ISSN 0254-4725

Manuals of food
quality control
1. The food control laboratory

FAO
FOOD AND
NUTRITION
PAPER

Rev. 1

Food
and
Agriculture
Organization
of
the
United
Nations

Manuals of food
quality control
1. The food control laboratory

FAO
FOODAND
NUTRITION
PAPER

14/1

Rev. 1

by
P.G. Martin

revised by
J. Weatherwax

and
P.G. Martin

p r e p a r e d with the support of the

S w e d i s h International Development Authority (SIDA)

Food
and
Agriculture
Organization
of
the
United
Nations

Rome, 1997

Reprinted 1997

The designations employed and the presentation of material in this

publication do not imply the expression of any opinion whatsoever on
the part of the Food and Agriculture Organization of the United
Nations concerning the legal status of any country, territory, city or
area or of its authorities, orconcerning the delimitation of its frontiers
or boundaries.

M-87
ISBN 92-5-102489-8

All rights reserved. No part of this publication may be reproduced, stored in a

retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying or otherwise, without the priorpermission of the copyright owner.
Applications for such permission, with a statement of the purpose and extent of the
reproduction, should be addressed to the Director, Information Division, Food and
Agriculture Organization of the United Nations, Viale delle Terme di Caracalla,
00100 Rome, Italy.
FAO 1986

FOREWORD

T h e c o n t r o l of food safety and quality is an integral part of n a t i o n a l

programmes for development.
National food control systems are designed to
protect the health and welfare of the consumer, to promote the development of
trade in food and food products, and to protect the interests of the fair and
h o n e s t food p r o d u c e r , processor or m a r k e t e r against dishonest and unfair
competition.
Emphasis is placed on the prevention of chemical and biological
hazards which result from contamination, adulteration or simple mishandling of
foods.
Also important are the maintenance of general food quality and the
control of the use of food additives and food processing procedures.
In order
must :

to

establish

a workable

food

control

system,

national

government

1.

Enact food control legislation.

2.

Promulgate regulations to enforce that legislation.

3.

Create an agency to cond uct the enforcement.

4.

Establish food inspection

agencies concerned.

5.

Provide physical facilities including a food control laboratory.

and

analysis

staff

within

the

agency

or

To assist the national governments of developing countries in this process, FAO,

with the support of the Swedish International Development Authority (SIDA) has
published the series Manuals of Food Quality Control. These are incorporated as
part of the FAO Food and Nutrition Paper Series No. 14, and include:
No. 14/1 rev. 1

The Food Control Laboratory (revised, 1986)

No. 14/2

Additives, Contaminants, and Techniques

by No. 14/7)

No. 14/3

Commodities (replaced by No. 14/8)

No. 14/4

Microbiological Analysis

No. 14/5

Food

No. 14/6

Food for Export

No. 14/7

Food Analysis: General Techniques, Additives,

Contaminants, and Composition

No. 14/8

Food Analysis:
Identity

(replaced

Inspection

Quality, Adulteration, and Tests of

In a d d i t i o n , FAO, WHO and UNEP jointly have published many guidelines and other
documents designed to further assist developing countries in forming adequate
food control systems. These publications include:
Methods of Sampling and Analysis of Contaminants in Food A Report of the Second Joint FAO/WHO Expert Consultation,
Rome - 1978
Guidelines for Establishing or Strengthening National Food
C o n t a m i n a t i o n M o n i t o r i n g Programmes - FAO Food Control
Series No. 5 - 1979

iii

Guidelines for the Study of Dietary Intakes of Chemical

Contaminants - WHO Offset Publication No. 87 - 1985
Guide
to
Codex
Recommendations
concerning
Residues, Part 2 - Maximum Limits for Pesticide
Second Preliminary Issue - Rome - 1985

Pesticide
Residues,

Recommended Practices for the Prevention of Mycotoxins in

F o o d , Feed and their Products - FAO Food and N u t r i t i o n
Paper No. 10, Rome - 1979
Food Standards, Codes of Practice and Methods of Analysis
Recommended by the Codex Alimentarius Commission - Joint
FAO/WHO Food Standards Programme (several titles)
Food Additive Evaluations and Specifications of Purity and
I d e n t i t y - Reports and M o n o g r a p h s of the Joint F A 0 / W H 0
Expert Committee on Food Additives (several titles)
The above publications, and others, are available to persons and organizations.
FAO
is also
interested
in receiving
comments
regarding
this volume
and
suggestions for future improvement. Please send to:
The Chief
Food Quality and Standards Service
Food Policy and Nutrition Division
Food and Agriculture Organization of the
United Nations
Via delle Terme di Caracalla
00100 Rome, Italy
FAO wishes
Development
of M r . J.*
preparation

to acknowledge the generous support of the Swedish International

Authority (SIDA), in the preparation of this volume, and the efforts
W e a t h e r w a x and M r . P.G. Martin who were responsible for the
of the text.

TABLE OF CONTENTS

FOREWORD

1.

SCOPE OF THE FOOD CONTROL LABORATORY MANUAL

2.

LABORATORY
2.1
2.2
2.3
2.4
2.5
2.6
2.7

3.

Establishing the Laboratory

Organizational Structure
Head of the Laboratory
Supervisors
Team Leaders
Analytical Staff
Support Staff

2
3
3
4
5
5
6

General Considerations
Basic Structure of the Building
Safety Features
Ventilation and Air Conditioning
Space Utilization
Equipment and Instruments
Utilities
Design References

7
7
10
12
13
15
16
18

LABORATORY ADMINISTRATION
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9

5.

ORGANIZATION

LABORATORY DESIGN
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8

4.

Sample Collection
Sample Receipt and Assignment
Sample Storage and Disposal
Budget
Purchasing
Supplies Management
Equipment Maintenance
Housekeeping
Training

LABORATORY
5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8

20
21
22
23
23
26
26
28
28

OPERATIONS

Workp lans
Priorities for Analysis
Analysis Assignment
Analysis Control
Analysis Reporting
Analysis Review
Method Validation
Confirming Analysis

. . . . .

29
31
31
32
32
33
34
34

6.

LABORATORY
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.8

7.

SAFETY

The Safety Programme

Basic Safety Rules
Fire Safety
Chemical Hazards
Biological Hazards
Physical Hazards
Safety and Emergency Equipment
First Aid

LABORATORY QUALITY ASSURANCE

7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8

35
35
36
37
38
40
42
43

(QA)

Introduction
Establishing a QA Programme
QA of Reference Standards
QA of Instruments
QA of Analytical Reports
Check Sample Examination
Other QA Activities
Text References

46
46
49
. . 55
58
61
66
66

vi

1.

SCOPE OF THE FOOD CONTROL LABORATORY M A N U A L

This m a n u a l is p r i m a r i l y a p r a c t i c a l h a n d b o o k on the e s t a b l i s h m e n t of a food

control laboratory.
The v a r i o u s organizational, administrative, operational,
and d e s i g n c r i t e r i a are d i s c u s s e d in s o m e d e t a i l .
A l s o i n c l u d e d is a
discussion of laboratory safety to stress the importance of safe operation and
the inherent hazards always present in an analytical laboratory.
The manual is designed for laboratory management and administration personnel,
but the o p e r a t i n g a n a l y s t can g a i n good i n f o r m a t i o n and i n s i g h t s into the
problems involved in establishing and operating a food control laboratory.
The u s e r of this m a n u a l should a l w a y s k e e p in m i n d that the i n f o r m a t i o n and
principles presented are advisory only and represent recommendations on how a
food control laboratory may be organized, arranged, etc., not how it must be.
This manual is intended as a guide, to help a new laboratory get off to a good
s t a r t , or to g u i d e an e s t a b l i s h e d l a b o r a t o r y in w h i c h w o r k is e x p a n d i n g and
diversifying.
As time goes by, experience builds up and a laboratory tends to
develop new methods, modify existing ones or adapt them to other products.
All
this valuable information should be retained and, if possible, combined with
this manual and manuals No. 14/2 and 14/3 in a readily accessible form. At the
s a m e t i m e , the a n a l y s t m u s t r e m e m b e r that r e l i a b l e r e s u l t s w i l l o n l y be
o b t a i n e d by s t r i c t a d h e r e n c e to the d e t a i l s that m a t t e r and to c a r e f u l and
professional work. Analytical chemistry is an exact science, very demanding on
the manipulative skills of the worker at the bench. There is no substitute for
e x p e r i e n c e but it is hoped this m a n u a l w i l l form a u s e f u l guide w h i l e that
experience is developing as well as during routine laboratory operations.
Any
c o m m e n t s or s u g g e s t i o n s for i m p r o v e m e n t s w i l l be w e l c o m e .
T h e s e should be
addressed to the address given in the Foreword.
The first e d i t i o n of this m a n u a l w a s w r i t t e n in 1977 by Mr. Peter G. M a r t i n ,
p r e s e n t l y of L y n e , M a r t i n and R a d f o r d , P u b l i c A n a l y s t s , R e a d i n g , B e r k s h i r e ,
England.
The p r e s e n t r e v i s e d e d i t i o n has b e e n p r e p a r e d w i t h Mr. M a r t i n ' s
support and assistance by Mr. John Weatherwax, retired Laboratory Director for
the United States Food and Drug Administration, Los Angeles, California, USA.

2.

2.1

Establishing

the

LABORATORY

ORGANIZATION

Laboratory

The publication, "Guidelines for Developing an Effective National Food Control

System", F A O / W H O / U N E P , FAO, Rome, 1976, details the formation of a food control
system embodied in a national food quality control service.
The purposes of a
n a t i o n a l food q u a l i t y c o n t r o l s e r v i c e are to e n s u r e a s u p p l y of s a f e ,
nutritious and honestly presented food; to protect consumers from foods which
are c o n t a m i n a t e d , decomposed, adulterated, injurious or packaged or labelled in
a false or misleading way; to promote better quality control of foods by food
p r o c e s s o r s and d i s t r i b u t o r s and t h e r e b y e n c o u r a g e d e v e l o p m e n t of the food
i n d u s t r y and to i m p r o v e e x p o r t p o t e n t i a l and e n a b l e b e t t e r c o n t r o l of food
import s.
When consumers and buyers have confidence in the quality and safety of foods,
trade increases at both local and international levels.
Increased local demand
e n c o u r a g e s i n d u s t r y and i n t e r n a t i o n a l t r a d e brings better returns in foreign
exchange capital.
T h i s c a n a l s o lead to n a t i o n a l d i e t s b e c o m i n g m o r e v a r i e d
and n u t r i t i o u s w i t h l o c a l p r o d u c t s o f t e n s u b s t i t u t e d for c o s t l y i m p o r t s .
B e s i d e s the o b v i o u s e c o n o m i c and p u b l i c h e a l t h b e n e f i t s , the a d v a n t a g e s in
social terms can also be considerable.
In m a n y g o v e r n m e n t s t r u c t u r e s t h e r e are s t a f f and f a c i l i t i e s l o c a t e d in
d i f f e r e n t a g e n c i e s that a r e i n v o l v e d in s o m e or all a s p e c t s of food c o n t r o l ,
b u t t h e i r e f f o r t s are o f t e n not h i g h l y e f f e c t i v e due to lack of f a c i l i t i e s ,
expertise or an adequate legal or a d m i n i s t r a t i v e f r a m e w o r k .
These resources
s h o u l d be b r o u g h t t o g e t h e r into a u n i f i e d s t r u c t u r e in such a w a y that the
p e r s o n n e l a r e b e s t u t i l i z e d and h a v e c l e a r o b j e c t i v e s w i t h the f a c i l i t i e s to
c a r r y t h e m out.
T h e r e s u l t w o u l d be a p r o p e r l y l i n k e d i n s p e c t o r a t e and
l a b o r a t o r y w i t h the n e c e s s a r y a d m i n i s t r a t i v e and l e g a l s u p p o r t i n c l u d i n g ,
w h e n e v e r possible, an Advisory Board to provide guidance and coordination at
national l e v e l .
This manual deals only with the establishment of the food control laboratory,
a l t h o u g h it is o n l y o n e c o m p o n e n t of a n a t i o n a l food c o n t r o l s e r v i c e .
It
laboratory
there must
be a
should
be n o t e d
that
f o r an e f f e c t i v e
correspondingly effective inspectorate.
In a f e w c o u n t r i e s t h e r e is no
p r o v i s i o n for an i n s p e c t o r a t e and s a m p l e s are o f t e n o b t a i n e d by the a n a l y s t ,
thereby using potential analytical time.
Having samples submitted by the food
industry saves sample collection time, but is inherently a bad practice because
the samples cannot be assured of being representative.
A food c o n t r o l l a b o r a t o r y is a c o s t l y f a c i l i t y to e s t a b l i s h , so b e s t r e s u l t s
will be achieved if the functions of the laboratory are confined to activities
r e s u l t i n g f r o m the e n f o r c e m e n t of food l a w , g e n e r a l s u r v e y s on q u a l i t y of
f o o d s , e x p o r t / i m p o r t i n s p e c t i o n w o r k and w o r k of an i n v e s t i g a t i o n a l n a t u r e
relating to food quality.
However, it may, for reasons of economy and o p t i m u m
u t i l i z a t i o n of the f a c i l i t i e s , b e c o m e n e c e s s a r y to t a k e up o t h e r s e l e c t e d
analytical work provided the laboratory is appropriately equipped.
Advice or
a n a l y s i s on a fee b a s i s to l o c a l i n d u s t r y m a y be j u s t i f i e d if t h i s d o e s n o t
conflict with statutory duties or other government bodies and there are clear
guidelines.
Such analyses are carried out for advisory purposes and in no way
are a substitute for normal food control work.

2.2

Organizational

The staffing

Structure

structure

of a typical

food

Head of

Analytical
Staff

control

laboratory

is as

follows:

Laboratory

Support
Staff

Administrative
Staff

The o f f i c e of Head of L a b o r a t o r y ( o t h e r t i t l e s such as " C h i e f " or " D i r e c t o r "

a r e o f t e n u s e d ) m a y i n c l u d e a D e p u t y if the l a b o r a t o r y s t a f f is s u f f i c i e n t l y
large.
U s u a l l y , h o w e v e r , the d u t i e s of the H e a d , in h i s or her a b s e n c e , are
assumed by a senior supervisor of the analytical staff.
The analytical and support staffs are discussed b e l o w in Sections 2.6 and 2.7,
respectively.
The administrative staff includes all administrative assistance
such as a s e c r e t a r y , t y p i n g and f i l i n g c l e r k s , a m a n a g e m e n t a s s i s t a n t and a
librarian (if the laboratory library is of a size to need one).
Basically the
a d m i n i s t r a t i v e s t a f f are t h o s e p e r s o n s g e n e r a l l y i n v o l v e d in " o f f i c e " or
"paperwork" functions.
This staff is very important to the smooth operation of
a laboratory.
It is false e c o n o m y to u n d e r s t a f f the a d m i n i s t r a t i v e g r o u p
because their work often m u s t then be done in part by the analytical or support
staffs .
The secretary for the laboratory generally works directly for the Head.
good practice, h o w e v e r , to m a k e the secretary responsive to secretarial
of the supervisors.

2.3

Head

of the

It is
needs

Laboratory

The H e a d of the l a b o r a t o r y s h o u l d be a g r a d u a t e c h e m i s t or m i c r o b i o l o g i s t
trained in food analysis.
A postgraduate d i p l o m a particularly relevant to this
w o r k is h i g h l y d e s i r a b l e .
A l t h o u g h the d u t i e s of the h e a d of the l a b o r a t o r y
are m a n y , s o m e m a y be d e l e g a t e d and o t h e r s u n d e r t a k e n b y o t h e r p a r t s of the
food control administration.
It is therefore not appropriate to do more than
d r a w a t t e n t i o n to c e r t a i n a s p e c t s .
The o b j e c t i v e of the l a b o r a t o r y is to
analyze a large number of samples correctly, quickly and cheaply.
This means
t h a t a t t e n t i o n m u s t be paid to c a r e f u l s p e n d i n g of the b u d g e t , p r o m o t i o n of
good staff relations and maintenance of the highest possible level of technical
efficiency and expertise.
The laboratory Head may have to give evidence in court or write documents used
in c o u r t , in w h i c h c a s e he m u s t h a v e a t h o r o u g h u n d e r s t a n d i n g of food and
related law and court procedure.
There will also be involvement in c o m m i t t e e
work and relations with other organizations.
The laboratory Head is usually
the spokesman for the laboratory in many instances.
The Head must prepare work
p l a n s w i t h the i n s p e c t o r a t e and o v e r a l l food c o n t r o l a u t h o r i t i e s .
Sampling
p l a n s a g r e e d w i t h the i n s p e c t o r a t e s h o u l d aim at a r e a s of c o n c e r n and m a j o r
abuses.
In the e a r l i e r y e a r s or w h i l e the l a b o r a t o r y r e m a i n s s m a l l , the Head of the
laboratory is the one who makes most of the m a n a g e m e n t decisions.
The Head is
also the person who interacts with higher m a n a g e m e n t .
This is a most important
aspect as the laboratory m u s t be fully integrated into the executive s tructure
in a m e a n i n g f u l w a y .
It w o u l d be f u t i l e for a l a b o r a t o r y to w o r k in an
administrative v a c u u m , producing r e s u l t s s h o w i n g , for e x a m p l e , that s a m p l e s

were contaminated or that there were consignments of food in the distribution

c h a i n r e q u i r i n g r e g u l a t o r y a c t i o n , if the food c o n t r o l o r g a n i z a t i o n and
i n s p e c t o r a t e took no a c t i o n , or if a t t e m p t e d a c t i o n w a s c o u n t e r m a n d e d at a
h i g h e r level.
The e x e c u t i v e a r m of the g o v e r n m e n t in this a r e a , the food
c o n t r o l s e r v i c e , n e e d s the s a n c t i o n and s u p p o r t of m o r e senior levels of the
administration.
To play an effective role, the Head of the laboratory must be
assured of necessary finance, staff and facilities.
When difficulties arise in
the supply of these three essential ingredients, it must be possible to bring
these difficulties to the attention of persons in positions of higher authority
for appropriate action.

2.4

Supervisors

S u p e r v i s o r s s h o u l d a l s o be g r a d u a t e c h e m i s t s or m i c r o b i o l o g i s t s w i t h
considerable food analysis experience.
The supervisor is the on-site manager
of the laboratory.
Having supervisors assigned to specific units or areas of
work permits the Head to more effectively plan (and execute) the total workload
of the laboratory.
S u p e r v i s o r s can be e x p e c t e d to do a n a l y t i c a l w o r k in a d d i t i o n to their
supervisory duties.
H o w e v e r , if their g r o u p e x c e e d s five p r o f e s s i o n a l
a n a l y s t s , it is best not to r e q u i r e a d d i t i o n a l a n a l y t i c a l w o r k e x c e p t for
occasional problem solving and trouble-shooting.
A reasonable m a x i m u m number
of a n a l y s t s for one p e r s o n to s u p e r v i s e is 10 to 12. T h i s can be m o r e if n o n professional support staff is added.
A supervisor's duties can include many or all of the
1.
Assisting the Head in overall
the work of the group supervised.
2.

posed

Receiving

and assigning

samples

laboratory

5.
Ensuring
do the work.

the

that

reports

the

of

6.
Ensuring that proper
followed by the group.

work

the necessary

laboratory

planning

in s o l v i n g

completed

group has

work

for analysis, within

3.
A n s w e r i n g q u e s t i o n s and a s s i s t i n g
by individual analysts.

4.
Reviewing
recommendations.

following:

and

and

the group.

analytical

making

supplies

planning

and

safety and housekeeping

problems

appropriate

equipment

practices

to

are

7.
R e c o m m e n d i n g to the Head n e w i n s t r u m e n t s or e q u i p m e n t n e e d e d , and
training needs of individual analysts.
8.
Taking appropriate disciplinary
laboratory rules or regulations.
9.

Acting

to manage the entire

action

laboratory

when

needed

to

enforce

in the absence of the Head.

Supervisors should train one or more analysts in their group to serve as backups, to supervise the group in the supervisor's absence.
The back-ups should
be given some formal classroom training in supervision in addition to on-thejob experience.
A good supervisor is indispensable to the smooth operation of a laboratory.
In
s e l e c t i n g a s u p e r v i s o r , the Head m u s t k e e p in m i n d that the p r i m a r y job of a
s u p e r v i s o r is to m a n a g e , so that s k i l l s in w o r k i n g w i t h p e o p l e are m o r e
i m p o r t a n t than s c i e n t i f i c e x p e r t i s e .
T h e r e f o r e , a top a d m i n i s t r a t o r w i t h

m e d i o c r e science ability is m o s t often a better choice than a top scientist w h o

is only a m e d i o c r e (or bad) a d m i n i s t r a t o r .
(This p r i n c i p l e h o l d s even m o r e for
s e l e c t i o n of the H e a d of the l a b o r a t o r y . )
O f t e n the b e s t a n a l y s t s are g i v e n
s u p e r v i s o r jobs as a r e w a r d for their b e n c h e x p e r t i s e .
T h i s not only r e m o v e s
t h e m (at l e a s t in p a r t ) f r o m t h e i r m o s t v a l u a b l e r o l e as a n a l y s t , b u t it a l s o
puts them in the o f t e n u n c o m f o r t a b l e role of s u p e r v i s o r .
This can result in an
overall d e c r e a s e in that i n d i v i d u a l ' s e f f e c t i v e n e s s .
T h i s is n o t to s a y t h a t a t o p a n a l y s t c a n n o t b e a t o p s u p e r v i s o r ,
many
fortunate o r g a n i z a t i o n s have such persons.
They are rare, h o w e v e r , and a Head
selecting a supervisor s h o u l d be w i l l i n g
to a c c e p t
lesser
scientific
c r e d e n t i a l s if the other attributes rank s u f f i c i e n t l y high.

2.5

Team

Leaders

A n o t h e r i m p o r t a n t , and o f t e n o v e r l o o k e d , p o s i t i o n is T e a m L e a d e r .
A team
leader is a senior analyst w h o h a s b e e n assigned a s m a l l g r o u p , u s u a l l y no m o r e
t h a n 4 , to do a s p e c i f i c
t a s k or t y p e of a n a l y s i s .
T h e l e a d e r h a s no
s u p e r v i s o r y functions as such, but is the c o o r d i n a t o r of the g r o u p ' s a c t i v i t i e s
and is the contact point for the supervisor.
T e a m l e a d e r s are m o s t u s e f u l w h e n a l a r g e n u m b e r of a r e p e t i t i v e type of
a n a l y s i s is to be done in a specified period of time.
This could be a specific
a n a l y t i c a l s u r v e y or a n e m e r g e n c y p u b l i c h e a l t h p r o b l e m r e q u i r i n g s c r e e n i n g
analyses.
T h e l e a d e r u s u a l l y w o r k s a l o n g w i t h the g r o u p in a d d i t i o n to the
coordinative function.
S u c h e x p e r i e n c e is o f t e n u s e f u l to d e t e r m i n e if t h e
assigned leader has potential as a future supervisor.

2.6

Analytical

Staff

The basic job of the analytical staff is to analyze the s a m p l e s received and to
issue a report.
They m a y also be required to a p p e a r in court as fact or expert
w i t n e s s e s to give e v i d e n c e in r e l a t i o n to a report.
They m a y also be called on
to o f f e r a d v i c e to i n d u s t r y and t r a d e , to a s s i s t in i m p r o v e m e n t o f f o o d
q u a l i t y , or advise on c o n f o r m i t y w i t h s t a n d a r d s or other legal r e q u i r e m e n t s .
T h i s c a n i n v o l v e t h e l a b o r a t o r y s t a f f in f a c t o r y v i s i t s a n d e v e n r e q u e s t s to
c a r r y out e x p e r i m e n t a l w o r k .
W h e t h e r or n o t the l a b o r a t o r y u n d e r t a k e s s u c h
w o r k w i l l be a m a t t e r of o r g a n i z a t i o n a l policy.
The d e c i s i o n w i l l depend on a
n u m b e r of f a c t o r s , i n c l u d i n g the a v a i l a b i l i t y of a l t e r n a t i v e facilities, the
n a t u r e of i n d i v i d u a l o w n e r s h i p ,
etc.
T h e i n t e g r i t y of the a n a l y s t
is
p a r a m o u n t , and s u p e r i o r s m u s t be i n f o r m e d of a n y c o n f l i c t of i n t e r e s t t h a t
a r i s e s . A s in t h e c a s e o f f o o d i n s p e c t o r s , it is p r o p e r f o r t h e a n a l y s t s to
have no vested interest in regulated industries.
This r e q u i r e m e n t is m a n d a t o r y
in m a n y countries.
A n a l y t i c a l staff can be d r a w n from three levels, u n i v e r s i t y g r a d u a t e s , trained
t e c h n i c i a n s f r o m t e c h n i c a n t r a i n i n g c o l l e g e s and u n q u a l i f i e d s t a f f w h o h a v e
received o n - t h e - j o b training.
The g r a d u a t e s can be c h e m i s t s , m i c r o b i o l o g i s t s ,
food scientists or fi od t e c h n o l o g i s t s .
U n i v e r s i t y d e g r e e s are only a starting
q u a l i f i c a t i o n and the-p. w i l l still be a r e q u i r e m e n t for specialized training
a n d e x p e r i e n c e in f o o d . n a l y s i s .
S t a f f s h o u l d be e n c o u r a g e d to c o n t i n u e to
w o r k for s u i t a b l e p o s t g r a d u a t e q u a l i f i c a t i o n s to e n a b l e t h e m to c o m p e t e for
h i g h e r posts in the laboratory.
S p e c i a l l y trained l a b o r a t o r y t e c h n i c i a n s w h o
h a v e f o l l o w e d a t w o to t h r e e y e a r p r a c t i c a l t r a i n i n g c o u r s e in l a b o r a t o r y
a n a l y s i s a f t e r c o m p l e t i n g s e c o n d a r y s c h o o l c a n be p a r t i c u l a r l y u s e f u l in
carrying out a n u m b e r of routine or even h i g h l y c o m p l e x food analyses.
As in
the c a s e w i t h u n i v e r s i t y g r a d u a t e s , s p e c i a l i z e d o n - t h e - j o b t r a i n i n g w i l l b e
needed for particular types of food analysis.

S o m e people w i t h little or no theoretical b a c k g r o u n d often s h o w m a n i p u l a t i v e

a n d p r a c t i c a l s k i l l s in t h e l a b o r a t o r y as g o o d or b e t t e r t h a n u n i v e r s i t y
graduates.
This type of person is often m o r e happy and fulfilled in carrying
out c e r t a i n r o u t i n e l a b o r a t o r y tasks than are graduates.
E v e r y a t t e m p t should
be m a d e to e n c o u r a g e s u c h p e r s o n n e l in t h e i r w o r k and the l a b o r a t o r y H e a d
s h o u l d a t t e m p t to s e t u p p a y s c a l e s a n d o t h e r i n c e n t i v e s to r e w a r d
such
workers.
T h e s e w o r k e r s m a y a l s o be e n c o u r a g e d to t a k e c o u r s e s and o b t a i n
q u a l i f i c a t i o n s in p r a c t i c a l a s p e c t s o f the w o r k , s u c h as
glass-blowing,
i n s t r u m e n t r e p a i r , e l e c t r o n i c s , m e t a l - w o r k and o t h e r f i e l d s r e l a t e d to the
m a i n t e n a n c e of l a b o r a t o r y e q u i p m e n t .
These skills are o f t e n scarce, and just
as d i f f i c u l t to m a s t e r , as t h o s e of the g r a d u a t e a n a l y s t and t h e r e is e v e r y
j u s t i f i c a t i o n for r e w a r d i n g their a c c o m p l i s h m e n t .
It is m o s t i m p o r t a n t that
staff e m p l o y e d for repair o p e r a t i o n s are qualified and t h o r o u g h l y trained.
In
p a r t i c u l a r , e l e c t r o n i c e q u i p m e n t s h o u l d be s e r v i c e d and r e p a i r e d only by
qualified i n s t r u m e n t a t i o n technicians.

2.7

Support

Staff

T h e s u p p o r t s t a f f of a l a b o r a t o r y a r e all of t h o s e p e r s o n s w o r k i n g in and for

the l a b o r a t o r y w h o are not c o n d u c t i n g
a n a l y s e s or are n o t i n v o l v e d
in
a d m i n i s t r a t i v e duties.
S o m e e x a m p l e s of duties include:
1.

Glassware

washing.

2.

Cleaning

and

3.

Disposal

of s a m p l e

4.

Pest

control.

5.

Heavy

lifting

housekeeping

and

maintenance.

reserves

( w h e n no

longer

required).

moving.

Support staff t y p i c a l l y have little or no e d u c a t i o n a l q u a l i f i c a t i o n s beyond

a b i l i t y to read and w r i t e .
H o w e v e r , they m u s t be w i l l i n g and able to learn
o n l y their d u t i e s , but also laboratory safety p r o c e d u r e s .

the
not

It is m o s t i m p o r t a n t t h a t s u f f i c i e n t p e r s o n s a r e h i r e d as s u p p o r t .
The w o r k
t h e y do m u s t be d o n e by s o m e o n e and t h i s is u s u a l l y an a n a l y s t or t e c h n i c i a n
w h e n there is i n s u f f i c i e n t support staff.
There is no fixed m o d u l e for n u m b e r s
of s u p p o r t w o r k e r s , b u t 1 5 - 2 0 % of the n u m b e r of a n a l y t i c a l s t a f f is o f t e n
sufficient.

3.

3.1

LABORATORY DESIGN

General Considerations

W h e n a new laboratory is being built, two people hold the key positions in
producing the right building at the right cost - the architect who designs it
and guides its construction, and the analyst (preferably the laboratory Head)
w h o explains the technical needs, and w o r k s in close p a r t n e r s h i p w i t h the
architect through every stage so that the end result is properly suited to the
requirements of the users.
It is not often that the analyst has the chance to
take part in the planning of a complete new laboratory, more usually he has to
make do with old or inadequate buildings. However, these are often more easily
extended, changed or adapted as the nature of the w o r k changes, than a n e w e r
building, so may in some ways be more advantageous.
Indeed, an important point
in designing a new laboratory is that provision should be made for future
expansion, however unlikely that may seem at the time. The design should also
be left as flexible as possible so that changes of emphasis in the work can be
a c c o m m o d a t e d . The laboratory should be located a w a y from urban centres and
industrial areas in order to minimize problems of contamination.
The information in this chapter was taken in part from Industrial Research and
D e v e l o p m e n t N e w s , VII No. 3, UN, N.Y., 1975.
The principles given apply to
food control l a b o r a t o r i e s in general, w h e t h e r n e w c o n s t r u c t i o n or space
converted to laboratory use.

3.2

Basic Structure of the Building

An example of the smallest laboratory that would be adequate for a food control
programme is shown in Figure 3.1. This design was originally intended to serve
120,000 people although in general this may be regarded as too small a
p o p u l a t i o n to justify a separate laboratory.
It is intended to be part of a
larger b u i l d i n g , but the disposition of r o o m s can be changed to suit local
c i r c u m s t a n c e s . Space for essential services such as solvent storage and the
usual administrative support must also be provided.
Sample preparation should
be carried out as far as possible from laboratories working on trace analysis
and microbiology or using sensitive instruments.
It must be stressed that the
figure s h o w n is only an e x a m p l e .
New l a b o r a t o r i e s m u s t be c u s t o m - b u i l t to
cater for the needs of the situation under consideration.
It is best to allow l a b o r a t o r i e s to r e m a i n o p e n - p l a n as far as p o s s i b l e ,
including the areas used as offices. Exceptions are areas where the activities
carried out cause c o n t a m i n a t i o n or are sensitive to it, such as s a m p l e
preparation, weighing, microbiology, trace analysis and use of instruments such
as gas-liquid chromatographs and spectrophotometers.
Lack of v i b r a t i o n is important and therefore concrete is a better structural
m a t e r i a l in m u l t i - s t o r e y
buildings.
S t e e l - f r a m e b u i l d i n g s m a y cause
d i f f i c u l t y with some i n s t r u m e n t s .
A two storey laboratory adequate for a
modest food control programme is shown in Figures 3.2 and 3.3. It consists of
a ground floor m a i n l y composed of offices and services and a first floor for
analytical work.
In addition there should be a flammable solvent storage area
separate from the building. W o r k s h o p and g l a s s b l o w i n g facilities are often
advantageous and if not otherwise available should be included.

1 ni i

>

Food
additives
and
toxicants

Food
standards
and nutrition
Corridor

Overall
length
21 m

Microbiology

Media
prparai ion

Office
Balance
room

Sample
prparai ion

1vK
Entrance
6.2 m

6.2 m

Figure 3.1
A Minimum Sized Food Control Laboratory

Figure 3.2
Ground Floor Plan
(mainly office and administrative

space)

Figure 3.3
First Floor Plan
(laboratory space)

3.3

Safety

Features

The building
including :
1.

The

and

laboratory

fire

design

should

a r e a s of c o r r i d o r s

include

a number

s h o u l d be f o r m e d

of

safety

of c o n c r e t e

features

blocks.

2.
Services should include a shower sprinkler system near each d o o r w a y
so t h a t a w o r k e r c a n t a k e an i m m e d i a t e s h o w e r , c l o t h e s and a l l , in the c a s e of
a c c i d e n t a l g e n e r a l c o n t a c t w i t h c o r r o s i v e or p o i s o n o u s l i q u i d s or f i r e .

10

3.
wash

There

stations

should

be

(obtainable

built-in
from

most

eye

wash

chemical

fountains,
supply

or

at

least

portable

eye

firms).

4.
The t r a f f i c
flow,
the e g r e s s p a t t e r n and the p r o p o r t i o n s of
the
l a b o r a t o r y are a l l s a f e t y c o n s i d e r a t i o n s .
I t m u s t a l w a y s be p o s s i b l e to l e a v e
the l a b o r a t o r y s a f e l y i r r e s p e c t i v e of the i n i t i a l s i t e of a f i r e .
Serious
t h o u g h t m u s t be g i v e n to t h e n u m b e r and l o c a t i o n o f f i r e e x t i n g u i s h e r s
and
s t a n d p i p e s y s t e m s , and to the a v a i l a b i l i t y of s p r i n k l e r
systems.
5.
L a b o r a t o r i e s s h o u l d b e w e l l - l i t so t h a t t h e o p e r a t o r d o e s n o t h a v e
to p e e r too c l o s e l y o v e r p o t e n t i a l l y h a z a r d o u s m a t e r i a l i n o r d e r to see w h a t he
is doing.
T h e r e s h o u l d be a m p l e w o r k i n g s p a c e and b e n c h t o p s and o t h e r s u r f a c e s
s h o u l d be k e p t c l e a r of a l l m a t e r i a l e x c e p t t h a t i n c u r r e n t u s e .
6.
Benches are best w i t h o u t s h e l v e s , only s e r v i c e s , these being operated
from the f r o n t so t h a t the o p e r a t o r d o e s not h a v e to s t r e t c h a c r o s s the b e n c h .
I t i s s t i l l common to s e e r e a g e n t s on s h e l v i n g at t h e b a c k o f b e n c h e s ( o r a b o v e
the c e n t r e of d o u b l e - w i d t h b e n c h e s ) b u t i t i s p r o b a b l y s a f e r i f such r e a g e n t s
c a n be k e p t on s i d e - s h e l v e s or i n t r a y s w h i c h a r e b r o u g h t to t h e b e n c h as
required .
7.
F l o o r i n g n e e d s to b e o f a n o n - s l i p m a t e r i a l , r e s i s t a n t to a c i d s a n d
s o l v e n t s , b u t n o t so h a r d a s to b e t i r i n g to s t a n d on f o r a f e w h o u r s at a
time.
No m a t e r i a l i s e n t i r e l y s a t i s f a c t o r y .
W e l l - l a i d l i n o l e u m and a f i l l e d
e p o x y r e s i n on top of c o n c r e t e a r e a m o n g t h e b e s t a v a i l a b l e .
It is a d v i s a b l e
n o t to p o l i s h l a b o r a t o r y
floors.
8.
P o l l u t a n t s g e n e r a t e d w i t h i n t h e l a b o r a t o r y m u s t be r e m o v e d s a f e l y ,
q u i c k l y and e f f i c i e n t l y .
I n p a r t i c u l a r , t o x i c or n o x i o u s g a s e s m u s t be r e m o v e d
e x p e d i t i o u s l y t h r o u g h a d u c t s y s t e m t h a t d o e s n o t e x h a u s t n e a r the b u i l d i n g a i r
conditioning
intake.
9.
The b u i l d i n g must be p l a n n e d f o r s e c u r i t y .
R e s t r i c t i o n of a c c e s s i s
of c o n s i d e r a b l e i m p o r t a n c e b e c a u s e of the e x t r e m e l y v a l u a b l e and
sensitive
e q u i p m e n t u s e d i n t h e l a b o r a t o r y w o r k a s w e l l as t o p r o t e c t t h e i n t e g r i t y o f
official
samples.
10.
I t i s v e r y a d v i s a b l e to h a v e an e f f i c i e n t f i r e a n d s m o k e d e t e c t i o n
system w i t h appropriate alarms.
Common f i r e d e t e c t i o n e q u i p m e n t is
usually
e i t h e r r a t e - o f - t e m p e r a t u r e - r i s e or f i x e d - t e m p e r a t u r e d e t e c t o r u s i n g a s u b s t a n c e
of known m e l t i n g p o i n t .
T h e r e a r e a d v a n t a g e s ( a n d d i s a d v a n t a g e s ) to e a c h t y p e
of d e t e c t o r and the l a b o r a t o r y Head s h o u l d s e l e c t the one he f e e l s b e s t f i t s
his laboratory.
D e s i g n i n g a l a b o r a t o r y to a f f o r d p r o t e c t i o n a g a i n s t e v e r y k i n d o f h a z a r d w o u l d
be a l m o s t i m p o s s i b l e .
The a i m s h o u l d be to d e t e r m i n e t h e l e v e l o f s a f e t y
for
t h e most g e n e r a l a p p l i c a t i o n s and to p r o v i d e s u p p l e m e n t a r y s y s t e m s in a r e a s o f
higher h a z a r d .
A s a f e s o l v e n t s t o r a g e a r e a i s i d e a l l y s e p a r a t e from t h e l a b o r a t o r y b u i l d i n g i n
a stand-alone structure.
I t c a n be a s m a l l b u i l d i n g of one room and
some
p o s s i b l e d e s i g n f e a t u r e s a r e : ( r e a s o n s are g i v e n in p a r e n t h e s i s )
1.
materials

Construction
s u r r o u n d the

of
cement
solvents.)

blocks

or

bricks.

(Only

non-flammable

2.
For a s t a n d - a l o n e b u i l d i n g , d o u b l e w a l l s w i t h i n s u l a t i o n
between.
The e x t e r i o r
w a l l c a n be m a t e r i a l
other
than block
or b r i c k .
(Provides
i n s u l a t i o n from the sun and m a k e s a i r c o n d i t i o n i n g more e f f e c t i v e . )
3.
An e p o x y f i l m to c o v e r t h e e n t i r e
walls.
( A n y s o l v e n t s p i l l a g e w i l l p o o l and
t h e f l o o r s or w a l l s . )

11

floor plus
evaporate,

10 cm up t h e b a s e of t h e
r a t h e r than soak through

4.
A c o p p e r pipe (about 25 m m ) inside the r o o m , w h i c h goes t h r o u g h the
floor and is e m b e d d e d a b o u t 2 m in earth.
(A g r o u n d pipe to bleed off any
static e l e c t r i c i t y c h a r g e s - w h i c h o f t e n build up w h e n s o l v e n t s are poured).
All metal objects in the room are to be attached to the pipe using heavy guage
single strand copper wire.
Also, attach a short wire with an alligator clip.
(This g r o u n d s all m e t a l .
The clip is used to g r o u n d any m e t a l cans used for
s o l v e n t transfer.)
5.
grounding

Storage
pipe.

shelves of metal

and connected

by wire

to each other and

the

6.
Air c o n d i t i o n i n g is e x t e r n a l , w i t h the e n t r a n c e duct at the top of
one c o r n e r of the r o o m and the exit d u c t at the b a s e of the o p p o s i t e c o r n e r .
( T h e r o o m m u s t be c o o l e d as m a n y s o l v e n t s w i l l b o i l at h o t o u t s i d e
temperatures. The air entrance on top and exit on the bottom diagonally across
the r o o m , w i l l cool the room and w i l l also serve to s w e e p and r e m o v e any
solvent fumes on the floor - solvent fumes are generally heavier than air and
will pool on the floor.)
7.
The door is of m e t a l and f i r e - r a t e d for at least one h o u r , w i t h a
positive closure.
It must seal well when closed. The door sill is at least 10
cm high.
(Fire doors are metal sheathed around cement.
The closure, the seal
and the h i g h sill all act to p r e v e n t e s c a p e of s o l v e n t , e i t h e r floor s p i l l a g e
or fumes.)
8.
An air c o n d i t i o n e r exit duct w i t h a fire b a f f l e (to p r e v e n t flash
b a c k ) and d u c t e d to exit in the o u t s i d e air at b u i l d i n g r o o f h e i g h t .
(Fumes
h a v e a b e t t e r c h a n c e of being carried a w a y by b r e e z e s and s o m e o n e s m o k i n g
nearby will not present a fire risk.)
9.
An extinguisher system,
and not water sprinklers.

3.4

Ventilation and Air

which

should

be carbon dioxide or Freon type

Conditioning

An ordinary laboratory may have amounts of lead in the air passing through it
in a day which can be measured in milligrams.
Natural ventilation, which may
provide large quantities of air without cooling, is not generally suitable for
laboratories.
T h i s is e s p e c i a l l y true in u r b a n a r e a s w h e r e m o t o r t r a f f i c is
high.
This means that air conditioning is essential for the modern laboratory.
A i r c o n d i t i o n i n g not only p r e v e n t s s o m e f o r m s of c o n t a m i n a t i o n , it also
p r o v i d e s a s t a b l e t e m p e r a t u r e e n v i r o n m e n t for s e n s i t i v e and s o p h i s t i c a t e d
analytical instruments. Most v o l u m e t r i c g l a s s w a r e is c a l i b r a t e d at 20C and
must be recalibrated if used at significantly different temperatures.
This is
s t i l l a n o t h e r a r g u m e n t for air c o n d i t i o n i n g .
T h e i m p o r t a n c e of a i r
conditioning to overall laboratory accuracy cannot be overstressed.
The exhaust fans in fume hoods result in a negative pressure in the laboratory
and in an urban or industrial area this aggravates contamination of the whole
l a b o r a t o r y area.
A p o s i t i v e p r e s s u r e s y s t e m is c o s t l y as it h a s to be
s u f f i c i e n t l y p o w e r f u l to p r o v i d e a c l e a n filtered air s u p p l y w h i c h p a s s e s
t h r o u g h f u m e hood e x h a u s t fans as w e l l as o t h e r o u t l e t s .
V e n t i l a t i o n by
p o s i t i v e p r e s s u r e a s s i s t s the e x h a u s t fans in f u m e h o o d s and is to be
preferred.
Each f u m e hood should h a v e a s e p a r a t e fan, as there is d a n g e r of
cross c o n t a m i n a t i o n from a c o m m o n d u c t i n g s y s t e m .
Such a s y s t e m can be
essential if the vicinity of the laboratory is prone to contamination and it is
necessary to carry out low-level trace analysis.
Toxic fumes must be confined
as far as possible to fume hoods.
These should be away from cross-currents of
air and pedestrian traffic.
The recommended m i n i m u m air-flow through the open
face of a f u m e hood is 0.5 m / s e c .
V e n t i l a t i o n s h o u l d be such as to give at
least 5 air changes per hour.

12

V a c u u m p u m p s used to evaporate solvents should have the exhaust to the outside

a i r , o t h e r w i s e t o x i c l e v e l s of the s o l v e n t m a y be r e a c h e d in the l a b o r a t o r y
atmosphere.
W a t e r aspirator p u m p s are quite safe w i t h w a t e r - s o l u b l e solvents
or acid f u m e s , but not w i t h w a t e r - i m m i s i b l e s o l v e n t s such as p e t r o l e u m ether.

3.5

Space

Utilization

L a b o r a t o r y s p a c e m u s t be a r r a n g e d for m a x i m u m u t i l i z a t i o n as w e l l as p r o p e r
w o r k flow.
It is usual to a l l o w about 10 square m e t e r s of laboratory space and
3 m e t e r s of b e n c h s u r f a c e p e r a n a l y s t .
An e x a m p l e of a l a b o r a t o r y for 8
a n a l y s t s is in Figure 3.4.

Sx
FC
Fr
DS
Kj

Figure

"
=
=
=
=

Soxhlet bench
fume cupboard
freezer
sink unit
Kjeldahl apparatus

3.4

N o t e that e a c h a n a l y s t h a s a l a t e r a l b e n c h a r e a to w o r k at.
T h i s f o r m a t is
termed 'peninsular' and is quite e f f i c i e n t .
An a l t e r n a t e f o r m a t uses 'islands'
w h i c h have access on all sides.
An e x a m p l e is Figure 3.5.

13

0.7b m

1.50 m

0.75 m

1.50 m

0.75 m

1.50 m

0.75 m

Consider as island
benches accessible
from every side, or
consider as the floor
space remaining, the
area B being occupied
by benches

Figure

3m

3.5

T h e o p t i m u m w i d t h f o r a s i n g l e b e n c h ( a b o u t 75 cm) i s r o u g h l y t h e s a m e as t h e
width
of
the
space
required
by a s t a n d i n g
individual.
It
is
therefore
convenient,
to c o n s i d e r t h e p r o s and c o n s o f i s l a n d b e n c h e s and
peninsular
b e n c h e s w i t h the a s s i s t a n c e of F i g u r e 3 . 5 .
I t c a n r e a d i l y be s e e n t h a t the
m a x i m u m b e n c h a r e a i s o b t a i n e d w i t h p e n i n s u l a r b e n c h e s (B a r e a s ) , h o w e v e r ,
the
w o r k i n g s u r f a c e is more a c c e s s i b l e on i s l a n d b e n c h e s (A a r e a s ) .
The
services
a r e m o r e a c c e s s i b l e f o r r e p a i r on i s l a n d b e n c h e s , b u t t h e r e i s l e s s
space
available
for s h e l v i n g
close
to t h e b e n c h e s .
In the c a s e of
peninsular
b e n c h e s , t h e a n a l y s t w o r k i n g i n a b a y h a s a c c e s s i n e f f e c t to t h r e e w o r k i n g
s u r f a c e s at o n c e and t h i s i s v e r y c o n v e n i e n t i f t h e r e a r e s e v e r a l
different
a n a l y s e s i n p r o g r e s s at the same t i m e .
H o w e v e r , the s p a c e b e t w e e n p e n i n s u l a r s
s h o u l d a l w a y s be e n o u g h for two p e o p l e to w o r k c o m f o r t a b l y b a c k to b a c k ( a b o u t
1.5 m).
I s l a n d b e n c h e s make the c h o i c e of s i t e for w i n d o w s and d o o r s
less
critical.
P e n i n s u l a r b e n c h e s m a y be p r e f e r r e d i f s p a c e i s a t a p r e m i u m a n d
t h e y may be s l i g h t l y s a f e r ,
as the r o u t e s by w h i c h p e o p l e w a l k a b o u t
the
l a b o r a t o r y t e n d to be m o r e r e s t r i c t e d and p r e d i c t a b l e .
W h i c h e v e r is c h o s e n ,
w h a t i s m o s t i m p o r t a n t i s t h a t t h e s i z e o f t h e r o o m i s c o r r e c t to t a k e a n
i n t e g r a l n u m b e r of b e n c h u n i t s w i t h t h e i r a c c o m p a n y i n g
floor space.
Usually
t h e p r o b l e m c a n be p a r t l y s o l v e d b y a w a l l b e n c h at one end or s i d e of t h e
l a b o r a t o r y but a l l too o f t e n l a b o r a t o r i e s have such a s i z e or shape t h a t f l o o r
s p a c e h a s b e e n w a s t e d , or an e x t r a b e n c h h a s b e e n i n c o n v e n i e n t l y s q u e e z e d
in.
The s t o r a g e a r e a s in the b e n c h e s s h o u l d be m o d u l a r to a l l o w f l e x i b i l i t y .
Many
laboratory
bench
manufacturers
have
units
where
the
storage
areas
are
interchangeable.
Some s a m p l e s of b e n c h a s s e m b l i e s a r e g i v e n in F i g u r e 3 . 6 ,
w i t h w i d t h s in c e n t i m e t e r s .

14

KO

ra

to

1M

(O

m m m
I

f-

"t-

22

to

'

to

110

120

4-

120

10

120

2%0

120

2$o

120

4-

2 tO

120

2so

tO

+4-

4-4-

4"

120

IM

120

4-4rara
1

II

II

4-

220

H
t-

rap nu
+

Il

ira
m m
m rap ra
era
to

M U

4-

SO (O

>0

110

4"

HI

..

Figure

--

--

'

3.6

The o p t i m u m working depth of benches for standing w o r k has been found to be 60

cm for the w o r k i n g s u r f a c e , p l u s 15 cm for the a c c o m m o d a t i o n of a b o v e - b e n c h
fitments (such as gas service, electrical sockets and shelves) giving a total
depth of 75 cm.
The bench heights, h o w e v e r , have always caused some problems
b e c a u s e of the v a r i e t y of b e n c h t o p s a v a i l a b l e .
Their thickness varies with
the different coverings and supporting bases used:
6 cm for ceramic tiles, 4
cm for P y r o c e r a m , 3.7 cm for a c i d - p r o o f s t o n e w a r e , and 2.8 cm for p l a s t i c s .
H e i g h t d i f f e r e n c e s in a d j a c e n t b e n c h u n i t s always cause inconvenience to the
user.
Therefore purchases of new benches m u s t expressly indicate that desks
and benches with different coverings must have uniform heights.
(Differences
c a n be c o m p e n s a t e d for b y u n d e r l a y i n g the b e n c h tops.) B e n c h m o d u l e l e n g t h s
are u s u a l l y 60 cm for s i n g l e u n i t s and 90 or 120 cm for d o u b l e u n i t s .
This
modulus of length in 30 cm steps allows adaptation to nearly any room size.
W o r k flow is a very important part of proper space utilization.
There should
be a l o g i c a l and s y s t e m a t i c a r r a n g e m e n t of s p a c e to p e r m i t f l o w of a n a l y s i s
w o r k f r o m s a m p l e r e c e i p t , p r e p a r a t i o n and a n a l y s i s to d i s p o s a l or s t o r a g e .
This entails examining the average sample annual workload in relation to the
areas and people involved in the various analyses.
The best work flow system
(within physical constraints of the building) is usually readily apparent.

3.6

Equipment

and

Instruments

The complexity of equipping a laboratory and the consequent delay in production

of u s e f u l r e s u l t s s h o u l d n o t be u n d e r e s t i m a t e d .
In the e a r l y s t a g e s , the
requirements for equipment may seem large and complex but once the laboratory
is e s t a b l i s h e d , the r u n n i n g c o s t s a r e r e l a t i v e l y l o w .
It is s o m e t i m e s n o t
appreciated by the non-technical administrator that an analysis may require 10
or 20 i n d i v i d u a l i t e m s and that if e v e n o n e is n o t a v a i l a b l e the a n a l y s i s
cannot be carried out.
On the other hand, many items are c o m m o n to different

15

a n a l y s e s so t h a t , o n c e the m a n y h u n d r e d s of i t e m s r e q u i r e d in a food c o n t r o l
l a b o r a t o r y h a v e b e e n p r o v i d e d , t h e r e c o m e s a p o i n t at w h i c h p r o d u c t i v i t y c a n
rise s h a r p l y and i n v e s t m e n t decrease.
The logistical p r o b l e m s of m a i n t e n a n c e ,
r e p a i r and r e p l a c e m e n t of e q u i p m e n t are also c o n s i d e r a b l e .
Adequate provision
m u s t be m a d e for obtaining spares and r e p l a c e m e n t parts and for their storage.
It is false e c o n o m y if staff are being paid but c a n n o t do an i m p o r t a n t part of
their w o r k due to a lack of r e l a t i v e l y i n e x p e n s i v e e q u i p m e n t .
S o m e of the i n s t r u m e n t s and e q u i p m e n t needed for c h e m i c a l a n a l y s i s by a m o d e r n
food c o n t r o l l a b o r a t o r y are:
(for purposes of this listing, ' i n s t r u m e n t s ' are
m e a s u r i n g d e v i c e s and ' e q u i p m e n t ' are p r o c e s s i n g d e v i c e s .
Apparatus made
p r i m a r i l y of glass are not included).

Instruments

A n a l y t i c a l balance
pH m e t e r
Spectrophotometer, UV-visible, double-beam
S p e c t r o p h o t o m e t e r , atomic a b s o r p t i o n
H i g h P e r f o r m a n c e Liquid C h r o m a t o g r a p h (with UV and d i f f e r e n t i a l r e f r a c t i v e
index d e t e c t o r s )
Gas C h r o m a t o g r a p h (with flame i o n i z a t i o n and e l e c t r o n capture d e t e c t o r s )

Equipment

Blender
Grinder
Pulverizing hammer mill
Air o v e n , forced draft
V a c u u m o v e n , with pump
M u f f l e furnace
Centrifuge
Refrigerator
Freezer
H e a t e r s and hot plates
Steam and w a t e r b a t h s
W a t e r still or d e i o n i z e r

All of the above e q u i p m e n t and i n s t r u m e n t s are m o v e a b l e , a l t h o u g h the larger or

m o r e s e n s i t i v e units are g e n e r a l l y not m o v e d , once placed.
The m a j o r i t e m s of
fixed e q u i p m e n t constructed in place are the fume hoods.
The e x t e n s i v e use of
s o l v e n t s , a s h i n g and n o x i o u s c h e m i c a l s in f o o d a n a l y s i s , r e q u i r e s m o r e f u m e
h o o d s t h a n o t h e r t y p e s of l a b o r a t o r y w o r k .
In f a c t , to e x p e r i e n c e d
food
a n a l y s t s , t h e r e n e v e r s e e m to b e e n o u g h h o o d s , e v e n in a w e l l
equipped
laboratory.
F u m e h o o d s m a y be p u r c h a s e d p r e - f a b r i c a t e d w i t h o u t l e t s for
services.
The m a t e r i a l of c o n s t r u c t i o n is m o s t i m p o r t a n t , e s p e c i a l l y if the
hood has to w i t h s t a n d acid fumes in general and p e r c h l o r i c acid in p a r t i c u l a r .
The s u p p l i e r m u s t be g i v e n full d e t a i l s of the use to w h i c h the fume hood w i l l
be put.
H o o d s c a n be c o n s t r u c t e d
out of l o c a l m a t e r i a l s s u c h as w o o d ,
p r e f e r a b l y hard w o o d s , coated w i t h epoxy resins.
Such should n e v e r be used for
acid d i g e s t i o n s , but only for solvent e x t r a c t i o n work.

3.7

Utilities

E l e c t r i c i t y m u s t either be a stable supply, or the voltage m u s t be stabilized

by e i t h e r one large s t a b i l i z e r for the w h o l e l a b o r a t o r y , or by a unit for each
of the i n s t r u m e n t s r e q u i r i n g it.
A b o u t 40 w a t t s per s q u a r e m e t e r has b e e n

16

suggested.
The laboratory pictured in Figure 3.3 has 160 double 13-amp socket
outlets.
This apparently large n u m b e r adds considerably to the efficiency of
a n a l y t i c a l o p e r a t i o n s and to their s a f e t y .
The s a m e l a b o r a t o r y has 110 gas
p o i n t s , e x c l u d i n g t h o s e to the f u m e h o o d s .
T h e r e m u s t b e s e v e r a l cold w a t e r
taps per b e n c h to a l l o w for r i n s i n g , c o n d e n s e r s , etc., but h o t w a t e r can be
restricted to those sinks w h e r e apparatus is washed.
In a larger laboratory a
distribution system for distilled or deionized water would be advantageous.

The following utilities

for fume hoods have been

Fume Hood Length

():

Gas taps (front controlled)

Water taps (front controlled)
Cup sinks
Compressed air valves (front
controlled)
Two-phased electrical sockets
Three-phased electrical
sockets

suggested:

1.2

1.5

1.8

2
2
1

2
3
2

3
4
2

1
2

1
3

1
4

S p e c i a l m e t h o d s , s u c h as t r a c e a n a l y s i s , u s u a l l y r e q u i r e d i s t i l l a t i o n f r o m
g l a s s a p p a r a t u s of w a t e r i n i t i a l l y p a r t i a l l y p u r i f i e d by d i s t i l l a t i o n or
deionization.
The initial purification produces water very low in salts, but
if the o r i g i n a l s u p p l y c o n t a i n s o r g a n i c m a t t e r t h i s m a y n o t be r e m o v e d , and
traces of resin material m a y be present.
A s t e a d y s u p p l y of c o m p r e s s e d air is r e q u i r e d for an a t o m i c
absorption
s p e c t r o p h o t o m e t e r (AAS) and is v e r y u s e f u l to h a v e a v a i l a b l e at the b e n c h . A
c o m p r e s s o r is s u i t a b l e for use w i t h the i n s t r u m e n t but if used for o t h e r
purposes at the same time it m u s t be capable of supplying those needs without
a f f e c t i n g the AAS s u p p l y . A p a r t f r o m the i n a c c u r a c y that w i l l r e s u l t from a
change in the flame characteristics, sudden failure of the air m a y result in a
flashback, which is expensive if the mixing chamber is destroyed, and could be
dangerous.
H o w e v e r , it m u s t be emphasized that m a n u f a c t u r e r s design this part
of the i n s t r u m e n t to be as safe as p o s s i b l e u n d e r f l a s h b a c k c o n d i t i o n s .
Therefore, in m a n y ways it is probably better to have a separate air supply to
the AAS.
T h i s i n s t r u m e n t a l s o has to be p r o v i d e d w i t h a v e n t i l a t i o n h o o d to
remove gases formed during operation, particularly if nitrous oxide is used as
the fumes are very toxic.
Utility services require a large space but need to be concealed for aesthetic
r e a s o n s , y e t r e q u i r e an e a s y a c c e s s for r e p a i r p u r p o s e s .
To s a t i s f y t h e s e
conflicting demands, the main runs may be in voids above false ceilings and in
floor ducts.
Secondary services are then run to outlet points on benches taken
from floor level along the wall behind benches in voids especially incorporated
in the design of the bench fittings.
Frequent access points are provided for
maintenance purposes.
Drain pipes should be of high density polythene or copolymer polypropylene with
screwed joints.
T h e s e s h o w g o o d r e s i s t a n c e to m o s t o r g a n i c and i n o r g a n i c
chemicals.
The d r a i n a g e l i n e s m a y be e m b e d d e d in the f l o o r i n g . As it is not
acceptable to discharge laboratory w a s t e s d i r e c t l y i n t o t h e s e w e r a g e s y s t e m ,
all w a s t e from l a b o r a t o r y sinks and o t h e r w a s t e f i t t i n g s s h o u l d be led f i r s t
into dilution pots (about 5 litre capacity) before being released into the m a i n
sewers.
Buildings can be designed to include a large dilution tank where all
l a b o r a t o r y sink w a s t e is d i r e c t e d b e f o r e e n t e r i n g the s e w e r a g e s y s t e m .
For
laboratories with high mineral acid use, sink traps of inert duriron often work
well.

17

3.8

Design

References

1.

B e c k , H. L u f t u n g s e i g e n s c h a f t e n von L a b o r a b z u g e n ( V e n t i l a t i o n p o w e r of
laboratory fume cupboard).
Weinheim, Chemie-Ingenieur-Technik, 1964 (No.
3 6 ) (in G e r m a n ) .

2.

Be r u f s g e n o s s e n s c h a f t fur d i e c h e m i s c h e I n d u s t r i e , R i c h t l i n i e n fur
c h e m i s c h e L a b o r a t o r i e n Nr. 12 ( D i r e c t i v e s for c h e m i c a l l a b o r a t o r i e s no.
12) Weinheim, Verlag-Chemie, 1972 (in German).

3.

DECHEMA Erfahrungs austausch;

Laborbau (DECHEMA sharing
laboratory design).
Frankfurt/M. DECHEMA, 1969 (in German).

4.

Decken,
C.B. v.d. a n d
B. H u n d o r f .
Untersuchungen
uber
die
stromungstechnischen Vorgange in der Kapelle eines Laborabzug (Experiments
about flow within the cabin of a fume cupboard).
Darmstadt, GIT 1968 (No.
8) (in G e r m a n ) .

5.

D e u t s c h e r V e r e i n von Gas und W a s s e r f a c h m a n n e r n ( D V G W ) N o r m e n

F e d e r a t i o n of Gas and W a t e r S p e c i a l i s t S t a n d a r d s ) E s c h b o r n ,
Republic of Germany (in German).

(German
Federal

a.

Was serversorgung; Verbrauchanlagen

D W G W W 503-1966.

piping)

b.

T e c h n i s c h e R e g e l n fur Bau und P r u f u n g von v o r g e f e r t i g t e n B a u t e i l e n

mit Gas und Wasserinstallation ( S p e c i f i c a t i o n for c o n s t r u c t i o n and
testing of prefabricated appliances with gas and water installations)
D V G W GW 3 (1968).

c.

Technische Regeln fur die Installation von Gasanlagen in Laboratorien

(Specifications for gas service installations in laboratories) DVGW G
621 (1971).
(Pressure

experience:

(Water supply: service

gas regulation) Koln, Carl Heymann's Verlag

6.

Druckgasverordnung
(in G e r m a n ) .

7.

Dunkl/Geyer.
R a t i o n a l e L o s u n g e n von L a b o r b a u und L a b o r e i n r i c h tungsprob1emen
in H o c h s c h u l e n ,
Industrieunternehmumgen
und i m
Gesundheitswesen der USA (Rational solutions of problems in the design of
laboratory building and equipment for u n i v e r s i t i e s , i n d u s t r y and p u b l i c
h e a l t h in the U n i t e d States).
In B e i t r a g e zur U n i v e r s i t a t s p l a n u n g
( C o n t r i b u t i o n s to the p l a n n i n g of u n i v e r s i t i e s ) . F r a n k f u r t / M . D E C H E M A ,
1970 (Heft 6) (in G e r m a n ) .

8.

F e u r i c h , H. R o h r n e t z e fur S a u e r s t o f f , D r u c k l u f t , V a c u u m , K o h l e n s a u r e in
K r a n k e n h a u s e r n und L a b o r a t o r i e n (Service p i p i n g for o x y g e n , c o m p r e s s e d
air, vacuum and carbon dioxide in hospitals and laboratories) Darmstadt,
G I T 1 9 6 4 (nos. 8, 9 and 10) (in G e r m a n ) .

9.

D e u t s c h e I n d u s t r i e N o r m t'DIN) ( G e r m a n
Beuth-Vertrieb G m b H (all in German)
plant;

principles,

Industrial

a.

Ventilation
English).

b.

Fire resistance
4102-1970.

c.

Space lighting by daylight; principles.

DIN 4034-1969.

d.

Laboratory furniture;
12 912-1973.

laboratory

of building

DIN

Standard).

materials

ceramic

18

tiles

1946-1960,

and

for

Part

structural

Berlin,

(also

elements.

bench

tops.

in

DIN

DIN

e.

Laboratory furniture; cup sinks.

DIN

12-914-1973.

f.

Laboratory
1973.

g.

L a b o r a t o r y furniture; large-size
DIN 12 916-1972.

h.

Colour code for fluids on h a n d l e v e r s and h a n d w h e e l s of laboratory

taps.
DIN 12-920-1971.

i.

Laboratory furniture; benches, dimensions.

j.

Laboratory
1972.

k.

Heating plant,
English).

1.

Traffic ways in buildings.

m.

Ventilation of laboratories. VID 2051-1966.

furniture; sinks w i t h integrated o v e r f l o w . DIN 12 915-

furniture;

smoke

fume

tiles

cupboards,

stacks.

DIN

DIN

18

for laboratory bench

tops.

DIN 12 922-1972.
dimensions.

160-1968;

DIN

part

12

923-

1 (also

in

18-225-1958.

10.

Geyer, F. A n f o r d e r u n g e n an L a b o r b a u t e n ( R e q u i r e m e n t s for laboratory

b u i l d i n g ) D a r m s t a d t , GIT (No. 1 2, 1 967 and No. 1 1968) (in German).

11.

/Richtlinien fur die Planung und den Bau von Laboratorien (Principles for
design and building of laboratories) Weinheim, C h e m i e - I n g e n i e u r - T e c h n i k ,
1971. (No. 11) (in German).

12.

Role et interet de la normalisation dans 1 ' amnagement et l'equipement des

l a b o r a t o i r e s , Courrier de la N o r m a l i s a t i o n , No. 228 n o v e m b r e - d e c e m b r e ,
1972 (in French).

13.

The role and significance of standarization of laboratory equipment and

furniture.
Laboratory Practice (London) No. 4, 1973.

14.

Laboratory furniture and fittings: BS 3202-1959, London, British

Institution.

15.

Strangmann, W. Wasserverbrauch in chemischen und biologischen Laboratorien

(Water consumption in chemical and biological laboratories).
Darmstadt,
GIT, 1964 (No. 6) (in German).

16.

Unfallverhutungsvorschrift:
Medizinische Laboratoriumsarbeiten (Prescription for accident prevention: work in medical laboratories) Frankfurt/M.
H G U V V ) (in German).

17.

United States Department of Health, Education and Welfare, Health Research

Laboratory Design, Bethesda, Maryland NIH 1968 (Publication 1807).

18.

V e r b a n d D e u t s c h e r E 1 e k t r o t e c h n i k e r ( V D E ) N o r m e n (Union of G e r m a n
E l e c t r i c a l Engineers s t a n d a r d s ) O f f e n b a c h / M a i n , Federal Republic of
Germany (in German).

19.

A Literature Survey and Design Study of Fume Cupboards and

Systems, Hughes, D., 1980, Science Reviews Ltd., London.

19

Standards

Fume-Dispersal

4.

4.1

LABORATORY ADMINISTRATION

Sample Collection

Work scheduling is greatly facilitated by arranging a sampling programme for

r o u t i n e m o n i t o r i n g w i t h the i n s p e c t o r a t e .
Close c o o p e r a t i o n w i t h
the
inspectorate will pay great dividends in improved efficiency in sampling.
It
i s o f t e n a l s o n e c e s s a r y to h a v e part of the l a b o r a t o r y staff a v a i l a b l e for
urgent work and for samples such as consumer complaints, export certification
and c h e c k i n g of i m p o r t s , w h e r e t h e r e is o f t e n l i t t l e n o t i c e g i v e n b e f o r e the
arrival of the sample.
S i n c e the l a b o r a t o r y r e l i e s on the i n s p e c t o r a t e for a s t e a d y w o r k l o a d , the
inspectorate and laboratory supervisors must be in frequent contact in order to
m a i n t a i n the w o r k l o a d in the l a b o r a t o r y at a r e a s o n a b l e level. As part of a
general food control programme, there is need to:
1.
Regularly inspect foods at different stages in the manufacturing
distribution chains using planned surveillance programmes.

and

2.
C a r r y out g e n e r a l s u r v e y s of the q u a l i t y of the food s u p p l y t h r o u g h
random sampling and analysis, samples being taken from factories, warehouses
and retailers.
3.
Monitor certain specific problem areas with regard to food safety specific foods or classes of foods for specific potential risks, (e.g. level of
metallic contaminants, pesticide residues, mycotoxins, etc.).
4.

Inspect foods for export, for certification of quality

(if needed).

5.
Inspect
food
imports.
This
is b e s t d o n e on a l l
c o n s i g n m e n t s by f o r m a l s a m p l i n g c a r r i e d out s y s t e m a t i c a l l y in
representative of the lot.

imported
a manner

6.
Formal sampling should also be done on locally produced food products
b a s e d o n t h e f o o d i n s p e c t o r s ' o b s e r v a t i o n s , or b e c a u s e a r a n d o m o r
investigatory sample under the regular programme was unsatisfactory, or because
the product is one that requires thorough surveillance.
Analysis of formal and
informal samples is also necessary in an emergency such as an outbreak of foodpoisoning .
National sampling programmes yield important benefits in terms of efficiency.
The I n s p e c t o r a t e and the L a b o r a t o r y a s s i s t e d and g u i d e d by o t h e r a g e n c y
o f f i c i a l s or an a d v i s o r y b o a r d , as a p p r o p r i a t e , should p e r i o d i c a l l y plan
overall programmes to locate and deal with different problems in the areas of
food q u a l i t y and c o n s u m e r p r o t e c t i o n .
In each case the o b j e c t i v e s of the
p r o g r a m m e should be clearly defined.
A l t h o u g h s a m p l e s m a y be c l a s s i f i e d in a n u m b e r of w a y s , it is c o n v e n i e n t to
consider two broad divisions, "formal" samples and "informal" samples.
Formal
samples are those taken to determine if the foods comply with national or local
l a w s or r e g u l a t i o n s .
R e g u l a t o r y a c t i o n m a y r e s u l t from r e p o r t s r e c e i v e d on
such samples.
Informal samples may be taken for purposes of monitoring or as
part of survey work. Formal follow-up samples can be taken if informal samples
receive adverse laboratory reports.
Formal or informal samples will also be
taken under other circumstances, such as a follow-up to a consumer complaint.
When samples are
of the nature and
required from the
e x p e r i e n c e , from
from the r o u t i n e

sent to the laboratory, the inspector must send full details

purpose of sampling and any other relevant data.
The results
analysis will usually be clear, either from the analyst's own
p r i o r d i s c u s s i o n w i t h the i n s p e c t o r or h i s s u p e r v i s o r s , or
i n f o r m a t i o n g i v e n w i t h the s a m p l e .
A w e l l q u a l i f i e d and

20

t r a i n e d i n s p e c t o r m a y a l s o w i s h to d i s c u s s the need for an a n a l y s i s that the

a n a l y s t w o u l d not r o u t i n e l y c a r r y out.
It is the d u t y of the l a b o r a t o r y H e a d
to decide how these requests are to be met.
The inspector's sample submission form should give all necessary details about
the sample.
These details may include the product n a m e , place of collection,
reason for collection, type of samples (consumer c o m p l a i n t , official, survey,
etc.),
inspector's name,
m o d e of s a m p l i n g ,
lot n u m b e r ,
s h i p p e r if so
transported, size of consignment and similar relevant details, together with
any s p e c i a l i n f o r m a t i o n that m a y be of a s s i s t a n c e to the a n a l y s t , such as
suspected contamination.
T h e s a m p l e s h o u l d a l s o be s e a l e d by the i n s p e c t o r
with an official seal.

4.2

Sample Receipt and

Assignment

W h e n a food s a m p l e is r e c e i v e d for a n a l y s i s , t h e r e m u s t be a s y s t e m to t r a c k
the sample throughout it's initial storage, analysis and later reserve storage.
This is usually embodied in a record keeping system which is keyed to a unique
n u m b e r a s s i g n e d to the s a m p l e at the t i m e of s a m p l i n g .
T h i s n u m b e r c a n be
sequential (i.e. 0001 to 9999) or can be devised to give information (i.e. 0245 - 0 7 , the 2 4 t h s a m p l e t a k e n in 1 985 u n d e r s a m p l i n g p r o g r a m m e n u m b e r 7).
The
r e c o r d m u s t s h o w each m o v e m e n t of a s a m p l e , its r e c e i p t , a s s i g n m e n t to a
l a b o r a t o r y p e r s o n for a n a l y s i s , r e t u r n to the s a m p l e c u s t o d i a n , and e v e n t u a l
disposition.
One of the a d m i n i s t r a t i v e s t a f f s h o u l d be g i v e n this r e c o r d
keeping function and closely supervised by a senior administrator, as well as
supervised in general by the laboratory Head.
It is usually best to use a card record system rather than a log book as cards
are more flexibly handled and may be filed in groups under different headings.
M a n y card record systems have been devised including 5x8 cards with coded sites
on the periphery for punching.
Other cards are pre-printed with spaces to be
filled in w i t h appropriate data.
Regardless of the card system selected, there
are certain items of information which should be on each card:

1.

Sample

number.

2.

Product

3.

Date

4.

Date received

5.

Type of sample

6.

Method

7.

Storage

8.

Date assigned

9.

To whom assigned

name.

sampled.
at the

laboratory.

(survey, complaint,

of storage

etc.).

(dry, refrigeration,

location (coded
for

for easy

freezing,

etc.).

finding).

analysis.
(the analyst

10.

Date returned

(from

11.

From whom returned

12.

Reserve

13.

Final disposition

should

initial

to show

receipt).

analyst).
(may be different

storage method

and

from

the original

analyst).

location.

or disposal

of sample, method

21

and

date.

Note that the above uses the sample record only to record physical m o v e m e n t and
location, not analytical results.
The reason is that the analytical worksheet
and the sample record are usually in two different locations.
T h e s a m p l e r e c o r d card s h o u l d be p r e p a r e d and in the c u s t o d y of one p e r s o n
until the reserve sample is destroyed.
This person is often called the Sample
Custodian and in small laboratories could have other duties as well.
The job
of S a m p l e C u s t o d i a n is c r i t i c a l to the o p e r a t i o n of m o s t l a b o r a t o r i e s .
The
person employed in this post m u s t be very reliable, but m a y find the duties of
the job s l i g h t l y m o n o t o n o u s .
C o m b i n i n g the d u t i e s of s a m p l e c u s t o d i a n w i t h
k e e p i n g the l a b o r a t o r y s t o r e is o f t e n d o n e in m e d i u m
or l a r g e r
sized
laboratories.
The laboratory store of chemicals, glassware and other fittings
r e q u i r e s c a r e f u l c o n t r o l as d o e s r e o r d e r i n g of m a t e r i a l s in s h o r t s u p p l y ,
issuance of supplies to analysts, etc.
Combining the jobs of Sample Custodian
and S t o r e K e e p e r c a n c r e a t e a c h a l l e n g i n g and i n t e r e s t i n g p o s t .
Another
approach to the job of Sample Custodian in smaller laboratories is to split the
job b e t w e e n several people with different senior assistants under the various
section leaders being responsible for samples from a particular source, or for
particular groups of products.
W h e n a s a m p l e is a s s i g n e d , the a n a l y s t s h o u l d p h y s i c a l l y sign or i n i t a l the
s a m p l e c a r d to s h o w c u s t o d y .
W h e n a s a m p l e r e s e r v e is r e t u r n e d to the
C u s t o d i a n , the C u s t o d i a n w o u l d sign or i n i t i a l .
A f t e r a s s i g n i n g the s a m p l e ,
the S u p e r v i s o r m u s t h a v e s o m e m e a n s of t r a c k i n g s a m p l e s u n d e r a n a l y s i s w i t h
proposed or possible completion dates.
The sample card could be used for this.
The card would then be in the hands of the Supervisor during analysis and would
be returned to the Custodian on completion.

4.3

Sample Storage

and

Disposal

S a m p l e s t o r a g e , b o t h i n i t i a l and r e s e r v e , is c r i t i c a l to a s a m p l e a n a l y s i s .
Improper storage can completely i n v a l i d a t e a n y a n a l y t i c a l r e s u l t s .
Ideally,
the s a m p l e is to be s t o r e d in a m a n n e r to p r e v e n t a c h a n g e in the a t t r i b u t e
being examined, from the time of sampling, through analysis, and into reserve
storage.
To i l l u s t r a t e the i m p o r t a n c e of p r o p e r s t o r a g e , if a fresh food
sample to be examined for decomposition is not hard frozen until examination,
it very likely will decompose even further.
The analyst is then not sure how
m u c h of the d e c o m p o s i t i o n found is due to sample mishandling.
The usual storage areas are dry (room temperature storage), refrigeration and
freezing.
K e e p in m i n d t h i n g s that c a n h a p p e n d u r i n g s t o r a g e .
For e x a m p l e ,
insects or other vermin can attack dry storage, mould frequently occurs during
refrigeration, and frozen products often have "freezer burn" where the food has
desiccated.
Steps to m i n i m i z e these problems include using correct containers
(i.e. glass or m e t a l for dry storage, no paper bags), proper sample preparation
(i.e. g l a z i n g f r o z e n s a m p l e s w h e r e p o s s i b l e , to r e d u c e d e h y d r a t i o n ) , and
frequent checks on those stored samples which are m o s t subject to change.
Sample disposal is, or can be, a relatively simple matter.
The only problems
arise w h e n there is a hazard involved in the destruction, or where the sample
r e m a i n s must have special treatment.
An e x a m p l e is a s a m p l e of g r o u n d n u t s
heavily contaminated with aflatoxin.
The sample itself presents a hazard to
the disposer and may be a hazard to others if not detoxified.
The analyst best
k n o w s any h a z a r d s i n v o l v e d , so s h o u l d i n f o r m the S a m p l e C u s t o d i a n of a n y
special disposal requirements.

22

4.4

Budget

The need should be appreciated for as flexible a budgetary system as possible.

C o n t i n g e n c y funds are i m p o r t a n t for the r u n n i n g of a l a b o r a t o r y .
Budgets
should be a r r a n g e d so that funds are r e a d i l y a v a i l a b l e for u r g e n t s u p p l i e s ,
s p a r e s and r e p a i r s and the o t h e r d a y - t o - d a y n e e d s of the l a b o r a t o r y w h i c h
cannot wait for the usually slow cycle of fiscal machinery utilized for annual
budgets in most governments.
The Laboratory Head must have adequate control of
the b u d g e t and o p e r a t e it under c l e a r l y d e f i n e d rules.
T h e s e should be
s u f f i c i e n t l y f l e x i b l e that he or she r e t a i n s d i s c r e t i o n a r y p o w e r s e n a b l i n g
t r a n s f e r of funds b e t w e e n c e r t a i n b u d g e t c l a s s e s as o c c a s i o n d e m a n d s .
For
e x a m p l e , funds for c a p i t a l e q u i p m e n t w i l l u s u a l l y be n o n - t r a n s f e r a b 1 e w h i l e
funds in two s e p a r a t e c l a s s e s for c h e m i c a l s and e x p e n d a b l e e q u i p m e n t m a y
reasonably be transferred between one another.
The b u d g e t p r e p a r a t i o n p r o c e s s should i n v o l v e all l e v e l s of l a b o r a t o r y
management from the Supervisors to the Head.
Supervisors especially gain an
a p p r e c i a t i o n for h o w m o n i e s can or c a n n o t be spent by p r e p a r i n g a b u d g e t
increment for their group.
B u d g e t s t y p i c a l l y are planned for one y e a r , but should be d i v i d a b l e into
quarters, seasons, projects or s o m e o t h e r l o g i c a l d i s t r i b u t i o n f o r m a t .
Each
Supervisor should have the responsibility (overseen and approved by the Head)
for the b u d g e t p u r c h a s e s by h i s group.
All o f f - b u d g e t i t e m s m u s t be fully
justified.
If sufficiently important, an off-budget item may take precedence
over the purchase of budgeted material.

4.5

Purchasing

The s e l e c t i o n and s p e c i f i c a t i o n of l a b o r a t o r y e q u i p m e n t t o g e t h e r w i t h the

p l a n n i n g of space r e q u i r e m e n t s ( i n c l u d i n g f l e x i b i l i t y for f u t u r e e x p a n s i o n )
should always precede, or at least go hand in hand with, building design.
Less
industrial countries often lack l a b o r a t o r y s u p p l i e s and e q u i p m e n t , t e c h n i c a l
assistance and maintenance services. The limited over-all marketing potential,
and the large variety of laboratory and scientific instruments available from
foreign suppliers and manufacturers, make it generally uneconomical for local
businessmen to establish stocks or to employ qualified service engineers.
The
p r o b l e m in m a n y c o u n t r i e s is c o m p o u n d e d by f o r e i g n e x c h a n g e and i m p o r t
r e s t r i c t i o n s w h i c h o f t e n do not e v e n p e r m i t the c o m m e r c i a l i m p o r t of spare
parts.
As a result, scientific laboratories in developing countries cannot, or
can only to a l i m i t e d e x t e n t , find t e c h n i c a l a s s i s t a n c e locally.
They m u s t
r e l y on the support and c o o p e r a t i o n of s u p p l i e r s based p e r h a p s t h o u s a n d s of
miles away.
Several conclusions can be drawn from this situation.
One of them
is that b e f o r e s e l e c t i n g any e q u i p m e n t , a c a r e f u l study should be m a d e to
determine :
1.
Which of the many possible suppliers and manufacturers of equipment
h a v e local r e p r e s e n t a t i v e s or o f f i c e s c a p a b l e of p r o v i d i n g i n s t a l l a t i o n and
maintenance services?
2.
W h a t e x p e r i e n c e do p o t e n t i a l s u p p l i e r s h a v e in d e a l i n g
special conditions obtaining in less industrialized countries?

with

the

E q u i p m e n t s p e c i f i c a t i o n s m u s t be p r e p a r e d very carefully and clearly.

There
are countless examples of cases where lack of detail in specifying has led to
the p u r c h a s e of i n c o m p l e t e or u n s u i t a b l e a p p a r a t u s .
It should be u n d e r s t o o d
that s u p p l e m e n t a r y e q u i p m e n t or a c c e s s o r i e s , if not s p e c i f i e d , w i l l not be
quoted for in the s u p p l i e r ' s bid. M o s t b r o c h u r e s or c a t a l o g u e s p u b l i s h e d by
equipment manufacturers give only general information, without complete order
specifications.
A s e l e c t i o n based p u r e l y on such l i t e r a t u r e o f t e n leads to
misunderstandings.
No indication is usually given of essential accessories not

23

included in the basic instrument, of optional accessories with explanations for

t h e i r p a r t i c u l a r a p p l i c a t i o n , or o f e s s e n t i a l o p e r a t i n g s u p p l i e s
and
r e c o m m e n d e d spare parts.
S c i e n t i f i c i n s t i t u t i o n s in less i n d u s t r i a l i z e d
countries have had the experience that because of insufficient specifications
(or lack of e x p e r i e n c e on the part of the s u p p l i e r s ) they w e r e s u p p l i e d w i t h
incomplete equipment.
W h i l e the s u p p l i e r m a y b e l i e v e that n o n - s p e c i f i e d e q u i p m e n t is a l r e a d y
a v a i l a b l e , the s c i e n t i s t in the l a b o r a t o r y m a y be s u f f e r i n g s e r i o u s and
annoying delays in putting the equipment into operation. New orders have to be
processed, and up to a year may be required to obtain the necessary additional
supplies.
Most manufacturers restrict their supplies to the parts they produce
in t h e i r o w n w o r k s .
T h e y a r e u s e d to the s i t u a t i o n w i t h i n t h e i r o w n c o u n t r y
w h e r e m i n o r a c c e s s o r i e s such as s t a n d s , c l a m p s , t u b i n g , g l a s s w a r e and e v e n
small instruments like pH-meters, balances and thermostats c o m m o n l y found in a
laboratory are either available i m m e d i a t e l y or may be obtained quickly from a
local dealer.
W h e n dealing with less industrialized countries, h o w e v e r , it is
frequently wrong to assume that the same situation obtains.
Large laboratory supply companies offer a m o r e comprehensive range of supplies
than individual manufacturers as their delivery p r o g r a m m e usually includes a
full range of instruments and auxiliary equipment.
Another advantage offered
by the l a r g e c o m p a n i e s is the e c o n o m y g a i n e d by d e a l i n g w i t h o n l y one s o u r c e
rather than having to deal with a n u m b e r of individual manufacturers.
Service
f a c i l i t i e s for i n s t a l l a t i o n and m a i n t e n a n c e of the e q u i p m e n t can also be
coordinated and provided m u c h m o r e easily by a large organization.
If experts
h a v e to be c o m m i s s i o n e d for each i n d i v i d u a l p i e c e of c o m p l e x e q u i p m e n t , the
expense b e c o m e s prohibitive.
C o m p l e x a p p a r a t u s r e q u i r e s s p e c i a l t r a i n i n g for the o p e r a t o r s .
Engineers
p e r f o r m i n g the installation usually provide some basic training.
Depending on
the experience of the scientist who is to work with the equipment, h o w e v e r , a
m o r e f a r - r e a c h i n g p r o g r a m m e of t r a i n i n g m a y be n e c e s s a r y , w h i c h c a n n o t be
i m p a r t e d by the e n g i n e e r in the field.
In such c a s e s , s p e c i a l t r a i n i n g
p r o g r a m m e s should be arranged in advance of the purchase, preferably before the
equipment is delivered.
P r o c u r e m e n t r u l e s d e m a n d , a l m o s t e v e r y w h e r e , that the c h e a p e s t o f f e r s be
accepted.
Applied to the purchase of scientific e q u i p m e n t , strict observation
of such r u l e s m a y turn out to be a v e r y e x p e n s i v e w a y of e q u i p p i n g a
laboratory.
Precise specifications are a good m e a n s of obtaining correct and
reliable offers.
O n l y such o f f e r s a l l o w a just c o m p a r i s o n of the s c o p e of
d e l i v e r y and the p r i c e s of d i f f e r e n t b i d d e r s .
In o r d e r to o b t a i n a n
u n d i s t o r t e d p i c t u r e of c o m p a r a t i v e d a t a , o n l y t e c h n i c a l l y e x p e r i e n c e d and
c o m m e r c i a l l y capable manufacturers and suppliers should be invited to submit
offers.
Only a limited number of firms that can satisfy every requirement as
to q u a l i t y , e x p e r i e n c e in h a n d l i n g c o m p r e h e n s i v e s u p p l i e s , r e l i a b i l i t y in
c o n n e c t i o n w i t h d e l i v e r y s c h e d u l e s , t e c h n i c a l a s s i s t a n c e and m a i n t e n a n c e
s e r v i c e s h o u l d be i n v i t e d to t e n d e r .
T h i s m a y e v e n lead to i n d i v i d u a l f i r m s
being selected as suppliers for entire laboratory equipment lots or specialized
instruments on a proprietary or s ingle-tender basis.
I n v i t a t i o n s to bid s h o u l d a l w a y s g i v e c l e a r i n d i c a t i o n s of the c u r r e n c y and
t e r m s in w h i c h o f f e r s are to be s u b m i t t e d ; if i n d i v i d u a l p r i c e s a r e to be
q u o t e d e x - w o r k s , f.o.b. port of s h i p m e n t , c & f. or c.i.f. p o r t of d e s t i n a t i o n ;
if s h i p m e n t is d e s i r e d b y air or sea; and w h e t h e r or n o t the c o s t of p a c k i n g
should be included.
It is worth pointing out that North A m e r i c a n firms have a
d i f f e r e n t i n t e r p r e t a t i o n of the t e r m "f.o.b." (free on b o a r d s h i p ) f r o m
European suppliers.
The latter observe the internationally accepted definition
of the t e r m , a c c o r d i n g to w h i c h f.o.b. p r i c e s i n c l u d e c o s t and all c h a r g e s of
delivery including packing, up to "on board ship" in the seaport or airport of
shipment.
In the U n i t e d S t a t e s of A m e r i c a , h o w e v e r , "f.o.b." is n o r m a l l y
u n d e r s t o o d as f.o.b. f a c t o r y , and p r i c e s do not i n c l u d e p a c k i n g ,
inland

24

f r e i g h t , l o a d i n g c h a r g e s , d o c u m e n t a t i o n or e x p o r t h a n d l i n g , all of w h i c h are
charged separately.
The term f.a.s. is used to denote "free alongside ship".
If a b i d d e r d e v i a t e s from the t e r m s laid d o w n in the t e n d e r i n v i t a t i o n , h i s
o f f e r s h o u l d be c a r e f u l l y e x a m i n e d as it m a y h a v e b e e n i n t e n d e d to o b t a i n a
superficial advantage in price comparison only.
A careful technical scrutiny
of the s p e c i f i c a t i o n s g i v e n in a b i d d e r ' s o f f e r and a c o m p a r i s o n w i t h the
i l l u s t r a t e d l i t e r a t u r e a t t a c h e d to the bid w i l l , in m a n y c a s e s , e l i m i n a t e
q u o t a t i o n s w h i c h at f i r s t g l a n c e look c h e a p e r .
Accessories may have been
p u r p o s e l y left out to g a i n an a d v a n t a g e over o t h e r b i d d e r s .
Sometimes minor
b u t i m p o r t a n t d i f f e r e n c e s in p e r f o r m a n c e d a t a c a u s e c o n s i d e r a b l e
price
variations.
M a n y n a t i o n a l and i n t e r n a t i o n a l o r g a n i z a t i o n s i n v i t e o f f e r s from o r i g i n a l
manufacturers only, demand ing that the c o m m i s s ion usually allowed to agents be
offered as a discount.
The disadvantages of this procedure are that orders are
quite frequently placed w i t h firms which readily accept these conditions but
which have neither experience nor agents in the purchasing country.
Thus, the
scientists in less industrali zed countries are denied the benefit of any kind
of t e c h n i c a l a s s i s t a n c e .
W h e n c o m p a r i n g p r i c e q u o t a t i o n s , the o f f e r of an
i n t e r n a t i o n a l l a b o r a t o r y e q u i p m e n t s u p p l i e r m a y o c c a s i o n a l l y be found to b e
substantially higher than that of a manufacturer.
In such cases it can only be
r e c o m m e n d e d t h a t the e x p e r i e n c e and a f t e r - s a l e s s e r v i c e i n c o r p o r a t e d in the
offer should be carefully considered.
One aspect of equipment purchase that causes problems is the time given for the
s u b m i s s i o n of o f f e r s .
O f t e n it is far too s h o r t .
It s h o u l d be r e a l i z e d t h a t
long lists of specifications prepared for a project over an extended period of
time cannot normally be quoted for in a space of only two or three weeks - the
t i m e that m i g h t be left to a s u p p l i e r a f t e r d e l a y s in m a i l are t a k e n into
account.
The q u a l i t y of o f f e r s m i g h t be c o n s i d e r a b l y i m p r o v e d if m o r e t i m e
were allowed.
D e c i s i o n s on bid a c c e p t a n c e s h o u l d n o t be d e l a y e d b e y o n d the
n o r m a l validity of offers.
Another serious problem that is often encountered concerns damage in transit
Extensive d a m a g e and even total loss
and the insurance covering such damage.
can result from the rough handling of consignments in ports where no mechanized
m e a n s of t r a n s p o r t (such as f o r k - l i f t t r u c k s ) is a v a i l a b l e .
D e l a y s m a y be
e n c o u n t e r e d in c l e a r i n g c o n s i g n m e n t s t h r o u g h c u s t o m s , and s h e l t e r e d s t o r a g e
facilities are often quite inadequate.
Cases containing expensive equipment
m a y be s u b j e c t e d to the m o s t a d v e r s e c l i m a t i c c o n d i t i o n s - h u m i d i t y , h e a v y
tropical rains, extreme heat and dust.
No economically justifiable method of
p a c k i n g can p r e v e n t d a m a g e to e q u i p m e n t u n d e r such c o n d i t i o n s .
Sometimes,
b e c a u s e of c u s t o m s f o r m a l i t i e s and a d m i n i s t r a t i v e d e l a y s in h a v i n g the
consignments unpacked and examined, insurance coverage has already expired by
the t i m e the e q u i p m e n t a r r i v e s at its d e s t i n a t i o n and a c l a i m can be l o d g e d .
T h e n , m o r e t i m e and e f f o r t is u s u a l l y s p e n t on f i x i n g r e s p o n s i b i l i t y than on
how the situation might be avoided in the future.
Replacement parts required to repair transport damage should be obtainable with
a m i n i m u m of delay and administrative red tape.
Laboratories should have the
authority, in an emergency, to place small orders direct with suppliers.
With
or without such emergency order facilities, h o w e v e r , scientists usually depend
on (and prefer cooperation with) the experienced and flexible supplier who is
in regular contact w i t h his customer, who extends unbureaucratic help and who
even provides, when necessary, free replacements and repair facilities in order
to c o n t r i b u t e to the p r i m e o b j e c t i v e in the e s t a b l i s h m e n t of a s c i e n t i f i c
institute, useful and effective work and uninterrupted operation.

25

4.6

Supplies

Management

Supplies routinely used by a laboratory include solvents, reagents, chemicals,

g l a s s w a r e and o t h e r a n a l y t i c a l m a t e r i a l s .
By d e f i n i t i o n ,
s u p p l i e s are
considered to be consumables and must be constantly replaced as used.
T h e r e m u s t t h e r e f o r e b e an a c c u r a t e a c c o u n t i n g s y s t e m to r e c o r d r e c e i p t , u s e
and f u t u r e n e e d .
T h i s is d o n e in a v a r i e t y of w a y s but a card s y s t e m is the
m o s t versatile.
The Supplies Record Card can contain such data as:

Name of product
Date purchased
Where purchased
Amount (including units if more than one
Expiration date (if any)
Special storage requirements (if any)
Amount dispensed.

container)

S m a l l m e t a l t a g s p a i n t e d w i t h b r i g h t c o l o u r s can be p u r c h a s e d and d i f f e r e n t
tags affixed to cards for flagging purposes.
For e x a m p l e , a red tag m a y m e a n
the supply is low and should be reordered within a given time.
Having a w o r k a b l e supplies m a n a g e m e n t s y s t e m t e n d s to p r e v e n t c i r c u m s t a n c e s
w h e r e a n a l y s e s h a v e s t o p p e d b e c a u s e a c r i t i c a l m a t e r i a l is s u d d e n l y u s e d up.
L i k e b u d g e t i n g , it is a p r o c e s s of m a i n t a i n i n g c o n t r o l of a c r i t i c a l a r e a to
promote overall smooth operation of the laboratory.

4.7

Equipment

Maintenance

W h e n the food analyst goes beyond organoleptic examinations, he or she must use
s o m e i t e m of e q u i p m e n t to p r o c e s s or to m e a s u r e the s a m p l e a t t r i b u t e of
interest.
It is critically important, therefore, that all items of equipment
be properly and promptly maintained, and repaired when needed.
T h e d e g r e e of s o p h i s t i c a t i o n of e q u i p m e n t v a r i e s d r a m a t i c a l l y from a
straightforward pH m e t e r to a complex spectrophotometer.
M a n y laboratories in
developing
countries have great difficulty
in o b t a i n i n g r e p a i r of any
e q u i p m e n t , sophisticated or otherwise.
It is therefore
reasonable to require
that proper maintenance of the equipment be routinely scheduled and completed,
hopefully to delay the day when outright repairs are necessary.
T h e b e s t c i r c u m s t a n c e , of c o u r s e , is to e s t a b l i s h an o p e r a t i n g r e p a i r and
m a i n t e n a n c e w o r k s h o p w i t h qualified technical staff.
This can be essential for
l a r g e i n s t i t u t e s h a v i n g a d i s p r o p o r t i o n a t e l y l a r g e i n v e s t m e n t in e x p e n s i v e
equipment.
E v e n in the a b s e n c e of an o r g a n i z e d w o r k s h o p , s o m e a n a l y s t s or
technicians can be given training in repair and maintenance techniques, often
by local instrument suppliers.
If adequate service is available locally, serious consideration should be given
to purchase of service contracts.
The usual service contract involves checking
the e q u i p m e n t at s p e c i f i e d i n t e r v a l s and p e r f o r m i n g n e c e s s a r y m a i n t e n a n c e .
E m e r g e n c y r e p a i r s are u s u a l l y d i s c o u n t e d in p r i c e b e c a u s e of the s e r v i c e
contract.
Service contracts are especially important for analytical balances,
to m a i n t a i n proper calibration.
A history of an instrument's maintenance and repair can become very important.
It p r o v i d e s a s u m m a r y of the i n s t r u m e n t ' s o p e r a t i o n o v e r a g i v e n p e r i o d , b u t
m o r e i m p o r t a n t l y , it can p r o v i d e a j u s t i f i c a t i o n for r e p l a c e m e n t of old and
o u t w o r n items.
Recording the cost is important as it is then readily apparent

26

w h e n an i n s t r u m e n t c o s t s m o r e to k e e p o p e r a t i n g t h a n it is w o r t h .
A preprinted
5 x 8 c a r d c a n c o n v e n i e n t l y b e u s e d to r e c o r d s u c h i n f o r m a t i o n .
An e x a m p l e of
s u c h a c a r d ( f r o n t a n d r e a r ) is s h o w n in F i g u r e s 4.1 a n d 4 . 2 .

T y p e of Machin*

MACHINE
PART I -

DETAILS

OF

HISTORY

CARD

MACHINE

B r a n d a n d Modal N o .

Vendor

L o c a t i o n of m a c h i n e
(State dept./scction)

H o w o p e r a t e d ( T i c k in appropriate b o x )

Machine N o .

C o u n t r y of Manufacture

Data of P u r c h a i e

Purchase Price

Guarantee P e r i o d

T e r m s of Guarantee

P A R T II -

Manual

Etactrk

Electronic

DETAILS OF MAINTENANCE
Service A g e n t

Per lOd

Maintenance C o n t r a c t

Name

From

Cott ($)
(per a n n u m )

To

Spare parts
included?
Yes

No

N u m b e r of

C o m m e n t o n f i r m ' service

(per a n n u m )

Figure 4.1
Front Side

F A R T HI -

OF

BREAKDOWNS
S e r v i c i n g / R e o a i r details
(State cause of b r e a k d o w n a n d
parts c h a n g e d , etc!

Date

P A R T IV

OETAILS

COMMON D E F E C T S

I d n c n b * with d . u i l i

pm

Response
time of
Service A g e n t

f r * j . n y . cHactsl

Figure 4.2
Rear Side

27

Cumulative
Cost

C o s t of
Repair

Time taken
to repair

4.8

Housekeeping

L a b o r a t o r y c l e a n l i n e s s is very i m p o r t a n t , not only to m a i n t a i n a good

appearance,
but to p r e v e n t s o m e f o r m s of c o n t a m i n a t i o n .
Housekeeping
a c t i v i t i e s go beyond c l e a n i n g and tidying in the l a b o r a t o r y .
It i n c l u d e s
i n s e c t and o t h e r pest c o n t r o l .
M o s t l a b o r a t o r i e s m u s t do their o w n pest
control to minimize contamination from control agents. Commercial pest control
firms usually do not have an appreciation of laboratory contamination problems.
L a b o r a t o r i e s m u s t be r o d e n t - p r o o f in c o n s t r u c t i o n .
E l e c t r i c a l d e v i c e s are
available for killing flying insects.
Food may arrive contaminated with insect
eggs so that proper storage is inadequate without fumigation.
Fumigation by
halogenated hydrocarbons or use of organochlorine compounds against insects are
l i k e l y s o u r c e s of l a b o r a t o r y c o n t a m i n a t i o n and are best a v o i d e d w h e n e v e r
possible.
T h e y all h a v e a s i g n i f i c a n t v a p o u r p r e s s u r e and m u s t be kept w e l l
a w a y from s e n s i t i v e e q u i p m e n t such as gas c h r o m a t o g r a p h s and from s a m p l e s
requiring analysis for pesticide residues.
H o u s e k e e p i n g should involve s c h e d u l e d as w e l l as ad hoc c l e a n i n g and pest
control.
O f t e n a good t i m e is the last h o u r of a w o r k w e e k .
A scheduled
activity quickly becomes routine and is consequently in the awareness of the
laboratory analysts.
This awareness is important because, as can be shown by
e x p e r i e n c e , not all p e r s o n s are n e a t , c l e a n and tidy in their e v e r y d a y
activities.
M a n a g e m e n t m u s t d e m o n s t r a t e a c o n t i n u i n g c o m m i t m e n t to good
housekeeping principles if the analysts are to accept those principles.

4.9

Training

W h e n an a n a l y s t is first hired in a food c o n t r o l l a b o r a t o r y , a c o n t i n u i n g

s e r i e s of t r a i n i n g and e d u c a t i o n a l e x p e r i e n c e s b e g i n .
The n e w a n a l y s t is
t a u g h t , u s u a l l y on the job, the v a r i e d a n a l y s e s and m e t h o d s used by the
laboratory.
Most often this is by what amounts to an apprenticeship approach
where the new analyst is assigned to work with a senior.
It is best, however,
to have a formal, structured training programme designed to acquaint the new
analyst with the work in a logical sequence.
Otherwise the training becomes
haphazard with the training sequence dependent on incoming work.
O n c e past the f o r m a l initial t r a i n i n g , the a n a l y s t s t a r t s a c o n t i n u i n g
knowledge updating process.
Food analysis is a rapidly changing subject and it
is i m p o r t a n t that a n a l y s t s attend s y m p o s i a , r e f r e s h e r c o u r s e s and other
educational programmes in order to keep up to date. In developing countries it
may be necessary to schedule travel to other areas from time to time for such
t r a i n i n g . T h i s e f f o r t is e n h a n c e d if the l a b o r a t o r y is a b l e to s u b s c r i b e to
the more active research journals in food analysis.
The analysts are then able
to keep abreast of new advances, especially newer analytical methods.
Should an a n a l y s t s h o w i n t e r e s t and a p t i t u d e for s u p e r v i s i o n , then he or she
s h o u l d be g i v e n f o r m a l c l a s s r o o m t r a i n i n g in s u p e r v i s o r y p r i n c i p l e s .
This
w o u l d be in a d d i t i o n to o n - t h e - j o b e x p e r i e n c e under the t u t e l a g e of a
supervisor or the Head.
It is important that the classroom instruction be done
because it is here that the analyst learns supervision and management theory
and techniques other than those used by his laboratory.
On-the-job experience
as an acting supervisor is necessary but tends to be one dimensional because it
teaches only the systems and techniques used by that laboratory.

28

5.

5.1

LABORATORY

OPERATIONS

Workplans

T h e a n n u a l w o r k p l a n is the c o r n e r s t o n e to m a n a g i n g a food c o n t r o l l a b o r a t o r y .
It p r o v i d e s a m e a n s of e s t i m a t i n g s t a f f a n d r e s o u r c e s n e c e s s a r y to do a f i x e d
n u m b e r of a n a l y s e s .
C o n v e r s e l y , g i v e n a f i x e d s t a f f , the w o r k p l a n can e s t i m a t e
h o w m u c h w o r k can be d o n e .
W o r k p l a n d a t a is a l w a y s o n l y an e s t i m a t e , a l t h o u g h its a c c u r a c y o f t e n
w i t h u s e d u e t o r e f i n i n g o f t i m e m o d u l e s u s e d in c a l c u l a t i o n s .
i m p o r t a n t t i m e m o d u l e s in w o r k p l a n n i n g are:

improves
The two

1.
T h e a n a l y s t p r o d u c t i v e y e a r : T h i s is t h a t t o t a l t i m e i n a n a v e r a g e
year that one a n a l y s t s p e n d s doing o n l y s a m p l e a n a l y s i s .
Time spent during
w o r k h o u r s d o i n g o t h e r t h i n g s is d e d u c t e d .
A n e x a m p l e of t h e d e t e r m i n a t i o n of
t h i s m o d u l e is as f o l l o w s :

Total

time a v a i l a b l e

(based

on 4 0 h o u r w o r k

week)

2080 hr s

Time deductions N a t i o n a l and l o c a l h o l i d a y s

Illness
P e r s o n a l leave time
Training
A d m i n i s t r a t i v e time
Other n o n - a n a l y s i s time
Total time d e d u c t i o n s
Total analysis

time

(2080 -

80
40
80
200
80
400
880

hr s
hrs
hr s
hrs
hrs
hrs
hrs

1200 hrs

880)

T h i s m e a n s ( b a s e d on the a b o v e e x a m p l e ) that for n a n a l y s t s , the

e x p e c t n x 1 2 0 0 h o u r s of p r o d u c t i v e w o r k d u r i n g t h e y e a r .

laboratory

can

T h e a b o v e t i m e d e d u c t i o n f i g u r e s w e r e t a k e n for e x a m p l e p u r p o s e s o n l y .
Each
i n d i v i d u a l l a b o r a t o r y w i l l be d i f f e r e n t .
In d e t e r m i n i n g d e d u c t i o n s , c o n s i d e r
the f o l l o w i n g :
a.

Holiday

time

is u s u a l l y

fixed

b.

I l l n e s s and p e r s o n a l t i m e a v e r a g e s can be t a k e n f r o m
staff
The
a d m i n i s t r a t i v e r e c o r d s f o r t h e p r e c e e d i n g o n e or t w o y e a r s .
a v e r a g e of the p r e v i o u s y e a r is b e s t u s e d as the m o d u l e . T h e r e a s o n
is that the s t a f f u s u a l l y h a v e m o r e p e r s o n a l t i m e m a d e a v a i l a b l e to
t h e m as t h e i r s e n i o r i t y i n c r e a s e s .

c.

M a n a g e m e n t m u s t d e c i d e h o w m u c h t i m e w i l l be set a s i d e e a c h y e a r for
t r a i n i n g . N o t e in the e x a m p l e t h a t t r a i n i n g t i m e is a b o u t 10% of the
t o t a l . If the s t a f f is r e l a t i v e l y y o u n g and i n e x p e r i e n c e d , m o r e t i m e
w i l l be r e q u i r e d .
C o n v e r s e l y an a l l - s e n i o r s t a f f m a y r e q u i r e l e s s .

d.

A d m i n i s t r a t i v e t i m e is d i f f i c u l t to e s t i m a t e as t h e r e are u s u a l l y few
or no r e c o r d s to go b y .
It i n c l u d e s t i m e a s a c t i n g
supervisor,
general
library reading,
and o t h e r a s s i g n e d
or
incidental
administrative activities.

e.

O t h e r n o n - a n a l y s i s t i m e is also o n l y an e s t i m a t e , a l t h o u g h s o m e t i m e
r e c o r d s m a y be a v a i l a b l e .
It i n c l u d e s g e n e r a l r e s e a r c h o r m e t h o d
development
activities,
quality
assurance
work,
equipment
m a i n t e n a n c e , t i m e s p e n t s e r v i n g as a t r a i n e r , a n d a n y o t h e r n o n a n a l y s i s w o r k time not included e l s e w h e r e .

29

by government

policy.

2.
T h e a n a l y t i c a l h o u r s r e q u i r e d per s a a p l e :
The f i r s t step is to
d e f i n e w h a t is i n c l u d e d in a s a m p l e a n a l y s i s , as t h i s o b v i o u s l y a f f e c t s the
total time.
Activities which are suggested to be included are:
a.

Sample receipt and

preparation.

b.

Analysis.

c.

M e t h o d d e v e l o p m e n t or p r o b l e m s o l v i n g r e q u i r e d of a g i v e n s a m p l e .
(As o p p o s e d to g e n e r a l d e v e l o p m e n t or r e s e a r c h , w h i c h w o u l d b e
included in non-analysis time.)

d.

S t a n d a r d i z a t i o n a c t i v i t i e s r e l a t e d to a g i v e n s a m p l e .
standard solutions and curves for example.)

e.

Preparation

of analytical

report and

(Preparing

calculations.

The next step is to prepare a list of all the different analyses conducted and
e s t i m a t e individual analytical times based on experience.
If some analyses are
d o n e b y t e a m s in a p r o d u c t i o n - 1 i n e a r r a n g e m e n t , e s t i m a t e the t o t a l t i m e
required by totalling the time and correcting to an individual analyst basis.
For e x a m p l e , if 4 analysts working as a team can produce 32 completed samples
in an 8 h o u r p e r i o d ,
t h e n t h e a v e r a g e a b s o l u t e s a m p l e t i m e is 0.25
hours/analysis.
H o w e v e r , it required 4 analysts and to correct the time to an
i n d i v i d u a l a n a l y s t b a s i s - 4 x 0.25 = 1.0 h o u r s / ana 1 ys i s . T h i s w o u l d be the
figure used in calculations.
*

The laboratory is now able to make good estimates on what and h o w m u c h work can
be d o n e .
It is a s i m p l e m a t t e r of m u l t i p l y i n g the n u m b e r s of a n a l y s t s
a v a i l a b l e d u r i n g the y e a r t i m e s the p r o d u c t i v e y e a r t i m e m o d u l e to g a i n the
total analytical hours available.
This can then be spread among the types of
a n a l y s e s to be d o n e , u s i n g the h o u r s / a n a l y s i s m o d u l e s .
A l t h o u g h m a n y of the
m o d u l e s are e s t i m a t e s , it is still a better and m o r e accurate w a y to d e t e r m i n e
w h a t can be d o n e , than r e l y i n g on m e m o r y and s h e e r g u e s s e s .
( R e g a r d i n g the
n u m b e r s of a n a l y s t s a v a i l a b l e d u r i n g the y e a r , k e e p in m i n d t h a t t h i s m a y
change by new hires or projected losses, so include these future projections in
the annual estimate).
T h e a b o v e c a l c u l a t i o n m e c h a n i c s of a w o r k p l a n do not a d d r e s s the m e a n s of
d e c i d i n g the a n n u a l w o r k p r i o r i t i e s .
T h i s is u s u a l l y d o n e in p a r t b y
organizational policy and in part by m e e t i n g s of senior operational managers,
s u c h as the L a b o r a t o r y and I n s p e c t o r a t e H e a d s .
All p l a n n e d w o r k and t i m e
modules depend on proper work scheduling and flow.
If samples are collected
too fast or too slow, the laboratory efficiency suffers.
There m u s t therefore
be an extremely close working relationship and liaison b e t w e e n the inspectorate
and l a b o r a t o r y .
No work plan would be complete without some form of contingency planning.
The
o l d a d a g e s t a t e s t h a t , "... If s o m e t h i n g c a n go w r o n g , it w i l l
...".
T h e r e f o r e , t h e r e s h o u l d be at least a p r o v i s i o n in a a n n u a l w o r k p l a n for
e m e r g e n c i e s or u n e x p e c t e d p r o b l e m s .
A m a j o r p u b l i c h e a l t h d i s a s t e r , for
e x a m p l e , could require an all-out laboratory effort, negating workplan work for
some period of time.
The contingency plan would simply and clearly state w h a t
t y p e s of a n a l y s e s ( u s u a l l y the l o w e s t p r i o r i t y ) w o u l d be e l i m i n a t e d in the
event of an emergency.

30

5.2

Priorities

for

General analytical
laboratory policy.

Analysis

priorities are usually s o m e w h a t fixed by organizational

H o w e v e r , a suggested priority structure would be:

Priority 1

Poisonings or
public health

Priority 2

K n o w n or
resulting

Priority 3

Informational

injury complaints
analyses.

s u s p e c t e d law or
in direct injury.
surveys

and

health

other

emergency

violations,

and other routine

or

not

work.

M o s t of the w o r k of a l a b o r a t o r y is u s u a l l y in the t h i r d p r i o r i t y c a t e g o r y ,
with a smattering of priority two and only infrequently, priority one.
W i t h i n a g i v e n p r i o r i t y , the w o r k c a n be s u b - g r o u p e d by r e l a t i v e i m p o r t a n c e .
It is conceivable that work of very low importance never gets done because of
the continuing press of higher priority analyses.
If it appears that such is
the c a s e , the s u p e r v i s o r m u s t a d v i s e the H e a d of the p r o b l e m s and s u g g e s t
r e v i s i o n of the p l a n n e d w o r k load for the s u p e r v i s o r ' s g r o u p .
The w o r k p l a n s
discussed in the previous Section often undergo mid-year or periodic revision
based on such happenings.

5.3

Analysis

Assignaient

A s s u m i n g the p r i o r i t y nas b e e n p r e v i o u s l y a s s i g n e d , the a n a l y s i s a s s i g n m e n t

includes two key considerations, n a m e l y w h a t is to be done and what analytical
method to use.
T h e a n a l y s i s to be c a r r i e d out on a s a m p l e m a y be p r e d e t e r m i n e d as p a r t of a
planned sampling p r o g r a m m e or by legal requirements.
Experience gained by the
analyst may enable him to have firm views on the tests to be done.
The purpose
of the a n a l y s i s m u s t be b o r n e c l e a r l y in m i n d , e.g. for e x p o r t c e r t i f i c a t i o n ,
the t e s t s r e q u i r e d by the i m p o r t i n g c o u n t r y m u s t be c a r r i e d o u t , for e x c i s e
purposes, the constituent that fixes the duty payable and so on.
When samples
are examined under the general and specific provisions of laws pertaining to
consumer protection and food quality, the analysis m u s t be designed to answer
certain questions such as:
Does the food meet established m i n i m u m quality and
safety standards?
Is it of the quality, substance and nature demanded by the
purchaser?
Is it correctly labelled?
Are any claims on the label justifiable
and l e g a l ?
D o e s it c o n t a i n n o n - p e r m i t t e d a d d i t i v e s or p e r m i t t e d o n e s in
excess?
Are any contaminants present at unacceptable levels?
R o u t i n e t e s t s on the p h y s i c a l c h a r a c t e r i s t i c s of m o s t c o m m o n food s a m p l e s
should be carried out.
Less frequently, tests may be made for preservatives,
prohibited colours and other a d u l t e r a n t s .
T h e a d u l t e r a n t s , c o n t a m i n a n t s and
compositional deficiencies looked for should be changed from time to time to
show if previously unsuspected infringements are present.
The analyst m u s t be
aware of the problems facing manufacturers and of developments in technology
and choose non-routine tests in the light of this information.
In this way the
r e g u l a t o r y a n a l y s t acts as a s u p p o r t to the l e g i t i m a t e m a n u f a c t u r e r w h i l e
protecting the consumer.
The analyst must establish that he can obtain reliable results with the method
used.
G e n e r a l l y , it is p r e f e r a b l e to use a m e t h o d t h a t h a s b e e n s u b j e c t e d to
collaborative study.
If the analyst has difficulty
with such a method it is
likely to be due to a deficiency in training or in facilities, rather than the
method itself.
Sometimes
it is d u e to p o o r e x p r e s s i o n of t h e e x a c t

31

e x p e r i m e n t a l d e t a i l s in the m e t h o d as published.
R e f e r e n c e to the source w i l l
usually resolve such difficulty.
It is n o t a l w a y s n e c e s s a r y
to u s e a
collaborated method.
H o w e v e r , s u c h m e t h o d s s h o u l d be f i r s t c h o i c e if the
p a r a m e t e r is b e i n g d e t e r m i n e d in t h e l a b o r a t o r y f o r t h e f i r s t t i m e or if a
p r o d u c t has not been a n a l y z e d p r e v i o u s l y .
It is i m p o r t a n t to f o l l o w the
p r o c e d u r e s ior v a l i d a t i n g a m e t h o d .
M a n y o t h e r m e t h o d s m a y be e q u a l l y g o o d ,
but m a y not, for v a r i o u s reasons, have been subjected to c o l l a b o r a t i v e studies
or r u g g e d n e s s t e s t s .
As a r e s u l t
the a n a l y s t m a y run into
unexpected
d i f f i c u l t i e s if he h a s to t a k e the m e t h o d d i r e c t l y f r o m a b o o k .
If a m e t h o d
has b e e n in use and found to give r e l i a b l e results it should not be changed for
another
until
the n e w m e t h o d
has been s h o w n
to be of e q u a l or b e t t e r
r e l i a b i l i t y in that p a r t i c u l a r l a b o r a t o r y ( i r r e s p e c t i v e o f i t s c o l l a b o r a t i v e
status).
C o n s i d e r a b l e stress is quite r i g h t l y put on c o l l a b o r a t i v e testing at
the p r e s e n t t i m e , but it should not be f o r g o t t e n that a r e l i a b l e m e t h o d is only
a p r e c o n d i t i o n to o b t a i n i n g the r i g h t a n s w e r .
T h e a b i l i t y of the a n a l y s t to
use the m e t h o d
is the e s s e n t i a l r e q u i r e m e n t
and the p e r s o n t a k i n g
the
r e s p o n s i b i l i t y for the result, w h e t h e r the analyst h i m s e l f or the s u p e r v i s o r ,
m u s t be c o n f i d e n t of this.

5.4

Analysis

Control

C o n t r o l is a v e r y i m p o r t a n t s u p e r v i s o r y f u n c t i o n .
It is n o t s u f f i c i e n t to
s i m p l y a s s i g n w o r k and w a i t for r e s u l t s .
T h e r e m u s t be s o m e type of a c t i v e
control in the form of expected c o m p l e t i o n datas, f o l l o w - u p i n q u i r i e s , or other
i n d i c a t i o n s of active interest.
This does not m e a n p e e r i n g over the a n a l y s t ' s
s h o u l d e r , but it does m e a n that the s u p e r v i s o r has c e r t a i n fixed e x p e c t a t i o n s
on w o r k c o m p l e t i o n and e n f o r c e s those e x p e c t a t i o n s .
T h e r e are several m e t h o d s of control but one of the m o r e e f f e c t i v e is also one
of the s i m p l e s t .
The s u p e r v i s o r p r e p a r e s a card for each a n a l y s t .
When a
s a m p l e is a s s i g n e d to the a n a l y s t , the s a m p l e n u m b e r is r e c o r d e d on the c a r d
along w i t h a p r o j e c t e d date of c o m p l e t i o n .
W h e n an a n a l y s i s report is r e c e i v e d
the entry is lined through.
W h e n a'card has been filled, it is discarded and a
n e w one p r e p a r e d .
The p r o j e c t e d c o m p l e t i o n d a t e r e p r e s e n t s t h e s u p e r v i s o r ' s
e s t i m a t e of an a c c e p t a b l e analysis t i m e , a s s u m i n g no p r o b l e m s .
The s u p e r v i s o r
s c a n s t h e c a r d s of a l l a n a l y s t s e v e r y d a y or so a n d if a d a t e h a s e x p i r e d b u t
no report r e c e i v e d , the supervisor inquires of the s a m p l e status.
The analyst
m a y be h a v i n g d i f f i c u l t y a n d h a d n o t m e n t i o n e d it.
A f t e r d i s c u s s i o n , the
s u p e r v i s o r d e c i d e s if a n a l y s i s s h o u l d c o n t i n u e and if so, a s s i g n s a n e w
projected c o m p l e t i o n date.
The s u p e r v i s o r m u s t also a s s i g n n e w dates w h e n
ongoing w o r k m u s t be interrupted by a s s i g n m e n t of h i g h e r p r i o r i t y analyses.

5.5

Analysis

Reporting

A n a l y s i s r e p o r t s are the end p r o d u c t of all of the w o r k of the l a b o r a t o r y and

t h e r e f o r e m u s t be b o t h c o m p l e t e a n d a c c u r a t e .
R e s u l t s of a n a l y s i s are o f t e n
i m p o r t a n t facts in legal p r o c e e d i n g s .
The w a y in w h i c h the technical results
p r o d u c e d by the l a b o r a t o r y reach the court is d i f f e r e n t u n d e r d i f f e r e n t legal
codes.
O n e e x t r e m e is the U.K. w h e r e a c e r t i f i c a t e of a n a l y s i s is a l e g a l l y
v a l i d d o c u m e n t w h i c h m a y b e a c c e p t e d as p r i m a f a c i e e v i d e n c e o f t h e f a c t s
stated therein.
Under R o m a n law, the l a b o r a t o r y report is a technical but not
l e g a l d o c u m e n t w h i c h the c o u r t is e m p o w e r e d to a c c e p t or r e j e c t .
In t h e
U.S.A., f e d e r a l a c t i o n is u s u a l l y i n i t i a t e d by a d o c u m e n t o r i g i n a t i n g in the
J u s t i c e D e p a r t m e n t on the basis of i n f o r m a t i o n from a t e c h n i c a l source.
Under
both R o m a n law and in the U.S.A., all prepared laboratory and technical records
r e l e v a n t to t h e s a m p l e m a y h a v e to be p r o d u c e d in c o u r t and t h e s a m p l e r and
analyst cross-examined.
T h i s o c c u r s l e s s f r e q u e n t l y u n d e r U.K. l a w w h e r e
c r o s s - e x a m i n a t i o n of the expert w i t n e s s is u s u a l l y all that is done, a l t h o u g h
if he did refer to original notes or c a l c u l a t i o n s they w o u l d b e c o m e a v a i l a b l e
to the c o u r t as in the U.S.A.
T h u s , it is m a i n l y u n d e r l e g a l c o d e s d e r i v e d

32

from Roman and c o m m o n law that the report or certificate of the analyst assumes
greater importance.
U n d e r b o t h R o m a n and U.S.A. l a w the e n t i r e l a b o r a t o r y
records relating to the sample must be capable of wi ths tand ing the scrutiny of
the c o u r t and d e f e n s e l a w y e r s .
The p r a c t i c a l e f f e c t of t h e s e d i f f e r e n c e s is
not great. Under any system it is necessary for the regulatory chemist to have
legally impeccable laboratory data records and to report against samples in a
w a y that is u n d e r s t a n d a b l e to the l a y m a n , b r i e f , s u c c i n c t , and free from
irrelevancy.
T h e f o r m a t of an a n a l y s i s r e p o r t is d i c t a t e d by the a d m i n i s t r a t i v e and legal
needs of the organization.
The report form should be preprinted with blocks or
l i n e s of i n f o r m a t i o n p l a c e d in d e s i g n a t e d a r e a s on the f o r m .
This p e r m i t s
faster and m o r e uniform write-up, as well as easier final review (the reviewer
knows where to look on the form for different information).
A complete report
form would have spaces for the following information:

Sample number
Product name
Product description and amount
Date received for analysis
Labelling (if any)
Analysis method used
Analysis results
Reserve product amount
Date completed
Total analysis time in hours (if needed

for time

modules).

Raw work data and standardization information can be placed on the reverse side
of the analysis report or can be kept separately in notebooks.
In any case it
s h o u l d be a c c e s s i b l e to the r e v i e w e r in the e v e n t of q u e s t i o n .
It is b e s t to
include all raw data so that the entire sequence of work can be reconstructed
later if needed.
Calculations m u s t be clear w i t h all equations stated.
There
is no w a y to d e t e r m i n e if a c a l c u l a t i o n is c o r r e c t w i t h o u t c h e c k i n g the
T h i s , of c o u r s e , m e a n s
c a l c u l a t i o n s y s t e m u s e d , as w e l l as the a r i t h m e t i c .
that all dilutions or other operations affecting the final calculation must be
clearly stated in the raw data.
R e s u l t s m u s t a l w a y s be r e p o r t e d o n l y to a n u m b e r of s i g n i f i c a n t
figures
j u s t i f i e d by the a c c u r a c y and p r e c i s i o n of the m e t h o d .
In g e n e r a l , it is
p r u d e n t to r e p o r t to as few s i g n i f i c a n t f i g u r e s as p o s s i b l e c o n s o n a n t w i t h
stating the facts the report has to convey.
For e x a m p l e , for most purposes it
m a y be a d e q u a t e to r e p o r t a s a m p l e as c o n t a i n i n g "not less ( m o r e ) than 70
percent of y".
The report m u s t be clear and confined to factual information,
and statements which cannot be substantiated must not be made.

5.6

Analysis

Review

T h e a n a l y s t should not d r a w c o n c l u s i o n s from the w o r k r e p o r t e d .

T h i s is
r i g h t f u l l y the job of the s u p e r v i s o r , w h o is n o r m a l l y the a n a l y s i s r e p o r t
reviewer.
The reviewer should ask himself a number of questions while reading
the report.
Any negative answers should be clarified by the analyst before the
report is accepted.
Some possible questions are:
Is the report generally complete?
(Any missing required information?)
Are the product descriptions adequate?
Was the correct method used?
Has sufficient work been done to draw a conclusion?
Have the proper standards and reagents been used?
Is there a blank?
Are the calculations easy to follow and accurate?
Are any strike-outs or discarded data explained?

33

5.7

Method

Validation

As discussed e l s e w h e r e , it is correct and proper to use collaboratively studied

methods w h e r e possible.
Such methods have already been shown to be capable of
use in different laboratories.
H o w e v e r , it is often necessary or advisable to
use a locally developed method or one which was selected from the literature,
but a b o u t w h i c h l i t t l e is k n o w n .
In such c a s e s the m e t h o d m u s t be v a l i d a t e d
for use in the local laboratory.
Method validation can take many forms, but the usual procedure is to examine a
k n o w n s a m p l e , or a k n o w n m a t e r i a l a d d e d to a s a m p l e , to d e t e r m i n e the m e t h o d
accuracy and precision.
For a contaminant residue, as example, a k n o w n amount
of reference grade contaminant would be added to a blank sample and replicate
assays done to determine the percentage recoveries.
In this type of recovery
v a l i d a t i o n it is i m p o r t a n t to be s u r e w h a t p a r t or p a r t s of the a n a l y s i s are
being evaluated.
A g a i n u s i n g the c o n t a m i n a n t e x a m p l e , a d d i t i o n of the
r e f e r e n c e c o n t a m i n a n t to the s a m p l e e x t r a c t s o l u t i o n d o e s n o t e v a l u a t e the
e x t r a c t i o n of the c o n t a m i n a n t , o n l y its p a s s a g e t h r o u g h c l e a n - u p and f i n a l
assay.
C o n t i n u i n g r e c o r d s of m e t h o d v a l i d a t i o n s should be kept for future reference
and to d e m o n s t r a t e the u s e f u l n e s s of the m e t h o d s .
N e g a t i v e d a t a is a l s o
desirable.
For e x a m p l e , if a method was tried and could not be satisfactorily
validated, that information should be recorded to avoid future attempts.
T h e r e c o v e r y d e t e r m i n a t i o n is o n l y one type of d i r e c t v a l i d a t i o n .
T h e r e are
also indirect validations where concurrent analyses are run on a given sample
using a new method as well as an established, accepted method. This provides a
direct experimental comparison.
T h i s is a good s y s t e m w h e n an a l t e r n a t e
procedure is needed for an official or referee method.

5.8

Confirming

Analysis

W h e n an o r i g i n a l a n a l y s i s s h o w s the s a m p l e to be in v i o l a t i o n of l a w or
regulations in some m a n n e r , the supervisor m u s t decide if a second analysis by
the o r i g i n a l a n a l y s t is n e e d e d .
T h i s s h o u l d o n l y be d o n e if t h e r e is s o m e
doubt that the original analysis w a s done correctly.
In the event that there are no apparent errors in the original analysis, then a
c o n f i r m i n g a n a l y s i s b y a s e c o n d a n a l y s t s h o u l d be d o n e as f o l l o w s :
A fresh
p o r t i o n of s a m p l e s h o u l d be p r e p a r e d ( u n l e s s it is n e c e s s a r y or d e s i r a b l e to
u s e the o r i g i n a l ) and a n a l y z e d u s i n g a s e c o n d m e t h o d (if p o s s i b l e ) and n e w
standard reference material.
If the a d v e r s e f i n d i n g s are r e p e a t e d by the
c o n f i r m i n g analyst, then it is extremely likely that a violation exists.
If,
h o w e v e r , t h e r e is no c o n f i r m a t i o n , then the s u p e r v i s o r m u s t m e e t w i t h b o t h
a n a l y s t s and d e c i d e w h a t is to be d o n e .
It m a y be t h a t the m e t h o d s are n o t
c o m p a t i b l e , if so a recheck using the original method might be in order.
It is
a l s o o f t e n v e r y u s e f u l to c r o s s c h e c k the s t a n d a r d s u s e d b y e a c h a n a l y s t to
ensure they compare.
Confirming analysis is basically an attempt to ensure that any violation of law
The e n f o r c e m e n t laboratory
or regulation has substance and is not a mistake.
c a n n o t a f f o r d to m a k e any m i s t a k e s , so it is n e c e s s a r y to p r o v e that all
adverse results are correct.

34

6.

6.1

The Safety

LABORATORY

SAFETY

Programme

The Head of the laboratory and supervisors must emphasize to all the laboratory
staff, their c o m m i t m e n t and d e t e r m i n a t i o n to e n s u r e s a f e l a b o r a t o r y w o r k i n g
conditions.
One staff m e m b e r s h o u l d be a p p o i n t e d the " S a f e t y O f f i c e r " and
given the responsibility to m o n i t o r safety procedures, practices and equipment
on a routine periodic basis.
In a large laboratory, the Safety Officer may be
assisted by a c o m m i t t e e of two or three analysts.
The d u t i e s of the S a f e t y O f f i c e r (and c o m m i t t e e w h e r e a p p r o p r i a t e ) s h o u l d be
d e t a i l e d in the l a b o r a t o r y S a f e t y P r o g r a m m e .
This p r o g r a m m e would indicate
safety requirements, hazards, equipment and emergency procedures.
Items which
can be included in a laboratory Safety P r o g r a m m e are discussed in the following
sections.
It should be r e m e m b e r e d that the Head h a s the final a u t h o r i t y as
w e l l as r e s p o n s i b i l i t y for l a b o r a t o r y s a f e t y , so t h a t the S a f e t y O f f i c e r m a y
only make recommendations.

6.2

Basic

Safety

Rules

E a c h l a b o r a t o r y s h o u l d d e v e l o p its o w n set of g e n e r a l s a f e t y r u l e s , and m a k e

sure that all m e m b e r s of staff are aware of them by supplying personal copies
of the r u l e s and by p o s t i n g c o p i e s on n o t i c e - b o a r d s .
T h e r u l e s s h o u l d be
changed and developed in the light of experience.
Some that should be included
are listed below:
1.
B e c o m e f a m i l i a r w i t h the l o c a t i o n and use of e m e r g e n c y
(e.g., f i r e e x t i n g u i s h e r ; e y e w a s h f o u n t a i n s ; s a f e t y s h o w e r s ;
cabinets).
Know where to go in case of fire.

equipment,
f i r s t aid

2.
Before beginning a sample analysis, review possible hazards connected
w i t h the a s s i g n m e n t and take the n e c e s s a r y p r e c a u t i o n s to e l i m i n a t e or
counteract the hazard.
3.
Use, when appropriate, the safety equipment provided for protection,
(e.g., s a f e t y g o g g l e s ; face s h i e l d s ; v a r i o u s t y p e s
of g l o v e s ) .
Wear a
laboratory coat routinely since its purpose is to serve as protective clothing.
4.
Bring all accidents and hazardous
supervisor or Head immediately.

conditions

to the attention of

the

5.
W h e n l i f t i n g h e a v y o b j e c t s , use the legs i n s t e a d of the b a c k .
Bend
the knees and hold the back straight so that the lifting effort is accomplished
w i t h the legs r a t h e r than the back.
L i f t s l o w l y to j u d g e the w e i g h t of the
object.
If too heavy, obtain assistance and/or use a lifting device.
6.
Be
jewelry (like
equipment.
entangled in

extremely careful of loose clothing, neckties, scarves, dangling

necklaces) and long h a i r w h e n u s i n g r e v o l v i n g or r e c i p r o c a t i n g
K e e p such i t e m s b o u n d or c o n f i n e d so that they w i l l not be
the equipment.

7.
T u r n off l a b o r a t o r y s e r v i c e s (gas, w a t e r , etc.) at the s e r v i c e c o c k
w h e n not in use. Changes in pressure m a y suddenly dislodge tubing connected to
an apparatus and lead to an accident or possible injury.
8.
Always use mechanical aids, such as safety bulbs
when pipetting hazardous material.
Never use the mouth.

35

or pipette

fillers,

9.
Use fume hoods for any analytical operations
of solvents, or w h e n noxious fumes will be generated.

their

10.
Keep the
contents.

work

area

neat

11.
Any chemicals, whether
m u s t be washed off immediately.

even

12.
Keep fire escape
temporarily.

routes

and

tidy,

toxic

and

13.
No one s h o u l d w o r k a l o n e
available in the event of accident.

with

or not,

doors

in the

all

which

clear

involving

large

containers

are

at all

laboratory,

labelled

spilled

times.

so that

amounts

on

the

Do not

with

hands

block,

assistance

is

14.
The last person to leave the laboratory at the end of the working day
m u s t c h e c k that all e q u i p m e n t t h a t s h o u l d be t u r n e d o f f h a s b e e n .
(This d o e s
not release each individual operator from his duty to turn off the equipment no
longer in use.)
The laboratory Head in consultation with staff m a y prefer to
operate a duty roster for opening the laboratory in the morning and closing at
the end of the w o r k i n g day.

6.3

Fire

Safety

A laboratory m u s t unfortunately be regarded as one of the more likely places in

w h i c h a fire w i l l o c c u r and it is t h e r e f o r e p r u d e n t to h a v e the l o c a l c h i e f
fire officer visit the building, be familiarized with the problems and advise
the laboratory staff about local fire regulations and further safety m e a s u r e s
that s h o u l d be t a k e n .
F i r e and s m o k e d e t e c t o r s m a y be i n s t a l l e d in the
b u i l d i n g and c o n n e c t e d so t h a t in the e v e n t of f i r e , an a l a r m is g i v e n at a
fire s t a t i o n .
C a r e m u s t be taken that s m o k e d e t e c t o r s are not set off
a c c i d e n t a l l y by b e g i n n i n g the a s h i n g of s a m p l e s in the o p e n l a b o r a t o r y or
excessive formation of smoke in other ways.
S t a f f m u s t h a v e c l e a r i n s t r u c t i o n s of the a c t i o n to be t a k e n in c a s e of fire.
Such i n s t r u c t i o n s s h o u l d be p o s t e d p r o m i n e n t l y in v a r i o u s p a r t s of the
building.
O c c a s i o n a l l y t h e r e s h o u l d be a fire d r i l l to c h e c k that e v e r y o n e
k n o w s w h a t to do in the case of a s e r i o u s fire and to m a k e sure that the
building can be evaculated in an orderly and rapid manner.
Once evacuated, a
r o l l c a l l is t a k e n to c h e c k that no one r e m a i n s in the b u i l d i n g .
Such a roll
call m u s t be completed in a very few minutes and therefore should be called in
groups if the total staff exceeds about 20-30.
A fire evacuation must include
switching off the electricity supply to the affected area, as short-circuits
may result in further fire hazard.
Isolation switches are important to enable
restricted areas of the building to be cut off from the supply.
H o w e v e r , for a
p r a c t i c e d r i l l , the s w i t c h i n g off can be s i m u l a t e d .
W h e n n e w s t a f f are
introduced, they m u s t have the drill explained to them and be shown where fire
e x t i n g u i s h e r s , b l a n k e t s , h o s e s and b u c k e t s are k e p t , and h o w the s p r i n k l e r
system w o r k s if there is one.
Breathing apparatus should be available at two or three points in the building,
and an adequate n u m b e r of people instructed in its use. In dealing with a fire
in a laboratory toxic fumes are always possible.
F i r e e x t i n g u i s h e r s in the l a b o r a t o r y s h o u l d be of the c a r b o n d i o x i d e type.
Pressurized dry chemical extinguishers are suitable for general use, but should
n o t be u s e d a r o u n d c o m p u t e r s or o t h e r s e n s i t i v e e l e c t r o n i c e q u i p m e n t .
The
r e a s o n is that it is n e a r l y i m p o s s i b l e to c l e a n the dry c h e m i c a l out of the
instrument., and the instrument could be irreparably damaged.
Carbon dioxide
units work best.
Everyone in the laboratory should have used an extinguisher
at l e a s t o n c e , so t h a t t h e y k n o w h o w to r e m o v e the s a f e t y p i n as r a p i d l y as
possible and are not disconcerted by the sudden noise when it is activated.
If

36

any s t r u c t u r a l part of the b u i l d i n g a p p e a r s a f f e c t e d by a s m a l l f i r e , it is

a d v i s a b l e to i n f o r m the fire s t a t i o n , s i n c e a f i r e that m a y a p p e a r to b e
extinguished in fact may be smouldering behind a panel or other structure and
break out again several hours later, perhaps after the laboratory is closed for
the night.
A d i s c u s s i o n of b u l k s o l v e n t s t o r a g e and c o n s t r u c t i o n of a s t o r a g e r o o m is
contained in Section 3.3 of this manual.
The quantitites of f l a m m a b l e liquids
in the laboratory should be kept at a m i n i m u m .
Bottles should be stored away
f r o m h e a t , s u n l i g h t and any s o u r c e of n a k e d f l a m e .
V a p o u r s such as t h o s e of
diethyl ether can flow along surfaces such as floors and benches and thus, by
c o n t a c t w i t h a n a k e d f l a m e or a h o t s u r f a c e (such as
a m u f f l e f u r n a c e or
h o t p l a t e ) b e c o m e i g n i t e d . S o l v e n t s m u s t be s t o r e d in an e x p l o s i o n - p r o o f
refrigerator, separately from acids and other reagents.
Some chemicals ignite
spontaneously on mixing, for example concentrated nitric acid with alcohols.
E l e c t r i c a l e q u i p m e n t m a y be the s o u r c e of a fire d u e to f a u l t y
wiring,
inadequate earthing, failure causing sparks or local overheating or switchgear
sparks.
A l l e l e c t r i c a l e q u i p m e n t s h o u l d c a r r y a f u s e w h i c h b l o w s at an
amperage
s l i g h t l y in e x c e s s of that r e q u i r e d by the e q u i p m e n t .
It is
c o m m o n p l a c e to find that equipment drawing only one or two amps have a 13 or 15
Flammable
amp fuse which is unlikely to be of any use if anything goes wrong.
vapour near electrical equipment represents a fire hazard unless the instrument
h a s b e e n r e n d e r e d " e x p l o s i o n p r o o f " by s e a l i n g t h o s e s e c t i o n s w h e r e a s p a r k
could occur.
Motors m u s t be serviced regularly.
Lack of attention m a y result
in o v e r h e a t i n g and s u b s e q u e n t fire.
C e n t r i f u g i n g of v o l a t i l e
flammable
s o l v e n t s is h a z a r d o u s
if the c e n t r i f u g e m o t o r
is n o t e x p 1 o s i o n - p r o o f ,
especially if the tube breaks.
S t a t i c e l e c t r i c i t y and s t a t i c s p a r k s can be a real p r o b l e m in a h o t and dry
climate.
They can result from wearing clothes m a d e of synthetic m a t e r i a l s , or
by simply walking across a carpet.

6.4

Chemical

Hazards

All c h e m i c a l s s h o u l d be c o n s i d e r e d as p o t e n t i a l l y h a z a r d o u s and s h o u l d be
treated with caution.
As far as possible, dangerous c h e m i c a l s should be stored
away from the laboratory and away from others with which they violently react.
Y e l l o w p h o s p h o r u s and p i c r i c acid m u s t be k e p t u n d e r w a t e r , s o d i u m and
potassium metal under oil.
Explosive peroxides can be formed in diethyl ether.
T h e y s h o u l d a l w a y s be r e m o v e d if f o u n d to be p r e s e n t , as an e x p l o s i v e
concentration
of p e r o x i d e m a y b e f o r m e d
if t h e e t h e r is d i s t i l l e d .
Distillation should be stopped while there is plenty of solvent remaining in
the d i s t i l l a t i o n flask and care s h o u l d be t a k e n not to o v e r h e a t the flask.
D u s t m a y c a u s e the e x p l o s i v e d e c o m p o s i t i o n of h y d r o g e n p e r o x i d e of o v e r 30
percent concentration.
Peroxides in general can be explosive, and must not be
allowed to come into contact with reducing agents or f l a m m a b l e solvents.
They
should be kept in dark bottles in a refrigerator.
Hydrogen fluoride solution
is e x t r e m e l y dangerous as contact w i t h the skin may result in lesions that fail
to heal.
Disposable plastic gloves must always be worn when this solution is
being handled.
Calcium gluconate gel or solution or another antidote should be
available in the first-aid cabinet.
Toxic levels of nitrogen dioxide can be produced during the use of the nitrous
oxide-acetylene flame in atomic absorption spectrophotometry and consequently
ventilation must be good.
The recommended threshold limit value (TLV) for 40
m i n u t e s exposure is 5 ppm.
Tubes for testing contaminated air
are available
c o m m e r c i a l l y from laboratory supply firms.
It is important that bottles containing sodium and potassium (for example w h e n
these have been used for drying ether) are
not left near a washing-up area in
case an inexperienced or unobservant person attempts to wash the bottle in the

37

u s u a l way.
In fact, all c o n t a i n e r s ( b e a k e r s , e t c ) c o n t a i n i n g h a z a r d o u s
material must first be rinsed or otherwise treated by the analyst to remove the
h a z a r d , b e f o r e giving to g l a s s w a r e w a s h i n g .
The need for this is o b v i o u s
as the analyst is the only one who knows of the hazard and how to eliminate it.
All reagent bottles, flasks or other containers must be properly labelled, even
if the c o n t e n t s are c o n s i d e r e d h a r m l e s s .
A d h e s i v e w a r n i n g s t i c k e r s can be
p u r c h a s e d from c h e m i c a l s u p p l y f i r m s .
T h e s e can be used in a d d i t i o n to the
container label to highlight hazards.
When emptying acids and chromic acid cleaning solutions into the drains, first
fill the sink with water, pour the acid or cleaning solution into the sink, and
then let the w a t e r run out.
A l l o w the tap to r e m a i n on full for a few
additional minutes.
Dilution should always be sufficient to reduce the acid
concentration to less than one normal.
Store acid containers in inert trays if
the acid c o n c e n t r a t i o n is g r e a t e r than 2N. P o l y e t h y l e n e t r a y s are s u i t a b l e .
Handle concentrated ammonium hydroxide and solutions of potassium and sodium
hydroxide which are ION or above as if they were concentrated acids and observe
the s a m e p r e c a u t i o n s as for acids. Do not store A L K A L I in the s a m e tray w i t h
ACID.
Do not store concentrated alkalies in glass-stoppered bottles.

6.5

Biological

Hazards

This manual is concerned primarily with a chemical analysis laboratory rather

than a m i c r o b i o l o g i c a l one.
H o w e v e r , t h e r e are b i o l o g i c a l h a z a r d s in the
typical chemical analysis laboratory.
The m o s t s e r i o u s of these are the
c a r c i n o g e n i c r e a g e n t s or r e f e r e n c e m a t e r i a l s c o m m o n to f o o d c o n t r o l
laboratories.
Carcinogens must always be handled with extreme care, using all
available protective gear.
The f o l l o w i n g listing is of s u b s t a n c e s used in a food c o n t r o l l a b o r a t o r y , or
found as food contaminants, which are suspected or k n o w n to be carcinogens:
Category

Reference

Aflatoxins

Potent

carcinogen

6,7

4-(or p-) Aminobiphenyl

Biphenylamine

Potent

carcinogen

1,2,6

Asbestos

Carc inogen

Auramine, or 4,4'dimethylaminobenzophenonimide

Suspected

carcinogen

2,6

Benzene, benzol(e)

Suspected

carcinogen

4,5,6

Benzidine,
diamide,

Potent

carcinogen

2,6

3,4-(or 1,2-) Benzpyrene

Potent

carcinogen

Cadmium and Compounds

(mainly inorganic)

Suspected

Carbon

Carc inogen

4,4'-biphenyldiaminobiphenyl

tetrachloride

Suspected

Chloroform (trichlorome thane)

Chromium

salts (3 and

6+)

Carc inogen

38

3,6

carcinogen

6,9

6
carcinogen

3,6,7

Ne

Catetory

Reference

Coal tar, Creosote oils

(polycyclic mixtures)

Care inogen

3,4,6

DDT

Suspected

(p,p*

or o,p')

o-Dianisidine

Care inogen

Diazomethane

Suspected

Dichloroethane

Carcinogen

4-Diethylaminoazobenzene
(Butter Y e l l o w )

Suspected

N,N-Dimethylnitrosamine

Potent

Dimethyl

Carcinogen

sulphide

1,4-Dioxane
ether

(diethylene

carcinogen

2,6
carcinogen

4,5,6
-

carcinogen

carcinogen

6,8
-

6,9

Carcinogen

Teratogen

Formamide

5,6

Suspected

carcinogen

Magenta basic or Basic

fuchsin (basic red 9,
basic violet, 14 rosaniline)

Suspected

carcinogen

2,6

Mineral

Carc inogen

3,6

1-Naphthylamine
(1-amino-naphthalene)

Care inogen

2,6

2-Naphthylamine
(2-amino-naphthalene)

Potent

Nickel

Carcinogen

4,6

Nitrobenzene

Carcinogen

Nitrosamines

Potent

Patulin

Suspected

carcinogen

Rhodamine B

Suspected

carcinogen

Suspected

carcinogen

Magenta

acid or Acid

oils

and

fuchsin

(heavy)

salts

Sodium diethyl
Soot, carbon

dithiocarbamate

black

carcinogen

carcinogen

Carcinogen

1,2,6

3,6

Tannins

Suspected

carcinogen

5,6

Thioacetamide

Suspected

carcinogen

4,5,6

Thiourea

Suspected

carcinogen

4,5,6

Trichloroethylene

Suspected

carcinogen

Vinylchloride

Carcinogen

Zearalenone

monomer

Suspected

39

10
carcinogen

11,12

The references noted

in the listing

are:

1.

Bo y 1 and, E. (1 963). "The B i o c h e m i s t r y of B l a d d e r Cancer."

Springfield, Illinois.

2.

C h e s t e r B e a t t y R e s e a r c h I n s t i t u t e (1966).
" P r e c a u t i o n s for L a b o r a t o r y
Workers who handle Carcinogenic Aromatic Amines."
The Institute, London;
reprinted with additional notes 1971, i. 7 pp.

3.

Clayson, D.B.

4.

D e w h u r s t , F. (1972).
10, 57-85, passim.

5.

Hueper,
Cancer."

6.

From International Agency for Research on Cancer, IARC Monographs on the

" E v a l u a t i o n of C a r c i n o g e n i c Risk of C h e m i c a l s to Man."
IARC, L y o n / W H O ,
Geneva/HMSO, London.

7.

R o e , F.J.C. and L a n c a s t e r , M.C. (1964), " N a t u r a l M e t a l l i c

Br. med. Bull., 2J)> 127-133.
Substances as Carcinogens."

8.

S e a r l e , C.E. (1972).

9.

National Institute of Occupational S a f e t y and H e a l t h (1975) - " S u s p e c t e d

C a r c i n o g e n s List." U n i t e d S t a t e s D e p a r t m e n t of H e a l t h E d u c a t i o n and
Welfare Publication No. (NIOSH) 75-188.

10.

Maltoni,

11.

Ueno, Y. and Kubota, K., (1976), Cancer Research, 36_ (2) 445-451.

12.

Schoental, R. , (1974), Br. J. Cancer, 30, ISS _2, 181.

6.6

Physical

(1962).

"Chemical Carcinogenesis."
"Carcinogens

C.C. T h o m a s ,

Churchill.

in the L a b o r a t o r y . "

W.C. and C o n w a y , W.D. (1964).

"Chemical
C.C. Thomas, Springfield, Illinois.

Lab. Equip. Dig.,

Carcinogenesis

and

and

other

" C h e m i c a l C a r c i n o g e n s . " C h e m . Ind., (3) 1 1 1 - 1 1 6 .

C. and Lefemine, G., (1974), Environmental

Research, _7, p.387.

Hazards

There are many physical hazards in a laboratory.

Most are avoidable by use of
c o m m o n sense.
It is advisable, however, to prepare some instructions for new
e m p l o y e e s and p e r i o d i c a l l y r e m i n d o t h e r s . The f o l l o w i n g are s o m e p r o p o s e d
instructions, grouped by operation.

Glassware Handling

1.
Do not use b r o k e n or chipped g l a s s w a r e or r e t u r n it to s t o r a g e .
If
it is b e y o n d r e p a i r , d i s p o s e of it. W h e n in d o u b t r e g a r d i n g p r o p e r d i s p o s a l ,
consult the supervisor.
Always use gloves in handling broken glass.
2.
R e m o v e s h a r p or jagged e d g e s from g l a s s w a r e b e f o r e u s i n g it.
polish the edges on all glass tubing.

Fire

3.
Broken glass in sinks present a definite hazard since glass may not
be v i s i b l e in the p r e s e n c e of w a t e r .
W h e n b r o k e n in the sink, r e m o v e it
promptly.
F u r t h e r m o r e , c o n s i d e r the p o s s i b i l i t y of the p r e s e n c e of b r o k e n
glass when reaching into the sink for any purpose.

40

4.
Inserting tubing into stoppers or rubber tubing can result in serious
cuts, which can be prevented if the following precautions are observed:
a.
b.
c.
d.
e.

Wet the tubing and/or stopper or rubber tubing.

Wear gloves or wrap a towel around the palms of the hands.
Do not use e x c e s s i v e force - cut the h o l e b i g g e r or b o r e a n e w
hole .
Use the fingers and not the hands when making the insertion.
Insert glass or metal tubing entirely through stoppers to assure
that the end may not be closed over by heat or solvent action on
the stopper.

5.
To remove glass tubing or thermometers from rubber, preferably cut
a w a y the r u b b e r . T h i s is p a r t i c u l a r l y true if the t u b i n g or s t o p p e r has b e e n
in place over an extended period of time or has been subjected to heat.
6.
In handling beakers, support them by grasping around the sides, never
over the top. If one hand will not reach more than half way around the beaker,
use both hands. Support large beakers (one litre or more) from the bottom when
in use.
7.
W h e n h e a t i n g l i q u i d s in g l a s s by m e a n s of a gas f l a m e , p r o t e c t the
glass from direct contact with the flame by use of a wire gauze or a centered
wire gauze.
8.
W h e n p l a c i n g l i q u i d s in b o t t l e s w h i c h h a v e a p o s i t i v e c l o s u r e ,
reserve more than 5 percent of the volume as air space to allow for expansion
due to temperature changes.
9.
Do not force s t o p c o c k s or ground g l a s s s t o p p e r s .
Use a s t o p c o c k
puller.
If the n a t u r e of the c o n t e n t s of the v e s s e l p e r m i t s , cool the shell
until the plug is cold, then heat the shell of the joint momentarily.
Withdraw
the plug quickly before it too has been expanded by the heat.

Vacuus Operations

1.
Protect glassware under vacuum from physical
cracks and result in collapse with explosive violence.

shock which might

2.
Do not subject flat-bottom flasks
heavy walls specifically for such service.

unless

to vacuum

cause

constructed

with

3.
Guard s t a n d a r d - w a l 1 ( s p h e r i c a l ) flasks larger than one l i t r e , w h e n
used in v a c u u m s e r v i c e , by a shield that is a d e q u a t e to stop all flying g l a s s
if collapse should occur.
4.
C h o o s e cork or r u b b e r s t o p p e r s used in v a c u u m s e r v i c e c a r e f u l l y .
They must be of such size that they will not be drawn through the opening which
they are intended to close.
5.

Relieve vacuum before attempting

to disassemble

equipment.

6.
Do not s t o p p e r h o t flasks c o n t a i n i n g u n c o n d e n s e d v a p o u r s or
To do so will subject them to vacuum on cooling.

41

steam.

Equipment

Handling

1.
W h e n using a m a n u a l cork b o r e r , do not hold the s t o p p e r in the p a l m
of the hand.
Place the stopper large end down on a soft, flat surface and hold
in p l a c e w i t h the t h u m b and f o r e f i n g e r .
K e e p the b o r e r sharp and l u b r i c a t e
with water or glycerine to prevent binding. Do not force the borer through the
stopper but twist to cut the material.
Use stout gloves for added protection
in case of slippage.
2.
Do
not lift the cover of a c e n t r i f u g e until r o t a t i o n has
Keep the cover closed when the centrifuge is not in use.

stopped.

3.
C y l i n d e r s c o n t a i n i n g i n d u s t r i a l gases must be properly anchored by
chains or heavy straps or held in stands.
Reactive gases should be stored away
from each other (e.g. do not store a c e t y l e n e near oxygen).
Gas s u p p l i e s for
gas liquid chromatography and atomic absorption spectroscopy are best kept on
the other side of the wall from the instrument and connected via a small duct
in the w a l l .
C y l i n d e r s t o r a g e p o i n t s s h o u l d be p r o t e c t e d from the w e a t h e r ,
p a r t i c u l a r l y in dusty areas w h e r e grit can get into the c y l i n d e r v a l v e , but
they s h o u l d be s u f f i c i e n t l y w e l l - v e n t i l a t e d to p r e v e n t l e a k i n g gas f r o m
reaching dangerous levels.
4.
Flexible tubing attached to gas supplies must be wired on or held by
clips and must be able to withstand any likely pressure.
The sudden bursting
or b l o w i n g off of a piece of tubing is s t a r t l i n g and m a y c a u s e an a c c i d e n t if
someone nearby is carrying out a hazardous operation.
5.
A rapid decrease of cooling water due to a fall in mains pressure or
a cut in the supply can damage equipment such as a still and also be hazardous.
A c o n s t a n t head d e v i c e in a t r a n s p a r e n t c o n t a i n e r w i l l give s o m e w a r n i n g of
this. However, if water pressure fluctuations are a frequent problem, a header
tank in the roof of the building may be advisable. Electrical equipment can be
fitted with automatic cutouts that turn off the electricity supply in case of
water failure.

6.7

Safety and Emergency

Equipment

" S a f e t y " e q u i p m e n t is that d e s i g n e d to p r o t e c t a n d / o r p r e v e n t i n j u r y and is

used b e f o r e an a c c i d e n t h a p p e n s .
" E m e r g e n c y " e q u i p m e n t is used a f t e r an
accident (or other emergency) to minimize the injury or damage. Therefore, eye
goggles are "safety" and eye wash fountains are "emergency" equipment.
U s i n g these d e f i n i t i o n s , the f o l l o w i n g are lists of safety and
equipment which every laboratory should include in their inventory:

emergency

Safety Equipment

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

Rubber aprons.
Eye goggles.
Face shields..
Disposable plastic or rubber gloves.
Bench shields (portable, clear plastic).
Pipetting bulbs.
Heavy rubber carriers for acid and alkali bottles.
Metal safety cans for flammable solvents.
M e t a l solvent s t o r a g e c a b i n e t s (about 45 g a l l o n
storage of solvents used daily in the laboratory).
Respirator filter masks (for dust or fumes).
42

capacity).

(For

Emergency

1.
2.
3.
4.
5.
6.

Equipment

Hand-held fire extinguishers (carbon dioxide preferably, see Section

6.3) .
Fire blankets (wall mounted).
Eye wash stations (built-in fountains or portable kits).
S p i l l a g e a b s o r b e n t kits for both a c i d s and s o l v e n t s ( a v a i l a b l e
commercially or can be assembled locally).
Emergency shower (in the laboratory, drenching full-on or -off valve
operated by a pull chain or loop).
Respirator mask with oxygen supply.

A major item of emergency equipment not included in the above list is the
aid cabinet.
This is discussed in detail in Section 6.8.

first

All such e q u i p m e n t is u s e l e s s if e i t h e r not a v a i l a b l e or not in s e r v i c e a b l e

condition.
The Safety Officer (see Section 6.1) should periodically check both
the s t o r a g e l o c a t i o n s (if n o t in u s e ) and the c o n d i t i o n of all safety and
emergency equipment.
The laboratory staff must also be trained in the use of
the equipment and use must be enforced when necessary.

6.8

First

Aid

First aid by definition is that initial assistance given to lessen the effect
of injury.
If the injury is sufficiently minor, then first aid will probably
s u f f i c e for t r e a t m e n t .
H o w e v e r , for s e r i o u s and e v e n m o d e r a t e l y s e r i o u s
i n j u r i e s , m e d i c a l h e l p m u s t be g i v e n as soon as p o s s i b l e .
Any first aid
m e a s u r e s w o u l d be only to give t e m p o r a r y h e l p u n t i l m e d i c a l t r e a t m e n t is
available.
S o m e o n e on the l a b o r a t o r y s t a f f s h o u l d be t r a i n e d in f i r s t - a i d ,
particularly in giving artificial respiration techniques.
Some chemicals such
as c y a n i d e are q u i c k - a c t i n g and there is r a r e l y t i m e to w a i t for a d o c t o r to
arrive, or transfer the patient to the hospital.
T h o u g h t s h o u l d be g i v e n to the l o c a l h a z a r d s that m i g h t be e x p e c t e d and the
c o n t e n t s of a first aid c a b i n e t d e s i g n e d to m a t c h .
The c a b i n e t should be
l o c a t e d in the l a b o r a t o r y p r o p e r and be a c c e s s i b l e .
A first-aid cabinet
suitable for a laboratory of 10-50 employees could contain the following:
1.

A copy of a leaflet giving advice on first aid

2.
A s u f f i c i e n t n u m b e r (not l e s s
unmedicated dressings for injured fingers.

than

12)

treatment.
of

small

sterilized

3.
A s u f f i c i e n t n u m b e r (not less than 6 ) of m e d i u m - s i z e d
unmedicated dressings for injured hands or feet.

sterilized

4.
A sufficient number (not less than 6) of large sterilized
dressings for other injured parts.

unmedicated

5.
A sufficient number (not less than 24) of adhesive wound
an approved type and of assorted sizes.
6.
A s u f f i c i e n t n u m b e r (not less than 4 ) of
unbleached calico, the longest size of which measures
and each of the other sides not less than 36 inches.
7.

small

A sufficient supply of adhesive

8.
A sufficient
packets.

supply

t r i a n g u l a r b a n d a g e s of
not less than 51 inches

plaster.

of a b s o r b e n t

43

dressings of

sterilized

cotton

in

individual

9.
approved

A sufficient supply of approved

type and size.

10. A sufficient n u m b e r
separate sealed packets.

(not

less

eye o i n t m e n t

than 4 ) of

11.

A rubber bandage or pressure bandage.

12.

Safety pins.

13.

A tube of antiseptic

in a container

sterilized

of an

eye-pads

in

cream.

It is suggested that, in addition to the above provisions (which cater

primarily for cuts and heat burns) each chemical laboratory first aid cabinet
should contain:
1.
2.
3.
4.

A tablespoon.
Bottle of Epsom salts (magnesium sulphate).
Bottle of milk of magnesia (dose - two tablespoonfuls).
Bottle of 1 percent acetic acid.

Hydrogen cyanide, soluble cyanides and nitriles which hydrolyse readily to HCN
when inhaled or ingested may call for treatment with capsules (0.3 ml) of amyl
nitrite w h i c h are easily crushed in a cloth from w h i c h the vapour can be
inhaled.
The following antidote for cyanide ingestion casualties consists of
two solutions which should be made up and left ready for immediate use:

S o l u t i o n A:
158 g ferrous sulphate crystals and 3 g citric acid crystals
in a litre of cold distilled w a t e r (the solution m u s t be inspected regularly
and be replaced if any deterioration has occurred).
S o l u t i o n B:
distilled water.

60 g anhydrous

sodium

carbonate

dissolved

in a litre

of

50 ml of solution A is placed in a 170 ml w i d e - n e c k e d bottle closed by a

p o l y t h e n e - c o v e r e d cork and labelled clearly "CYANIDE A N T I D O T E A".
50 ml of
solution B is s i m i l a r l y bottled and labelled "CYANIDE A N T I D O T E B".
Both
b o t t l e s should bear the legend "Mix the w h o l e contents of bottles "A" and "B"
and swallow the mixture".
The merit of the basic ferrous hydroxide suspension
is that when swallowed it is likely to induce vomiting while at the same time
forming insoluble non-toxic iron c o m p l e x e s with the cyanide.
It m u s t be
s t r e s s e d , h o w e v e r , that the i m m e d i a t e s u m m o n i n g of a doctor,
w h o can
a d m i n i s t e r an approved injection, is of the u t m o s t i m p o r t a n c e in cases of
cyanide poisoning.
Kits for the intravenous treatment of cyanide poisoning by
doctors are available.
A kit should be at hand in any o r g a n i z a t i o n w h e r e
cyanides are handled regularly.
I o d i n e , if i n g e s t e d , s h o u l d be t r e a t e d w i t h sodium thio s ul pha te.
An
appropriate weight of the crystals in a bottle to make up a 1 percent solution
when water is added to a set mark, will provide the right solution for taking
internally and also for swabbing on skin contaminated with iodine.
In some o r g a n i z a t i o n s , the a d m i n i s t r a t i o n of oxygen through a f a c e - m a s k has
become part of first aid procedures for certain types of casualty.
When it is
certain that a casualty has stopped breathing, artificial respiration should be
applied immediately.
The "mouth-to-nose" and "mouth-to-mouth" procedures are
now the methods of first choice and are described in "New Essential First-Aid"
by A. Ward Gardner and C. J. Roylande (Pan Books), among others.
The mouth-tomouth procedure must be used when the casualty has a nasal obstruction.
Where
injuries to the face and m o u t h m a k e the use of these m e t h o d s i m p o s s i b l e , or
w h e r e cyanide poisoning is k n o w n or suspected, the Sylvester method can be

44

used.
This is described in "First Aid" (2nd E d i t i o n 1965) published by St.
John A m b u l a n c e A s s o c i a t i o n , The St. A n d r e w A m b u l a n c e A s s o c i a t i o n and the
British Red Cross Society, as well as in standard medical texts.
Bromine, formic acid, hydrofluoric acid and other acid burns on the skin can be
treated with magnesia/glycerol paste prepared by triturating 200 g magnesium
oxide with 240 ml glycerol, the paste being applied liberally over the affected
areas. Dilute ammonia (1 volume ammonia added to 15 volumes of water) has also
been found e f f e c t i v e in reducing the degree of b u r n i n g w i t h b r o m i n e , formic
acid and hydrofluoric acid.
The laboratory should have at least one book (preferably more) on first aid and
laboratory safety.
There are m a n y such available.
Some of the better ones
are :
1.

"Handbook of L a b o r a t o r y Safety", Steere, N.V., C h e m i c a l Rubber

Cleveland, Ohio.

2.

"Hazards in the Chemical Laboratory",

C h e m i s t r y , U.K. 1 977.

3.

"Fire P r o t e c t i o n for L a b o r a t o r i e s Using C h e m i c a l s " ,

National
Protection Association, Batterymarch Park, Quincy, MA 02269.

4.

American Chemical Society, "Safety in the Chemical Laboratory" Vol 1 ACS

1967 (reprinted from "Journal of C h e m i c a l Education", January 1964 January 1967), and Vol 2, ACS 1971.

5.

M a n u f a c t u r i n g C h e m i s t s ' A s s o c i a t i o n Guide for safety

Laboratory, 2nd Ed, Van Nostrand Reinhold, 1972.

6.

Medical
1973 .

Muir.

G.D. (Ed.) Royal

Company,

Institute

of

Fire

in the

Chemical

in Laboratories",

MRC, U.K.

7.

P r e c a u t i o n s for L a b o r a t o r y W o r k e r s who Handle Carcinogenic

Amines, The Chester Beatty Research Institute, London, 1966.

Aromatic

8.

Reference Book of P r o t e c t i v e
Association, London, 1981-82.

Research

Council, "Safety

Precautions

E q u i p m e n t , Industrial Safety Manufacturers

45

7. LABORATORY QUALITY ASSURANCE

7.1

(QA)

Introduction

A laboratory engaged in food control analysis must have some means of assuring
that their analytical results are of the highest quality.
Errors in analysis
can o f t e n m e a n s e r i o u s e c o n o m i c l o s s e s for the food i n d u s t r y or i m p o r t e r , as
well as possible illness or injury to the consuming public.
This assurance of
quality is not limited to confirming that a food found to be unacceptable, is
in fact b a d .
It is e q u a l l y i m p o r t a n t to a s s u r e that f o o d s f o u n d to b e
a c c e p t a b l e , are in fact good.
To do this r e q u i r e s an u n d e r s t a n d i n g and
c o m m i t m e n t by the laboratory m a n a g e m e n t as well as the operating staff, that
high quality in analysis is the foremost objective.
O f t e n , the t e r m s " Q u a l i t y C o n t r o l " and " Q u a l i t y A s s u r a n c e " are used
interchangeably when discussing analytical quality.
H o w e v e r , G a r f i e l d (1)
m a k e s a d i s t i n c t i o n b e t w e e n the t w o .
He d e f i n e s Q u a l i t y c o n t r o l a s , "...a
p l a n n e d s y s t e m of a c t i v i t i e s w h o s e p u r p o s e is to p r o v i d e a q u a l i t y p r o d u c t . "
Conversely, he defines Quality Assurance as, "...a planned system of activities
w h o s e p u r p o s e is to p r o v i d e a s s u r a n c e that the q u a l i t y c o n t r o l p r o g r a m is
actually effective."
Therefore, Quality Control encompasses all of the myriad
r e v i e w , checking and operational procedures routinely used by the laboratory to
m a i n t a i n high analytical quality.
( M a n y of t h e s e are d i s c u s s e d in the
preceeding Chapters 4 and 5.) The following discussions of Quality Assurance
u s e s G a r f i e l d ' s d e f i n i t i o n and c o v e r s t h o s e p r o c e d u r e s u s e d to c o n f i r m t h a t
high quality is being maintained.

7.2

Establishing

a QA

Programme

To be successful, quality assurance must be a formal planned activity which is

designed to fit the needs of the laboratory.
A formal QA p r o g r a m m e is prepared
by establishing:
1.

The acceptable

quality

for a given

2.

A periodic review to confirm this

3.

A system of documentation

4.

Appropriate

laboratory

function.

quality.

to record

the results of the

follow-up to correct any deficiencies

reviews.

found.

The first step is to decide the functions that should have formal review.
Some
s u g g e s t i o n s a r e s t a n d a r d s s t o r a g e and h a n d l i n g , p r e p a r a t i o n of a n a l y s i s
r e p o r t s , i n s t r u m e n t m a i n t e n a n c e and l a b o r a t o r y s a f e t y .
T h e l a b o r a t o r y Head
should carefully examine the entire laboratory operation, by audit review if
n e c e s s a r y , and s e l e c t those f u n c t i o n s w h i c h need i m p r o v e m e n t or w h i c h w o u l d
benefit from periodic monitoring.
A QA p r o g r a m m e should be d y n a m i c and subject
to change when needed. Therefore a detailed QA review could be conducted until
it is felt that the function under review will continue to operate smoothly, at
w h i c h t i m e the r e v i e w could be l e s s e n e d and a n o t h e r f u n c t i o n g i v e n i n - d e p t h
coverage .
T h e r e v i e w i t s e l f is n o r m a l l y l i m i t e d to the c r i t i c a l p a r t s of the f u n c t i o n
under review.
For e x a m p l e , a r e v i e w of s t a n d a r d s t o r a g e and h a n d l i n g c o u l d
include: accounting for all standards by inventory and checking proper storage;
c h e c k i n g t h a t no s t a n d a r d h a s e x c e e d e d its e x p i r a t i o n or d i s p o s a l d a t e ; and
visual,
p h y s i c a l a n d / o r c h e m i c a l c h e c k s to i n d i c a t e
s t a n d a r d s are not
contaminated or decomposed.

46

The "acceptable quality" standard is set by the laboratory.

If some error rate
is acceptable in daily practice, then that rate b e c o m e s the quality standard.
The laboratory will always be striving for perfection, and the QA p r o g r a m m e is
one means to identify those areas which need improvement towards the ideal.
Quality Assurance programmes
are u s u a l l y a l s o r e q u i r e d
for
laboratory
certification.
An e x a m p l e is G u i d e 25 of the I n t e r n a t i o n a l O r g a n i z a t i o n for
S t a n d a r d i z a t i o n ( I S O ) (2).
U n d e r P a r t 4, " Q u a l i t y S y s t e m " it s t a t e s the
following :

1.
The laboratory shall operate an internal quality assurance p r o g r a m m e
a p p r o p r i a t e to the t y p e , r a n g e and v o l u m e of w o r k p e r f o r m e d .
The quality
assurance p r o g r a m m e shall be documented in a quality manual which is available
for u s e b y the l a b o r a t o r y s t a f f .
T h e q u a l i t y m a n u a l s h a l l be m a i n t a i n e d
relevant and current by a responsible m e m b e r of the laboratory staff. A person
or persons having responsibility for q u a l i t y a s s u r a n c e w i t h i n the l a b o r a t o r y
shall be designated by the laboratory m a n a g e m e n t and have direct access to top
management.

2.

The quality manual

shall contain

information

regarding:

a.

The structure of the laboratory

(organizational

charts);

b.

The operational and functional duties and services pertaining to

quality, so that each person concerned will know the extent and
the limits of his responsibility;

c.

General quality assurance

d.

Quality assurance
appropriate ;

e.

Where
appropriate,
m a t e r i a l , etc.;

f.

S a t i s f a c t o r y a r r a n g e m e n t s for f e e d b a c k and c o r r e c t i v e
whenever testing discrepancies are detected;

g.

Procedure

procedures;

procedures

proficiency

specific

testing,

for dealing with technical

for

use

each

of

test,

as

reference

action

complaints.

3.
The quality system shall be systematically and periodically reviewed
by or on b e h a l f of m a n a g e m e n t to e n s u r e the c o n t i n u e d e f f e c t i v e n e s s of the
arrangements, and corrective action initiated.
Such reviews shall be recorded
together with details of any corrective action taken.

This clearly states the importance that m u s t be placed on QA in the analytical

laboratory.
N o t e the key p r o g r a m m e e l e m e n t s are r e v i e w , d o c u m e n t a t i o n and
follow-up.
It
A Quality Assurance p r o g r a m m e must obviously be tailored to specific needs.
c a n be (and o f t e n is) an e x t e n s i v e and c o m p l e x d o c u m e n t w h i c h c o v e r s all
aspects of the laboratory work.
An example is the Quality Manual recommended
for t e s t i n g l a b o r a t o r i e s b y the I L A C (3). T h e v a r i o u s s u b j e c t s i n c l u d e d in a
complete Manual, listed alphabetically, are:

47

DEFINITIONS
Quality Manual
Quality System
Terminology
Testing Laboratory
Test Method
Test Report
ENVIRONMENT
External
Internal

Controls
Controls

E Q U I P M E N T , TESTING AND

MEASURING

Calibration
Identification
Inter laboratory Correlation
P r i o r to U s e
Programmes
U s e of I n - S e r v i c e T e s t E q u i p m e n t
U s e of R e f e r e n c e S t a n d a r d s
External
In-house
O v e r l o a d e d or M i s h a n d l e d
Periodic Maintenance
P u r c h a s i n g and A c c e p t a n c e P r o c e d u r e s
Records
LABORATORY DESCRIPTION
Confidential Information
Employee Responsibility
F i e l d s of A c t i v i t y
Identification
Minimizing Improper Influence
Organizational Structure
Proprietary Rights
Technical Management Personnel
QUALITY MANAGEMENT SYSTEM
Corrective Action
F i e l d s of T e s t i n g A c t i v i t i e s
Obj ec t i v e
P r o f i c i e n c y and I n t e r l a b o r a t o r y C o m p a r i s o n T e s t i n g
Quality Assurance Management
Q u a l i t y M a n u a l - R e v i s i o n and D i s t r i b u t i o n
Quality Policy
Quality System Audit
R e s p o n s i b i l i t y for Q u a l i t y A s s u r a n c e S y s t e m
Reference Materials
Resources Employed
Scope
S u b c o n t r a c ting
Technical Complaints
U p d a t i n g and C o n t r o l of D o c u m e n t s
U s e of E x t e r n a l F a c i l i t i e s
RECORDS
C o n f i d e n t i a l i t y and S e c u r i t y
H i s t o r i c a l F i l e of T e s t M e t h o d s
Maintenance

48

SAMPLES/ITEMS TO BE TESTED
P r o t e c t i o n from Damage
R e c e i p t and D i s p o s a l
Security
STAFF
Deputy Assignments
Job D e s c r i p t i o n s
P e r s o n n e l Records
S u p e r v i s ion
Other Measures
TEST METHODS AND PROCEDURES
I n d e x of Documents
S e l e c t i o n of Test Methods
Use of Non-Standard Test Methods
TEST REPORTS/TEST
Computerized
Format
Revision
Verification

DOCUMENTS
Date

of

Dsta

T h e a b o v e i l l u s t r a t e s h o w c o m p l e x and t h o r o u g h the d o c u m e n t a t i o n f o r a QA
programme can b e .
O b v i o u s l y , not a l l l a b o r a t o r i e s w i l l need such c o m p l e t e n e s s .
H o w e v e r , t h e r e i s a m i n i m u m QA p r o g r a m m e w h i c h s h o u l d be d o n e e v e n in the
s m a l l e s t of food c o n t r o l l a b o r a t o r i e s .
T h i s should i n c l u d e the four key a r e a s
where q u a l i t y c h e c k i n g is needed most.
These are r e f e r e n c e standard m a t e r i a l
used in a n a l y s i s ,
laboratory measuring instruments,
a n a l y s i s r e p o r t s and the
t e c h n i c a l p r o f i c i e n c y of the a n a l y t i c a l s t a f f .
The l a t t e r can be r e v i e w e d in
p a r t by use of a c h e c k s a m p l e a n a l y s i s p r o g r a m m e .
T h e s e f o u r QA c h e c k a r e a s
a r e d i s c u s s e d in d e t a i l in s u c c e e d i n g S e c t i o n s 7 . 3 to 7 . 6 .
O t h e r r e l a t e d QA
a c t i v i t i e s are d i s c u s s e d under S e c t i o n 7 . 7 .

7.3

QA of R e f e r e n c e

Standards

F o r p u r p o s e s of t h i s S e c t i o n , a " R e f e r e n c e S t a n d a r d " i s a p u r e c h e m i c a l or
b i o l o g i c a l s u b s t a n c e w h i c h may be used for c o m p a r i s o n d u r i n g the q u a n t i t a t i v e
a n d / o r q u a l i t a t i v e a n a l y s i s of a c o n s t i t u e n t or a t t r i b u t e of a f o o d .
Of
c o u r s e , " p u r e " is a r e l a t i v e term.
Some m e t a l e l e m e n t s c a n be r o u t i n e l y
o b t a i n e d in 9 9 . 9 9 9 % p u r i t y , w h i l e many o r g a n i c s u b s t a n c e s would be c o n s i d e r e d
" p u r e " at 9 5 % .
The a n a l y s t m u s t j u d g e i f t h e r e f e r e n c e s t a n d a r d u s e d i s
s u f f i c i e n t l y pure for a n a l y s i s p u r p o s e s .
R e f e r e n c e s t a n d a r d s can be d i v i d e d
i n t o three g r o u p s :

1.
Primary:
These are m a t e r i a l s which have been a n a l y z e d and
c e r t i f i e d by a n a t i o n a l s t a n d a r d s o r g a n i z a t i o n or o t h e r a c c e p t a b l e
organization.
2.
Secondary:
S u b s t a n c e s whose p u r i t y is
commercial s u p p l i e r s or o r g a n i z a t i o n s o t h e r than the

certified
above.

by

the p u r i t y
certifying

analysis

by

3.
Other:
This i n c l u d e s a l l r e f e r e n c e s t a n d a r d s w h i c h are c o n s i d e r e d
a c c e p t a b l e by t h e u s e r , b u t w h i c h do n o t f a l l i n t h e a b o v e t w o g r o u p i n g s .
T h e s e can i n c l u d e l o c a l l y o b t a i n e d m a t e r i a l s w h i c h h a v e u n d e r g o n e r e p l i c a t e
a n a l y s i s and have been compared to p r i m a r y or s e c o n d a r y r e f e r e n c e s t a n d a r d s , to
calculate purity.

49

S u b s t a n c e s l a b e l l e d , " p u r e " , " c h e m i c a l l y p u r e " , "c.p.", " p u r i f i e d " or " h i g h e s t

p u r i t y " s h o u l d a l w a y s b e c o n s i d e r e d s u s p e c t as t h e i r a c t u a l p u r i t y o f t e n v a r i e s
widely.
T h e y m u s t be c o m p a r e d to s u i t a b l e r e f e r e n c e s t a n d a r d s b e f o r e u s e as a
standard themselves.
As p r i m a r y and s o m e s e c o n d a r y r e f e r e n c e s t a n d a r d s a r e o f t e n q u i t e e x p e n s i v e , it
c a n b e e c o n o m i c a l to o b t a i n a s u p p l y o f a c h e a p e r p u r e m a t e r i a l a s a w o r k i n g
standard.
It c a n b e a n a l y z e d in c o m p a r i s o n to t h e p r i m a r y ( o r s e c o n d a r y )
r e f e r e n c e s t a n d a r d and the p u r i t y d e t e r m i n e d .
The analyst m u s t be c a r e f u l ,
h o w e v e r , to a v o i d i m p u r i t i e s in the l o c a l m a t e r i a l , w h i c h w i l l c r e a t e p r o b l e m s
during analysis.
T h e f o l l o w i n g is a l i s t o f s o m e s o u r c e s in t h e U n i t e d S t a t e s
s e c o n d a r y r e f e r e n c e s t a n d a r d s of t h e i n d i c a t e d m a t e r i a l s :

Reference

Standards

for p r i m a r y

Source

Number

Alcohols

21

Alkenes

21

Antibiotics

(Chlortetracycline

HC1)

(Erythromycin)

15

(Monensin

14

Sodium)

(Oxytetracycline
(Penicillin

Base)

"G" P r o c a i n e )

(Streptomycin

Sulfate)

(Tylosin)
Atomic

Absorption

Bacterial
Blood

(Metals)

Reference

12
11
12
14
22

Cultures

1, 2 , 3, 4

Group/Typing

Chemicals, Industrial

1 9 , 3 2 , 38

Contaminants, Drinking Water

Drugs

13

1 0 , 34

(Animal)

1 8 , 2 5 , 31

(U.S. Schedules

I, II)

1 6 , 1 7 , 18

(U.S. Schedules

III, IV, V, VI)

18

Ethanol, Absolute

37

Fibers, Synthetic

21

Fuels, Motor

35

Lead

(Alcoholic Beverages)

34

(Blood)

20

(Motor Fuels)

22

50

or

Reference

Standards

Source

Metals (Foods, Feeds, Fertilizers)

Htmber

23, 30, 36

(Fish, Sediments, Fuel Oil)

23

(Sludge)

34
17,

Mycotoxins
Pesticides

21, 24, 25, 26

19, 21, 32, 33

Phenylalanine (PKU)

3, 4

Salmonella Typing & Grouping Antisera

1, 3

Shigella Grouping Antisera

1, 5

Species (Known Fish)

27, 28

(Known Meats)

29

Spirits (Distilled Congeners)

36

Streptococcus

Thallium (Standard 1000 ppm)

19

Trichinosis

Tuleremia

Viral Agent Antisera

1, 6, 7

Wine (Reference)

23

The U.S. sources referred to above, listed by number are:

1.

Department of Health and Human Services

Public Health Service
Centers for Disease Control
Atlanta, GA 30333

2.

American Type Culture Collection

12301 Parklawn Drive
Rockville, MD 20852

3.

Difco Laboratories
P.O. Box 1058
Detroit, MI 48232

4.

BBL Microbiology Systems

P.O. Box 243
Cockeysville, MD 21030

5.

Fisher Scientific
7633 Hull Street Road
Suite 2000D
Richmond, VA 23235

6.

M A Bioproducts
Briggs Ford Road
Building 100
Walkersville, MD 21793
51

7.

Flow Laboratories, Inc.

7655 Old Springhouse Road
McLean, VA 22102

8.

Wellcome Diagnostics
Research Triangle Park
North Carolina 27709

9.

American Dade
P.O. Box 520672
Miami, FL 33152

10

Environmental Resource Associates

5540 Marshall
Arvada, CO 80002

11

ICN Nutritional Biochemicals

P.O. Box 28050
Cleveland, OH 44128

12

Pfizer Laboratories
235 E. 42nd Street
New York, NY 10017

13

Lederle Laboratories
Division of American Cyanamid
One Cyanamid Plaza
Wayne, NJ 07470

14

Eli Lilly and Company

307 E. McCarty Street
Indianapolis, IN 46285

15

Aldrich Chemical Company

Milwaukee, WI 53233

16

U.S. Drug Enforcement Administration

Special Testing Laboratory
7704 Old Springhouse Road
McLean, VA 22102

17

Applied Science
P.O. Box 440
State College, PA 16801

18

United States Pharmacopeia Convention Inc.

12601 Twinbrook Parkway
Rockville, MD 20852

19

Aldrich Chemical Company

P.O. Box 355
Milwaukee, WI 53201

20,

E. S. A. Inc.
45 Wiggins Avenue
Bedford, MA 01730

21,

Supelco Inc.
Supelco Park
Bellefonte , PA 16823

22,

Fisher Scientific Company

711 Forbes Avenue
Pittsburgh, PA 15219

Division

52

(US-DEA)

23.

National Bureau of Standards

Office of Standard -and Reference Materials
Room B 311, Chemistry Building
Washington, DC 20234

24.

The Myco Laboratory Company

P.O. Box 321
Chesterfield, MO 63017

25.

Sigma Chemical Company

P.O. Box 14508
St. Louis, MO 63178

26.

Eureka
215 - 26th Street
Sacramento, CA 95816

27.

U.S. Department of Commerce

National Oceanic and Atmospheric
Northeast Inspection Office
P.O. Box 1188, Emerson Avenue
Gloucester, MA 01930

Admin.

28.

VA Institute of Marine Science

College of William and Mary
Gloucester Point, VA 23062

29.

VA Dept. of Agriculture and Consumer

Division of Animal Health
1 North 14th Street
Richmond, VA 23219

30.

American Dade Division

American Hospital Supply Corp.
Miami, FL 33152

31.

Pfaltz and Bower Inc.

375 Fairfield Avenue
Stamford, CN 06902

32.

U.S. Environmental Protection Agency

Pesticides, Industrial Chemicals Repository
Research Triangle Park, NC 27711

33.

U.S. Environmental Protection Agency

Analytical Chemistry Section
Building 306, Room 101, ARC - East
Beltsville, MD 20705

34.

U.S. Environmental Protection Agency

EMSL - Cincinnati
26 West St. Clair Street
Cincinnati, OH 45268

35.

Phillips Chemical Company

Drawer 0
Borger, TX 79007

36.

J. T. Baker Chemical Company

222 Red School Lane
Phillipsburg, NJ 08865

37.

U.S. Industrial Chemical Company

Tuscola, IL 61953

53

Services

(MD-8)

38.

Chem Service
P.O. Box 194
West Chester, PA

19380

Once a stock of appropriate reference standards has been obtained, they must be
recorded, used and stored properly.
A records book or file cards can be used,
with the following information noted for each standard:
1.

Standard name and date

2.

Source

3.

Code or lot number.

4.

Purity.

5.

Expiration date

(if any).

6.

Special

storage

requirements.

7.

Storage

location.

(from where

received.

obtained).

M a n y laboratories assign a number to the standard container for accountability

purposes.
If the s t a n d a r d is o n e w h i c h m a y d e t e r i o r a t e on s t o r a g e , t h e n the
record should also include dates and results when stability checks were m a d e .
If it is deemed necessary for control, there could be a check-out and - i n sheet
for the s t a n d a r d , w h i c h the a n a l y s t w o u l d d a t e and i n i t i a l w h e n u s i n g the
material.
T h i s is n o t u s u a l l y d o n e e x c e p t for e x t r e m e l y d a n g e r o u s or h i g h l y
sensitive substances which must be accounted for.
It is o f t e n c o n v e n i e n t to s t o r e r e f e r e n c e s t a n d a r d s in a r e a s n e a r w h e r e t h e
a n a l y s e s are b e i n g d o n e (i.e. p e s t i c i d e s t a n d a r d s in the p e s t i c i d e s r e s i d u e
analysis section of a larger food laboratory).
H o w e v e r , the storage area m u s t
be separate from other chemical storage and clearly marked as to its contents.
E x a m p l e s are a marked refrigerator section or cabinet with clear warnings or
i n s t r u c t i o n s that o n l y s p e c i f i c r e f e r e n c e s t a n d a r d s are to be s t o r e d t h e r e .
T h i s p e r m i t s a c c o u n t i n g for a s t a n d a r d l o c a t i o n as w e l l as e n s u r i n g t h a t a
reference standard is not mistakenly used as a non-standard chemical.
If periodic testing is done to check stability, then the test protocol should
be k e p t w i t h the s t a n d a r d r e c o r d .
The r e c o r d w o u l d also c o n t a i n the test
r e s u l t s , d a t e , a n a l y s t n a m e and a n y s u p p o r t i n g d o c u m e n t s s u c h as s p e c t r a or
chromatograms.
W i t h all Quality Control procedures in
would consist of a periodic review of:
1.
Records
c o n d i t i o n of the
correct times?)

for?

the

Quality

Assurance

checking

(Are they complete and current?

Do they reflect the actual
standard?
H a v e a p p r o p r i a t e s t a b i l i t y t e s t s b e e n r u n at

2.
Storage
(is
If not, w h y ? )

3.
review?

place,

the

storage proper?

Are the stored

standards

Physical Condition
( W h e r e w a s the s t a n d a r d at the
Any physical evidence of deterioration or m i s h a n d l i n g ? )

accounted

time

of

the

The t i m i n g of the r e v i e w w o u l d d e p e n d on n e e d .
An i n i t i a l c y c l e of t h r e e
m o n t h s is s u g g e s t e d .
T h i s c a n b e i n c r e a s e d or d e c r e a s e d as c o n d i t i o n s and
review results dictate.

54

M a n a g e m e n t and e a c h a n a l y s t m u s t r e m e m b e r that r e f e r e n c e s t a n d a r d s are

e x t r e m e l y i m p o r t a n t to an a n a l y t i c a l l a b o r a t o r y , a n d m u s t b e
treated
accordingly.
The p e r s o n m a k i n g the QA r e v i e w s h o u l d be a s e n i o r a n a l y s t or
s u p e r v i s o r w h o h a s a k n o w l e d g e and a p p r e c i a t i o n for p r o b l e m s t h a t i m p r o p e r ,
contaminated or deteriorated reference standards can create for the analyst.

7.4

QA of

Instruments

A f t e r r e f e r e n c e s t a n d a r d s , m e a s u r i n g i n s t r u m e n t s are the m o s t s e n s i t i v e and

troublesome items for an a n a l y t i c a l l a b o r a t o r y .
I n s t r u m e n t m a i n t e n a n c e and
r e p a i r are o b v i o u s l y i m p o r t a n t and are d i s c u s s e d e l s e w h e r e .
Of e q u a l (or
possibly greater) importance is an o r g a n i z e d p r o c e d u r e to p e r i o d i c a l l y c h e c k
the instrument performance.
If the performance parameters to be checked are
s e l e c t e d c a r e f u l l y , t h e n the a n a l y s t h a s a r e a s o n a b l e m e a s u r e of w h e t h e r the
i n s t r u m e n t is o p e r a t i n g p r o p e r l y , on a c o n t i n u i n g b a s i s . O n c e a p e r f o r m a n c e
c h e c k i n g p r o t o c o l is d e c i d e d u p o n , an i n d i v i d u a l p e r f o r m a n c e r e c o r d c a n b e
p r e p a r e d for e a c h i n s t r u m e n t .
T h i s can be a s e p a r a t e n o t e b o o k w h i c h is k e p t
p h y s i c a l l y n e a r the i n s t r u m e n t , or c a n be p a r t of the m a i n t e n a n c e and r e p a i r
record kept for each instrument.
The frequency of performance checking varies considerably, again depending on
c i r c u m s t a n c e and p r e v i o u s c h e c k r e s u l t s .
If a c h e c k r e s u l t
indicates
maintenance or repair, then a follow-up check (after the repair, etc.) should
be scheduled before the next routine QA check time.
The routine use of m a n y instruments involves some form of performance checking.
An example is a working standard injection into a gas chromatograph first thing
in the m o r n i n g , to c h e c k i n s t r u m e n t r e s p o n s e .
T h i s is n e c e s s a r y and h a s its
place to assure the analyst that the instrument is operating properly for that
day.
For p u r p o s e s of a QA p e r f o r m a n c e c h e c k , h o w e v e r , t h e r e s h o u l d be a
separate and distinct checking programme.
S o m e l a b o r a t o r i e s m a k e a d i s t i n c t i o n b e t w e e n r o u t i n e i n s t r u m e n t s used by
e s s e n t i a l l y all a n a l y s t s (i.e. b a l a n c e s , s p e c t r o p h o t o m e t e r s , etc.) and t h o s e
used o n l y by h i g h l y t r a i n e d s p e c i a l i s t s (i.e. m a s s s p e c t r o m e t e r s , etc.).
The
p e r f o r m a n c e c h e c k i n g of the f o r m e r c a n b e d o n e b y any a s s i g n e d a n a l y s t .
The
latter, h o w e v e r , should be checked by trained analyst only.
A suggested performance checking protocol
laboratory instruments is as follows:

Analytical

1.

and

schedule

for

some

general

Balances

Sensitivity

(bimonthly)

Check balance sensitivity using three standard weights (10g, lg and

100 mg).
Weight used should be traceable to certified weights of at
l e a s t U.S. C l a s s S.
S e n s i t i v i t y s h o u l d be w i t h i n the
balance
specifications.

2.

Calibration

(annual)

Best done in connection

using standard weights.

with

annual

55

cleaning

and

maintenance,

again

Spectrophotometers

1.

(ultraviolet and

Wavelength

Accuracy

visible)

(bimonthly)

Check by recording over entire UV-visible w a v e l e n g t h range using

H o l m i u m and D i d y m i u m f i l t e r s ( u s u a l l y o b t a i n a b l e f r o m t h e i n s t r u m e n t
m a n u f a c t u r e r or a l a r g e s u p p l y f i r m ) .
Run two spectra
for
comparison.
Results should not differ from published values more
t h a n + 1.0 n m at a n y w a v e l e n g t h .

2.

Photometric

Accuracy

(bimonthly)

P r e p a r e a s o l u t i o n of 60 _+ 0.25 m g p o t a s s i u m d i c h r o m a t e in o n e l i t r e
of 0.01N s u l p h u r i c a c i d .
( T h i s s o l u t i o n is q u i t e s t a b l e a n d o n c e
p r e p a r e d can be used a long time).
S c a n this s o l u t i o n f r o m 2 1 0 to
450 n m .
T h e f o l l o w i n g a b s o r b a n c e s (+ 1% f u l l s c a l e ) s h o u l d o c c u r at
the i n d i c a t e d w a v e l e n g t h s :

Wavelength

(nm)

Absorbance

235
257
313
350

0.747
0.869
0.293
0.644

A l t e r n a t i v e l y , t h e U.S. N a t i o n a l B u r e a u of S t a n d a r d s h a s a v a i l a b l e
for p u r c h a s e S R M 9 3 0 , a g l a s s f i l t e r w h i c h c a n b e u s e d s i m i l a r l y and
which has certified wavelength/absorbance values.

Spectrophotometer

1.

(infrared)

Wavelength Accuracy

(trimonthly)

Scan a standard polystyrene film.

The following peaks
indicated w a v e n u m b e r s w i t h i n the listed a c c u r a c y :

Wavenumber

(cm

1.

Baseline

(atomic

+
_+
+
+

absorption)

(daily when

Absorbance

the

6
6
2
2

used)

U s i n g f l a m e o n l y , the r e c o r d e r b a s e l i n e s h o u l d
.005 a b s o r b a n c e u n i t s in a f i v e m i n u t e p e r i o d .

2.

at

Accuracy

2851
1601
1028
907

Spectrophotometer

occur

(daily when

not vary m o r e

than +

used)

T h r e e c o n s e c u t i v e a b s o r b a n c e c h e c k s of the
v a r y m o r e t h a n _+ .005 a b s o r b a n c e u n i t s .

56

same

solution

should

not

3.

Detection Limit

(monthly)

Prepare a solution of a metal standard sufficiently dilute to give a

response of two times the baseline absorbance under ideal conditions.
T h i s b e c o m e s the ' d e t e c t i o n l i m i t ' s t a n d a r d .
M a k e four r e p l i c a t e
aspirations to check reproducibility.

Gas

Chromatograph

1.

Column Oven

(semiannual)

Check column oven temperature using

2.

Gas Flow Rate

pyrometer.

(monthly)

C h e c k f l o w rates of all c a r r i e r
bubble meter or other device.

3.

a calibrated

Detector Response

(daily when

and

detector

gases

u s e d , using

used)

Compare present detector response with the response obtained when new
or w h e n last c l e a n e d and c a l i b r a t e d .
(in s o m e d e t e c t o r s , n o t a b l y
e l e c t r o n c a p t u r e , a d e t e r i o r a t i n g r e s p o n s e i n d i c a t e s a need for
cleaning).

High Performance Liquid

1.

Chrcmatograph

Column Resolution (daily when

used)

Prepare a solution of two or more substances which the column should

resolve under normal analytical conditions. Use this to check column
performance each time the column is used.

2.

Detector Response (daily when used)

C h e c k d e t e c t o r r e s p o n s e using a k n o w n c o n c e n t r a t i o n standard and
compare to a response previously obtained under ideal conditions.

The above p e r f o r m a n c e c h e c k s are only s u g g e s t i o n s .

The best a p p r o a c h is to
read the o p e r a t i o n s m a n u a l for e a c h i n s t r u m e n t and s e l e c t key o p e r a t i n g
p a r a m e t e r s or s p e c i f i c a t i o n s of i n t e r e s t to p r e p a r e the p r o t o c o l .
Also,
instruments or equipment other than those mentioned above should be considered
for a p e r f o r m a n c e check p r o g r a m m e .
The g o v e r n i n g factor should be the
instrument or equipment importance to the laboratory.
The QA p r o g r a m m e on i n s t r u m e n t p e r f o r m a n c e c h e c k i n g m u s t also include a
p e r i o d i c r e v i e w to i n s u r e the c h e c k s are b e i n g m a d e and that a p p r o p r i a t e
follow-up action is taken if a check discloses a possible performance problem.
This follow-up could be maintenance, cleaning, repair, calibration, etc.
Any
follow-up action should be recorded in the notebook kept with the instrument.

57

7.5

QA of Analytical

Reports

As discussed in preceding Section 5.5, the analytical report is the culmination

of all of the l a b o r a t o r y ' s e f f o r t s .
T h e r e are m a n y t y p e s and f o r m a t s for
analysis reports.
T h e y v a r y from s i m p l e to d e t a i l e d , but all are s u b j e c t to
the same problem, h u m a n error.
A Quality Assurance p r o g r a m m e for analytical
reports is basically an after-the-fact or retrospective review of a document
w h i c h h a s a l r e a d y b e e n t h r o u g h the n o r m a l s u p e r v i s o r y and m a n a g e m e n t r e v i e w
process.
It is d e s i g n e d to d e t e c t r e p o r t w r i t e - u p and r e v i e w e r r o r s so that
appropriate procedures can be instituted to prevent their reoccurrence.
Although report formats m a y vary according to organizational need, the report
m u s t be c o m p l e t e enough to enable the reviewer to reconstruct the analysis and
to c h e c k the a n a l y t i c a l r e a s o n i n g as w e l l as d a t a and c a l c u l a t i o n s .
For
e x a m p l e , in ISO Guide 25 (2) under part 12, "Test Reports", it states:

1.
The work carried out by the testing laboratory shall be covered by a
report w h i c h accurately, clearly and u n a m b i g u o u s l y p r e s e n t s the t e s t r e s u l t s
and all other relevant information.

2.

Each test report

shall

include at least

the following

information:

a.

Name and address of testing

b.

Unique identification of
each page of the report.

c.

Name and address of

d.

Description and identification of the test

e.

D a t e of r e c e i p t of test
tests, as appropriate.

f.

A s t a t e m e n t to the e f f e c t that the test r e s u l t s r e l a t e o n l y to

the items tested.

g.

Identification

h.

Description of sampling

i.

Any d e v i a t i o n s ,
additions
specification, and any other
test .

j.

Disclosure
ut ilized.

k.

M e a s u r e m e n t s , e x a m i n a t i o n s and d e r i v e d r e s u l t s , s u p p o r t e d by
t a b l e s , g r a p h s , s k e t c h e s , p h o t o g r a p h s as a p p r o p r i a t e , and any
failure identified.

1.

A statement on measurement

m.

A s i g n a t u r e a n d t i t l e of p e r s o n ( s ) a c c e p t i n g
technical
responsibility for the test report and date of issue.

n.

A s t a t e m e n t that t h e r e p o r t s h a l l n o t be r e p r o d u c e d
full without the approval of the testing laboratory.

of

report

(such

as serial

number),

and

of

performance

of

client.

of the test

any

company.

item

and

date(s)

of

specification, method

procedure, where

and

procedure.

relevant.

to or e x c l u s i o n s from the test

information relevant to a specific

non-standard

58

item.

test

uncertainty

method

(where

or

procedure

relevant).

except

in

3.
Particular care and attention shall be paid to the arrangement of the
test report, especially with regard to presentation of the test data and ease
of assimilation by the reader.
The format shall be carefully and specifically
a s s i g n e d for e a c h type of test c a r r i e d o u t , but the h e a d i n g s shall be
standardized as far as possible.
The U.S. Food and Drug A d m i n i s t r a t i o n " A n a l y s t W o r k s h e e t "
good example for purposes of discussing an analytical report
is relatively complete and includes space for all pertinent
analytical summary.
The r e v e r s e of the form w o u l d be used
and calculations as the analysis progresses.

(Figure 7.1) is a
QA programme.
It
data including an
for r a w w o r k d a t a

An a n a l y t i c a l r e p o r t QA p r o g r a m m e should i n v o l v e r e v i e w of a p r e d e t e r m i n e d
n u m b e r of c o m p l e t e d r e p o r t s on a m o n t h l y or b i m o n t h l y b a s i s .
The r e p o r t s
should be r e p r e s e n t a t i v e of the k i n d s of w o r k d o n e , w i t h a b o u t as m a n y w h i c h
s h o w law v i o l a t i o n s as are u s u a l l y e n c o u n t e r e d .
An e x a m p l e could be ten
r e p o r t s w i t h t w o b e i n g v i o l a t i v e ( a s s u m i n g the v i o l a t i o n rate is about 20%).
The object is to gain a relatively representative sampling of completed reports
in order to evaluate overall report writing.
If some section of the laboratory
has substandard reports, then their coverage can be selectively increased until
it a p p e a r s that the r e p o r t s are s a t i s f a c t o r y .
T h i s is one of the p r i m e
f u n c t i o n s of QA r e v i e w s ( w h a t e v e r the t y p e ) - to p i n p o i n t p r o b l e m areas and
give them visibility until the problem is solved.
An example of an analytical report review protocol is one which has been used
by the U.S. Food and Drug A d m i n i s t r a t i o n for QA r e v i e w of their A n a l y t i c a l
Worksheets.
Their protocol consists of a listing of performance factors that
their Worksheet (Figure 7.1) must meet, as follows:
1.

2.

Accuracy and

Completeness

a.

Worksheet clearly describes

received by the analyst.

b.

Worksheet fully and accurately reflects continuity and

of sample.

c.

Information on the
Collection Report.

d.

T h e u s e of a p p r o p r i a t e
equipment is described.

e.

C a l c u l a t i o n s are a c c u r a t e , easy to f o l l o w , and are c h e c k e d .

This includes checking of conversion factors, normality factors,
etc., for accuracy of recording.

f.

If m o r e than one p e r s o n p a r t i c i p a t e d in
worksheet clearly indicates who did what.

g.

Sample reserve or disposition is correctly

h.

E r r o r s are noted by s t r i k i n g t h r o u g h the i n c o r r e c t

inserting, initialing and dating the new entry.

i.

Any discarded

Analytical

worksheet

results are

the

sample

and

is compatible

standards,

condition

with

reagents,

the

the

and

when

integrity

Inspection

special

analysis,

the

reported.
entry

and

explained.

Methodology

The a p p r o p r i a t e m e t h o d
is used and is r e f e r e n c e d on the
worksheet.
Analyses performed and methods used are consistent
with appropriate instructions or as directed by the Supervisor.

59

ANALYST WORKSHEET
3. S E A L S

NONE

INTACT

BROKEN

1. P R O D U C T

4. D A T E

REC'D

2. S A M P L E

5. R E C E I V E D

FROM

NUMBER

6. D I S T R I C T O R L A B O R A T O R Y

7. D E S C R I P T I O N O F S A M P L E

8.
NET
CONTENTS

NOT APPLICABLE

DECLARE/UNIT

NOT DETERMINED

AMOUNT

UNITS E X A M I N E D

% OF

10. S U M M A R Y O F

11. R E S E R V E

.ORIGINAL(S)
LABELING

FOUND.

DECLARED

.COPIES

SUBMITTED

SUBMITTED

NONE

ANALYSIS

SAMPLE

1 2 . L. A N A L Y S T S I G N A T U R E (Broke

Seal

)
WORKSHEET
CHECK
14. D A T E

FORM FD 431 (1/77)

P R E V I O U S E D I T I O N IS O B S O L E T E .

Figure
USFDA

Analyst

60

7.1
Worksheet

REPORTED

PAGE

OF

PAGES

3.

4.

b.

Sample is analyzed so
laws or regulations.

c.

Deviations
worksheet.

d.

Any unofficial method

Supervisory

from

the

as

to

permit

referenced

used

application

method

are

of

appriopriate

explained

on

the

is validated.

Review

a.

The a n a l y s i s and m e t h o d o l o g y w a s a p p r o p r i a t e
indicated on the inspection collection report.

b.

L a b o r a t o r y c o n c l u s i o n s and final d e c i s i o n
supported by information on the worksheet.

c.

If the sample is classified

performed (if possible).

Time

Frames

a.

Sample analysis

violative,

to

are

the

problem

accurate

a confirming

analysis

and

is

time frames are met.

Any deviations from the above which are found during the r e v i e w , are recorded
and an a t t e m p t m a d e to d e t e r m i n e h o w they o c c u r r e d .
T h e r e v i e w e r m a y find a
p a t t e r n s u c h as c e r t a i n e r r o r s a r e c o n s i s t e n t l y m a d e , i n d i c a t i n g a n e e d for
specific training.
A l l f o l l o w - u p a c t i v i t i e s and a c t i o n s t a k e n to c o r r e c t
p r o b l e m s , m u s t be detailed and documented to provide laboratory m a n a g e m e n t with
a continuing basis to evaluate improvement.

7.6

Check Sampl

Examination

O n e of the m o s t c o m m o n w a y s to e v a l u a t e o v e r a l l i n d i v i d u a l or l a b o r a t o r y
p e r f o r m a n c e in a g i v e n a n a l y s i s , is b y u s e of k n o w n c h e c k s a m p l e s .
This
i n c l u d e s b o t h i n t r a ( w i t h i n ) the l a b o r a t o r y and i n t e r ( b e t w e e n ) like
laboratories.
The A m e r i c a n Chemical Society (ACS) in their 1980 Guidelines for
Data Quality Evaluation, stated:
"At the o u t s e t , a l a b o r a t o r y s h o u l d d e m o n s t r a t e its p r o f i c i e n c y u s i n g
prototype and non-critical samples, thereby reducing the probability that bad
d a t a w i l l be g e n e r a t e d on c r i t i c a l s a m p l e s , e s p e c i a l l y t h o s e i n v o l v i n g
complicated unknown mixtures.
An i n t r a l a b o r a t o r y q u a l i t y c o n t r o l p r o g r a m
s h o u l d i n c l u d e the use of b l i n d s a m p l e s in a d d i t i o n to c h e c k s a m p l e s w h o s e
v a l u e s are k n o w n to the a n a l y s t s .
A l l a n a l y s t s s h o u l d be m o n i t o r e d b y the
quality control procedures, and any assessment of laboratory performance should
include all of the analysts involved, or at least a random selection of those
analysts.
I n t e r l a b o r a t o r y Q u a l i t y A s s u r a n c e p r o g r a m s s h o u l d also use b l i n d
s a m p l e s in a d d i t i o n to c h e c k s a m p l e s ,
in o r d e r to p r o v i d e a r e a l i s t i c
assessment of the performance of the method that is achievable in the field."
L a t e r , in 1 9 8 2 , the A C S m a d e an a d d i t i o n a l s t a t e m e n t
reliability and acceptability of analysis data:

regarding

improving

" I d e a l l y , for a g i v e n m e t h o d , i n t e r l a b o r a t o r y v a r i a b i l i t y s h o u l d b e the

s a m e as i n t r a l a b o r a t o r y v a r i a b i l i t y :
In real s i t u a t i o n s , h o w e v e r , the
i n t e r l a b o r a t o r y v a r i a b i l i t y is a l m o s t a l w a y s g r e a t e r .
T h e r e f o r e , it is
necessary to determine for a given method the variability of the m e a s u r e m e n t s
( r a n d o m e r r o r ) b e t w e e n l a b o r a t o r i e s in o r d e r to m a k e a l l o w a n c e s for t h o s e
differences
in i n t e r p r e t i n g
the r e s u l t s of a n a l y s e s .
For any p r o p e r l y

61

validated procedure, however, interlaboratory results will be consistent with

i n t r a 1 a b o r a t o r y r e s u l t s / t h a t is, t h e u n c e r t a i n t y i n t e r v a l s
(including
s y s t e m a t i c error b o u n d s ) for all q u a l i f i e d l a b o r a t o r i e s ( i n d i v i d u a l l y and
collectively) will overlap the true value. (This presumes that the measurement
method, itself, has negligible bias.)"
The various

factors

influencing

final

analysis data are shown in Figure 7.2.

DATA

Figure 7.2

During 1984, the U.S. Association of Food and Drug Officials (AFDO) assembled a
listing of proficiency and check sample programs available through various U.S.
a g e n c i e s and o r g a n i z a t i o n s .
The listing is as f o l l o w s , giving c h e c k s a m p l e
type, the product involved and the check sample program sponsor:

Check Sample Type

Program
Sponsor

Product(s)

Aflatoxins

Milk, Corn

Alcohol

Blood

Antibiotics

Meat

Antibiotics

Milk

Arsenic

Meat, Poultry

Filters

Asbestos

(Number of Fibres)

Bacteriology

Milk, General

Bioassay of Antibiotics

Feed s

Cations

Water

Cereal

Water

Cereal

Components

Coliforms

62

Food

6,7

Drinking Water,
Fatty

Prograai
Sponsor

Product(s)

Check Sample Type

Contaminants

Water

Fats and

Acids

Oils

Fertilizers

Frtilizers

13

Fibre

Fibre

11

Flammables

Various

11

Fluoride

Water

Food

Various

Characterization

Components

Herbicides and
Industrial
Lead and

Chemicals

FEP

Medicated
Metals

Organics

Feeds

(Cations)

Metals and

Foods

Urine and

17

Water

10

Fish

Blood

Feed s

Food

Water

Minerals

Microb iology
Microscopic

14

Various
Characterization

Products

18,19

Feed s

15

Mould s

Mycology

Organic

Chemicals

Water

Organic

Solvents

Charcoal

Organics

Semi-Volatile

Organochlorine

Tube

Synthetic

Compounds

PCB's and Chlorinated

14

Organics

Leachate

12

Plasma

10

Fat, Blood
Meats,

Poultry

Phosphatase

Milk

Protein/Moisture/Fat/Salt

Meat

Residues,

Meats,

Pesticide

Poultry

Pesticides/Herbicides

Water

Pesticides/Herbicides

Vegetables,

Smalley Oil

Feed s

Milk

Somatic

Cell

Meals
Count

and Drinking

Sulfonamide s

Meats,

Vitamins

Milk, Feed,

Waste Water

Parameters

Water

63

Foods

Poultry
Foods

Water

9,10,14
6,16

4
1
9

The U . S . s p o n s o r s

for the above c h e c k sample p r o g r a m s

1.

A m e r i c a n A s s o c i a t i o n of C e r e a l
3340 P i l o t K n o b Road
St. P a u l , MN 55121

2.

A m e r i c a n Oil C h e m i s t s Society
508 South Sixth Street
C h a m p a i g n , IL 61820

3.

U . S . D e p a r t m e n t of T r a n s p o r t a t i o n
Transportation Systems Center, Kendall
Cambridge, MA 02142

are

Chemists

Square

4.

U . S . D e p a r t m e n t of A g r i c u l t u r e , FSIS
P . O . Box 5080
S t . L o u i s , MO 63115

5.

N a t i o n a l I n s t i t u t e of O c c u p a t i o n a l Safety and H e a l t h
C h e m i c a l R e f e r e n c e L a b o r a t o r y (PAT) (R-3)
4676 C o l o m b i a P a r k w a y
C i n c i n n a t i , OH 4 5 2 2 6

6.

U . S . Food and D r u g A d m i n i s t r a t i o n
1090 T u s c u l u m A v e n u e
C i n c i n n a t i , OH 4 5 2 2 6

7.

U . S . C e n t e r for D i s e a s e C o n t r o l
Chief, Performance Evaluation Branch, Laboratory
P r o g r a m O f f i c e , A t l a n t a , GA 3 0 3 3 3
Telephone: (404) 329-3847

8.

A m e r i c a n A s s o c i a t i o n of Feed C o n t r o l
c/o L a w and C o m p a n y
P . O . B o x 1558
A t l a n t a , GA 30301

9.

U . S . Environmental Protection
QA B r a n c h , EMSL
C i n c i n n a t i , OH 4 5 2 6 8

10.

U . S . E n v i r o n m e n t a l P r o t e c t i o n A g e n c y , QA D i v i s i o n
E M S L , P . O . Box 15027
Las V e g a s , NV 89114
T e l e p h o n e : (702) 7 9 8 - 2 1 0 0

11.

Forensic Science Foundation

Collaborative Testing Services, Inc.
8343-A Greensboro Drive
M c L e a n , V A 22102

12.

A m e r i c a n S o c i e t y for Testing
1916 R a c e S t r e e t
P h i l a d e l p h i a , PA 19103

13.

A s s o c i a t i o n of A m e r i c a n Plant Food C o n t r o l O f f i c i a l s
c/o W . Penn Z e n t m e y e r
V A D e p a r t m e n t of A g r i c u l t u r e and C o n s u m e r S e r v i c e s
P . O . Box 1163
R i c h m o n d , VA 23201
Telephone: (804) 786-3511

Officials

Agency

Material

64

14.

U.S. Geological Survey

5293 Ward Road
Arvada, CO 80002
Telephone: (303) 234-3975

15.

American Association of Feed

Attn: Mrs. Janet Windsor
1118 Apple Drive
Mechanicsburg, PA 17055

16.

Association of Food and Drug Officials of the Southern States

c/o George Fong
Division of Chemistry
Florida Department of Agriculture and Consumer Services
3125 Connor Boulevard
Tallahassee, FL 32301

17.

National Food Processors Association

1133 20th Street, NW
Washington, DC 20016
Telephone: (202) 331-5955

18.

College of American Pathologists

7400 N. Skokie Boulevard
Skokie, IL 60077
Telephone: (312) 677-3500

19.

American Association of Bioanalysts

Proficiency Testing Service
205 W. Levee Street
Brownsville, TX 78520
Telephone: (512) 546-5315

Microscopists

It is a d v i s a b l e to p a r t i c i p a t e in as m a n y i n t e r - 1 a b o r a t o r y c h e c k s a m p l e
p r o g r a m s as are a v a i l a b l e in the a r e a s of i n t e r e s t to the l a b o r a t o r y .
The
s p o n s o r i n g o r g a n i z a t i o n s u s u a l l y p r o v i d e a s u m m a r y r e p o r t to p a r t i c p a t i n g
l a b o r a t o r i e s , w h i c h g i v e s an e v a l u a t i o n of the l a b o r a t o r y ' s p e r f o r m a n c e as
compared
to o t h e r p a r t i c i p a n t s .
T h e i n t e r - 1 a b o r a t o r y p r o g r a m can be
supplemented by an intra program to highlight specific areas of concern which
W h e n s e l e c t i n g s a m p l e s for an
are n o t c o v e r e d in the inter p a r t i c i p a t i o n .
intra program, the following considerations should be taken into account:
1.

The capability
laboratory.

to analyze

the

sample must be w i d e l y available

2.

The analytical method must be one that

3.

The sample should cover a variety of analytical

identification steps if possible.

4.

The product must be readily available and reasonable

is generally

in the

employed.

techniques,

including

in cost.

A l w a y s keep in mind that the evaluation of check sample results must include
all aspects of the analysis.
In cases where there is a large discrepancy from
the expected or true result, the laboratory must investigate all aspects of the
analysis (as given in Figure 7.2) to d e t e r m i n e w h a t specific analysis area or
areas are suspect.
From this, the laboratory should take appropriate action to
prevent reoccurrence of a similar difficulty.

65

7.7

Other QA Activities

Some important QA review programmes were discussed in the preceding Sections.

Many other areas of laboratory operations would also benefit from QA review.
Keeping in mind the definition for Quality Assurance given in Section 7.1, any
l a b o r a t o r y o p e r a t i o n can be r e v i e w e d to d e t e r m i n e if c o r r e c t p r o c e d u r e s are
being followed and to identify procedural weaknesses.' Examples are:

1.
S a f e t y - The laboratory safety programme can be periodically reviewed
(about every three months) to determine that safety and emergency materials are
on hand and b e i n g used. T h i s w o u l d i n c l u d e a c h e c k of any i n j u r y or a c c i d e n t
records and a review that appropriate follow-up corrective measures were taken.
2.
S u p p l y M a n a g e m e n t - R e f e r e n c e s t a n d a r d h a n d l i n g and s t o r a g e w a s
discussed earlier.
The s a m e g e n e r a l p r i n c i p l e s a p p l y to all l a b o r a t o r y
supplies, such as glassware, chemicals, solvents and others. A QA review would
focus on whether supplies are being ordered, stored and distributed properly.
3.
S a m p l e M a n a g e m e n t - The s a m p l e s r e c e i v e d by the l a b o r a t o r y for
analysis must be accounted for. This is even more critical when the laboratory
is i n v o l v e d in food l a w e n f o r c e m e n t .
An a c c o u n t a b i l i t y s y s t e m s h o u l d be
e s t a b l i s h e d and in o p e r a t i o n (see S e c t i o n s 4.2 and 4.3). The QA r e v i e w w o u l d
determine that the system is working properly and that samples are accounted
for throughout their receipt, storage, analysis and final disposition.
4.
T r a i n i n g - This m a y s e e m an odd area for QA r e v i e w , but it r a n k s in
importance to most other laboratory operations.
A QA review of training could
i n c l u d e c h e c k s of o n g o i n g f o r m a l t r a i n i n g p r o g r a m m e s for n e w a n a l y s t s and
checks of training needs and records for experienced analysts.
The importance
of t r a i n i n g c a n n o t be o v e r e m p h a s i z e d and a QA r e v i e w p r o g r a m m e o f t e n g i v e s
training needed visibility to management.

The above are only examples and laboratory management must select with care the
o p e r a t i o n a l areas n e e d e d for Q u a l i t y A s s u r a n c e r e v i e w .
R e m e m b e r that any
laboratory function can be (and often should be) subject to QA review.

7.8

Text

1.

G A R F I E L D , F.M.,
Laboratories, 2.
VA, U.S.A.

2.

ISO Guide 25, 1982.

General Requirements for the Technical Competence
Testing Laboratories.
International Organization for Standards.

3.

INTERNATIONAL LABORATORY
Report of Task Force D.

Farther

References
1985.
Q u a l i t y A s s u r a n c e P r i n c i p l e s for A n a l y t i c a l
Association of Official Analytical Chemists, Arlington,

ACCREDATION

CONFERENCE,

London.

Oct.

of

1984.

Reading

B E R M A N , G.A. (Ed.) 1980.

Testing Laboratory Performance:
Accreditation, NBS
P u b l i c a t i o n 591, National Bureau
Gaithersburg, MD, U.S.A.

E v a l u a t i o n and
of
Standards,

Chemistry Quality Assurance Handbook, Volume 1, Principles, U.S. Department

Agriculture, Food Safety and Inspection Service, Washington, DC, U.S.A.

66

of

D U N C A N , A.J.
1974.
Q u a l i t y C o n t r o l and I n d u s t r i a l
Richard D. Irwin, Inc., Homewood, IL., U.S.A.

Statistics,

4th

Ed.,

G A R F I E L D , F.M. et al (Ed.) 1980. O p t i m i z i n g C h e m i c a l L a b o r a t o r y P e r f o r m a n c e

T h r o u g h the A p p l i c a t i o n of Q u a l i t y A s s u r a n c e P r i n c i p l e s , A s s o c i a t i o n of
Official Analytical Chemists, Arlington, VA, U.S.A.
H O R W I T Z , W.
1981.
A C S S y m p o s i u m S e r i e s No. 1 6 0 , T h e P e s t i c i d e C h e m i s t and
Modern Toxicology, "Analytical M e a s u r e m e n t s : H o w Do You K n o w Your Results Are
Right". American Chemical Society, Washington, DC, U . S . A .
INHORN, S.L. (Ed.) 1977.
Quality Assurance Practices for Health
American Public Health Association, Washington, DC, U.S.A.
JURAN, J.M. & GRYNA, F.M.
J U R A N , J.M.,
McGraw-Hill.

GRYNA,

1980.

Quality

F.M. & B I N G H A M ,

Planning

B.S.

1974.

and Analysis,
Quality

Laboratories,

McGraw-Hill.

Control

Handbook,

SHERMA, J. (Ed.) 1976.

Manual of Analytical Quality Control for Pesticides in
H u m a n and Environmental Media, U.S. Environmental Protection Agency, Research
Triangle Park, NC, U.S.A.
Y O U D E N , W.J. & S T E I N E R , E.H.
1975.
S t a t i s t i c a l M a n u a l of
Association of Official Analytical Chemists, Arlington, VA, U.S.A.

67

the

AOAC,

F A O T E C H N I C A L PAPERS
F A O F O O D A N D N U T R I T I O N PAPERS
1/1
1/2

R e v i e w of f o o d c o n s u m p t i o n surveys 1 9 7 7 Vol. 1. Europe, N o r t h A m e r i c a , Oceania, 1 9 7 7 (E)

R e v i e w of f o o d c o n s u m p t i o n s u r v e y s 1 9 7 7 V o l . 2 . A f r i c a , Latin A m e r i c a , Near East, Far East,
1 9 7 9 (E)

Report of t h e joint F A O / W H O / U N E P c o n f e r e n c e o n
m y c o t o x i n s , 1 9 7 7 (E F S)

Report o f a j o i n t F A O / W H O expert c o n s u l t a t i o n o n
dietary f a t s and oils in h u m a n nutrition,

JECFA s p e c i f i c a t i o n s for i d e n t i t y and purity of

t h i c k e n i n g a g e n t s , a n t i c a k i n g agents,
a n t i m i c r o b i a l s , a n t i o x i d a n t s and emulsifiers,

18 Rev. 1

Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 8 4 (E)

18 Rev. 2

Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 8 7 (E)

18 Rev. 3

Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 9 0 (E)

19

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of

carrier s o l v e n t s , emulsifiers and stabilizers,
e n z y m e preparations, f l a v o u r i n g a g e n t s , f o o d
colours, s w e e t e n i n g agents and o t h e r f o o d
additives, 1 9 8 1 (E F)

20
21
22

Legumes in h u m a n n u t r i t i o n , 1 9 8 2 (E F S)
M y c o t o x i n surveillance - a guideline, 1 9 8 2 (E)
Guidelines for agricultural t r a i n i n g curricula in
A f r i c a , 1 9 8 2 (E F)

23

M a n a g e m e n t of g r o u p f e e d i n g p r o g r a m m e s ,
1 9 8 2 (E F P S)
Food and n u t r i t i o n in t h e m a n a g e m e n t of g r o u p
feeding p r o g r a m m e s , 1 9 9 3 (E F S)
Evaluation o f n u t r i t i o n i n t e r v e n t i o n s , 1 9 8 2 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
b u f f e r i n g agents, salts; e m u l s i f i e r s , t h i c k e n i n g
a g e n t s , stabilizers; f l a v o u r i n g a g e n t s , f o o d
colours, s w e e t e n i n g agents and m i s c e l l a n e o u s
f o o d additives, 1 9 8 2 (E F)
Food c o m p o s i t i o n tables for t h e Near East,

1 9 7 7 (E F S)

1 9 7 8 (E)
5
5 Rev. 1
5 Rev. 2

JECFA - guide t o s p e c i f i c a t i o n s , 1 9 7 8 (E F)
JECFA - guide t o s p e c i f i c a t i o n s , 1 9 8 3 (E F)
JECFA - guide t o s p e c i f i c a t i o n s , 1 9 9 1 (E)

The f e e d i n g of w o r k e r s in developing countries,

1 9 7 6 (E S)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
f o o d c o l o u r s , e n z y m e preparations and other f o o d
a d d i t i v e s , 1 9 7 8 (E F)

W o m e n in f o o d p r o d u c t i o n , f o o d handling and
n u t r i t i o n , 1 9 7 9 (E F S)

A r s e n i c and t i n in f o o d s : r e v i e w s of c o m m o n l y
u s e d m e t h o d s of analysis, 1 9 7 9 (E)

10
11
12

P r e v e n t i o n of m y c o t o x i n s , 1 9 7 9 (E F S)
The e c o n o m i c value of breast-feeding, 1 9 7 9 (E F)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and purity of
f o o d c o l o u r s , f l a v o u r i n g agents and other f o o d
a d d i t i v e s , 1 9 7 9 (E F)

2 3 Rev. 1
24
25

26
27
28

1 9 8 3 (E)
Review of f o o d c o n s u m p t i o n s u r v e y s 1 9 8 1 ,
1 9 8 3 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
b u f f e r i n g agents, salts, e m u l s i f i e r s , stabilizers,
t h i c k e n i n g agents, e x t r a c t i o n s o l v e n t s , f l a v o u r i n g
agents, s w e e t e n i n g agents and m i s c e l l a n e o u s
f o o d additives, 1 9 8 3 (E F)
Post-harvest losses in quality of f o o d grains,
1 9 8 3 (E F)

13

Perspective o n m y c o t o x i n s , 1 9 7 9 (E F S)

14
14/1
1 4 / 1 Rev.1

Manuals of food quality

control:
Food c o n t r o l l a b o r a t o r y , 1 9 7 9 (Ar E)
The f o o d c o n t r o l laboratory, 1 9 8 6 (E)

14/2

A d d i t i v e s , c o n t a m i n a n t s , t e c h n i q u e s , 1 9 8 0 (E)

14/3
14/4

C o m m o d i t i e s , 1 9 7 9 (E)
M i c r o b i o l o g i c a l analysis, 1 9 7 9 (E F S)

30

F A O / W H O f o o d additives d a t a s y s t e m , 1 9 8 4 (E)

3 0 Rev. 1

14/5
14/6
1 4 / 6 Rev.1
14/7

Food
Food
Food
Food

31/1

F A O / W H O f o o d additives data s y s t e m , 1 9 8 5 (E)

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
f o o d colours, 1 9 8 4 (E F)

c o n t a m i n a n t s and c o m p o s i t i o n , 1 9 8 6 (C E)
Food analysis: q u a l i t y , adulteration and t e s t s of

32

14/8

i d e n t i t y , 1 9 8 6 (E)
I n t r o d u c t i o n t o f o o d s a m p l i n g , 1 9 8 8 (Ar C E F S)
T r a i n i n g in m y c o t o x i n s analysis, 1 9 9 0 (E S)
M a n a g e m e n t of f o o d c o n t r o l p r o g r a m m e s ,

33

14/9
14/10
14/11

1 9 9 1 (E)
Q u a l i t y a s s u r a n c e in the f o o d c o n t r o l
m i c r o b i o l o g i c a l laboratory, 1 9 9 2 (E F S)
Pesticide residue analysis in t h e f o o d c o n t r o l
l a b o r a t o r y , 1 9 9 3 (E F)
Q u a l i t y assurance in t h e f o o d c o n t r o l chemical

35

R e v i e w of f o o d c o n s u m p t i o n s u r v e y s 1 9 8 5 ,
1 9 8 6 (E)

36

Guidelines for c a n m a n u f a c t u r e r s and f o o d

canners, 1 9 8 6 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
certain f o o d additives, 1 9 8 6 (E F)

l a b o r a t o r y , 1 9 9 3 (E)
I m p o r t e d f o o d inspection, 1 9 9 3 (E F)
Radionuclides in f o o d , 1 9 9 4 (E)
C a r b o h y d r a t e s in h u m a n nutrition, 1 9 8 0 (E F S)
A n a l y s i s of f o o d c o n s u m p t i o n s u r v e y data for
d e v e l o p i n g c o u n t r i e s , 1 9 8 0 (E F S)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
s w e e t e n i n g a g e n t s , e m u l s i f y i n g agents, f l a v o u r i n g
a g e n t s and other f o o d additives, 1 9 8 0 (E F)
Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 8 1 (E)

38

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of

certain f o o d additives, 1 9 8 8 (E)

39

Quality c o n t r o l in f r u i t and v e g e t a b l e p r o c e s s i n g ,
1 9 8 8 (E F S)
D i r e c t o r y of f o o d and n u t r i t i o n i n s t i t u t i o n s in the
Near East, 1 9 8 7 (E)
Residues of s o m e v e t e r i n a r y d r u g s in animals and
f o o d s , 1 9 8 8 (E)

14/12
14/13
14/14
14/15
14/16
15
16
17

18

inspection, 1981
for e x p o r t , 1 9 7 9
for e x p o r t , 1 9 9 0
analysis: general

(Ar E) (Rev. 1 9 8 4 , E S)
(E S)
(E S)
t e c h n i q u e s , additives,

29

31/2

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of

f o o d additives, 1 9 8 4 (E F)

34

37

40
41
41/2

Residues of v e t e r i n a r y d r u g s in f o o d s ,
1 9 8 5 (E/F/S)
Nutritional implications of f o o d aid: an a n n o t a t e d
bibliography, 1 9 8 5 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
certain f o o d additives, 1 9 8 6 (E F)

Residues of s o m e v e t e r i n a r y d r u g s in animals and

f o o d s . T h i r t y - f o u r t h m e e t i n g of t h e j o i n t
F A O / W H O Expert C o m m i t t e e o n Food A d d i t i v e s ,
1 9 9 0 (E)

41/3

41/4

Residues of s o m e veterinary drugs in animals and

f o o d s . T h i r t y - s i x t h m e e t i n g of the joint F A O / W H O
Expert C o m m i t t e e o n Food A d d i t i v e s , 1 9 9 1 (E)
Residues of s o m e v e t e r i n a r y drugs in animals and

55

Sampling plans for a f l a t o x i n analysis in p e a n u t s

and c o r n , 1 9 9 3 (E)

56

Body m a s s index - A m e a s u r e of c h r o n i c energy

d e f i c i e n c y in adults, 1 9 9 4 (E F S)
Fats and oils in h u m a n n u t r i t i o n , 1 9 9 5 (Ar E F S)

f o o d s . T h i r t y - e i g h t h m e e t i n g of t h e joint
F A O / W H O Expert C o m m i t t e e o n Food A d d i t i v e s ,
1 9 9 1 (E)

57
58

The use of hazard analysis critical c o n t r o l point

(HACCP) principles in f o o d c o n t r o l , 1 9 9 5 (E F S)

41/5

Residues of s o m e veterinary drugs in animals and

59
60

N u t r i t i o n e d u c a t i o n for t h e public, 1 9 9 5 (E F S)
Food f o r t i f i c a t i o n : t e c h n o l o g y and quality c o n t r o l ,
1 9 9 6 (E)

41/6

f o o d s . Fortieth m e e t i n g of t h e J o i n t F A O / W H O
Expert C o m m i t t e e on Food A d d i t i v e s , 1 9 9 3 (E)
Residues of s o m e v e t e r i n a r y drugs in animals and

61
62

B i o t e c h n o l o g y and f o o d s a f e t y , 1 9 9 6 (E)
N u t r i t i o n e d u c a t i o n for t h e public - D i s c u s s i o n
papers of t h e FAO Expert C o n s u l t a t i o n , 1 9 9 6 (E)

63
64

Street f o o d s , 1 9 9 7 (E/F/S)
W o r l d w i d e regulations for m y c o t o x i n s 1 9 9 5 - A
c o m p e n d i u m , 1 9 9 7 (E)
Risk m a n a g e m e n t and f o o d s a f e t y , 1 9 9 7 (E)

f o o d s . F o r t y - s e c o n d m e e t i n g of the J o i n t
F A O / W H O Expert C o m m i t t e e on Food A d d i t i v e s ,
1 9 9 4 (E)
41/7

41/8

Residues of s o m e
f o o d s . Forty-third
Expert C o m m i t t e e
Residues of s o m e

veterinary d r u g s in animals and

m e e t i n g of t h e J o i n t F A O / W H O
o n Food A d d i t i v e s , 1 9 9 4 (E)
veterinary drugs in animals and

41/9

f o o d s . F o r t y - f i f t h m e e t i n g of t h e J o i n t F A O / W H O
Expert C o m m i t t e e o n Food A d d i t i v e s , 1 9 9 6 (E)
Residues of s o m e v e t e r i n a r y drugs in animals and
f o o d s . F o r t y - s e v e n t h m e e t i n g of t h e J o i n t
F A O / W H O Expert C o m m i t t e e o n Food A d d i t i v e s ,
1 9 9 7 (E)

65

Availability: November 1 9 9 7
Ar

Arabic

C
E
F

Chinese
English
French

Multil

Multilingual
Out of print
In preparation

42
42/1

Traditional f o o d plants, 1 9 8 8 (E)

Edible plants of Uganda. The value o f w i l d and

Portuguese

Spanish

43

c u l t i v a t e d plants as f o o d , 1 9 8 9 (E)
Guidelines for agricultural training curricula in A r a b
c o u n t r i e s , 1 9 8 8 (Ar)

44

R e v i e w of f o o d c o n s u m p t i o n s u r v e y s 1 9 8 8 ,

FAO Sales Agents

FAO. Viale delle Terme di Caracalla, 00100Rome,

45
46

1 9 8 8 (E)
Exposure of i n f a n t s and children t o lead, 1 9 8 9 (E)
S t r e e t f o o d s , 1 9 9 0 (E/F/S)

47/1

Utilization of t r o p i c a l f o o d s : cereals, 1 9 8 9 (E F S)

47/2
47/3
47/4

Utilization of t r o p i c a l f o o d s : roots and t u b e r s ,

1 9 8 9 (E F S)
Utilization of t r o p i c a l f o o d s : trees, 1 9 8 9 (E F S)
Utilization o f t r o p i c a l f o o d s : tropical beans,

47/5

1 9 8 9 (E F S)
Utilization of t r o p i c a l f o o d s : t r o p i c a l oil seeds,
1 9 8 9 (E F S)

47/6
47/7
47/8

Utilization of t r o p i c a l f o o d s : sugars, spices and

s t i m u l a n t s , 1 9 8 9 (E F S)
Utilization of t r o p i c a l f o o d s : fruits and leaves,
1 9 9 0 (E F S)
Utilization of t r o p i c a l f o o d s : animal p r o d u c t s ,
1 9 9 0 (E F S)

48

N u m b e r not assigned

49

JECFA s p e c i f i c a t i o n s for i d e n t i t y and purity of

c e r t a i n f o o d additives, 1 9 9 0 (E)

50
51

Traditional f o o d s in the Near East, 1 9 9 1 (E)

Protein quality evaluation. Report of t h e J o i n t
F A O / W H O Expert C o n s u l t a t i o n , 1 9 9 1 (E F)

52/1

C o m p e n d i u m of f o o d additive s p e c i f i c a t i o n s V o l . 1, 1 9 9 3 (E)
C o m p e n d i u m of f o o d additive s p e c i f i c a t i o n s -

52/2

V o l . 2 , 1 9 9 3 (E)
52 Add. 1
52 Add. 2
52 Add. 3
52 Add. 4
52 Add. 5
53
54

C o m p e n d i u m of f o o d additive
A d d e n d u m 1, 1 9 9 2 (E)
C o m p e n d i u m of f o o d additive
A d d e n d u m 2, 1 9 9 3 (E)
C o m p e n d i u m of f o o d additive
A d d e n d u m 3, 1 9 9 5 (E)
C o m p e n d i u m of f o o d additive
A d d e n d u m 4 , 1 9 9 6 (E)

specifications specifications specifications specifications -

C o m p e n d i u m of f o o d additive s p e c i f i c a t i o n s A d d e n d u m 5, 1 9 9 7 (E)
M e a t and m e a t p r o d u c t s in h u m a n n u t r i t i o n in
d e v e l o p i n g c o u n t r i e s , 1 9 9 2 (E)
N u m b e r not assigned

The FAO Technical Papers are available

or directly

through

the

authorized

from Sales and Marketing

Italy

Group,

- --

'

'

'

- - -

'

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ISBN 92-5-102489-8

9
M

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7 8 9 2 5 1

ISSN 0254-4725

0 2 4 8 9 8
T0432E/2/9.97/500

ISSN 0254-4725

Manuals of food
quality control
1. The food control laboratory

FAO
FOOD AND
NUTRITION
PAPER

Rev. 1

Food
and
Agriculture
Organization
of
the
United
Nations

Manuals of food
quality control
1. The food control laboratory

FAO
FOODAND
NUTRITION
PAPER

14/1

Rev. 1

by
P.G. Martin

revised by
J. Weatherwax

and
P.G. Martin

p r e p a r e d with the support of the

S w e d i s h International Development Authority (SIDA)

Food
and
Agriculture
Organization
of
the
United
Nations

Rome, 1997

Reprinted 1997

The designations employed and the presentation of material in this

publication do not imply the expression of any opinion whatsoever on
the part of the Food and Agriculture Organization of the United
Nations concerning the legal status of any country, territory, city or
area or of its authorities, orconcerning the delimitation of its frontiers
or boundaries.

M-87
ISBN 92-5-102489-8

All rights reserved. No part of this publication may be reproduced, stored in a

retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying or otherwise, without the priorpermission of the copyright owner.
Applications for such permission, with a statement of the purpose and extent of the
reproduction, should be addressed to the Director, Information Division, Food and
Agriculture Organization of the United Nations, Viale delle Terme di Caracalla,
00100 Rome, Italy.
FAO 1986

FOREWORD

T h e c o n t r o l of food safety and quality is an integral part of n a t i o n a l

programmes for development.
National food control systems are designed to
protect the health and welfare of the consumer, to promote the development of
trade in food and food products, and to protect the interests of the fair and
h o n e s t food p r o d u c e r , processor or m a r k e t e r against dishonest and unfair
competition.
Emphasis is placed on the prevention of chemical and biological
hazards which result from contamination, adulteration or simple mishandling of
foods.
Also important are the maintenance of general food quality and the
control of the use of food additives and food processing procedures.
In order
must :

to

establish

a workable

food

control

system,

national

government

1.

Enact food control legislation.

2.

Promulgate regulations to enforce that legislation.

3.

Create an agency to cond uct the enforcement.

4.

Establish food inspection

agencies concerned.

5.

Provide physical facilities including a food control laboratory.

and

analysis

staff

within

the

agency

or

To assist the national governments of developing countries in this process, FAO,

with the support of the Swedish International Development Authority (SIDA) has
published the series Manuals of Food Quality Control. These are incorporated as
part of the FAO Food and Nutrition Paper Series No. 14, and include:
No. 14/1 rev. 1

The Food Control Laboratory (revised, 1986)

No. 14/2

Additives, Contaminants, and Techniques

by No. 14/7)

No. 14/3

Commodities (replaced by No. 14/8)

No. 14/4

Microbiological Analysis

No. 14/5

Food

No. 14/6

Food for Export

No. 14/7

Food Analysis: General Techniques, Additives,

Contaminants, and Composition

No. 14/8

Food Analysis:
Identity

(replaced

Inspection

Quality, Adulteration, and Tests of

In a d d i t i o n , FAO, WHO and UNEP jointly have published many guidelines and other
documents designed to further assist developing countries in forming adequate
food control systems. These publications include:
Methods of Sampling and Analysis of Contaminants in Food A Report of the Second Joint FAO/WHO Expert Consultation,
Rome - 1978
Guidelines for Establishing or Strengthening National Food
C o n t a m i n a t i o n M o n i t o r i n g Programmes - FAO Food Control
Series No. 5 - 1979

iii

Guidelines for the Study of Dietary Intakes of Chemical

Contaminants - WHO Offset Publication No. 87 - 1985
Guide
to
Codex
Recommendations
concerning
Residues, Part 2 - Maximum Limits for Pesticide
Second Preliminary Issue - Rome - 1985

Pesticide
Residues,

Recommended Practices for the Prevention of Mycotoxins in

F o o d , Feed and their Products - FAO Food and N u t r i t i o n
Paper No. 10, Rome - 1979
Food Standards, Codes of Practice and Methods of Analysis
Recommended by the Codex Alimentarius Commission - Joint
FAO/WHO Food Standards Programme (several titles)
Food Additive Evaluations and Specifications of Purity and
I d e n t i t y - Reports and M o n o g r a p h s of the Joint F A 0 / W H 0
Expert Committee on Food Additives (several titles)
The above publications, and others, are available to persons and organizations.
FAO
is also
interested
in receiving
comments
regarding
this volume
and
suggestions for future improvement. Please send to:
The Chief
Food Quality and Standards Service
Food Policy and Nutrition Division
Food and Agriculture Organization of the
United Nations
Via delle Terme di Caracalla
00100 Rome, Italy
FAO wishes
Development
of M r . J.*
preparation

to acknowledge the generous support of the Swedish International

Authority (SIDA), in the preparation of this volume, and the efforts
W e a t h e r w a x and M r . P.G. Martin who were responsible for the
of the text.

TABLE OF CONTENTS

FOREWORD

1.

SCOPE OF THE FOOD CONTROL LABORATORY MANUAL

2.

LABORATORY
2.1
2.2
2.3
2.4
2.5
2.6
2.7

3.

Establishing the Laboratory

Organizational Structure
Head of the Laboratory
Supervisors
Team Leaders
Analytical Staff
Support Staff

2
3
3
4
5
5
6

General Considerations
Basic Structure of the Building
Safety Features
Ventilation and Air Conditioning
Space Utilization
Equipment and Instruments
Utilities
Design References

7
7
10
12
13
15
16
18

LABORATORY ADMINISTRATION
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9

5.

ORGANIZATION

LABORATORY DESIGN
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8

4.

Sample Collection
Sample Receipt and Assignment
Sample Storage and Disposal
Budget
Purchasing
Supplies Management
Equipment Maintenance
Housekeeping
Training

LABORATORY
5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8

20
21
22
23
23
26
26
28
28

OPERATIONS

Workp lans
Priorities for Analysis
Analysis Assignment
Analysis Control
Analysis Reporting
Analysis Review
Method Validation
Confirming Analysis

. . . . .

29
31
31
32
32
33
34
34

6.

LABORATORY
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.8

7.

SAFETY

The Safety Programme

Basic Safety Rules
Fire Safety
Chemical Hazards
Biological Hazards
Physical Hazards
Safety and Emergency Equipment
First Aid

LABORATORY QUALITY ASSURANCE

7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8

35
35
36
37
38
40
42
43

(QA)

Introduction
Establishing a QA Programme
QA of Reference Standards
QA of Instruments
QA of Analytical Reports
Check Sample Examination
Other QA Activities
Text References

46
46
49
. . 55
58
61
66
66

vi

1.

SCOPE OF THE FOOD CONTROL LABORATORY M A N U A L

This m a n u a l is p r i m a r i l y a p r a c t i c a l h a n d b o o k on the e s t a b l i s h m e n t of a food

control laboratory.
The v a r i o u s organizational, administrative, operational,
and d e s i g n c r i t e r i a are d i s c u s s e d in s o m e d e t a i l .
A l s o i n c l u d e d is a
discussion of laboratory safety to stress the importance of safe operation and
the inherent hazards always present in an analytical laboratory.
The manual is designed for laboratory management and administration personnel,
but the o p e r a t i n g a n a l y s t can g a i n good i n f o r m a t i o n and i n s i g h t s into the
problems involved in establishing and operating a food control laboratory.
The u s e r of this m a n u a l should a l w a y s k e e p in m i n d that the i n f o r m a t i o n and
principles presented are advisory only and represent recommendations on how a
food control laboratory may be organized, arranged, etc., not how it must be.
This manual is intended as a guide, to help a new laboratory get off to a good
s t a r t , or to g u i d e an e s t a b l i s h e d l a b o r a t o r y in w h i c h w o r k is e x p a n d i n g and
diversifying.
As time goes by, experience builds up and a laboratory tends to
develop new methods, modify existing ones or adapt them to other products.
All
this valuable information should be retained and, if possible, combined with
this manual and manuals No. 14/2 and 14/3 in a readily accessible form. At the
s a m e t i m e , the a n a l y s t m u s t r e m e m b e r that r e l i a b l e r e s u l t s w i l l o n l y be
o b t a i n e d by s t r i c t a d h e r e n c e to the d e t a i l s that m a t t e r and to c a r e f u l and
professional work. Analytical chemistry is an exact science, very demanding on
the manipulative skills of the worker at the bench. There is no substitute for
e x p e r i e n c e but it is hoped this m a n u a l w i l l form a u s e f u l guide w h i l e that
experience is developing as well as during routine laboratory operations.
Any
c o m m e n t s or s u g g e s t i o n s for i m p r o v e m e n t s w i l l be w e l c o m e .
T h e s e should be
addressed to the address given in the Foreword.
The first e d i t i o n of this m a n u a l w a s w r i t t e n in 1977 by Mr. Peter G. M a r t i n ,
p r e s e n t l y of L y n e , M a r t i n and R a d f o r d , P u b l i c A n a l y s t s , R e a d i n g , B e r k s h i r e ,
England.
The p r e s e n t r e v i s e d e d i t i o n has b e e n p r e p a r e d w i t h Mr. M a r t i n ' s
support and assistance by Mr. John Weatherwax, retired Laboratory Director for
the United States Food and Drug Administration, Los Angeles, California, USA.

2.

2.1

Establishing

the

LABORATORY

ORGANIZATION

Laboratory

The publication, "Guidelines for Developing an Effective National Food Control

System", F A O / W H O / U N E P , FAO, Rome, 1976, details the formation of a food control
system embodied in a national food quality control service.
The purposes of a
n a t i o n a l food q u a l i t y c o n t r o l s e r v i c e are to e n s u r e a s u p p l y of s a f e ,
nutritious and honestly presented food; to protect consumers from foods which
are c o n t a m i n a t e d , decomposed, adulterated, injurious or packaged or labelled in
a false or misleading way; to promote better quality control of foods by food
p r o c e s s o r s and d i s t r i b u t o r s and t h e r e b y e n c o u r a g e d e v e l o p m e n t of the food
i n d u s t r y and to i m p r o v e e x p o r t p o t e n t i a l and e n a b l e b e t t e r c o n t r o l of food
import s.
When consumers and buyers have confidence in the quality and safety of foods,
trade increases at both local and international levels.
Increased local demand
e n c o u r a g e s i n d u s t r y and i n t e r n a t i o n a l t r a d e brings better returns in foreign
exchange capital.
T h i s c a n a l s o lead to n a t i o n a l d i e t s b e c o m i n g m o r e v a r i e d
and n u t r i t i o u s w i t h l o c a l p r o d u c t s o f t e n s u b s t i t u t e d for c o s t l y i m p o r t s .
B e s i d e s the o b v i o u s e c o n o m i c and p u b l i c h e a l t h b e n e f i t s , the a d v a n t a g e s in
social terms can also be considerable.
In m a n y g o v e r n m e n t s t r u c t u r e s t h e r e are s t a f f and f a c i l i t i e s l o c a t e d in
d i f f e r e n t a g e n c i e s that a r e i n v o l v e d in s o m e or all a s p e c t s of food c o n t r o l ,
b u t t h e i r e f f o r t s are o f t e n not h i g h l y e f f e c t i v e due to lack of f a c i l i t i e s ,
expertise or an adequate legal or a d m i n i s t r a t i v e f r a m e w o r k .
These resources
s h o u l d be b r o u g h t t o g e t h e r into a u n i f i e d s t r u c t u r e in such a w a y that the
p e r s o n n e l a r e b e s t u t i l i z e d and h a v e c l e a r o b j e c t i v e s w i t h the f a c i l i t i e s to
c a r r y t h e m out.
T h e r e s u l t w o u l d be a p r o p e r l y l i n k e d i n s p e c t o r a t e and
l a b o r a t o r y w i t h the n e c e s s a r y a d m i n i s t r a t i v e and l e g a l s u p p o r t i n c l u d i n g ,
w h e n e v e r possible, an Advisory Board to provide guidance and coordination at
national l e v e l .
This manual deals only with the establishment of the food control laboratory,
a l t h o u g h it is o n l y o n e c o m p o n e n t of a n a t i o n a l food c o n t r o l s e r v i c e .
It
laboratory
there must
be a
should
be n o t e d
that
f o r an e f f e c t i v e
correspondingly effective inspectorate.
In a f e w c o u n t r i e s t h e r e is no
p r o v i s i o n for an i n s p e c t o r a t e and s a m p l e s are o f t e n o b t a i n e d by the a n a l y s t ,
thereby using potential analytical time.
Having samples submitted by the food
industry saves sample collection time, but is inherently a bad practice because
the samples cannot be assured of being representative.
A food c o n t r o l l a b o r a t o r y is a c o s t l y f a c i l i t y to e s t a b l i s h , so b e s t r e s u l t s
will be achieved if the functions of the laboratory are confined to activities
r e s u l t i n g f r o m the e n f o r c e m e n t of food l a w , g e n e r a l s u r v e y s on q u a l i t y of
f o o d s , e x p o r t / i m p o r t i n s p e c t i o n w o r k and w o r k of an i n v e s t i g a t i o n a l n a t u r e
relating to food quality.
However, it may, for reasons of economy and o p t i m u m
u t i l i z a t i o n of the f a c i l i t i e s , b e c o m e n e c e s s a r y to t a k e up o t h e r s e l e c t e d
analytical work provided the laboratory is appropriately equipped.
Advice or
a n a l y s i s on a fee b a s i s to l o c a l i n d u s t r y m a y be j u s t i f i e d if t h i s d o e s n o t
conflict with statutory duties or other government bodies and there are clear
guidelines.
Such analyses are carried out for advisory purposes and in no way
are a substitute for normal food control work.

2.2

Organizational

The staffing

Structure

structure

of a typical

food

Head of

Analytical
Staff

control

laboratory

is as

follows:

Laboratory

Support
Staff

Administrative
Staff

The o f f i c e of Head of L a b o r a t o r y ( o t h e r t i t l e s such as " C h i e f " or " D i r e c t o r "

a r e o f t e n u s e d ) m a y i n c l u d e a D e p u t y if the l a b o r a t o r y s t a f f is s u f f i c i e n t l y
large.
U s u a l l y , h o w e v e r , the d u t i e s of the H e a d , in h i s or her a b s e n c e , are
assumed by a senior supervisor of the analytical staff.
The analytical and support staffs are discussed b e l o w in Sections 2.6 and 2.7,
respectively.
The administrative staff includes all administrative assistance
such as a s e c r e t a r y , t y p i n g and f i l i n g c l e r k s , a m a n a g e m e n t a s s i s t a n t and a
librarian (if the laboratory library is of a size to need one).
Basically the
a d m i n i s t r a t i v e s t a f f are t h o s e p e r s o n s g e n e r a l l y i n v o l v e d in " o f f i c e " or
"paperwork" functions.
This staff is very important to the smooth operation of
a laboratory.
It is false e c o n o m y to u n d e r s t a f f the a d m i n i s t r a t i v e g r o u p
because their work often m u s t then be done in part by the analytical or support
staffs .
The secretary for the laboratory generally works directly for the Head.
good practice, h o w e v e r , to m a k e the secretary responsive to secretarial
of the supervisors.

2.3

Head

of the

It is
needs

Laboratory

The H e a d of the l a b o r a t o r y s h o u l d be a g r a d u a t e c h e m i s t or m i c r o b i o l o g i s t
trained in food analysis.
A postgraduate d i p l o m a particularly relevant to this
w o r k is h i g h l y d e s i r a b l e .
A l t h o u g h the d u t i e s of the h e a d of the l a b o r a t o r y
are m a n y , s o m e m a y be d e l e g a t e d and o t h e r s u n d e r t a k e n b y o t h e r p a r t s of the
food control administration.
It is therefore not appropriate to do more than
d r a w a t t e n t i o n to c e r t a i n a s p e c t s .
The o b j e c t i v e of the l a b o r a t o r y is to
analyze a large number of samples correctly, quickly and cheaply.
This means
t h a t a t t e n t i o n m u s t be paid to c a r e f u l s p e n d i n g of the b u d g e t , p r o m o t i o n of
good staff relations and maintenance of the highest possible level of technical
efficiency and expertise.
The laboratory Head may have to give evidence in court or write documents used
in c o u r t , in w h i c h c a s e he m u s t h a v e a t h o r o u g h u n d e r s t a n d i n g of food and
related law and court procedure.
There will also be involvement in c o m m i t t e e
work and relations with other organizations.
The laboratory Head is usually
the spokesman for the laboratory in many instances.
The Head must prepare work
p l a n s w i t h the i n s p e c t o r a t e and o v e r a l l food c o n t r o l a u t h o r i t i e s .
Sampling
p l a n s a g r e e d w i t h the i n s p e c t o r a t e s h o u l d aim at a r e a s of c o n c e r n and m a j o r
abuses.
In the e a r l i e r y e a r s or w h i l e the l a b o r a t o r y r e m a i n s s m a l l , the Head of the
laboratory is the one who makes most of the m a n a g e m e n t decisions.
The Head is
also the person who interacts with higher m a n a g e m e n t .
This is a most important
aspect as the laboratory m u s t be fully integrated into the executive s tructure
in a m e a n i n g f u l w a y .
It w o u l d be f u t i l e for a l a b o r a t o r y to w o r k in an
administrative v a c u u m , producing r e s u l t s s h o w i n g , for e x a m p l e , that s a m p l e s

were contaminated or that there were consignments of food in the distribution

c h a i n r e q u i r i n g r e g u l a t o r y a c t i o n , if the food c o n t r o l o r g a n i z a t i o n and
i n s p e c t o r a t e took no a c t i o n , or if a t t e m p t e d a c t i o n w a s c o u n t e r m a n d e d at a
h i g h e r level.
The e x e c u t i v e a r m of the g o v e r n m e n t in this a r e a , the food
c o n t r o l s e r v i c e , n e e d s the s a n c t i o n and s u p p o r t of m o r e senior levels of the
administration.
To play an effective role, the Head of the laboratory must be
assured of necessary finance, staff and facilities.
When difficulties arise in
the supply of these three essential ingredients, it must be possible to bring
these difficulties to the attention of persons in positions of higher authority
for appropriate action.

2.4

Supervisors

S u p e r v i s o r s s h o u l d a l s o be g r a d u a t e c h e m i s t s or m i c r o b i o l o g i s t s w i t h
considerable food analysis experience.
The supervisor is the on-site manager
of the laboratory.
Having supervisors assigned to specific units or areas of
work permits the Head to more effectively plan (and execute) the total workload
of the laboratory.
S u p e r v i s o r s can be e x p e c t e d to do a n a l y t i c a l w o r k in a d d i t i o n to their
supervisory duties.
H o w e v e r , if their g r o u p e x c e e d s five p r o f e s s i o n a l
a n a l y s t s , it is best not to r e q u i r e a d d i t i o n a l a n a l y t i c a l w o r k e x c e p t for
occasional problem solving and trouble-shooting.
A reasonable m a x i m u m number
of a n a l y s t s for one p e r s o n to s u p e r v i s e is 10 to 12. T h i s can be m o r e if n o n professional support staff is added.
A supervisor's duties can include many or all of the
1.
Assisting the Head in overall
the work of the group supervised.
2.

posed

Receiving

and assigning

samples

laboratory

5.
Ensuring
do the work.

the

that

reports

the

of

6.
Ensuring that proper
followed by the group.

work

the necessary

laboratory

planning

in s o l v i n g

completed

group has

work

for analysis, within

3.
A n s w e r i n g q u e s t i o n s and a s s i s t i n g
by individual analysts.

4.
Reviewing
recommendations.

following:

and

and

the group.

analytical

making

supplies

planning

and

safety and housekeeping

problems

appropriate

equipment

practices

to

are

7.
R e c o m m e n d i n g to the Head n e w i n s t r u m e n t s or e q u i p m e n t n e e d e d , and
training needs of individual analysts.
8.
Taking appropriate disciplinary
laboratory rules or regulations.
9.

Acting

to manage the entire

action

laboratory

when

needed

to

enforce

in the absence of the Head.

Supervisors should train one or more analysts in their group to serve as backups, to supervise the group in the supervisor's absence.
The back-ups should
be given some formal classroom training in supervision in addition to on-thejob experience.
A good supervisor is indispensable to the smooth operation of a laboratory.
In
s e l e c t i n g a s u p e r v i s o r , the Head m u s t k e e p in m i n d that the p r i m a r y job of a
s u p e r v i s o r is to m a n a g e , so that s k i l l s in w o r k i n g w i t h p e o p l e are m o r e
i m p o r t a n t than s c i e n t i f i c e x p e r t i s e .
T h e r e f o r e , a top a d m i n i s t r a t o r w i t h

m e d i o c r e science ability is m o s t often a better choice than a top scientist w h o

is only a m e d i o c r e (or bad) a d m i n i s t r a t o r .
(This p r i n c i p l e h o l d s even m o r e for
s e l e c t i o n of the H e a d of the l a b o r a t o r y . )
O f t e n the b e s t a n a l y s t s are g i v e n
s u p e r v i s o r jobs as a r e w a r d for their b e n c h e x p e r t i s e .
T h i s not only r e m o v e s
t h e m (at l e a s t in p a r t ) f r o m t h e i r m o s t v a l u a b l e r o l e as a n a l y s t , b u t it a l s o
puts them in the o f t e n u n c o m f o r t a b l e role of s u p e r v i s o r .
This can result in an
overall d e c r e a s e in that i n d i v i d u a l ' s e f f e c t i v e n e s s .
T h i s is n o t to s a y t h a t a t o p a n a l y s t c a n n o t b e a t o p s u p e r v i s o r ,
many
fortunate o r g a n i z a t i o n s have such persons.
They are rare, h o w e v e r , and a Head
selecting a supervisor s h o u l d be w i l l i n g
to a c c e p t
lesser
scientific
c r e d e n t i a l s if the other attributes rank s u f f i c i e n t l y high.

2.5

Team

Leaders

A n o t h e r i m p o r t a n t , and o f t e n o v e r l o o k e d , p o s i t i o n is T e a m L e a d e r .
A team
leader is a senior analyst w h o h a s b e e n assigned a s m a l l g r o u p , u s u a l l y no m o r e
t h a n 4 , to do a s p e c i f i c
t a s k or t y p e of a n a l y s i s .
T h e l e a d e r h a s no
s u p e r v i s o r y functions as such, but is the c o o r d i n a t o r of the g r o u p ' s a c t i v i t i e s
and is the contact point for the supervisor.
T e a m l e a d e r s are m o s t u s e f u l w h e n a l a r g e n u m b e r of a r e p e t i t i v e type of
a n a l y s i s is to be done in a specified period of time.
This could be a specific
a n a l y t i c a l s u r v e y or a n e m e r g e n c y p u b l i c h e a l t h p r o b l e m r e q u i r i n g s c r e e n i n g
analyses.
T h e l e a d e r u s u a l l y w o r k s a l o n g w i t h the g r o u p in a d d i t i o n to the
coordinative function.
S u c h e x p e r i e n c e is o f t e n u s e f u l to d e t e r m i n e if t h e
assigned leader has potential as a future supervisor.

2.6

Analytical

Staff

The basic job of the analytical staff is to analyze the s a m p l e s received and to
issue a report.
They m a y also be required to a p p e a r in court as fact or expert
w i t n e s s e s to give e v i d e n c e in r e l a t i o n to a report.
They m a y also be called on
to o f f e r a d v i c e to i n d u s t r y and t r a d e , to a s s i s t in i m p r o v e m e n t o f f o o d
q u a l i t y , or advise on c o n f o r m i t y w i t h s t a n d a r d s or other legal r e q u i r e m e n t s .
T h i s c a n i n v o l v e t h e l a b o r a t o r y s t a f f in f a c t o r y v i s i t s a n d e v e n r e q u e s t s to
c a r r y out e x p e r i m e n t a l w o r k .
W h e t h e r or n o t the l a b o r a t o r y u n d e r t a k e s s u c h
w o r k w i l l be a m a t t e r of o r g a n i z a t i o n a l policy.
The d e c i s i o n w i l l depend on a
n u m b e r of f a c t o r s , i n c l u d i n g the a v a i l a b i l i t y of a l t e r n a t i v e facilities, the
n a t u r e of i n d i v i d u a l o w n e r s h i p ,
etc.
T h e i n t e g r i t y of the a n a l y s t
is
p a r a m o u n t , and s u p e r i o r s m u s t be i n f o r m e d of a n y c o n f l i c t of i n t e r e s t t h a t
a r i s e s . A s in t h e c a s e o f f o o d i n s p e c t o r s , it is p r o p e r f o r t h e a n a l y s t s to
have no vested interest in regulated industries.
This r e q u i r e m e n t is m a n d a t o r y
in m a n y countries.
A n a l y t i c a l staff can be d r a w n from three levels, u n i v e r s i t y g r a d u a t e s , trained
t e c h n i c i a n s f r o m t e c h n i c a n t r a i n i n g c o l l e g e s and u n q u a l i f i e d s t a f f w h o h a v e
received o n - t h e - j o b training.
The g r a d u a t e s can be c h e m i s t s , m i c r o b i o l o g i s t s ,
food scientists or fi od t e c h n o l o g i s t s .
U n i v e r s i t y d e g r e e s are only a starting
q u a l i f i c a t i o n and the-p. w i l l still be a r e q u i r e m e n t for specialized training
a n d e x p e r i e n c e in f o o d . n a l y s i s .
S t a f f s h o u l d be e n c o u r a g e d to c o n t i n u e to
w o r k for s u i t a b l e p o s t g r a d u a t e q u a l i f i c a t i o n s to e n a b l e t h e m to c o m p e t e for
h i g h e r posts in the laboratory.
S p e c i a l l y trained l a b o r a t o r y t e c h n i c i a n s w h o
h a v e f o l l o w e d a t w o to t h r e e y e a r p r a c t i c a l t r a i n i n g c o u r s e in l a b o r a t o r y
a n a l y s i s a f t e r c o m p l e t i n g s e c o n d a r y s c h o o l c a n be p a r t i c u l a r l y u s e f u l in
carrying out a n u m b e r of routine or even h i g h l y c o m p l e x food analyses.
As in
the c a s e w i t h u n i v e r s i t y g r a d u a t e s , s p e c i a l i z e d o n - t h e - j o b t r a i n i n g w i l l b e
needed for particular types of food analysis.

S o m e people w i t h little or no theoretical b a c k g r o u n d often s h o w m a n i p u l a t i v e

a n d p r a c t i c a l s k i l l s in t h e l a b o r a t o r y as g o o d or b e t t e r t h a n u n i v e r s i t y
graduates.
This type of person is often m o r e happy and fulfilled in carrying
out c e r t a i n r o u t i n e l a b o r a t o r y tasks than are graduates.
E v e r y a t t e m p t should
be m a d e to e n c o u r a g e s u c h p e r s o n n e l in t h e i r w o r k and the l a b o r a t o r y H e a d
s h o u l d a t t e m p t to s e t u p p a y s c a l e s a n d o t h e r i n c e n t i v e s to r e w a r d
such
workers.
T h e s e w o r k e r s m a y a l s o be e n c o u r a g e d to t a k e c o u r s e s and o b t a i n
q u a l i f i c a t i o n s in p r a c t i c a l a s p e c t s o f the w o r k , s u c h as
glass-blowing,
i n s t r u m e n t r e p a i r , e l e c t r o n i c s , m e t a l - w o r k and o t h e r f i e l d s r e l a t e d to the
m a i n t e n a n c e of l a b o r a t o r y e q u i p m e n t .
These skills are o f t e n scarce, and just
as d i f f i c u l t to m a s t e r , as t h o s e of the g r a d u a t e a n a l y s t and t h e r e is e v e r y
j u s t i f i c a t i o n for r e w a r d i n g their a c c o m p l i s h m e n t .
It is m o s t i m p o r t a n t that
staff e m p l o y e d for repair o p e r a t i o n s are qualified and t h o r o u g h l y trained.
In
p a r t i c u l a r , e l e c t r o n i c e q u i p m e n t s h o u l d be s e r v i c e d and r e p a i r e d only by
qualified i n s t r u m e n t a t i o n technicians.

2.7

Support

Staff

T h e s u p p o r t s t a f f of a l a b o r a t o r y a r e all of t h o s e p e r s o n s w o r k i n g in and for

the l a b o r a t o r y w h o are not c o n d u c t i n g
a n a l y s e s or are n o t i n v o l v e d
in
a d m i n i s t r a t i v e duties.
S o m e e x a m p l e s of duties include:
1.

Glassware

washing.

2.

Cleaning

and

3.

Disposal

of s a m p l e

4.

Pest

control.

5.

Heavy

lifting

housekeeping

and

maintenance.

reserves

( w h e n no

longer

required).

moving.

Support staff t y p i c a l l y have little or no e d u c a t i o n a l q u a l i f i c a t i o n s beyond

a b i l i t y to read and w r i t e .
H o w e v e r , they m u s t be w i l l i n g and able to learn
o n l y their d u t i e s , but also laboratory safety p r o c e d u r e s .

the
not

It is m o s t i m p o r t a n t t h a t s u f f i c i e n t p e r s o n s a r e h i r e d as s u p p o r t .
The w o r k
t h e y do m u s t be d o n e by s o m e o n e and t h i s is u s u a l l y an a n a l y s t or t e c h n i c i a n
w h e n there is i n s u f f i c i e n t support staff.
There is no fixed m o d u l e for n u m b e r s
of s u p p o r t w o r k e r s , b u t 1 5 - 2 0 % of the n u m b e r of a n a l y t i c a l s t a f f is o f t e n
sufficient.

3.

3.1

LABORATORY DESIGN

General Considerations

W h e n a new laboratory is being built, two people hold the key positions in
producing the right building at the right cost - the architect who designs it
and guides its construction, and the analyst (preferably the laboratory Head)
w h o explains the technical needs, and w o r k s in close p a r t n e r s h i p w i t h the
architect through every stage so that the end result is properly suited to the
requirements of the users.
It is not often that the analyst has the chance to
take part in the planning of a complete new laboratory, more usually he has to
make do with old or inadequate buildings. However, these are often more easily
extended, changed or adapted as the nature of the w o r k changes, than a n e w e r
building, so may in some ways be more advantageous.
Indeed, an important point
in designing a new laboratory is that provision should be made for future
expansion, however unlikely that may seem at the time. The design should also
be left as flexible as possible so that changes of emphasis in the work can be
a c c o m m o d a t e d . The laboratory should be located a w a y from urban centres and
industrial areas in order to minimize problems of contamination.
The information in this chapter was taken in part from Industrial Research and
D e v e l o p m e n t N e w s , VII No. 3, UN, N.Y., 1975.
The principles given apply to
food control l a b o r a t o r i e s in general, w h e t h e r n e w c o n s t r u c t i o n or space
converted to laboratory use.

3.2

Basic Structure of the Building

An example of the smallest laboratory that would be adequate for a food control
programme is shown in Figure 3.1. This design was originally intended to serve
120,000 people although in general this may be regarded as too small a
p o p u l a t i o n to justify a separate laboratory.
It is intended to be part of a
larger b u i l d i n g , but the disposition of r o o m s can be changed to suit local
c i r c u m s t a n c e s . Space for essential services such as solvent storage and the
usual administrative support must also be provided.
Sample preparation should
be carried out as far as possible from laboratories working on trace analysis
and microbiology or using sensitive instruments.
It must be stressed that the
figure s h o w n is only an e x a m p l e .
New l a b o r a t o r i e s m u s t be c u s t o m - b u i l t to
cater for the needs of the situation under consideration.
It is best to allow l a b o r a t o r i e s to r e m a i n o p e n - p l a n as far as p o s s i b l e ,
including the areas used as offices. Exceptions are areas where the activities
carried out cause c o n t a m i n a t i o n or are sensitive to it, such as s a m p l e
preparation, weighing, microbiology, trace analysis and use of instruments such
as gas-liquid chromatographs and spectrophotometers.
Lack of v i b r a t i o n is important and therefore concrete is a better structural
m a t e r i a l in m u l t i - s t o r e y
buildings.
S t e e l - f r a m e b u i l d i n g s m a y cause
d i f f i c u l t y with some i n s t r u m e n t s .
A two storey laboratory adequate for a
modest food control programme is shown in Figures 3.2 and 3.3. It consists of
a ground floor m a i n l y composed of offices and services and a first floor for
analytical work.
In addition there should be a flammable solvent storage area
separate from the building. W o r k s h o p and g l a s s b l o w i n g facilities are often
advantageous and if not otherwise available should be included.

1 ni i

>

Food
additives
and
toxicants

Food
standards
and nutrition
Corridor

Overall
length
21 m

Microbiology

Media
prparai ion

Office
Balance
room

Sample
prparai ion

1vK
Entrance
6.2 m

6.2 m

Figure 3.1
A Minimum Sized Food Control Laboratory

Figure 3.2
Ground Floor Plan
(mainly office and administrative

space)

Figure 3.3
First Floor Plan
(laboratory space)

3.3

Safety

Features

The building
including :
1.

The

and

laboratory

fire

design

should

a r e a s of c o r r i d o r s

include

a number

s h o u l d be f o r m e d

of

safety

of c o n c r e t e

features

blocks.

2.
Services should include a shower sprinkler system near each d o o r w a y
so t h a t a w o r k e r c a n t a k e an i m m e d i a t e s h o w e r , c l o t h e s and a l l , in the c a s e of
a c c i d e n t a l g e n e r a l c o n t a c t w i t h c o r r o s i v e or p o i s o n o u s l i q u i d s or f i r e .

10

3.
wash

There

stations

should

be

(obtainable

built-in
from

most

eye

wash

chemical

fountains,
supply

or

at

least

portable

eye

firms).

4.
The t r a f f i c
flow,
the e g r e s s p a t t e r n and the p r o p o r t i o n s of
the
l a b o r a t o r y are a l l s a f e t y c o n s i d e r a t i o n s .
I t m u s t a l w a y s be p o s s i b l e to l e a v e
the l a b o r a t o r y s a f e l y i r r e s p e c t i v e of the i n i t i a l s i t e of a f i r e .
Serious
t h o u g h t m u s t be g i v e n to t h e n u m b e r and l o c a t i o n o f f i r e e x t i n g u i s h e r s
and
s t a n d p i p e s y s t e m s , and to the a v a i l a b i l i t y of s p r i n k l e r
systems.
5.
L a b o r a t o r i e s s h o u l d b e w e l l - l i t so t h a t t h e o p e r a t o r d o e s n o t h a v e
to p e e r too c l o s e l y o v e r p o t e n t i a l l y h a z a r d o u s m a t e r i a l i n o r d e r to see w h a t he
is doing.
T h e r e s h o u l d be a m p l e w o r k i n g s p a c e and b e n c h t o p s and o t h e r s u r f a c e s
s h o u l d be k e p t c l e a r of a l l m a t e r i a l e x c e p t t h a t i n c u r r e n t u s e .
6.
Benches are best w i t h o u t s h e l v e s , only s e r v i c e s , these being operated
from the f r o n t so t h a t the o p e r a t o r d o e s not h a v e to s t r e t c h a c r o s s the b e n c h .
I t i s s t i l l common to s e e r e a g e n t s on s h e l v i n g at t h e b a c k o f b e n c h e s ( o r a b o v e
the c e n t r e of d o u b l e - w i d t h b e n c h e s ) b u t i t i s p r o b a b l y s a f e r i f such r e a g e n t s
c a n be k e p t on s i d e - s h e l v e s or i n t r a y s w h i c h a r e b r o u g h t to t h e b e n c h as
required .
7.
F l o o r i n g n e e d s to b e o f a n o n - s l i p m a t e r i a l , r e s i s t a n t to a c i d s a n d
s o l v e n t s , b u t n o t so h a r d a s to b e t i r i n g to s t a n d on f o r a f e w h o u r s at a
time.
No m a t e r i a l i s e n t i r e l y s a t i s f a c t o r y .
W e l l - l a i d l i n o l e u m and a f i l l e d
e p o x y r e s i n on top of c o n c r e t e a r e a m o n g t h e b e s t a v a i l a b l e .
It is a d v i s a b l e
n o t to p o l i s h l a b o r a t o r y
floors.
8.
P o l l u t a n t s g e n e r a t e d w i t h i n t h e l a b o r a t o r y m u s t be r e m o v e d s a f e l y ,
q u i c k l y and e f f i c i e n t l y .
I n p a r t i c u l a r , t o x i c or n o x i o u s g a s e s m u s t be r e m o v e d
e x p e d i t i o u s l y t h r o u g h a d u c t s y s t e m t h a t d o e s n o t e x h a u s t n e a r the b u i l d i n g a i r
conditioning
intake.
9.
The b u i l d i n g must be p l a n n e d f o r s e c u r i t y .
R e s t r i c t i o n of a c c e s s i s
of c o n s i d e r a b l e i m p o r t a n c e b e c a u s e of the e x t r e m e l y v a l u a b l e and
sensitive
e q u i p m e n t u s e d i n t h e l a b o r a t o r y w o r k a s w e l l as t o p r o t e c t t h e i n t e g r i t y o f
official
samples.
10.
I t i s v e r y a d v i s a b l e to h a v e an e f f i c i e n t f i r e a n d s m o k e d e t e c t i o n
system w i t h appropriate alarms.
Common f i r e d e t e c t i o n e q u i p m e n t is
usually
e i t h e r r a t e - o f - t e m p e r a t u r e - r i s e or f i x e d - t e m p e r a t u r e d e t e c t o r u s i n g a s u b s t a n c e
of known m e l t i n g p o i n t .
T h e r e a r e a d v a n t a g e s ( a n d d i s a d v a n t a g e s ) to e a c h t y p e
of d e t e c t o r and the l a b o r a t o r y Head s h o u l d s e l e c t the one he f e e l s b e s t f i t s
his laboratory.
D e s i g n i n g a l a b o r a t o r y to a f f o r d p r o t e c t i o n a g a i n s t e v e r y k i n d o f h a z a r d w o u l d
be a l m o s t i m p o s s i b l e .
The a i m s h o u l d be to d e t e r m i n e t h e l e v e l o f s a f e t y
for
t h e most g e n e r a l a p p l i c a t i o n s and to p r o v i d e s u p p l e m e n t a r y s y s t e m s in a r e a s o f
higher h a z a r d .
A s a f e s o l v e n t s t o r a g e a r e a i s i d e a l l y s e p a r a t e from t h e l a b o r a t o r y b u i l d i n g i n
a stand-alone structure.
I t c a n be a s m a l l b u i l d i n g of one room and
some
p o s s i b l e d e s i g n f e a t u r e s a r e : ( r e a s o n s are g i v e n in p a r e n t h e s i s )
1.
materials

Construction
s u r r o u n d the

of
cement
solvents.)

blocks

or

bricks.

(Only

non-flammable

2.
For a s t a n d - a l o n e b u i l d i n g , d o u b l e w a l l s w i t h i n s u l a t i o n
between.
The e x t e r i o r
w a l l c a n be m a t e r i a l
other
than block
or b r i c k .
(Provides
i n s u l a t i o n from the sun and m a k e s a i r c o n d i t i o n i n g more e f f e c t i v e . )
3.
An e p o x y f i l m to c o v e r t h e e n t i r e
walls.
( A n y s o l v e n t s p i l l a g e w i l l p o o l and
t h e f l o o r s or w a l l s . )

11

floor plus
evaporate,

10 cm up t h e b a s e of t h e
r a t h e r than soak through

4.
A c o p p e r pipe (about 25 m m ) inside the r o o m , w h i c h goes t h r o u g h the
floor and is e m b e d d e d a b o u t 2 m in earth.
(A g r o u n d pipe to bleed off any
static e l e c t r i c i t y c h a r g e s - w h i c h o f t e n build up w h e n s o l v e n t s are poured).
All metal objects in the room are to be attached to the pipe using heavy guage
single strand copper wire.
Also, attach a short wire with an alligator clip.
(This g r o u n d s all m e t a l .
The clip is used to g r o u n d any m e t a l cans used for
s o l v e n t transfer.)
5.
grounding

Storage
pipe.

shelves of metal

and connected

by wire

to each other and

the

6.
Air c o n d i t i o n i n g is e x t e r n a l , w i t h the e n t r a n c e duct at the top of
one c o r n e r of the r o o m and the exit d u c t at the b a s e of the o p p o s i t e c o r n e r .
( T h e r o o m m u s t be c o o l e d as m a n y s o l v e n t s w i l l b o i l at h o t o u t s i d e
temperatures. The air entrance on top and exit on the bottom diagonally across
the r o o m , w i l l cool the room and w i l l also serve to s w e e p and r e m o v e any
solvent fumes on the floor - solvent fumes are generally heavier than air and
will pool on the floor.)
7.
The door is of m e t a l and f i r e - r a t e d for at least one h o u r , w i t h a
positive closure.
It must seal well when closed. The door sill is at least 10
cm high.
(Fire doors are metal sheathed around cement.
The closure, the seal
and the h i g h sill all act to p r e v e n t e s c a p e of s o l v e n t , e i t h e r floor s p i l l a g e
or fumes.)
8.
An air c o n d i t i o n e r exit duct w i t h a fire b a f f l e (to p r e v e n t flash
b a c k ) and d u c t e d to exit in the o u t s i d e air at b u i l d i n g r o o f h e i g h t .
(Fumes
h a v e a b e t t e r c h a n c e of being carried a w a y by b r e e z e s and s o m e o n e s m o k i n g
nearby will not present a fire risk.)
9.
An extinguisher system,
and not water sprinklers.

3.4

Ventilation and Air

which

should

be carbon dioxide or Freon type

Conditioning

An ordinary laboratory may have amounts of lead in the air passing through it
in a day which can be measured in milligrams.
Natural ventilation, which may
provide large quantities of air without cooling, is not generally suitable for
laboratories.
T h i s is e s p e c i a l l y true in u r b a n a r e a s w h e r e m o t o r t r a f f i c is
high.
This means that air conditioning is essential for the modern laboratory.
A i r c o n d i t i o n i n g not only p r e v e n t s s o m e f o r m s of c o n t a m i n a t i o n , it also
p r o v i d e s a s t a b l e t e m p e r a t u r e e n v i r o n m e n t for s e n s i t i v e and s o p h i s t i c a t e d
analytical instruments. Most v o l u m e t r i c g l a s s w a r e is c a l i b r a t e d at 20C and
must be recalibrated if used at significantly different temperatures.
This is
s t i l l a n o t h e r a r g u m e n t for air c o n d i t i o n i n g .
T h e i m p o r t a n c e of a i r
conditioning to overall laboratory accuracy cannot be overstressed.
The exhaust fans in fume hoods result in a negative pressure in the laboratory
and in an urban or industrial area this aggravates contamination of the whole
l a b o r a t o r y area.
A p o s i t i v e p r e s s u r e s y s t e m is c o s t l y as it h a s to be
s u f f i c i e n t l y p o w e r f u l to p r o v i d e a c l e a n filtered air s u p p l y w h i c h p a s s e s
t h r o u g h f u m e hood e x h a u s t fans as w e l l as o t h e r o u t l e t s .
V e n t i l a t i o n by
p o s i t i v e p r e s s u r e a s s i s t s the e x h a u s t fans in f u m e h o o d s and is to be
preferred.
Each f u m e hood should h a v e a s e p a r a t e fan, as there is d a n g e r of
cross c o n t a m i n a t i o n from a c o m m o n d u c t i n g s y s t e m .
Such a s y s t e m can be
essential if the vicinity of the laboratory is prone to contamination and it is
necessary to carry out low-level trace analysis.
Toxic fumes must be confined
as far as possible to fume hoods.
These should be away from cross-currents of
air and pedestrian traffic.
The recommended m i n i m u m air-flow through the open
face of a f u m e hood is 0.5 m / s e c .
V e n t i l a t i o n s h o u l d be such as to give at
least 5 air changes per hour.

12

V a c u u m p u m p s used to evaporate solvents should have the exhaust to the outside

a i r , o t h e r w i s e t o x i c l e v e l s of the s o l v e n t m a y be r e a c h e d in the l a b o r a t o r y
atmosphere.
W a t e r aspirator p u m p s are quite safe w i t h w a t e r - s o l u b l e solvents
or acid f u m e s , but not w i t h w a t e r - i m m i s i b l e s o l v e n t s such as p e t r o l e u m ether.

3.5

Space

Utilization

L a b o r a t o r y s p a c e m u s t be a r r a n g e d for m a x i m u m u t i l i z a t i o n as w e l l as p r o p e r
w o r k flow.
It is usual to a l l o w about 10 square m e t e r s of laboratory space and
3 m e t e r s of b e n c h s u r f a c e p e r a n a l y s t .
An e x a m p l e of a l a b o r a t o r y for 8
a n a l y s t s is in Figure 3.4.

Sx
FC
Fr
DS
Kj

Figure

"
=
=
=
=

Soxhlet bench
fume cupboard
freezer
sink unit
Kjeldahl apparatus

3.4

N o t e that e a c h a n a l y s t h a s a l a t e r a l b e n c h a r e a to w o r k at.
T h i s f o r m a t is
termed 'peninsular' and is quite e f f i c i e n t .
An a l t e r n a t e f o r m a t uses 'islands'
w h i c h have access on all sides.
An e x a m p l e is Figure 3.5.

13

0.7b m

1.50 m

0.75 m

1.50 m

0.75 m

1.50 m

0.75 m

Consider as island
benches accessible
from every side, or
consider as the floor
space remaining, the
area B being occupied
by benches

Figure

3m

3.5

T h e o p t i m u m w i d t h f o r a s i n g l e b e n c h ( a b o u t 75 cm) i s r o u g h l y t h e s a m e as t h e
width
of
the
space
required
by a s t a n d i n g
individual.
It
is
therefore
convenient,
to c o n s i d e r t h e p r o s and c o n s o f i s l a n d b e n c h e s and
peninsular
b e n c h e s w i t h the a s s i s t a n c e of F i g u r e 3 . 5 .
I t c a n r e a d i l y be s e e n t h a t the
m a x i m u m b e n c h a r e a i s o b t a i n e d w i t h p e n i n s u l a r b e n c h e s (B a r e a s ) , h o w e v e r ,
the
w o r k i n g s u r f a c e is more a c c e s s i b l e on i s l a n d b e n c h e s (A a r e a s ) .
The
services
a r e m o r e a c c e s s i b l e f o r r e p a i r on i s l a n d b e n c h e s , b u t t h e r e i s l e s s
space
available
for s h e l v i n g
close
to t h e b e n c h e s .
In the c a s e of
peninsular
b e n c h e s , t h e a n a l y s t w o r k i n g i n a b a y h a s a c c e s s i n e f f e c t to t h r e e w o r k i n g
s u r f a c e s at o n c e and t h i s i s v e r y c o n v e n i e n t i f t h e r e a r e s e v e r a l
different
a n a l y s e s i n p r o g r e s s at the same t i m e .
H o w e v e r , the s p a c e b e t w e e n p e n i n s u l a r s
s h o u l d a l w a y s be e n o u g h for two p e o p l e to w o r k c o m f o r t a b l y b a c k to b a c k ( a b o u t
1.5 m).
I s l a n d b e n c h e s make the c h o i c e of s i t e for w i n d o w s and d o o r s
less
critical.
P e n i n s u l a r b e n c h e s m a y be p r e f e r r e d i f s p a c e i s a t a p r e m i u m a n d
t h e y may be s l i g h t l y s a f e r ,
as the r o u t e s by w h i c h p e o p l e w a l k a b o u t
the
l a b o r a t o r y t e n d to be m o r e r e s t r i c t e d and p r e d i c t a b l e .
W h i c h e v e r is c h o s e n ,
w h a t i s m o s t i m p o r t a n t i s t h a t t h e s i z e o f t h e r o o m i s c o r r e c t to t a k e a n
i n t e g r a l n u m b e r of b e n c h u n i t s w i t h t h e i r a c c o m p a n y i n g
floor space.
Usually
t h e p r o b l e m c a n be p a r t l y s o l v e d b y a w a l l b e n c h at one end or s i d e of t h e
l a b o r a t o r y but a l l too o f t e n l a b o r a t o r i e s have such a s i z e or shape t h a t f l o o r
s p a c e h a s b e e n w a s t e d , or an e x t r a b e n c h h a s b e e n i n c o n v e n i e n t l y s q u e e z e d
in.
The s t o r a g e a r e a s in the b e n c h e s s h o u l d be m o d u l a r to a l l o w f l e x i b i l i t y .
Many
laboratory
bench
manufacturers
have
units
where
the
storage
areas
are
interchangeable.
Some s a m p l e s of b e n c h a s s e m b l i e s a r e g i v e n in F i g u r e 3 . 6 ,
w i t h w i d t h s in c e n t i m e t e r s .

14

KO

ra

to

1M

(O

m m m
I

f-

"t-

22

to

'

to

110

120

4-

120

10

120

2%0

120

2$o

120

4-

2 tO

120

2so

tO

+4-

4-4-

4"

120

IM

120

4-4rara
1

II

II

4-

220

H
t-

rap nu
+

Il

ira
m m
m rap ra
era
to

M U

4-

SO (O

>0

110

4"

HI

..

Figure

--

--

'

3.6

The o p t i m u m working depth of benches for standing w o r k has been found to be 60

cm for the w o r k i n g s u r f a c e , p l u s 15 cm for the a c c o m m o d a t i o n of a b o v e - b e n c h
fitments (such as gas service, electrical sockets and shelves) giving a total
depth of 75 cm.
The bench heights, h o w e v e r , have always caused some problems
b e c a u s e of the v a r i e t y of b e n c h t o p s a v a i l a b l e .
Their thickness varies with
the different coverings and supporting bases used:
6 cm for ceramic tiles, 4
cm for P y r o c e r a m , 3.7 cm for a c i d - p r o o f s t o n e w a r e , and 2.8 cm for p l a s t i c s .
H e i g h t d i f f e r e n c e s in a d j a c e n t b e n c h u n i t s always cause inconvenience to the
user.
Therefore purchases of new benches m u s t expressly indicate that desks
and benches with different coverings must have uniform heights.
(Differences
c a n be c o m p e n s a t e d for b y u n d e r l a y i n g the b e n c h tops.) B e n c h m o d u l e l e n g t h s
are u s u a l l y 60 cm for s i n g l e u n i t s and 90 or 120 cm for d o u b l e u n i t s .
This
modulus of length in 30 cm steps allows adaptation to nearly any room size.
W o r k flow is a very important part of proper space utilization.
There should
be a l o g i c a l and s y s t e m a t i c a r r a n g e m e n t of s p a c e to p e r m i t f l o w of a n a l y s i s
w o r k f r o m s a m p l e r e c e i p t , p r e p a r a t i o n and a n a l y s i s to d i s p o s a l or s t o r a g e .
This entails examining the average sample annual workload in relation to the
areas and people involved in the various analyses.
The best work flow system
(within physical constraints of the building) is usually readily apparent.

3.6

Equipment

and

Instruments

The complexity of equipping a laboratory and the consequent delay in production

of u s e f u l r e s u l t s s h o u l d n o t be u n d e r e s t i m a t e d .
In the e a r l y s t a g e s , the
requirements for equipment may seem large and complex but once the laboratory
is e s t a b l i s h e d , the r u n n i n g c o s t s a r e r e l a t i v e l y l o w .
It is s o m e t i m e s n o t
appreciated by the non-technical administrator that an analysis may require 10
or 20 i n d i v i d u a l i t e m s and that if e v e n o n e is n o t a v a i l a b l e the a n a l y s i s
cannot be carried out.
On the other hand, many items are c o m m o n to different

15

a n a l y s e s so t h a t , o n c e the m a n y h u n d r e d s of i t e m s r e q u i r e d in a food c o n t r o l
l a b o r a t o r y h a v e b e e n p r o v i d e d , t h e r e c o m e s a p o i n t at w h i c h p r o d u c t i v i t y c a n
rise s h a r p l y and i n v e s t m e n t decrease.
The logistical p r o b l e m s of m a i n t e n a n c e ,
r e p a i r and r e p l a c e m e n t of e q u i p m e n t are also c o n s i d e r a b l e .
Adequate provision
m u s t be m a d e for obtaining spares and r e p l a c e m e n t parts and for their storage.
It is false e c o n o m y if staff are being paid but c a n n o t do an i m p o r t a n t part of
their w o r k due to a lack of r e l a t i v e l y i n e x p e n s i v e e q u i p m e n t .
S o m e of the i n s t r u m e n t s and e q u i p m e n t needed for c h e m i c a l a n a l y s i s by a m o d e r n
food c o n t r o l l a b o r a t o r y are:
(for purposes of this listing, ' i n s t r u m e n t s ' are
m e a s u r i n g d e v i c e s and ' e q u i p m e n t ' are p r o c e s s i n g d e v i c e s .
Apparatus made
p r i m a r i l y of glass are not included).

Instruments

A n a l y t i c a l balance
pH m e t e r
Spectrophotometer, UV-visible, double-beam
S p e c t r o p h o t o m e t e r , atomic a b s o r p t i o n
H i g h P e r f o r m a n c e Liquid C h r o m a t o g r a p h (with UV and d i f f e r e n t i a l r e f r a c t i v e
index d e t e c t o r s )
Gas C h r o m a t o g r a p h (with flame i o n i z a t i o n and e l e c t r o n capture d e t e c t o r s )

Equipment

Blender
Grinder
Pulverizing hammer mill
Air o v e n , forced draft
V a c u u m o v e n , with pump
M u f f l e furnace
Centrifuge
Refrigerator
Freezer
H e a t e r s and hot plates
Steam and w a t e r b a t h s
W a t e r still or d e i o n i z e r

All of the above e q u i p m e n t and i n s t r u m e n t s are m o v e a b l e , a l t h o u g h the larger or

m o r e s e n s i t i v e units are g e n e r a l l y not m o v e d , once placed.
The m a j o r i t e m s of
fixed e q u i p m e n t constructed in place are the fume hoods.
The e x t e n s i v e use of
s o l v e n t s , a s h i n g and n o x i o u s c h e m i c a l s in f o o d a n a l y s i s , r e q u i r e s m o r e f u m e
h o o d s t h a n o t h e r t y p e s of l a b o r a t o r y w o r k .
In f a c t , to e x p e r i e n c e d
food
a n a l y s t s , t h e r e n e v e r s e e m to b e e n o u g h h o o d s , e v e n in a w e l l
equipped
laboratory.
F u m e h o o d s m a y be p u r c h a s e d p r e - f a b r i c a t e d w i t h o u t l e t s for
services.
The m a t e r i a l of c o n s t r u c t i o n is m o s t i m p o r t a n t , e s p e c i a l l y if the
hood has to w i t h s t a n d acid fumes in general and p e r c h l o r i c acid in p a r t i c u l a r .
The s u p p l i e r m u s t be g i v e n full d e t a i l s of the use to w h i c h the fume hood w i l l
be put.
H o o d s c a n be c o n s t r u c t e d
out of l o c a l m a t e r i a l s s u c h as w o o d ,
p r e f e r a b l y hard w o o d s , coated w i t h epoxy resins.
Such should n e v e r be used for
acid d i g e s t i o n s , but only for solvent e x t r a c t i o n work.

3.7

Utilities

E l e c t r i c i t y m u s t either be a stable supply, or the voltage m u s t be stabilized

by e i t h e r one large s t a b i l i z e r for the w h o l e l a b o r a t o r y , or by a unit for each
of the i n s t r u m e n t s r e q u i r i n g it.
A b o u t 40 w a t t s per s q u a r e m e t e r has b e e n

16

suggested.
The laboratory pictured in Figure 3.3 has 160 double 13-amp socket
outlets.
This apparently large n u m b e r adds considerably to the efficiency of
a n a l y t i c a l o p e r a t i o n s and to their s a f e t y .
The s a m e l a b o r a t o r y has 110 gas
p o i n t s , e x c l u d i n g t h o s e to the f u m e h o o d s .
T h e r e m u s t b e s e v e r a l cold w a t e r
taps per b e n c h to a l l o w for r i n s i n g , c o n d e n s e r s , etc., but h o t w a t e r can be
restricted to those sinks w h e r e apparatus is washed.
In a larger laboratory a
distribution system for distilled or deionized water would be advantageous.

The following utilities

for fume hoods have been

Fume Hood Length

():

Gas taps (front controlled)

Water taps (front controlled)
Cup sinks
Compressed air valves (front
controlled)
Two-phased electrical sockets
Three-phased electrical
sockets

suggested:

1.2

1.5

1.8

2
2
1

2
3
2

3
4
2

1
2

1
3

1
4

S p e c i a l m e t h o d s , s u c h as t r a c e a n a l y s i s , u s u a l l y r e q u i r e d i s t i l l a t i o n f r o m
g l a s s a p p a r a t u s of w a t e r i n i t i a l l y p a r t i a l l y p u r i f i e d by d i s t i l l a t i o n or
deionization.
The initial purification produces water very low in salts, but
if the o r i g i n a l s u p p l y c o n t a i n s o r g a n i c m a t t e r t h i s m a y n o t be r e m o v e d , and
traces of resin material m a y be present.
A s t e a d y s u p p l y of c o m p r e s s e d air is r e q u i r e d for an a t o m i c
absorption
s p e c t r o p h o t o m e t e r (AAS) and is v e r y u s e f u l to h a v e a v a i l a b l e at the b e n c h . A
c o m p r e s s o r is s u i t a b l e for use w i t h the i n s t r u m e n t but if used for o t h e r
purposes at the same time it m u s t be capable of supplying those needs without
a f f e c t i n g the AAS s u p p l y . A p a r t f r o m the i n a c c u r a c y that w i l l r e s u l t from a
change in the flame characteristics, sudden failure of the air m a y result in a
flashback, which is expensive if the mixing chamber is destroyed, and could be
dangerous.
H o w e v e r , it m u s t be emphasized that m a n u f a c t u r e r s design this part
of the i n s t r u m e n t to be as safe as p o s s i b l e u n d e r f l a s h b a c k c o n d i t i o n s .
Therefore, in m a n y ways it is probably better to have a separate air supply to
the AAS.
T h i s i n s t r u m e n t a l s o has to be p r o v i d e d w i t h a v e n t i l a t i o n h o o d to
remove gases formed during operation, particularly if nitrous oxide is used as
the fumes are very toxic.
Utility services require a large space but need to be concealed for aesthetic
r e a s o n s , y e t r e q u i r e an e a s y a c c e s s for r e p a i r p u r p o s e s .
To s a t i s f y t h e s e
conflicting demands, the main runs may be in voids above false ceilings and in
floor ducts.
Secondary services are then run to outlet points on benches taken
from floor level along the wall behind benches in voids especially incorporated
in the design of the bench fittings.
Frequent access points are provided for
maintenance purposes.
Drain pipes should be of high density polythene or copolymer polypropylene with
screwed joints.
T h e s e s h o w g o o d r e s i s t a n c e to m o s t o r g a n i c and i n o r g a n i c
chemicals.
The d r a i n a g e l i n e s m a y be e m b e d d e d in the f l o o r i n g . As it is not
acceptable to discharge laboratory w a s t e s d i r e c t l y i n t o t h e s e w e r a g e s y s t e m ,
all w a s t e from l a b o r a t o r y sinks and o t h e r w a s t e f i t t i n g s s h o u l d be led f i r s t
into dilution pots (about 5 litre capacity) before being released into the m a i n
sewers.
Buildings can be designed to include a large dilution tank where all
l a b o r a t o r y sink w a s t e is d i r e c t e d b e f o r e e n t e r i n g the s e w e r a g e s y s t e m .
For
laboratories with high mineral acid use, sink traps of inert duriron often work
well.

17

3.8

Design

References

1.

B e c k , H. L u f t u n g s e i g e n s c h a f t e n von L a b o r a b z u g e n ( V e n t i l a t i o n p o w e r of
laboratory fume cupboard).
Weinheim, Chemie-Ingenieur-Technik, 1964 (No.
3 6 ) (in G e r m a n ) .

2.

Be r u f s g e n o s s e n s c h a f t fur d i e c h e m i s c h e I n d u s t r i e , R i c h t l i n i e n fur
c h e m i s c h e L a b o r a t o r i e n Nr. 12 ( D i r e c t i v e s for c h e m i c a l l a b o r a t o r i e s no.
12) Weinheim, Verlag-Chemie, 1972 (in German).

3.

DECHEMA Erfahrungs austausch;

Laborbau (DECHEMA sharing
laboratory design).
Frankfurt/M. DECHEMA, 1969 (in German).

4.

Decken,
C.B. v.d. a n d
B. H u n d o r f .
Untersuchungen
uber
die
stromungstechnischen Vorgange in der Kapelle eines Laborabzug (Experiments
about flow within the cabin of a fume cupboard).
Darmstadt, GIT 1968 (No.
8) (in G e r m a n ) .

5.

D e u t s c h e r V e r e i n von Gas und W a s s e r f a c h m a n n e r n ( D V G W ) N o r m e n

F e d e r a t i o n of Gas and W a t e r S p e c i a l i s t S t a n d a r d s ) E s c h b o r n ,
Republic of Germany (in German).

(German
Federal

a.

Was serversorgung; Verbrauchanlagen

D W G W W 503-1966.

piping)

b.

T e c h n i s c h e R e g e l n fur Bau und P r u f u n g von v o r g e f e r t i g t e n B a u t e i l e n

mit Gas und Wasserinstallation ( S p e c i f i c a t i o n for c o n s t r u c t i o n and
testing of prefabricated appliances with gas and water installations)
D V G W GW 3 (1968).

c.

Technische Regeln fur die Installation von Gasanlagen in Laboratorien

(Specifications for gas service installations in laboratories) DVGW G
621 (1971).
(Pressure

experience:

(Water supply: service

gas regulation) Koln, Carl Heymann's Verlag

6.

Druckgasverordnung
(in G e r m a n ) .

7.

Dunkl/Geyer.
R a t i o n a l e L o s u n g e n von L a b o r b a u und L a b o r e i n r i c h tungsprob1emen
in H o c h s c h u l e n ,
Industrieunternehmumgen
und i m
Gesundheitswesen der USA (Rational solutions of problems in the design of
laboratory building and equipment for u n i v e r s i t i e s , i n d u s t r y and p u b l i c
h e a l t h in the U n i t e d States).
In B e i t r a g e zur U n i v e r s i t a t s p l a n u n g
( C o n t r i b u t i o n s to the p l a n n i n g of u n i v e r s i t i e s ) . F r a n k f u r t / M . D E C H E M A ,
1970 (Heft 6) (in G e r m a n ) .

8.

F e u r i c h , H. R o h r n e t z e fur S a u e r s t o f f , D r u c k l u f t , V a c u u m , K o h l e n s a u r e in
K r a n k e n h a u s e r n und L a b o r a t o r i e n (Service p i p i n g for o x y g e n , c o m p r e s s e d
air, vacuum and carbon dioxide in hospitals and laboratories) Darmstadt,
G I T 1 9 6 4 (nos. 8, 9 and 10) (in G e r m a n ) .

9.

D e u t s c h e I n d u s t r i e N o r m t'DIN) ( G e r m a n
Beuth-Vertrieb G m b H (all in German)
plant;

principles,

Industrial

a.

Ventilation
English).

b.

Fire resistance
4102-1970.

c.

Space lighting by daylight; principles.

DIN 4034-1969.

d.

Laboratory furniture;
12 912-1973.

laboratory

of building

DIN

Standard).

materials

ceramic

18

tiles

1946-1960,

and

for

Part

structural

Berlin,

(also

elements.

bench

tops.

in

DIN

DIN

e.

Laboratory furniture; cup sinks.

DIN

12-914-1973.

f.

Laboratory
1973.

g.

L a b o r a t o r y furniture; large-size
DIN 12 916-1972.

h.

Colour code for fluids on h a n d l e v e r s and h a n d w h e e l s of laboratory

taps.
DIN 12-920-1971.

i.

Laboratory furniture; benches, dimensions.

j.

Laboratory
1972.

k.

Heating plant,
English).

1.

Traffic ways in buildings.

m.

Ventilation of laboratories. VID 2051-1966.

furniture; sinks w i t h integrated o v e r f l o w . DIN 12 915-

furniture;

smoke

fume

tiles

cupboards,

stacks.

DIN

DIN

18

for laboratory bench

tops.

DIN 12 922-1972.
dimensions.

160-1968;

DIN

part

12

923-

1 (also

in

18-225-1958.

10.

Geyer, F. A n f o r d e r u n g e n an L a b o r b a u t e n ( R e q u i r e m e n t s for laboratory

b u i l d i n g ) D a r m s t a d t , GIT (No. 1 2, 1 967 and No. 1 1968) (in German).

11.

/Richtlinien fur die Planung und den Bau von Laboratorien (Principles for
design and building of laboratories) Weinheim, C h e m i e - I n g e n i e u r - T e c h n i k ,
1971. (No. 11) (in German).

12.

Role et interet de la normalisation dans 1 ' amnagement et l'equipement des

l a b o r a t o i r e s , Courrier de la N o r m a l i s a t i o n , No. 228 n o v e m b r e - d e c e m b r e ,
1972 (in French).

13.

The role and significance of standarization of laboratory equipment and

furniture.
Laboratory Practice (London) No. 4, 1973.

14.

Laboratory furniture and fittings: BS 3202-1959, London, British

Institution.

15.

Strangmann, W. Wasserverbrauch in chemischen und biologischen Laboratorien

(Water consumption in chemical and biological laboratories).
Darmstadt,
GIT, 1964 (No. 6) (in German).

16.

Unfallverhutungsvorschrift:
Medizinische Laboratoriumsarbeiten (Prescription for accident prevention: work in medical laboratories) Frankfurt/M.
H G U V V ) (in German).

17.

United States Department of Health, Education and Welfare, Health Research

Laboratory Design, Bethesda, Maryland NIH 1968 (Publication 1807).

18.

V e r b a n d D e u t s c h e r E 1 e k t r o t e c h n i k e r ( V D E ) N o r m e n (Union of G e r m a n
E l e c t r i c a l Engineers s t a n d a r d s ) O f f e n b a c h / M a i n , Federal Republic of
Germany (in German).

19.

A Literature Survey and Design Study of Fume Cupboards and

Systems, Hughes, D., 1980, Science Reviews Ltd., London.

19

Standards

Fume-Dispersal

4.

4.1

LABORATORY ADMINISTRATION

Sample Collection

Work scheduling is greatly facilitated by arranging a sampling programme for

r o u t i n e m o n i t o r i n g w i t h the i n s p e c t o r a t e .
Close c o o p e r a t i o n w i t h
the
inspectorate will pay great dividends in improved efficiency in sampling.
It
i s o f t e n a l s o n e c e s s a r y to h a v e part of the l a b o r a t o r y staff a v a i l a b l e for
urgent work and for samples such as consumer complaints, export certification
and c h e c k i n g of i m p o r t s , w h e r e t h e r e is o f t e n l i t t l e n o t i c e g i v e n b e f o r e the
arrival of the sample.
S i n c e the l a b o r a t o r y r e l i e s on the i n s p e c t o r a t e for a s t e a d y w o r k l o a d , the
inspectorate and laboratory supervisors must be in frequent contact in order to
m a i n t a i n the w o r k l o a d in the l a b o r a t o r y at a r e a s o n a b l e level. As part of a
general food control programme, there is need to:
1.
Regularly inspect foods at different stages in the manufacturing
distribution chains using planned surveillance programmes.

and

2.
C a r r y out g e n e r a l s u r v e y s of the q u a l i t y of the food s u p p l y t h r o u g h
random sampling and analysis, samples being taken from factories, warehouses
and retailers.
3.
Monitor certain specific problem areas with regard to food safety specific foods or classes of foods for specific potential risks, (e.g. level of
metallic contaminants, pesticide residues, mycotoxins, etc.).
4.

Inspect foods for export, for certification of quality

(if needed).

5.
Inspect
food
imports.
This
is b e s t d o n e on a l l
c o n s i g n m e n t s by f o r m a l s a m p l i n g c a r r i e d out s y s t e m a t i c a l l y in
representative of the lot.

imported
a manner

6.
Formal sampling should also be done on locally produced food products
b a s e d o n t h e f o o d i n s p e c t o r s ' o b s e r v a t i o n s , or b e c a u s e a r a n d o m o r
investigatory sample under the regular programme was unsatisfactory, or because
the product is one that requires thorough surveillance.
Analysis of formal and
informal samples is also necessary in an emergency such as an outbreak of foodpoisoning .
National sampling programmes yield important benefits in terms of efficiency.
The I n s p e c t o r a t e and the L a b o r a t o r y a s s i s t e d and g u i d e d by o t h e r a g e n c y
o f f i c i a l s or an a d v i s o r y b o a r d , as a p p r o p r i a t e , should p e r i o d i c a l l y plan
overall programmes to locate and deal with different problems in the areas of
food q u a l i t y and c o n s u m e r p r o t e c t i o n .
In each case the o b j e c t i v e s of the
p r o g r a m m e should be clearly defined.
A l t h o u g h s a m p l e s m a y be c l a s s i f i e d in a n u m b e r of w a y s , it is c o n v e n i e n t to
consider two broad divisions, "formal" samples and "informal" samples.
Formal
samples are those taken to determine if the foods comply with national or local
l a w s or r e g u l a t i o n s .
R e g u l a t o r y a c t i o n m a y r e s u l t from r e p o r t s r e c e i v e d on
such samples.
Informal samples may be taken for purposes of monitoring or as
part of survey work. Formal follow-up samples can be taken if informal samples
receive adverse laboratory reports.
Formal or informal samples will also be
taken under other circumstances, such as a follow-up to a consumer complaint.
When samples are
of the nature and
required from the
e x p e r i e n c e , from
from the r o u t i n e

sent to the laboratory, the inspector must send full details

purpose of sampling and any other relevant data.
The results
analysis will usually be clear, either from the analyst's own
p r i o r d i s c u s s i o n w i t h the i n s p e c t o r or h i s s u p e r v i s o r s , or
i n f o r m a t i o n g i v e n w i t h the s a m p l e .
A w e l l q u a l i f i e d and

20

t r a i n e d i n s p e c t o r m a y a l s o w i s h to d i s c u s s the need for an a n a l y s i s that the

a n a l y s t w o u l d not r o u t i n e l y c a r r y out.
It is the d u t y of the l a b o r a t o r y H e a d
to decide how these requests are to be met.
The inspector's sample submission form should give all necessary details about
the sample.
These details may include the product n a m e , place of collection,
reason for collection, type of samples (consumer c o m p l a i n t , official, survey,
etc.),
inspector's name,
m o d e of s a m p l i n g ,
lot n u m b e r ,
s h i p p e r if so
transported, size of consignment and similar relevant details, together with
any s p e c i a l i n f o r m a t i o n that m a y be of a s s i s t a n c e to the a n a l y s t , such as
suspected contamination.
T h e s a m p l e s h o u l d a l s o be s e a l e d by the i n s p e c t o r
with an official seal.

4.2

Sample Receipt and

Assignment

W h e n a food s a m p l e is r e c e i v e d for a n a l y s i s , t h e r e m u s t be a s y s t e m to t r a c k
the sample throughout it's initial storage, analysis and later reserve storage.
This is usually embodied in a record keeping system which is keyed to a unique
n u m b e r a s s i g n e d to the s a m p l e at the t i m e of s a m p l i n g .
T h i s n u m b e r c a n be
sequential (i.e. 0001 to 9999) or can be devised to give information (i.e. 0245 - 0 7 , the 2 4 t h s a m p l e t a k e n in 1 985 u n d e r s a m p l i n g p r o g r a m m e n u m b e r 7).
The
r e c o r d m u s t s h o w each m o v e m e n t of a s a m p l e , its r e c e i p t , a s s i g n m e n t to a
l a b o r a t o r y p e r s o n for a n a l y s i s , r e t u r n to the s a m p l e c u s t o d i a n , and e v e n t u a l
disposition.
One of the a d m i n i s t r a t i v e s t a f f s h o u l d be g i v e n this r e c o r d
keeping function and closely supervised by a senior administrator, as well as
supervised in general by the laboratory Head.
It is usually best to use a card record system rather than a log book as cards
are more flexibly handled and may be filed in groups under different headings.
M a n y card record systems have been devised including 5x8 cards with coded sites
on the periphery for punching.
Other cards are pre-printed with spaces to be
filled in w i t h appropriate data.
Regardless of the card system selected, there
are certain items of information which should be on each card:

1.

Sample

number.

2.

Product

3.

Date

4.

Date received

5.

Type of sample

6.

Method

7.

Storage

8.

Date assigned

9.

To whom assigned

name.

sampled.
at the

laboratory.

(survey, complaint,

of storage

etc.).

(dry, refrigeration,

location (coded
for

for easy

freezing,

etc.).

finding).

analysis.
(the analyst

10.

Date returned

(from

11.

From whom returned

12.

Reserve

13.

Final disposition

should

initial

to show

receipt).

analyst).
(may be different

storage method

and

from

the original

analyst).

location.

or disposal

of sample, method

21

and

date.

Note that the above uses the sample record only to record physical m o v e m e n t and
location, not analytical results.
The reason is that the analytical worksheet
and the sample record are usually in two different locations.
T h e s a m p l e r e c o r d card s h o u l d be p r e p a r e d and in the c u s t o d y of one p e r s o n
until the reserve sample is destroyed.
This person is often called the Sample
Custodian and in small laboratories could have other duties as well.
The job
of S a m p l e C u s t o d i a n is c r i t i c a l to the o p e r a t i o n of m o s t l a b o r a t o r i e s .
The
person employed in this post m u s t be very reliable, but m a y find the duties of
the job s l i g h t l y m o n o t o n o u s .
C o m b i n i n g the d u t i e s of s a m p l e c u s t o d i a n w i t h
k e e p i n g the l a b o r a t o r y s t o r e is o f t e n d o n e in m e d i u m
or l a r g e r
sized
laboratories.
The laboratory store of chemicals, glassware and other fittings
r e q u i r e s c a r e f u l c o n t r o l as d o e s r e o r d e r i n g of m a t e r i a l s in s h o r t s u p p l y ,
issuance of supplies to analysts, etc.
Combining the jobs of Sample Custodian
and S t o r e K e e p e r c a n c r e a t e a c h a l l e n g i n g and i n t e r e s t i n g p o s t .
Another
approach to the job of Sample Custodian in smaller laboratories is to split the
job b e t w e e n several people with different senior assistants under the various
section leaders being responsible for samples from a particular source, or for
particular groups of products.
W h e n a s a m p l e is a s s i g n e d , the a n a l y s t s h o u l d p h y s i c a l l y sign or i n i t a l the
s a m p l e c a r d to s h o w c u s t o d y .
W h e n a s a m p l e r e s e r v e is r e t u r n e d to the
C u s t o d i a n , the C u s t o d i a n w o u l d sign or i n i t i a l .
A f t e r a s s i g n i n g the s a m p l e ,
the S u p e r v i s o r m u s t h a v e s o m e m e a n s of t r a c k i n g s a m p l e s u n d e r a n a l y s i s w i t h
proposed or possible completion dates.
The sample card could be used for this.
The card would then be in the hands of the Supervisor during analysis and would
be returned to the Custodian on completion.

4.3

Sample Storage

and

Disposal

S a m p l e s t o r a g e , b o t h i n i t i a l and r e s e r v e , is c r i t i c a l to a s a m p l e a n a l y s i s .
Improper storage can completely i n v a l i d a t e a n y a n a l y t i c a l r e s u l t s .
Ideally,
the s a m p l e is to be s t o r e d in a m a n n e r to p r e v e n t a c h a n g e in the a t t r i b u t e
being examined, from the time of sampling, through analysis, and into reserve
storage.
To i l l u s t r a t e the i m p o r t a n c e of p r o p e r s t o r a g e , if a fresh food
sample to be examined for decomposition is not hard frozen until examination,
it very likely will decompose even further.
The analyst is then not sure how
m u c h of the d e c o m p o s i t i o n found is due to sample mishandling.
The usual storage areas are dry (room temperature storage), refrigeration and
freezing.
K e e p in m i n d t h i n g s that c a n h a p p e n d u r i n g s t o r a g e .
For e x a m p l e ,
insects or other vermin can attack dry storage, mould frequently occurs during
refrigeration, and frozen products often have "freezer burn" where the food has
desiccated.
Steps to m i n i m i z e these problems include using correct containers
(i.e. glass or m e t a l for dry storage, no paper bags), proper sample preparation
(i.e. g l a z i n g f r o z e n s a m p l e s w h e r e p o s s i b l e , to r e d u c e d e h y d r a t i o n ) , and
frequent checks on those stored samples which are m o s t subject to change.
Sample disposal is, or can be, a relatively simple matter.
The only problems
arise w h e n there is a hazard involved in the destruction, or where the sample
r e m a i n s must have special treatment.
An e x a m p l e is a s a m p l e of g r o u n d n u t s
heavily contaminated with aflatoxin.
The sample itself presents a hazard to
the disposer and may be a hazard to others if not detoxified.
The analyst best
k n o w s any h a z a r d s i n v o l v e d , so s h o u l d i n f o r m the S a m p l e C u s t o d i a n of a n y
special disposal requirements.

22

4.4

Budget

The need should be appreciated for as flexible a budgetary system as possible.

C o n t i n g e n c y funds are i m p o r t a n t for the r u n n i n g of a l a b o r a t o r y .
Budgets
should be a r r a n g e d so that funds are r e a d i l y a v a i l a b l e for u r g e n t s u p p l i e s ,
s p a r e s and r e p a i r s and the o t h e r d a y - t o - d a y n e e d s of the l a b o r a t o r y w h i c h
cannot wait for the usually slow cycle of fiscal machinery utilized for annual
budgets in most governments.
The Laboratory Head must have adequate control of
the b u d g e t and o p e r a t e it under c l e a r l y d e f i n e d rules.
T h e s e should be
s u f f i c i e n t l y f l e x i b l e that he or she r e t a i n s d i s c r e t i o n a r y p o w e r s e n a b l i n g
t r a n s f e r of funds b e t w e e n c e r t a i n b u d g e t c l a s s e s as o c c a s i o n d e m a n d s .
For
e x a m p l e , funds for c a p i t a l e q u i p m e n t w i l l u s u a l l y be n o n - t r a n s f e r a b 1 e w h i l e
funds in two s e p a r a t e c l a s s e s for c h e m i c a l s and e x p e n d a b l e e q u i p m e n t m a y
reasonably be transferred between one another.
The b u d g e t p r e p a r a t i o n p r o c e s s should i n v o l v e all l e v e l s of l a b o r a t o r y
management from the Supervisors to the Head.
Supervisors especially gain an
a p p r e c i a t i o n for h o w m o n i e s can or c a n n o t be spent by p r e p a r i n g a b u d g e t
increment for their group.
B u d g e t s t y p i c a l l y are planned for one y e a r , but should be d i v i d a b l e into
quarters, seasons, projects or s o m e o t h e r l o g i c a l d i s t r i b u t i o n f o r m a t .
Each
Supervisor should have the responsibility (overseen and approved by the Head)
for the b u d g e t p u r c h a s e s by h i s group.
All o f f - b u d g e t i t e m s m u s t be fully
justified.
If sufficiently important, an off-budget item may take precedence
over the purchase of budgeted material.

4.5

Purchasing

The s e l e c t i o n and s p e c i f i c a t i o n of l a b o r a t o r y e q u i p m e n t t o g e t h e r w i t h the

p l a n n i n g of space r e q u i r e m e n t s ( i n c l u d i n g f l e x i b i l i t y for f u t u r e e x p a n s i o n )
should always precede, or at least go hand in hand with, building design.
Less
industrial countries often lack l a b o r a t o r y s u p p l i e s and e q u i p m e n t , t e c h n i c a l
assistance and maintenance services. The limited over-all marketing potential,
and the large variety of laboratory and scientific instruments available from
foreign suppliers and manufacturers, make it generally uneconomical for local
businessmen to establish stocks or to employ qualified service engineers.
The
p r o b l e m in m a n y c o u n t r i e s is c o m p o u n d e d by f o r e i g n e x c h a n g e and i m p o r t
r e s t r i c t i o n s w h i c h o f t e n do not e v e n p e r m i t the c o m m e r c i a l i m p o r t of spare
parts.
As a result, scientific laboratories in developing countries cannot, or
can only to a l i m i t e d e x t e n t , find t e c h n i c a l a s s i s t a n c e locally.
They m u s t
r e l y on the support and c o o p e r a t i o n of s u p p l i e r s based p e r h a p s t h o u s a n d s of
miles away.
Several conclusions can be drawn from this situation.
One of them
is that b e f o r e s e l e c t i n g any e q u i p m e n t , a c a r e f u l study should be m a d e to
determine :
1.
Which of the many possible suppliers and manufacturers of equipment
h a v e local r e p r e s e n t a t i v e s or o f f i c e s c a p a b l e of p r o v i d i n g i n s t a l l a t i o n and
maintenance services?
2.
W h a t e x p e r i e n c e do p o t e n t i a l s u p p l i e r s h a v e in d e a l i n g
special conditions obtaining in less industrialized countries?

with

the

E q u i p m e n t s p e c i f i c a t i o n s m u s t be p r e p a r e d very carefully and clearly.

There
are countless examples of cases where lack of detail in specifying has led to
the p u r c h a s e of i n c o m p l e t e or u n s u i t a b l e a p p a r a t u s .
It should be u n d e r s t o o d
that s u p p l e m e n t a r y e q u i p m e n t or a c c e s s o r i e s , if not s p e c i f i e d , w i l l not be
quoted for in the s u p p l i e r ' s bid. M o s t b r o c h u r e s or c a t a l o g u e s p u b l i s h e d by
equipment manufacturers give only general information, without complete order
specifications.
A s e l e c t i o n based p u r e l y on such l i t e r a t u r e o f t e n leads to
misunderstandings.
No indication is usually given of essential accessories not

23

included in the basic instrument, of optional accessories with explanations for

t h e i r p a r t i c u l a r a p p l i c a t i o n , or o f e s s e n t i a l o p e r a t i n g s u p p l i e s
and
r e c o m m e n d e d spare parts.
S c i e n t i f i c i n s t i t u t i o n s in less i n d u s t r i a l i z e d
countries have had the experience that because of insufficient specifications
(or lack of e x p e r i e n c e on the part of the s u p p l i e r s ) they w e r e s u p p l i e d w i t h
incomplete equipment.
W h i l e the s u p p l i e r m a y b e l i e v e that n o n - s p e c i f i e d e q u i p m e n t is a l r e a d y
a v a i l a b l e , the s c i e n t i s t in the l a b o r a t o r y m a y be s u f f e r i n g s e r i o u s and
annoying delays in putting the equipment into operation. New orders have to be
processed, and up to a year may be required to obtain the necessary additional
supplies.
Most manufacturers restrict their supplies to the parts they produce
in t h e i r o w n w o r k s .
T h e y a r e u s e d to the s i t u a t i o n w i t h i n t h e i r o w n c o u n t r y
w h e r e m i n o r a c c e s s o r i e s such as s t a n d s , c l a m p s , t u b i n g , g l a s s w a r e and e v e n
small instruments like pH-meters, balances and thermostats c o m m o n l y found in a
laboratory are either available i m m e d i a t e l y or may be obtained quickly from a
local dealer.
W h e n dealing with less industrialized countries, h o w e v e r , it is
frequently wrong to assume that the same situation obtains.
Large laboratory supply companies offer a m o r e comprehensive range of supplies
than individual manufacturers as their delivery p r o g r a m m e usually includes a
full range of instruments and auxiliary equipment.
Another advantage offered
by the l a r g e c o m p a n i e s is the e c o n o m y g a i n e d by d e a l i n g w i t h o n l y one s o u r c e
rather than having to deal with a n u m b e r of individual manufacturers.
Service
f a c i l i t i e s for i n s t a l l a t i o n and m a i n t e n a n c e of the e q u i p m e n t can also be
coordinated and provided m u c h m o r e easily by a large organization.
If experts
h a v e to be c o m m i s s i o n e d for each i n d i v i d u a l p i e c e of c o m p l e x e q u i p m e n t , the
expense b e c o m e s prohibitive.
C o m p l e x a p p a r a t u s r e q u i r e s s p e c i a l t r a i n i n g for the o p e r a t o r s .
Engineers
p e r f o r m i n g the installation usually provide some basic training.
Depending on
the experience of the scientist who is to work with the equipment, h o w e v e r , a
m o r e f a r - r e a c h i n g p r o g r a m m e of t r a i n i n g m a y be n e c e s s a r y , w h i c h c a n n o t be
i m p a r t e d by the e n g i n e e r in the field.
In such c a s e s , s p e c i a l t r a i n i n g
p r o g r a m m e s should be arranged in advance of the purchase, preferably before the
equipment is delivered.
P r o c u r e m e n t r u l e s d e m a n d , a l m o s t e v e r y w h e r e , that the c h e a p e s t o f f e r s be
accepted.
Applied to the purchase of scientific e q u i p m e n t , strict observation
of such r u l e s m a y turn out to be a v e r y e x p e n s i v e w a y of e q u i p p i n g a
laboratory.
Precise specifications are a good m e a n s of obtaining correct and
reliable offers.
O n l y such o f f e r s a l l o w a just c o m p a r i s o n of the s c o p e of
d e l i v e r y and the p r i c e s of d i f f e r e n t b i d d e r s .
In o r d e r to o b t a i n a n
u n d i s t o r t e d p i c t u r e of c o m p a r a t i v e d a t a , o n l y t e c h n i c a l l y e x p e r i e n c e d and
c o m m e r c i a l l y capable manufacturers and suppliers should be invited to submit
offers.
Only a limited number of firms that can satisfy every requirement as
to q u a l i t y , e x p e r i e n c e in h a n d l i n g c o m p r e h e n s i v e s u p p l i e s , r e l i a b i l i t y in
c o n n e c t i o n w i t h d e l i v e r y s c h e d u l e s , t e c h n i c a l a s s i s t a n c e and m a i n t e n a n c e
s e r v i c e s h o u l d be i n v i t e d to t e n d e r .
T h i s m a y e v e n lead to i n d i v i d u a l f i r m s
being selected as suppliers for entire laboratory equipment lots or specialized
instruments on a proprietary or s ingle-tender basis.
I n v i t a t i o n s to bid s h o u l d a l w a y s g i v e c l e a r i n d i c a t i o n s of the c u r r e n c y and
t e r m s in w h i c h o f f e r s are to be s u b m i t t e d ; if i n d i v i d u a l p r i c e s a r e to be
q u o t e d e x - w o r k s , f.o.b. port of s h i p m e n t , c & f. or c.i.f. p o r t of d e s t i n a t i o n ;
if s h i p m e n t is d e s i r e d b y air or sea; and w h e t h e r or n o t the c o s t of p a c k i n g
should be included.
It is worth pointing out that North A m e r i c a n firms have a
d i f f e r e n t i n t e r p r e t a t i o n of the t e r m "f.o.b." (free on b o a r d s h i p ) f r o m
European suppliers.
The latter observe the internationally accepted definition
of the t e r m , a c c o r d i n g to w h i c h f.o.b. p r i c e s i n c l u d e c o s t and all c h a r g e s of
delivery including packing, up to "on board ship" in the seaport or airport of
shipment.
In the U n i t e d S t a t e s of A m e r i c a , h o w e v e r , "f.o.b." is n o r m a l l y
u n d e r s t o o d as f.o.b. f a c t o r y , and p r i c e s do not i n c l u d e p a c k i n g ,
inland

24

f r e i g h t , l o a d i n g c h a r g e s , d o c u m e n t a t i o n or e x p o r t h a n d l i n g , all of w h i c h are
charged separately.
The term f.a.s. is used to denote "free alongside ship".
If a b i d d e r d e v i a t e s from the t e r m s laid d o w n in the t e n d e r i n v i t a t i o n , h i s
o f f e r s h o u l d be c a r e f u l l y e x a m i n e d as it m a y h a v e b e e n i n t e n d e d to o b t a i n a
superficial advantage in price comparison only.
A careful technical scrutiny
of the s p e c i f i c a t i o n s g i v e n in a b i d d e r ' s o f f e r and a c o m p a r i s o n w i t h the
i l l u s t r a t e d l i t e r a t u r e a t t a c h e d to the bid w i l l , in m a n y c a s e s , e l i m i n a t e
q u o t a t i o n s w h i c h at f i r s t g l a n c e look c h e a p e r .
Accessories may have been
p u r p o s e l y left out to g a i n an a d v a n t a g e over o t h e r b i d d e r s .
Sometimes minor
b u t i m p o r t a n t d i f f e r e n c e s in p e r f o r m a n c e d a t a c a u s e c o n s i d e r a b l e
price
variations.
M a n y n a t i o n a l and i n t e r n a t i o n a l o r g a n i z a t i o n s i n v i t e o f f e r s from o r i g i n a l
manufacturers only, demand ing that the c o m m i s s ion usually allowed to agents be
offered as a discount.
The disadvantages of this procedure are that orders are
quite frequently placed w i t h firms which readily accept these conditions but
which have neither experience nor agents in the purchasing country.
Thus, the
scientists in less industrali zed countries are denied the benefit of any kind
of t e c h n i c a l a s s i s t a n c e .
W h e n c o m p a r i n g p r i c e q u o t a t i o n s , the o f f e r of an
i n t e r n a t i o n a l l a b o r a t o r y e q u i p m e n t s u p p l i e r m a y o c c a s i o n a l l y be found to b e
substantially higher than that of a manufacturer.
In such cases it can only be
r e c o m m e n d e d t h a t the e x p e r i e n c e and a f t e r - s a l e s s e r v i c e i n c o r p o r a t e d in the
offer should be carefully considered.
One aspect of equipment purchase that causes problems is the time given for the
s u b m i s s i o n of o f f e r s .
O f t e n it is far too s h o r t .
It s h o u l d be r e a l i z e d t h a t
long lists of specifications prepared for a project over an extended period of
time cannot normally be quoted for in a space of only two or three weeks - the
t i m e that m i g h t be left to a s u p p l i e r a f t e r d e l a y s in m a i l are t a k e n into
account.
The q u a l i t y of o f f e r s m i g h t be c o n s i d e r a b l y i m p r o v e d if m o r e t i m e
were allowed.
D e c i s i o n s on bid a c c e p t a n c e s h o u l d n o t be d e l a y e d b e y o n d the
n o r m a l validity of offers.
Another serious problem that is often encountered concerns damage in transit
Extensive d a m a g e and even total loss
and the insurance covering such damage.
can result from the rough handling of consignments in ports where no mechanized
m e a n s of t r a n s p o r t (such as f o r k - l i f t t r u c k s ) is a v a i l a b l e .
D e l a y s m a y be
e n c o u n t e r e d in c l e a r i n g c o n s i g n m e n t s t h r o u g h c u s t o m s , and s h e l t e r e d s t o r a g e
facilities are often quite inadequate.
Cases containing expensive equipment
m a y be s u b j e c t e d to the m o s t a d v e r s e c l i m a t i c c o n d i t i o n s - h u m i d i t y , h e a v y
tropical rains, extreme heat and dust.
No economically justifiable method of
p a c k i n g can p r e v e n t d a m a g e to e q u i p m e n t u n d e r such c o n d i t i o n s .
Sometimes,
b e c a u s e of c u s t o m s f o r m a l i t i e s and a d m i n i s t r a t i v e d e l a y s in h a v i n g the
consignments unpacked and examined, insurance coverage has already expired by
the t i m e the e q u i p m e n t a r r i v e s at its d e s t i n a t i o n and a c l a i m can be l o d g e d .
T h e n , m o r e t i m e and e f f o r t is u s u a l l y s p e n t on f i x i n g r e s p o n s i b i l i t y than on
how the situation might be avoided in the future.
Replacement parts required to repair transport damage should be obtainable with
a m i n i m u m of delay and administrative red tape.
Laboratories should have the
authority, in an emergency, to place small orders direct with suppliers.
With
or without such emergency order facilities, h o w e v e r , scientists usually depend
on (and prefer cooperation with) the experienced and flexible supplier who is
in regular contact w i t h his customer, who extends unbureaucratic help and who
even provides, when necessary, free replacements and repair facilities in order
to c o n t r i b u t e to the p r i m e o b j e c t i v e in the e s t a b l i s h m e n t of a s c i e n t i f i c
institute, useful and effective work and uninterrupted operation.

25

4.6

Supplies

Management

Supplies routinely used by a laboratory include solvents, reagents, chemicals,

g l a s s w a r e and o t h e r a n a l y t i c a l m a t e r i a l s .
By d e f i n i t i o n ,
s u p p l i e s are
considered to be consumables and must be constantly replaced as used.
T h e r e m u s t t h e r e f o r e b e an a c c u r a t e a c c o u n t i n g s y s t e m to r e c o r d r e c e i p t , u s e
and f u t u r e n e e d .
T h i s is d o n e in a v a r i e t y of w a y s but a card s y s t e m is the
m o s t versatile.
The Supplies Record Card can contain such data as:

Name of product
Date purchased
Where purchased
Amount (including units if more than one
Expiration date (if any)
Special storage requirements (if any)
Amount dispensed.

container)

S m a l l m e t a l t a g s p a i n t e d w i t h b r i g h t c o l o u r s can be p u r c h a s e d and d i f f e r e n t
tags affixed to cards for flagging purposes.
For e x a m p l e , a red tag m a y m e a n
the supply is low and should be reordered within a given time.
Having a w o r k a b l e supplies m a n a g e m e n t s y s t e m t e n d s to p r e v e n t c i r c u m s t a n c e s
w h e r e a n a l y s e s h a v e s t o p p e d b e c a u s e a c r i t i c a l m a t e r i a l is s u d d e n l y u s e d up.
L i k e b u d g e t i n g , it is a p r o c e s s of m a i n t a i n i n g c o n t r o l of a c r i t i c a l a r e a to
promote overall smooth operation of the laboratory.

4.7

Equipment

Maintenance

W h e n the food analyst goes beyond organoleptic examinations, he or she must use
s o m e i t e m of e q u i p m e n t to p r o c e s s or to m e a s u r e the s a m p l e a t t r i b u t e of
interest.
It is critically important, therefore, that all items of equipment
be properly and promptly maintained, and repaired when needed.
T h e d e g r e e of s o p h i s t i c a t i o n of e q u i p m e n t v a r i e s d r a m a t i c a l l y from a
straightforward pH m e t e r to a complex spectrophotometer.
M a n y laboratories in
developing
countries have great difficulty
in o b t a i n i n g r e p a i r of any
e q u i p m e n t , sophisticated or otherwise.
It is therefore
reasonable to require
that proper maintenance of the equipment be routinely scheduled and completed,
hopefully to delay the day when outright repairs are necessary.
T h e b e s t c i r c u m s t a n c e , of c o u r s e , is to e s t a b l i s h an o p e r a t i n g r e p a i r and
m a i n t e n a n c e w o r k s h o p w i t h qualified technical staff.
This can be essential for
l a r g e i n s t i t u t e s h a v i n g a d i s p r o p o r t i o n a t e l y l a r g e i n v e s t m e n t in e x p e n s i v e
equipment.
E v e n in the a b s e n c e of an o r g a n i z e d w o r k s h o p , s o m e a n a l y s t s or
technicians can be given training in repair and maintenance techniques, often
by local instrument suppliers.
If adequate service is available locally, serious consideration should be given
to purchase of service contracts.
The usual service contract involves checking
the e q u i p m e n t at s p e c i f i e d i n t e r v a l s and p e r f o r m i n g n e c e s s a r y m a i n t e n a n c e .
E m e r g e n c y r e p a i r s are u s u a l l y d i s c o u n t e d in p r i c e b e c a u s e of the s e r v i c e
contract.
Service contracts are especially important for analytical balances,
to m a i n t a i n proper calibration.
A history of an instrument's maintenance and repair can become very important.
It p r o v i d e s a s u m m a r y of the i n s t r u m e n t ' s o p e r a t i o n o v e r a g i v e n p e r i o d , b u t
m o r e i m p o r t a n t l y , it can p r o v i d e a j u s t i f i c a t i o n for r e p l a c e m e n t of old and
o u t w o r n items.
Recording the cost is important as it is then readily apparent

26

w h e n an i n s t r u m e n t c o s t s m o r e to k e e p o p e r a t i n g t h a n it is w o r t h .
A preprinted
5 x 8 c a r d c a n c o n v e n i e n t l y b e u s e d to r e c o r d s u c h i n f o r m a t i o n .
An e x a m p l e of
s u c h a c a r d ( f r o n t a n d r e a r ) is s h o w n in F i g u r e s 4.1 a n d 4 . 2 .

T y p e of Machin*

MACHINE
PART I -

DETAILS

OF

HISTORY

CARD

MACHINE

B r a n d a n d Modal N o .

Vendor

L o c a t i o n of m a c h i n e
(State dept./scction)

H o w o p e r a t e d ( T i c k in appropriate b o x )

Machine N o .

C o u n t r y of Manufacture

Data of P u r c h a i e

Purchase Price

Guarantee P e r i o d

T e r m s of Guarantee

P A R T II -

Manual

Etactrk

Electronic

DETAILS OF MAINTENANCE
Service A g e n t

Per lOd

Maintenance C o n t r a c t

Name

From

Cott ($)
(per a n n u m )

To

Spare parts
included?
Yes

No

N u m b e r of

C o m m e n t o n f i r m ' service

(per a n n u m )

Figure 4.1
Front Side

F A R T HI -

OF

BREAKDOWNS
S e r v i c i n g / R e o a i r details
(State cause of b r e a k d o w n a n d
parts c h a n g e d , etc!

Date

P A R T IV

OETAILS

COMMON D E F E C T S

I d n c n b * with d . u i l i

pm

Response
time of
Service A g e n t

f r * j . n y . cHactsl

Figure 4.2
Rear Side

27

Cumulative
Cost

C o s t of
Repair

Time taken
to repair

4.8

Housekeeping

L a b o r a t o r y c l e a n l i n e s s is very i m p o r t a n t , not only to m a i n t a i n a good

appearance,
but to p r e v e n t s o m e f o r m s of c o n t a m i n a t i o n .
Housekeeping
a c t i v i t i e s go beyond c l e a n i n g and tidying in the l a b o r a t o r y .
It i n c l u d e s
i n s e c t and o t h e r pest c o n t r o l .
M o s t l a b o r a t o r i e s m u s t do their o w n pest
control to minimize contamination from control agents. Commercial pest control
firms usually do not have an appreciation of laboratory contamination problems.
L a b o r a t o r i e s m u s t be r o d e n t - p r o o f in c o n s t r u c t i o n .
E l e c t r i c a l d e v i c e s are
available for killing flying insects.
Food may arrive contaminated with insect
eggs so that proper storage is inadequate without fumigation.
Fumigation by
halogenated hydrocarbons or use of organochlorine compounds against insects are
l i k e l y s o u r c e s of l a b o r a t o r y c o n t a m i n a t i o n and are best a v o i d e d w h e n e v e r
possible.
T h e y all h a v e a s i g n i f i c a n t v a p o u r p r e s s u r e and m u s t be kept w e l l
a w a y from s e n s i t i v e e q u i p m e n t such as gas c h r o m a t o g r a p h s and from s a m p l e s
requiring analysis for pesticide residues.
H o u s e k e e p i n g should involve s c h e d u l e d as w e l l as ad hoc c l e a n i n g and pest
control.
O f t e n a good t i m e is the last h o u r of a w o r k w e e k .
A scheduled
activity quickly becomes routine and is consequently in the awareness of the
laboratory analysts.
This awareness is important because, as can be shown by
e x p e r i e n c e , not all p e r s o n s are n e a t , c l e a n and tidy in their e v e r y d a y
activities.
M a n a g e m e n t m u s t d e m o n s t r a t e a c o n t i n u i n g c o m m i t m e n t to good
housekeeping principles if the analysts are to accept those principles.

4.9

Training

W h e n an a n a l y s t is first hired in a food c o n t r o l l a b o r a t o r y , a c o n t i n u i n g

s e r i e s of t r a i n i n g and e d u c a t i o n a l e x p e r i e n c e s b e g i n .
The n e w a n a l y s t is
t a u g h t , u s u a l l y on the job, the v a r i e d a n a l y s e s and m e t h o d s used by the
laboratory.
Most often this is by what amounts to an apprenticeship approach
where the new analyst is assigned to work with a senior.
It is best, however,
to have a formal, structured training programme designed to acquaint the new
analyst with the work in a logical sequence.
Otherwise the training becomes
haphazard with the training sequence dependent on incoming work.
O n c e past the f o r m a l initial t r a i n i n g , the a n a l y s t s t a r t s a c o n t i n u i n g
knowledge updating process.
Food analysis is a rapidly changing subject and it
is i m p o r t a n t that a n a l y s t s attend s y m p o s i a , r e f r e s h e r c o u r s e s and other
educational programmes in order to keep up to date. In developing countries it
may be necessary to schedule travel to other areas from time to time for such
t r a i n i n g . T h i s e f f o r t is e n h a n c e d if the l a b o r a t o r y is a b l e to s u b s c r i b e to
the more active research journals in food analysis.
The analysts are then able
to keep abreast of new advances, especially newer analytical methods.
Should an a n a l y s t s h o w i n t e r e s t and a p t i t u d e for s u p e r v i s i o n , then he or she
s h o u l d be g i v e n f o r m a l c l a s s r o o m t r a i n i n g in s u p e r v i s o r y p r i n c i p l e s .
This
w o u l d be in a d d i t i o n to o n - t h e - j o b e x p e r i e n c e under the t u t e l a g e of a
supervisor or the Head.
It is important that the classroom instruction be done
because it is here that the analyst learns supervision and management theory
and techniques other than those used by his laboratory.
On-the-job experience
as an acting supervisor is necessary but tends to be one dimensional because it
teaches only the systems and techniques used by that laboratory.

28

5.

5.1

LABORATORY

OPERATIONS

Workplans

T h e a n n u a l w o r k p l a n is the c o r n e r s t o n e to m a n a g i n g a food c o n t r o l l a b o r a t o r y .
It p r o v i d e s a m e a n s of e s t i m a t i n g s t a f f a n d r e s o u r c e s n e c e s s a r y to do a f i x e d
n u m b e r of a n a l y s e s .
C o n v e r s e l y , g i v e n a f i x e d s t a f f , the w o r k p l a n can e s t i m a t e
h o w m u c h w o r k can be d o n e .
W o r k p l a n d a t a is a l w a y s o n l y an e s t i m a t e , a l t h o u g h its a c c u r a c y o f t e n
w i t h u s e d u e t o r e f i n i n g o f t i m e m o d u l e s u s e d in c a l c u l a t i o n s .
i m p o r t a n t t i m e m o d u l e s in w o r k p l a n n i n g are:

improves
The two

1.
T h e a n a l y s t p r o d u c t i v e y e a r : T h i s is t h a t t o t a l t i m e i n a n a v e r a g e
year that one a n a l y s t s p e n d s doing o n l y s a m p l e a n a l y s i s .
Time spent during
w o r k h o u r s d o i n g o t h e r t h i n g s is d e d u c t e d .
A n e x a m p l e of t h e d e t e r m i n a t i o n of
t h i s m o d u l e is as f o l l o w s :

Total

time a v a i l a b l e

(based

on 4 0 h o u r w o r k

week)

2080 hr s

Time deductions N a t i o n a l and l o c a l h o l i d a y s

Illness
P e r s o n a l leave time
Training
A d m i n i s t r a t i v e time
Other n o n - a n a l y s i s time
Total time d e d u c t i o n s
Total analysis

time

(2080 -

80
40
80
200
80
400
880

hr s
hrs
hr s
hrs
hrs
hrs
hrs

1200 hrs

880)

T h i s m e a n s ( b a s e d on the a b o v e e x a m p l e ) that for n a n a l y s t s , the

e x p e c t n x 1 2 0 0 h o u r s of p r o d u c t i v e w o r k d u r i n g t h e y e a r .

laboratory

can

T h e a b o v e t i m e d e d u c t i o n f i g u r e s w e r e t a k e n for e x a m p l e p u r p o s e s o n l y .
Each
i n d i v i d u a l l a b o r a t o r y w i l l be d i f f e r e n t .
In d e t e r m i n i n g d e d u c t i o n s , c o n s i d e r
the f o l l o w i n g :
a.

Holiday

time

is u s u a l l y

fixed

b.

I l l n e s s and p e r s o n a l t i m e a v e r a g e s can be t a k e n f r o m
staff
The
a d m i n i s t r a t i v e r e c o r d s f o r t h e p r e c e e d i n g o n e or t w o y e a r s .
a v e r a g e of the p r e v i o u s y e a r is b e s t u s e d as the m o d u l e . T h e r e a s o n
is that the s t a f f u s u a l l y h a v e m o r e p e r s o n a l t i m e m a d e a v a i l a b l e to
t h e m as t h e i r s e n i o r i t y i n c r e a s e s .

c.

M a n a g e m e n t m u s t d e c i d e h o w m u c h t i m e w i l l be set a s i d e e a c h y e a r for
t r a i n i n g . N o t e in the e x a m p l e t h a t t r a i n i n g t i m e is a b o u t 10% of the
t o t a l . If the s t a f f is r e l a t i v e l y y o u n g and i n e x p e r i e n c e d , m o r e t i m e
w i l l be r e q u i r e d .
C o n v e r s e l y an a l l - s e n i o r s t a f f m a y r e q u i r e l e s s .

d.

A d m i n i s t r a t i v e t i m e is d i f f i c u l t to e s t i m a t e as t h e r e are u s u a l l y few
or no r e c o r d s to go b y .
It i n c l u d e s t i m e a s a c t i n g
supervisor,
general
library reading,
and o t h e r a s s i g n e d
or
incidental
administrative activities.

e.

O t h e r n o n - a n a l y s i s t i m e is also o n l y an e s t i m a t e , a l t h o u g h s o m e t i m e
r e c o r d s m a y be a v a i l a b l e .
It i n c l u d e s g e n e r a l r e s e a r c h o r m e t h o d
development
activities,
quality
assurance
work,
equipment
m a i n t e n a n c e , t i m e s p e n t s e r v i n g as a t r a i n e r , a n d a n y o t h e r n o n a n a l y s i s w o r k time not included e l s e w h e r e .

29

by government

policy.

2.
T h e a n a l y t i c a l h o u r s r e q u i r e d per s a a p l e :
The f i r s t step is to
d e f i n e w h a t is i n c l u d e d in a s a m p l e a n a l y s i s , as t h i s o b v i o u s l y a f f e c t s the
total time.
Activities which are suggested to be included are:
a.

Sample receipt and

preparation.

b.

Analysis.

c.

M e t h o d d e v e l o p m e n t or p r o b l e m s o l v i n g r e q u i r e d of a g i v e n s a m p l e .
(As o p p o s e d to g e n e r a l d e v e l o p m e n t or r e s e a r c h , w h i c h w o u l d b e
included in non-analysis time.)

d.

S t a n d a r d i z a t i o n a c t i v i t i e s r e l a t e d to a g i v e n s a m p l e .
standard solutions and curves for example.)

e.

Preparation

of analytical

report and

(Preparing

calculations.

The next step is to prepare a list of all the different analyses conducted and
e s t i m a t e individual analytical times based on experience.
If some analyses are
d o n e b y t e a m s in a p r o d u c t i o n - 1 i n e a r r a n g e m e n t , e s t i m a t e the t o t a l t i m e
required by totalling the time and correcting to an individual analyst basis.
For e x a m p l e , if 4 analysts working as a team can produce 32 completed samples
in an 8 h o u r p e r i o d ,
t h e n t h e a v e r a g e a b s o l u t e s a m p l e t i m e is 0.25
hours/analysis.
H o w e v e r , it required 4 analysts and to correct the time to an
i n d i v i d u a l a n a l y s t b a s i s - 4 x 0.25 = 1.0 h o u r s / ana 1 ys i s . T h i s w o u l d be the
figure used in calculations.
*

The laboratory is now able to make good estimates on what and h o w m u c h work can
be d o n e .
It is a s i m p l e m a t t e r of m u l t i p l y i n g the n u m b e r s of a n a l y s t s
a v a i l a b l e d u r i n g the y e a r t i m e s the p r o d u c t i v e y e a r t i m e m o d u l e to g a i n the
total analytical hours available.
This can then be spread among the types of
a n a l y s e s to be d o n e , u s i n g the h o u r s / a n a l y s i s m o d u l e s .
A l t h o u g h m a n y of the
m o d u l e s are e s t i m a t e s , it is still a better and m o r e accurate w a y to d e t e r m i n e
w h a t can be d o n e , than r e l y i n g on m e m o r y and s h e e r g u e s s e s .
( R e g a r d i n g the
n u m b e r s of a n a l y s t s a v a i l a b l e d u r i n g the y e a r , k e e p in m i n d t h a t t h i s m a y
change by new hires or projected losses, so include these future projections in
the annual estimate).
T h e a b o v e c a l c u l a t i o n m e c h a n i c s of a w o r k p l a n do not a d d r e s s the m e a n s of
d e c i d i n g the a n n u a l w o r k p r i o r i t i e s .
T h i s is u s u a l l y d o n e in p a r t b y
organizational policy and in part by m e e t i n g s of senior operational managers,
s u c h as the L a b o r a t o r y and I n s p e c t o r a t e H e a d s .
All p l a n n e d w o r k and t i m e
modules depend on proper work scheduling and flow.
If samples are collected
too fast or too slow, the laboratory efficiency suffers.
There m u s t therefore
be an extremely close working relationship and liaison b e t w e e n the inspectorate
and l a b o r a t o r y .
No work plan would be complete without some form of contingency planning.
The
o l d a d a g e s t a t e s t h a t , "... If s o m e t h i n g c a n go w r o n g , it w i l l
...".
T h e r e f o r e , t h e r e s h o u l d be at least a p r o v i s i o n in a a n n u a l w o r k p l a n for
e m e r g e n c i e s or u n e x p e c t e d p r o b l e m s .
A m a j o r p u b l i c h e a l t h d i s a s t e r , for
e x a m p l e , could require an all-out laboratory effort, negating workplan work for
some period of time.
The contingency plan would simply and clearly state w h a t
t y p e s of a n a l y s e s ( u s u a l l y the l o w e s t p r i o r i t y ) w o u l d be e l i m i n a t e d in the
event of an emergency.

30

5.2

Priorities

for

General analytical
laboratory policy.

Analysis

priorities are usually s o m e w h a t fixed by organizational

H o w e v e r , a suggested priority structure would be:

Priority 1

Poisonings or
public health

Priority 2

K n o w n or
resulting

Priority 3

Informational

injury complaints
analyses.

s u s p e c t e d law or
in direct injury.
surveys

and

health

other

emergency

violations,

and other routine

or

not

work.

M o s t of the w o r k of a l a b o r a t o r y is u s u a l l y in the t h i r d p r i o r i t y c a t e g o r y ,
with a smattering of priority two and only infrequently, priority one.
W i t h i n a g i v e n p r i o r i t y , the w o r k c a n be s u b - g r o u p e d by r e l a t i v e i m p o r t a n c e .
It is conceivable that work of very low importance never gets done because of
the continuing press of higher priority analyses.
If it appears that such is
the c a s e , the s u p e r v i s o r m u s t a d v i s e the H e a d of the p r o b l e m s and s u g g e s t
r e v i s i o n of the p l a n n e d w o r k load for the s u p e r v i s o r ' s g r o u p .
The w o r k p l a n s
discussed in the previous Section often undergo mid-year or periodic revision
based on such happenings.

5.3

Analysis

Assignaient

A s s u m i n g the p r i o r i t y nas b e e n p r e v i o u s l y a s s i g n e d , the a n a l y s i s a s s i g n m e n t

includes two key considerations, n a m e l y w h a t is to be done and what analytical
method to use.
T h e a n a l y s i s to be c a r r i e d out on a s a m p l e m a y be p r e d e t e r m i n e d as p a r t of a
planned sampling p r o g r a m m e or by legal requirements.
Experience gained by the
analyst may enable him to have firm views on the tests to be done.
The purpose
of the a n a l y s i s m u s t be b o r n e c l e a r l y in m i n d , e.g. for e x p o r t c e r t i f i c a t i o n ,
the t e s t s r e q u i r e d by the i m p o r t i n g c o u n t r y m u s t be c a r r i e d o u t , for e x c i s e
purposes, the constituent that fixes the duty payable and so on.
When samples
are examined under the general and specific provisions of laws pertaining to
consumer protection and food quality, the analysis m u s t be designed to answer
certain questions such as:
Does the food meet established m i n i m u m quality and
safety standards?
Is it of the quality, substance and nature demanded by the
purchaser?
Is it correctly labelled?
Are any claims on the label justifiable
and l e g a l ?
D o e s it c o n t a i n n o n - p e r m i t t e d a d d i t i v e s or p e r m i t t e d o n e s in
excess?
Are any contaminants present at unacceptable levels?
R o u t i n e t e s t s on the p h y s i c a l c h a r a c t e r i s t i c s of m o s t c o m m o n food s a m p l e s
should be carried out.
Less frequently, tests may be made for preservatives,
prohibited colours and other a d u l t e r a n t s .
T h e a d u l t e r a n t s , c o n t a m i n a n t s and
compositional deficiencies looked for should be changed from time to time to
show if previously unsuspected infringements are present.
The analyst m u s t be
aware of the problems facing manufacturers and of developments in technology
and choose non-routine tests in the light of this information.
In this way the
r e g u l a t o r y a n a l y s t acts as a s u p p o r t to the l e g i t i m a t e m a n u f a c t u r e r w h i l e
protecting the consumer.
The analyst must establish that he can obtain reliable results with the method
used.
G e n e r a l l y , it is p r e f e r a b l e to use a m e t h o d t h a t h a s b e e n s u b j e c t e d to
collaborative study.
If the analyst has difficulty
with such a method it is
likely to be due to a deficiency in training or in facilities, rather than the
method itself.
Sometimes
it is d u e to p o o r e x p r e s s i o n of t h e e x a c t

31

e x p e r i m e n t a l d e t a i l s in the m e t h o d as published.
R e f e r e n c e to the source w i l l
usually resolve such difficulty.
It is n o t a l w a y s n e c e s s a r y
to u s e a
collaborated method.
H o w e v e r , s u c h m e t h o d s s h o u l d be f i r s t c h o i c e if the
p a r a m e t e r is b e i n g d e t e r m i n e d in t h e l a b o r a t o r y f o r t h e f i r s t t i m e or if a
p r o d u c t has not been a n a l y z e d p r e v i o u s l y .
It is i m p o r t a n t to f o l l o w the
p r o c e d u r e s ior v a l i d a t i n g a m e t h o d .
M a n y o t h e r m e t h o d s m a y be e q u a l l y g o o d ,
but m a y not, for v a r i o u s reasons, have been subjected to c o l l a b o r a t i v e studies
or r u g g e d n e s s t e s t s .
As a r e s u l t
the a n a l y s t m a y run into
unexpected
d i f f i c u l t i e s if he h a s to t a k e the m e t h o d d i r e c t l y f r o m a b o o k .
If a m e t h o d
has b e e n in use and found to give r e l i a b l e results it should not be changed for
another
until
the n e w m e t h o d
has been s h o w n
to be of e q u a l or b e t t e r
r e l i a b i l i t y in that p a r t i c u l a r l a b o r a t o r y ( i r r e s p e c t i v e o f i t s c o l l a b o r a t i v e
status).
C o n s i d e r a b l e stress is quite r i g h t l y put on c o l l a b o r a t i v e testing at
the p r e s e n t t i m e , but it should not be f o r g o t t e n that a r e l i a b l e m e t h o d is only
a p r e c o n d i t i o n to o b t a i n i n g the r i g h t a n s w e r .
T h e a b i l i t y of the a n a l y s t to
use the m e t h o d
is the e s s e n t i a l r e q u i r e m e n t
and the p e r s o n t a k i n g
the
r e s p o n s i b i l i t y for the result, w h e t h e r the analyst h i m s e l f or the s u p e r v i s o r ,
m u s t be c o n f i d e n t of this.

5.4

Analysis

Control

C o n t r o l is a v e r y i m p o r t a n t s u p e r v i s o r y f u n c t i o n .
It is n o t s u f f i c i e n t to
s i m p l y a s s i g n w o r k and w a i t for r e s u l t s .
T h e r e m u s t be s o m e type of a c t i v e
control in the form of expected c o m p l e t i o n datas, f o l l o w - u p i n q u i r i e s , or other
i n d i c a t i o n s of active interest.
This does not m e a n p e e r i n g over the a n a l y s t ' s
s h o u l d e r , but it does m e a n that the s u p e r v i s o r has c e r t a i n fixed e x p e c t a t i o n s
on w o r k c o m p l e t i o n and e n f o r c e s those e x p e c t a t i o n s .
T h e r e are several m e t h o d s of control but one of the m o r e e f f e c t i v e is also one
of the s i m p l e s t .
The s u p e r v i s o r p r e p a r e s a card for each a n a l y s t .
When a
s a m p l e is a s s i g n e d to the a n a l y s t , the s a m p l e n u m b e r is r e c o r d e d on the c a r d
along w i t h a p r o j e c t e d date of c o m p l e t i o n .
W h e n an a n a l y s i s report is r e c e i v e d
the entry is lined through.
W h e n a'card has been filled, it is discarded and a
n e w one p r e p a r e d .
The p r o j e c t e d c o m p l e t i o n d a t e r e p r e s e n t s t h e s u p e r v i s o r ' s
e s t i m a t e of an a c c e p t a b l e analysis t i m e , a s s u m i n g no p r o b l e m s .
The s u p e r v i s o r
s c a n s t h e c a r d s of a l l a n a l y s t s e v e r y d a y or so a n d if a d a t e h a s e x p i r e d b u t
no report r e c e i v e d , the supervisor inquires of the s a m p l e status.
The analyst
m a y be h a v i n g d i f f i c u l t y a n d h a d n o t m e n t i o n e d it.
A f t e r d i s c u s s i o n , the
s u p e r v i s o r d e c i d e s if a n a l y s i s s h o u l d c o n t i n u e and if so, a s s i g n s a n e w
projected c o m p l e t i o n date.
The s u p e r v i s o r m u s t also a s s i g n n e w dates w h e n
ongoing w o r k m u s t be interrupted by a s s i g n m e n t of h i g h e r p r i o r i t y analyses.

5.5

Analysis

Reporting

A n a l y s i s r e p o r t s are the end p r o d u c t of all of the w o r k of the l a b o r a t o r y and

t h e r e f o r e m u s t be b o t h c o m p l e t e a n d a c c u r a t e .
R e s u l t s of a n a l y s i s are o f t e n
i m p o r t a n t facts in legal p r o c e e d i n g s .
The w a y in w h i c h the technical results
p r o d u c e d by the l a b o r a t o r y reach the court is d i f f e r e n t u n d e r d i f f e r e n t legal
codes.
O n e e x t r e m e is the U.K. w h e r e a c e r t i f i c a t e of a n a l y s i s is a l e g a l l y
v a l i d d o c u m e n t w h i c h m a y b e a c c e p t e d as p r i m a f a c i e e v i d e n c e o f t h e f a c t s
stated therein.
Under R o m a n law, the l a b o r a t o r y report is a technical but not
l e g a l d o c u m e n t w h i c h the c o u r t is e m p o w e r e d to a c c e p t or r e j e c t .
In t h e
U.S.A., f e d e r a l a c t i o n is u s u a l l y i n i t i a t e d by a d o c u m e n t o r i g i n a t i n g in the
J u s t i c e D e p a r t m e n t on the basis of i n f o r m a t i o n from a t e c h n i c a l source.
Under
both R o m a n law and in the U.S.A., all prepared laboratory and technical records
r e l e v a n t to t h e s a m p l e m a y h a v e to be p r o d u c e d in c o u r t and t h e s a m p l e r and
analyst cross-examined.
T h i s o c c u r s l e s s f r e q u e n t l y u n d e r U.K. l a w w h e r e
c r o s s - e x a m i n a t i o n of the expert w i t n e s s is u s u a l l y all that is done, a l t h o u g h
if he did refer to original notes or c a l c u l a t i o n s they w o u l d b e c o m e a v a i l a b l e
to the c o u r t as in the U.S.A.
T h u s , it is m a i n l y u n d e r l e g a l c o d e s d e r i v e d

32

from Roman and c o m m o n law that the report or certificate of the analyst assumes
greater importance.
U n d e r b o t h R o m a n and U.S.A. l a w the e n t i r e l a b o r a t o r y
records relating to the sample must be capable of wi ths tand ing the scrutiny of
the c o u r t and d e f e n s e l a w y e r s .
The p r a c t i c a l e f f e c t of t h e s e d i f f e r e n c e s is
not great. Under any system it is necessary for the regulatory chemist to have
legally impeccable laboratory data records and to report against samples in a
w a y that is u n d e r s t a n d a b l e to the l a y m a n , b r i e f , s u c c i n c t , and free from
irrelevancy.
T h e f o r m a t of an a n a l y s i s r e p o r t is d i c t a t e d by the a d m i n i s t r a t i v e and legal
needs of the organization.
The report form should be preprinted with blocks or
l i n e s of i n f o r m a t i o n p l a c e d in d e s i g n a t e d a r e a s on the f o r m .
This p e r m i t s
faster and m o r e uniform write-up, as well as easier final review (the reviewer
knows where to look on the form for different information).
A complete report
form would have spaces for the following information:

Sample number
Product name
Product description and amount
Date received for analysis
Labelling (if any)
Analysis method used
Analysis results
Reserve product amount
Date completed
Total analysis time in hours (if needed

for time

modules).

Raw work data and standardization information can be placed on the reverse side
of the analysis report or can be kept separately in notebooks.
In any case it
s h o u l d be a c c e s s i b l e to the r e v i e w e r in the e v e n t of q u e s t i o n .
It is b e s t to
include all raw data so that the entire sequence of work can be reconstructed
later if needed.
Calculations m u s t be clear w i t h all equations stated.
There
is no w a y to d e t e r m i n e if a c a l c u l a t i o n is c o r r e c t w i t h o u t c h e c k i n g the
T h i s , of c o u r s e , m e a n s
c a l c u l a t i o n s y s t e m u s e d , as w e l l as the a r i t h m e t i c .
that all dilutions or other operations affecting the final calculation must be
clearly stated in the raw data.
R e s u l t s m u s t a l w a y s be r e p o r t e d o n l y to a n u m b e r of s i g n i f i c a n t
figures
j u s t i f i e d by the a c c u r a c y and p r e c i s i o n of the m e t h o d .
In g e n e r a l , it is
p r u d e n t to r e p o r t to as few s i g n i f i c a n t f i g u r e s as p o s s i b l e c o n s o n a n t w i t h
stating the facts the report has to convey.
For e x a m p l e , for most purposes it
m a y be a d e q u a t e to r e p o r t a s a m p l e as c o n t a i n i n g "not less ( m o r e ) than 70
percent of y".
The report m u s t be clear and confined to factual information,
and statements which cannot be substantiated must not be made.

5.6

Analysis

Review

T h e a n a l y s t should not d r a w c o n c l u s i o n s from the w o r k r e p o r t e d .

T h i s is
r i g h t f u l l y the job of the s u p e r v i s o r , w h o is n o r m a l l y the a n a l y s i s r e p o r t
reviewer.
The reviewer should ask himself a number of questions while reading
the report.
Any negative answers should be clarified by the analyst before the
report is accepted.
Some possible questions are:
Is the report generally complete?
(Any missing required information?)
Are the product descriptions adequate?
Was the correct method used?
Has sufficient work been done to draw a conclusion?
Have the proper standards and reagents been used?
Is there a blank?
Are the calculations easy to follow and accurate?
Are any strike-outs or discarded data explained?

33

5.7

Method

Validation

As discussed e l s e w h e r e , it is correct and proper to use collaboratively studied

methods w h e r e possible.
Such methods have already been shown to be capable of
use in different laboratories.
H o w e v e r , it is often necessary or advisable to
use a locally developed method or one which was selected from the literature,
but a b o u t w h i c h l i t t l e is k n o w n .
In such c a s e s the m e t h o d m u s t be v a l i d a t e d
for use in the local laboratory.
Method validation can take many forms, but the usual procedure is to examine a
k n o w n s a m p l e , or a k n o w n m a t e r i a l a d d e d to a s a m p l e , to d e t e r m i n e the m e t h o d
accuracy and precision.
For a contaminant residue, as example, a k n o w n amount
of reference grade contaminant would be added to a blank sample and replicate
assays done to determine the percentage recoveries.
In this type of recovery
v a l i d a t i o n it is i m p o r t a n t to be s u r e w h a t p a r t or p a r t s of the a n a l y s i s are
being evaluated.
A g a i n u s i n g the c o n t a m i n a n t e x a m p l e , a d d i t i o n of the
r e f e r e n c e c o n t a m i n a n t to the s a m p l e e x t r a c t s o l u t i o n d o e s n o t e v a l u a t e the
e x t r a c t i o n of the c o n t a m i n a n t , o n l y its p a s s a g e t h r o u g h c l e a n - u p and f i n a l
assay.
C o n t i n u i n g r e c o r d s of m e t h o d v a l i d a t i o n s should be kept for future reference
and to d e m o n s t r a t e the u s e f u l n e s s of the m e t h o d s .
N e g a t i v e d a t a is a l s o
desirable.
For e x a m p l e , if a method was tried and could not be satisfactorily
validated, that information should be recorded to avoid future attempts.
T h e r e c o v e r y d e t e r m i n a t i o n is o n l y one type of d i r e c t v a l i d a t i o n .
T h e r e are
also indirect validations where concurrent analyses are run on a given sample
using a new method as well as an established, accepted method. This provides a
direct experimental comparison.
T h i s is a good s y s t e m w h e n an a l t e r n a t e
procedure is needed for an official or referee method.

5.8

Confirming

Analysis

W h e n an o r i g i n a l a n a l y s i s s h o w s the s a m p l e to be in v i o l a t i o n of l a w or
regulations in some m a n n e r , the supervisor m u s t decide if a second analysis by
the o r i g i n a l a n a l y s t is n e e d e d .
T h i s s h o u l d o n l y be d o n e if t h e r e is s o m e
doubt that the original analysis w a s done correctly.
In the event that there are no apparent errors in the original analysis, then a
c o n f i r m i n g a n a l y s i s b y a s e c o n d a n a l y s t s h o u l d be d o n e as f o l l o w s :
A fresh
p o r t i o n of s a m p l e s h o u l d be p r e p a r e d ( u n l e s s it is n e c e s s a r y or d e s i r a b l e to
u s e the o r i g i n a l ) and a n a l y z e d u s i n g a s e c o n d m e t h o d (if p o s s i b l e ) and n e w
standard reference material.
If the a d v e r s e f i n d i n g s are r e p e a t e d by the
c o n f i r m i n g analyst, then it is extremely likely that a violation exists.
If,
h o w e v e r , t h e r e is no c o n f i r m a t i o n , then the s u p e r v i s o r m u s t m e e t w i t h b o t h
a n a l y s t s and d e c i d e w h a t is to be d o n e .
It m a y be t h a t the m e t h o d s are n o t
c o m p a t i b l e , if so a recheck using the original method might be in order.
It is
a l s o o f t e n v e r y u s e f u l to c r o s s c h e c k the s t a n d a r d s u s e d b y e a c h a n a l y s t to
ensure they compare.
Confirming analysis is basically an attempt to ensure that any violation of law
The e n f o r c e m e n t laboratory
or regulation has substance and is not a mistake.
c a n n o t a f f o r d to m a k e any m i s t a k e s , so it is n e c e s s a r y to p r o v e that all
adverse results are correct.

34

6.

6.1

The Safety

LABORATORY

SAFETY

Programme

The Head of the laboratory and supervisors must emphasize to all the laboratory
staff, their c o m m i t m e n t and d e t e r m i n a t i o n to e n s u r e s a f e l a b o r a t o r y w o r k i n g
conditions.
One staff m e m b e r s h o u l d be a p p o i n t e d the " S a f e t y O f f i c e r " and
given the responsibility to m o n i t o r safety procedures, practices and equipment
on a routine periodic basis.
In a large laboratory, the Safety Officer may be
assisted by a c o m m i t t e e of two or three analysts.
The d u t i e s of the S a f e t y O f f i c e r (and c o m m i t t e e w h e r e a p p r o p r i a t e ) s h o u l d be
d e t a i l e d in the l a b o r a t o r y S a f e t y P r o g r a m m e .
This p r o g r a m m e would indicate
safety requirements, hazards, equipment and emergency procedures.
Items which
can be included in a laboratory Safety P r o g r a m m e are discussed in the following
sections.
It should be r e m e m b e r e d that the Head h a s the final a u t h o r i t y as
w e l l as r e s p o n s i b i l i t y for l a b o r a t o r y s a f e t y , so t h a t the S a f e t y O f f i c e r m a y
only make recommendations.

6.2

Basic

Safety

Rules

E a c h l a b o r a t o r y s h o u l d d e v e l o p its o w n set of g e n e r a l s a f e t y r u l e s , and m a k e

sure that all m e m b e r s of staff are aware of them by supplying personal copies
of the r u l e s and by p o s t i n g c o p i e s on n o t i c e - b o a r d s .
T h e r u l e s s h o u l d be
changed and developed in the light of experience.
Some that should be included
are listed below:
1.
B e c o m e f a m i l i a r w i t h the l o c a t i o n and use of e m e r g e n c y
(e.g., f i r e e x t i n g u i s h e r ; e y e w a s h f o u n t a i n s ; s a f e t y s h o w e r s ;
cabinets).
Know where to go in case of fire.

equipment,
f i r s t aid

2.
Before beginning a sample analysis, review possible hazards connected
w i t h the a s s i g n m e n t and take the n e c e s s a r y p r e c a u t i o n s to e l i m i n a t e or
counteract the hazard.
3.
Use, when appropriate, the safety equipment provided for protection,
(e.g., s a f e t y g o g g l e s ; face s h i e l d s ; v a r i o u s t y p e s
of g l o v e s ) .
Wear a
laboratory coat routinely since its purpose is to serve as protective clothing.
4.
Bring all accidents and hazardous
supervisor or Head immediately.

conditions

to the attention of

the

5.
W h e n l i f t i n g h e a v y o b j e c t s , use the legs i n s t e a d of the b a c k .
Bend
the knees and hold the back straight so that the lifting effort is accomplished
w i t h the legs r a t h e r than the back.
L i f t s l o w l y to j u d g e the w e i g h t of the
object.
If too heavy, obtain assistance and/or use a lifting device.
6.
Be
jewelry (like
equipment.
entangled in

extremely careful of loose clothing, neckties, scarves, dangling

necklaces) and long h a i r w h e n u s i n g r e v o l v i n g or r e c i p r o c a t i n g
K e e p such i t e m s b o u n d or c o n f i n e d so that they w i l l not be
the equipment.

7.
T u r n off l a b o r a t o r y s e r v i c e s (gas, w a t e r , etc.) at the s e r v i c e c o c k
w h e n not in use. Changes in pressure m a y suddenly dislodge tubing connected to
an apparatus and lead to an accident or possible injury.
8.
Always use mechanical aids, such as safety bulbs
when pipetting hazardous material.
Never use the mouth.

35

or pipette

fillers,

9.
Use fume hoods for any analytical operations
of solvents, or w h e n noxious fumes will be generated.

their

10.
Keep the
contents.

work

area

neat

11.
Any chemicals, whether
m u s t be washed off immediately.

even

12.
Keep fire escape
temporarily.

routes

and

tidy,

toxic

and

13.
No one s h o u l d w o r k a l o n e
available in the event of accident.

with

or not,

doors

in the

all

which

clear

involving

large

containers

are

at all

laboratory,

labelled

spilled

times.

so that

amounts

on

the

Do not

with

hands

block,

assistance

is

14.
The last person to leave the laboratory at the end of the working day
m u s t c h e c k that all e q u i p m e n t t h a t s h o u l d be t u r n e d o f f h a s b e e n .
(This d o e s
not release each individual operator from his duty to turn off the equipment no
longer in use.)
The laboratory Head in consultation with staff m a y prefer to
operate a duty roster for opening the laboratory in the morning and closing at
the end of the w o r k i n g day.

6.3

Fire

Safety

A laboratory m u s t unfortunately be regarded as one of the more likely places in

w h i c h a fire w i l l o c c u r and it is t h e r e f o r e p r u d e n t to h a v e the l o c a l c h i e f
fire officer visit the building, be familiarized with the problems and advise
the laboratory staff about local fire regulations and further safety m e a s u r e s
that s h o u l d be t a k e n .
F i r e and s m o k e d e t e c t o r s m a y be i n s t a l l e d in the
b u i l d i n g and c o n n e c t e d so t h a t in the e v e n t of f i r e , an a l a r m is g i v e n at a
fire s t a t i o n .
C a r e m u s t be taken that s m o k e d e t e c t o r s are not set off
a c c i d e n t a l l y by b e g i n n i n g the a s h i n g of s a m p l e s in the o p e n l a b o r a t o r y or
excessive formation of smoke in other ways.
S t a f f m u s t h a v e c l e a r i n s t r u c t i o n s of the a c t i o n to be t a k e n in c a s e of fire.
Such i n s t r u c t i o n s s h o u l d be p o s t e d p r o m i n e n t l y in v a r i o u s p a r t s of the
building.
O c c a s i o n a l l y t h e r e s h o u l d be a fire d r i l l to c h e c k that e v e r y o n e
k n o w s w h a t to do in the case of a s e r i o u s fire and to m a k e sure that the
building can be evaculated in an orderly and rapid manner.
Once evacuated, a
r o l l c a l l is t a k e n to c h e c k that no one r e m a i n s in the b u i l d i n g .
Such a roll
call m u s t be completed in a very few minutes and therefore should be called in
groups if the total staff exceeds about 20-30.
A fire evacuation must include
switching off the electricity supply to the affected area, as short-circuits
may result in further fire hazard.
Isolation switches are important to enable
restricted areas of the building to be cut off from the supply.
H o w e v e r , for a
p r a c t i c e d r i l l , the s w i t c h i n g off can be s i m u l a t e d .
W h e n n e w s t a f f are
introduced, they m u s t have the drill explained to them and be shown where fire
e x t i n g u i s h e r s , b l a n k e t s , h o s e s and b u c k e t s are k e p t , and h o w the s p r i n k l e r
system w o r k s if there is one.
Breathing apparatus should be available at two or three points in the building,
and an adequate n u m b e r of people instructed in its use. In dealing with a fire
in a laboratory toxic fumes are always possible.
F i r e e x t i n g u i s h e r s in the l a b o r a t o r y s h o u l d be of the c a r b o n d i o x i d e type.
Pressurized dry chemical extinguishers are suitable for general use, but should
n o t be u s e d a r o u n d c o m p u t e r s or o t h e r s e n s i t i v e e l e c t r o n i c e q u i p m e n t .
The
r e a s o n is that it is n e a r l y i m p o s s i b l e to c l e a n the dry c h e m i c a l out of the
instrument., and the instrument could be irreparably damaged.
Carbon dioxide
units work best.
Everyone in the laboratory should have used an extinguisher
at l e a s t o n c e , so t h a t t h e y k n o w h o w to r e m o v e the s a f e t y p i n as r a p i d l y as
possible and are not disconcerted by the sudden noise when it is activated.
If

36

any s t r u c t u r a l part of the b u i l d i n g a p p e a r s a f f e c t e d by a s m a l l f i r e , it is

a d v i s a b l e to i n f o r m the fire s t a t i o n , s i n c e a f i r e that m a y a p p e a r to b e
extinguished in fact may be smouldering behind a panel or other structure and
break out again several hours later, perhaps after the laboratory is closed for
the night.
A d i s c u s s i o n of b u l k s o l v e n t s t o r a g e and c o n s t r u c t i o n of a s t o r a g e r o o m is
contained in Section 3.3 of this manual.
The quantitites of f l a m m a b l e liquids
in the laboratory should be kept at a m i n i m u m .
Bottles should be stored away
f r o m h e a t , s u n l i g h t and any s o u r c e of n a k e d f l a m e .
V a p o u r s such as t h o s e of
diethyl ether can flow along surfaces such as floors and benches and thus, by
c o n t a c t w i t h a n a k e d f l a m e or a h o t s u r f a c e (such as
a m u f f l e f u r n a c e or
h o t p l a t e ) b e c o m e i g n i t e d . S o l v e n t s m u s t be s t o r e d in an e x p l o s i o n - p r o o f
refrigerator, separately from acids and other reagents.
Some chemicals ignite
spontaneously on mixing, for example concentrated nitric acid with alcohols.
E l e c t r i c a l e q u i p m e n t m a y be the s o u r c e of a fire d u e to f a u l t y
wiring,
inadequate earthing, failure causing sparks or local overheating or switchgear
sparks.
A l l e l e c t r i c a l e q u i p m e n t s h o u l d c a r r y a f u s e w h i c h b l o w s at an
amperage
s l i g h t l y in e x c e s s of that r e q u i r e d by the e q u i p m e n t .
It is
c o m m o n p l a c e to find that equipment drawing only one or two amps have a 13 or 15
Flammable
amp fuse which is unlikely to be of any use if anything goes wrong.
vapour near electrical equipment represents a fire hazard unless the instrument
h a s b e e n r e n d e r e d " e x p l o s i o n p r o o f " by s e a l i n g t h o s e s e c t i o n s w h e r e a s p a r k
could occur.
Motors m u s t be serviced regularly.
Lack of attention m a y result
in o v e r h e a t i n g and s u b s e q u e n t fire.
C e n t r i f u g i n g of v o l a t i l e
flammable
s o l v e n t s is h a z a r d o u s
if the c e n t r i f u g e m o t o r
is n o t e x p 1 o s i o n - p r o o f ,
especially if the tube breaks.
S t a t i c e l e c t r i c i t y and s t a t i c s p a r k s can be a real p r o b l e m in a h o t and dry
climate.
They can result from wearing clothes m a d e of synthetic m a t e r i a l s , or
by simply walking across a carpet.

6.4

Chemical

Hazards

All c h e m i c a l s s h o u l d be c o n s i d e r e d as p o t e n t i a l l y h a z a r d o u s and s h o u l d be
treated with caution.
As far as possible, dangerous c h e m i c a l s should be stored
away from the laboratory and away from others with which they violently react.
Y e l l o w p h o s p h o r u s and p i c r i c acid m u s t be k e p t u n d e r w a t e r , s o d i u m and
potassium metal under oil.
Explosive peroxides can be formed in diethyl ether.
T h e y s h o u l d a l w a y s be r e m o v e d if f o u n d to be p r e s e n t , as an e x p l o s i v e
concentration
of p e r o x i d e m a y b e f o r m e d
if t h e e t h e r is d i s t i l l e d .
Distillation should be stopped while there is plenty of solvent remaining in
the d i s t i l l a t i o n flask and care s h o u l d be t a k e n not to o v e r h e a t the flask.
D u s t m a y c a u s e the e x p l o s i v e d e c o m p o s i t i o n of h y d r o g e n p e r o x i d e of o v e r 30
percent concentration.
Peroxides in general can be explosive, and must not be
allowed to come into contact with reducing agents or f l a m m a b l e solvents.
They
should be kept in dark bottles in a refrigerator.
Hydrogen fluoride solution
is e x t r e m e l y dangerous as contact w i t h the skin may result in lesions that fail
to heal.
Disposable plastic gloves must always be worn when this solution is
being handled.
Calcium gluconate gel or solution or another antidote should be
available in the first-aid cabinet.
Toxic levels of nitrogen dioxide can be produced during the use of the nitrous
oxide-acetylene flame in atomic absorption spectrophotometry and consequently
ventilation must be good.
The recommended threshold limit value (TLV) for 40
m i n u t e s exposure is 5 ppm.
Tubes for testing contaminated air
are available
c o m m e r c i a l l y from laboratory supply firms.
It is important that bottles containing sodium and potassium (for example w h e n
these have been used for drying ether) are
not left near a washing-up area in
case an inexperienced or unobservant person attempts to wash the bottle in the

37

u s u a l way.
In fact, all c o n t a i n e r s ( b e a k e r s , e t c ) c o n t a i n i n g h a z a r d o u s
material must first be rinsed or otherwise treated by the analyst to remove the
h a z a r d , b e f o r e giving to g l a s s w a r e w a s h i n g .
The need for this is o b v i o u s
as the analyst is the only one who knows of the hazard and how to eliminate it.
All reagent bottles, flasks or other containers must be properly labelled, even
if the c o n t e n t s are c o n s i d e r e d h a r m l e s s .
A d h e s i v e w a r n i n g s t i c k e r s can be
p u r c h a s e d from c h e m i c a l s u p p l y f i r m s .
T h e s e can be used in a d d i t i o n to the
container label to highlight hazards.
When emptying acids and chromic acid cleaning solutions into the drains, first
fill the sink with water, pour the acid or cleaning solution into the sink, and
then let the w a t e r run out.
A l l o w the tap to r e m a i n on full for a few
additional minutes.
Dilution should always be sufficient to reduce the acid
concentration to less than one normal.
Store acid containers in inert trays if
the acid c o n c e n t r a t i o n is g r e a t e r than 2N. P o l y e t h y l e n e t r a y s are s u i t a b l e .
Handle concentrated ammonium hydroxide and solutions of potassium and sodium
hydroxide which are ION or above as if they were concentrated acids and observe
the s a m e p r e c a u t i o n s as for acids. Do not store A L K A L I in the s a m e tray w i t h
ACID.
Do not store concentrated alkalies in glass-stoppered bottles.

6.5

Biological

Hazards

This manual is concerned primarily with a chemical analysis laboratory rather

than a m i c r o b i o l o g i c a l one.
H o w e v e r , t h e r e are b i o l o g i c a l h a z a r d s in the
typical chemical analysis laboratory.
The m o s t s e r i o u s of these are the
c a r c i n o g e n i c r e a g e n t s or r e f e r e n c e m a t e r i a l s c o m m o n to f o o d c o n t r o l
laboratories.
Carcinogens must always be handled with extreme care, using all
available protective gear.
The f o l l o w i n g listing is of s u b s t a n c e s used in a food c o n t r o l l a b o r a t o r y , or
found as food contaminants, which are suspected or k n o w n to be carcinogens:
Category

Reference

Aflatoxins

Potent

carcinogen

6,7

4-(or p-) Aminobiphenyl

Biphenylamine

Potent

carcinogen

1,2,6

Asbestos

Carc inogen

Auramine, or 4,4'dimethylaminobenzophenonimide

Suspected

carcinogen

2,6

Benzene, benzol(e)

Suspected

carcinogen

4,5,6

Benzidine,
diamide,

Potent

carcinogen

2,6

3,4-(or 1,2-) Benzpyrene

Potent

carcinogen

Cadmium and Compounds

(mainly inorganic)

Suspected

Carbon

Carc inogen

4,4'-biphenyldiaminobiphenyl

tetrachloride

Suspected

Chloroform (trichlorome thane)

Chromium

salts (3 and

6+)

Carc inogen

38

3,6

carcinogen

6,9

6
carcinogen

3,6,7

Ne

Catetory

Reference

Coal tar, Creosote oils

(polycyclic mixtures)

Care inogen

3,4,6

DDT

Suspected

(p,p*

or o,p')

o-Dianisidine

Care inogen

Diazomethane

Suspected

Dichloroethane

Carcinogen

4-Diethylaminoazobenzene
(Butter Y e l l o w )

Suspected

N,N-Dimethylnitrosamine

Potent

Dimethyl

Carcinogen

sulphide

1,4-Dioxane
ether

(diethylene

carcinogen

2,6
carcinogen

4,5,6
-

carcinogen

carcinogen

6,8
-

6,9

Carcinogen

Teratogen

Formamide

5,6

Suspected

carcinogen

Magenta basic or Basic

fuchsin (basic red 9,
basic violet, 14 rosaniline)

Suspected

carcinogen

2,6

Mineral

Carc inogen

3,6

1-Naphthylamine
(1-amino-naphthalene)

Care inogen

2,6

2-Naphthylamine
(2-amino-naphthalene)

Potent

Nickel

Carcinogen

4,6

Nitrobenzene

Carcinogen

Nitrosamines

Potent

Patulin

Suspected

carcinogen

Rhodamine B

Suspected

carcinogen

Suspected

carcinogen

Magenta

acid or Acid

oils

and

fuchsin

(heavy)

salts

Sodium diethyl
Soot, carbon

dithiocarbamate

black

carcinogen

carcinogen

Carcinogen

1,2,6

3,6

Tannins

Suspected

carcinogen

5,6

Thioacetamide

Suspected

carcinogen

4,5,6

Thiourea

Suspected

carcinogen

4,5,6

Trichloroethylene

Suspected

carcinogen

Vinylchloride

Carcinogen

Zearalenone

monomer

Suspected

39

10
carcinogen

11,12

The references noted

in the listing

are:

1.

Bo y 1 and, E. (1 963). "The B i o c h e m i s t r y of B l a d d e r Cancer."

Springfield, Illinois.

2.

C h e s t e r B e a t t y R e s e a r c h I n s t i t u t e (1966).
" P r e c a u t i o n s for L a b o r a t o r y
Workers who handle Carcinogenic Aromatic Amines."
The Institute, London;
reprinted with additional notes 1971, i. 7 pp.

3.

Clayson, D.B.

4.

D e w h u r s t , F. (1972).
10, 57-85, passim.

5.

Hueper,
Cancer."

6.

From International Agency for Research on Cancer, IARC Monographs on the

" E v a l u a t i o n of C a r c i n o g e n i c Risk of C h e m i c a l s to Man."
IARC, L y o n / W H O ,
Geneva/HMSO, London.

7.

R o e , F.J.C. and L a n c a s t e r , M.C. (1964), " N a t u r a l M e t a l l i c

Br. med. Bull., 2J)> 127-133.
Substances as Carcinogens."

8.

S e a r l e , C.E. (1972).

9.

National Institute of Occupational S a f e t y and H e a l t h (1975) - " S u s p e c t e d

C a r c i n o g e n s List." U n i t e d S t a t e s D e p a r t m e n t of H e a l t h E d u c a t i o n and
Welfare Publication No. (NIOSH) 75-188.

10.

Maltoni,

11.

Ueno, Y. and Kubota, K., (1976), Cancer Research, 36_ (2) 445-451.

12.

Schoental, R. , (1974), Br. J. Cancer, 30, ISS _2, 181.

6.6

Physical

(1962).

"Chemical Carcinogenesis."
"Carcinogens

C.C. T h o m a s ,

Churchill.

in the L a b o r a t o r y . "

W.C. and C o n w a y , W.D. (1964).

"Chemical
C.C. Thomas, Springfield, Illinois.

Lab. Equip. Dig.,

Carcinogenesis

and

and

other

" C h e m i c a l C a r c i n o g e n s . " C h e m . Ind., (3) 1 1 1 - 1 1 6 .

C. and Lefemine, G., (1974), Environmental

Research, _7, p.387.

Hazards

There are many physical hazards in a laboratory.

Most are avoidable by use of
c o m m o n sense.
It is advisable, however, to prepare some instructions for new
e m p l o y e e s and p e r i o d i c a l l y r e m i n d o t h e r s . The f o l l o w i n g are s o m e p r o p o s e d
instructions, grouped by operation.

Glassware Handling

1.
Do not use b r o k e n or chipped g l a s s w a r e or r e t u r n it to s t o r a g e .
If
it is b e y o n d r e p a i r , d i s p o s e of it. W h e n in d o u b t r e g a r d i n g p r o p e r d i s p o s a l ,
consult the supervisor.
Always use gloves in handling broken glass.
2.
R e m o v e s h a r p or jagged e d g e s from g l a s s w a r e b e f o r e u s i n g it.
polish the edges on all glass tubing.

Fire

3.
Broken glass in sinks present a definite hazard since glass may not
be v i s i b l e in the p r e s e n c e of w a t e r .
W h e n b r o k e n in the sink, r e m o v e it
promptly.
F u r t h e r m o r e , c o n s i d e r the p o s s i b i l i t y of the p r e s e n c e of b r o k e n
glass when reaching into the sink for any purpose.

40

4.
Inserting tubing into stoppers or rubber tubing can result in serious
cuts, which can be prevented if the following precautions are observed:
a.
b.
c.
d.
e.

Wet the tubing and/or stopper or rubber tubing.

Wear gloves or wrap a towel around the palms of the hands.
Do not use e x c e s s i v e force - cut the h o l e b i g g e r or b o r e a n e w
hole .
Use the fingers and not the hands when making the insertion.
Insert glass or metal tubing entirely through stoppers to assure
that the end may not be closed over by heat or solvent action on
the stopper.

5.
To remove glass tubing or thermometers from rubber, preferably cut
a w a y the r u b b e r . T h i s is p a r t i c u l a r l y true if the t u b i n g or s t o p p e r has b e e n
in place over an extended period of time or has been subjected to heat.
6.
In handling beakers, support them by grasping around the sides, never
over the top. If one hand will not reach more than half way around the beaker,
use both hands. Support large beakers (one litre or more) from the bottom when
in use.
7.
W h e n h e a t i n g l i q u i d s in g l a s s by m e a n s of a gas f l a m e , p r o t e c t the
glass from direct contact with the flame by use of a wire gauze or a centered
wire gauze.
8.
W h e n p l a c i n g l i q u i d s in b o t t l e s w h i c h h a v e a p o s i t i v e c l o s u r e ,
reserve more than 5 percent of the volume as air space to allow for expansion
due to temperature changes.
9.
Do not force s t o p c o c k s or ground g l a s s s t o p p e r s .
Use a s t o p c o c k
puller.
If the n a t u r e of the c o n t e n t s of the v e s s e l p e r m i t s , cool the shell
until the plug is cold, then heat the shell of the joint momentarily.
Withdraw
the plug quickly before it too has been expanded by the heat.

Vacuus Operations

1.
Protect glassware under vacuum from physical
cracks and result in collapse with explosive violence.

shock which might

2.
Do not subject flat-bottom flasks
heavy walls specifically for such service.

unless

to vacuum

cause

constructed

with

3.
Guard s t a n d a r d - w a l 1 ( s p h e r i c a l ) flasks larger than one l i t r e , w h e n
used in v a c u u m s e r v i c e , by a shield that is a d e q u a t e to stop all flying g l a s s
if collapse should occur.
4.
C h o o s e cork or r u b b e r s t o p p e r s used in v a c u u m s e r v i c e c a r e f u l l y .
They must be of such size that they will not be drawn through the opening which
they are intended to close.
5.

Relieve vacuum before attempting

to disassemble

equipment.

6.
Do not s t o p p e r h o t flasks c o n t a i n i n g u n c o n d e n s e d v a p o u r s or
To do so will subject them to vacuum on cooling.

41

steam.

Equipment

Handling

1.
W h e n using a m a n u a l cork b o r e r , do not hold the s t o p p e r in the p a l m
of the hand.
Place the stopper large end down on a soft, flat surface and hold
in p l a c e w i t h the t h u m b and f o r e f i n g e r .
K e e p the b o r e r sharp and l u b r i c a t e
with water or glycerine to prevent binding. Do not force the borer through the
stopper but twist to cut the material.
Use stout gloves for added protection
in case of slippage.
2.
Do
not lift the cover of a c e n t r i f u g e until r o t a t i o n has
Keep the cover closed when the centrifuge is not in use.

stopped.

3.
C y l i n d e r s c o n t a i n i n g i n d u s t r i a l gases must be properly anchored by
chains or heavy straps or held in stands.
Reactive gases should be stored away
from each other (e.g. do not store a c e t y l e n e near oxygen).
Gas s u p p l i e s for
gas liquid chromatography and atomic absorption spectroscopy are best kept on
the other side of the wall from the instrument and connected via a small duct
in the w a l l .
C y l i n d e r s t o r a g e p o i n t s s h o u l d be p r o t e c t e d from the w e a t h e r ,
p a r t i c u l a r l y in dusty areas w h e r e grit can get into the c y l i n d e r v a l v e , but
they s h o u l d be s u f f i c i e n t l y w e l l - v e n t i l a t e d to p r e v e n t l e a k i n g gas f r o m
reaching dangerous levels.
4.
Flexible tubing attached to gas supplies must be wired on or held by
clips and must be able to withstand any likely pressure.
The sudden bursting
or b l o w i n g off of a piece of tubing is s t a r t l i n g and m a y c a u s e an a c c i d e n t if
someone nearby is carrying out a hazardous operation.
5.
A rapid decrease of cooling water due to a fall in mains pressure or
a cut in the supply can damage equipment such as a still and also be hazardous.
A c o n s t a n t head d e v i c e in a t r a n s p a r e n t c o n t a i n e r w i l l give s o m e w a r n i n g of
this. However, if water pressure fluctuations are a frequent problem, a header
tank in the roof of the building may be advisable. Electrical equipment can be
fitted with automatic cutouts that turn off the electricity supply in case of
water failure.

6.7

Safety and Emergency

Equipment

" S a f e t y " e q u i p m e n t is that d e s i g n e d to p r o t e c t a n d / o r p r e v e n t i n j u r y and is

used b e f o r e an a c c i d e n t h a p p e n s .
" E m e r g e n c y " e q u i p m e n t is used a f t e r an
accident (or other emergency) to minimize the injury or damage. Therefore, eye
goggles are "safety" and eye wash fountains are "emergency" equipment.
U s i n g these d e f i n i t i o n s , the f o l l o w i n g are lists of safety and
equipment which every laboratory should include in their inventory:

emergency

Safety Equipment

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

Rubber aprons.
Eye goggles.
Face shields..
Disposable plastic or rubber gloves.
Bench shields (portable, clear plastic).
Pipetting bulbs.
Heavy rubber carriers for acid and alkali bottles.
Metal safety cans for flammable solvents.
M e t a l solvent s t o r a g e c a b i n e t s (about 45 g a l l o n
storage of solvents used daily in the laboratory).
Respirator filter masks (for dust or fumes).
42

capacity).

(For

Emergency

1.
2.
3.
4.
5.
6.

Equipment

Hand-held fire extinguishers (carbon dioxide preferably, see Section

6.3) .
Fire blankets (wall mounted).
Eye wash stations (built-in fountains or portable kits).
S p i l l a g e a b s o r b e n t kits for both a c i d s and s o l v e n t s ( a v a i l a b l e
commercially or can be assembled locally).
Emergency shower (in the laboratory, drenching full-on or -off valve
operated by a pull chain or loop).
Respirator mask with oxygen supply.

A major item of emergency equipment not included in the above list is the
aid cabinet.
This is discussed in detail in Section 6.8.

first

All such e q u i p m e n t is u s e l e s s if e i t h e r not a v a i l a b l e or not in s e r v i c e a b l e

condition.
The Safety Officer (see Section 6.1) should periodically check both
the s t o r a g e l o c a t i o n s (if n o t in u s e ) and the c o n d i t i o n of all safety and
emergency equipment.
The laboratory staff must also be trained in the use of
the equipment and use must be enforced when necessary.

6.8

First

Aid

First aid by definition is that initial assistance given to lessen the effect
of injury.
If the injury is sufficiently minor, then first aid will probably
s u f f i c e for t r e a t m e n t .
H o w e v e r , for s e r i o u s and e v e n m o d e r a t e l y s e r i o u s
i n j u r i e s , m e d i c a l h e l p m u s t be g i v e n as soon as p o s s i b l e .
Any first aid
m e a s u r e s w o u l d be only to give t e m p o r a r y h e l p u n t i l m e d i c a l t r e a t m e n t is
available.
S o m e o n e on the l a b o r a t o r y s t a f f s h o u l d be t r a i n e d in f i r s t - a i d ,
particularly in giving artificial respiration techniques.
Some chemicals such
as c y a n i d e are q u i c k - a c t i n g and there is r a r e l y t i m e to w a i t for a d o c t o r to
arrive, or transfer the patient to the hospital.
T h o u g h t s h o u l d be g i v e n to the l o c a l h a z a r d s that m i g h t be e x p e c t e d and the
c o n t e n t s of a first aid c a b i n e t d e s i g n e d to m a t c h .
The c a b i n e t should be
l o c a t e d in the l a b o r a t o r y p r o p e r and be a c c e s s i b l e .
A first-aid cabinet
suitable for a laboratory of 10-50 employees could contain the following:
1.

A copy of a leaflet giving advice on first aid

2.
A s u f f i c i e n t n u m b e r (not l e s s
unmedicated dressings for injured fingers.

than

12)

treatment.
of

small

sterilized

3.
A s u f f i c i e n t n u m b e r (not less than 6 ) of m e d i u m - s i z e d
unmedicated dressings for injured hands or feet.

sterilized

4.
A sufficient number (not less than 6) of large sterilized
dressings for other injured parts.

unmedicated

5.
A sufficient number (not less than 24) of adhesive wound
an approved type and of assorted sizes.
6.
A s u f f i c i e n t n u m b e r (not less than 4 ) of
unbleached calico, the longest size of which measures
and each of the other sides not less than 36 inches.
7.

small

A sufficient supply of adhesive

8.
A sufficient
packets.

supply

t r i a n g u l a r b a n d a g e s of
not less than 51 inches

plaster.

of a b s o r b e n t

43

dressings of

sterilized

cotton

in

individual

9.
approved

A sufficient supply of approved

type and size.

10. A sufficient n u m b e r
separate sealed packets.

(not

less

eye o i n t m e n t

than 4 ) of

11.

A rubber bandage or pressure bandage.

12.

Safety pins.

13.

A tube of antiseptic

in a container

sterilized

of an

eye-pads

in

cream.

It is suggested that, in addition to the above provisions (which cater

primarily for cuts and heat burns) each chemical laboratory first aid cabinet
should contain:
1.
2.
3.
4.

A tablespoon.
Bottle of Epsom salts (magnesium sulphate).
Bottle of milk of magnesia (dose - two tablespoonfuls).
Bottle of 1 percent acetic acid.

Hydrogen cyanide, soluble cyanides and nitriles which hydrolyse readily to HCN
when inhaled or ingested may call for treatment with capsules (0.3 ml) of amyl
nitrite w h i c h are easily crushed in a cloth from w h i c h the vapour can be
inhaled.
The following antidote for cyanide ingestion casualties consists of
two solutions which should be made up and left ready for immediate use:

S o l u t i o n A:
158 g ferrous sulphate crystals and 3 g citric acid crystals
in a litre of cold distilled w a t e r (the solution m u s t be inspected regularly
and be replaced if any deterioration has occurred).
S o l u t i o n B:
distilled water.

60 g anhydrous

sodium

carbonate

dissolved

in a litre

of

50 ml of solution A is placed in a 170 ml w i d e - n e c k e d bottle closed by a

p o l y t h e n e - c o v e r e d cork and labelled clearly "CYANIDE A N T I D O T E A".
50 ml of
solution B is s i m i l a r l y bottled and labelled "CYANIDE A N T I D O T E B".
Both
b o t t l e s should bear the legend "Mix the w h o l e contents of bottles "A" and "B"
and swallow the mixture".
The merit of the basic ferrous hydroxide suspension
is that when swallowed it is likely to induce vomiting while at the same time
forming insoluble non-toxic iron c o m p l e x e s with the cyanide.
It m u s t be
s t r e s s e d , h o w e v e r , that the i m m e d i a t e s u m m o n i n g of a doctor,
w h o can
a d m i n i s t e r an approved injection, is of the u t m o s t i m p o r t a n c e in cases of
cyanide poisoning.
Kits for the intravenous treatment of cyanide poisoning by
doctors are available.
A kit should be at hand in any o r g a n i z a t i o n w h e r e
cyanides are handled regularly.
I o d i n e , if i n g e s t e d , s h o u l d be t r e a t e d w i t h sodium thio s ul pha te.
An
appropriate weight of the crystals in a bottle to make up a 1 percent solution
when water is added to a set mark, will provide the right solution for taking
internally and also for swabbing on skin contaminated with iodine.
In some o r g a n i z a t i o n s , the a d m i n i s t r a t i o n of oxygen through a f a c e - m a s k has
become part of first aid procedures for certain types of casualty.
When it is
certain that a casualty has stopped breathing, artificial respiration should be
applied immediately.
The "mouth-to-nose" and "mouth-to-mouth" procedures are
now the methods of first choice and are described in "New Essential First-Aid"
by A. Ward Gardner and C. J. Roylande (Pan Books), among others.
The mouth-tomouth procedure must be used when the casualty has a nasal obstruction.
Where
injuries to the face and m o u t h m a k e the use of these m e t h o d s i m p o s s i b l e , or
w h e r e cyanide poisoning is k n o w n or suspected, the Sylvester method can be

44

used.
This is described in "First Aid" (2nd E d i t i o n 1965) published by St.
John A m b u l a n c e A s s o c i a t i o n , The St. A n d r e w A m b u l a n c e A s s o c i a t i o n and the
British Red Cross Society, as well as in standard medical texts.
Bromine, formic acid, hydrofluoric acid and other acid burns on the skin can be
treated with magnesia/glycerol paste prepared by triturating 200 g magnesium
oxide with 240 ml glycerol, the paste being applied liberally over the affected
areas. Dilute ammonia (1 volume ammonia added to 15 volumes of water) has also
been found e f f e c t i v e in reducing the degree of b u r n i n g w i t h b r o m i n e , formic
acid and hydrofluoric acid.
The laboratory should have at least one book (preferably more) on first aid and
laboratory safety.
There are m a n y such available.
Some of the better ones
are :
1.

"Handbook of L a b o r a t o r y Safety", Steere, N.V., C h e m i c a l Rubber

Cleveland, Ohio.

2.

"Hazards in the Chemical Laboratory",

C h e m i s t r y , U.K. 1 977.

3.

"Fire P r o t e c t i o n for L a b o r a t o r i e s Using C h e m i c a l s " ,

National
Protection Association, Batterymarch Park, Quincy, MA 02269.

4.

American Chemical Society, "Safety in the Chemical Laboratory" Vol 1 ACS

1967 (reprinted from "Journal of C h e m i c a l Education", January 1964 January 1967), and Vol 2, ACS 1971.

5.

M a n u f a c t u r i n g C h e m i s t s ' A s s o c i a t i o n Guide for safety

Laboratory, 2nd Ed, Van Nostrand Reinhold, 1972.

6.

Medical
1973 .

Muir.

G.D. (Ed.) Royal

Company,

Institute

of

Fire

in the

Chemical

in Laboratories",

MRC, U.K.

7.

P r e c a u t i o n s for L a b o r a t o r y W o r k e r s who Handle Carcinogenic

Amines, The Chester Beatty Research Institute, London, 1966.

Aromatic

8.

Reference Book of P r o t e c t i v e
Association, London, 1981-82.

Research

Council, "Safety

Precautions

E q u i p m e n t , Industrial Safety Manufacturers

45

7. LABORATORY QUALITY ASSURANCE

7.1

(QA)

Introduction

A laboratory engaged in food control analysis must have some means of assuring
that their analytical results are of the highest quality.
Errors in analysis
can o f t e n m e a n s e r i o u s e c o n o m i c l o s s e s for the food i n d u s t r y or i m p o r t e r , as
well as possible illness or injury to the consuming public.
This assurance of
quality is not limited to confirming that a food found to be unacceptable, is
in fact b a d .
It is e q u a l l y i m p o r t a n t to a s s u r e that f o o d s f o u n d to b e
a c c e p t a b l e , are in fact good.
To do this r e q u i r e s an u n d e r s t a n d i n g and
c o m m i t m e n t by the laboratory m a n a g e m e n t as well as the operating staff, that
high quality in analysis is the foremost objective.
O f t e n , the t e r m s " Q u a l i t y C o n t r o l " and " Q u a l i t y A s s u r a n c e " are used
interchangeably when discussing analytical quality.
H o w e v e r , G a r f i e l d (1)
m a k e s a d i s t i n c t i o n b e t w e e n the t w o .
He d e f i n e s Q u a l i t y c o n t r o l a s , "...a
p l a n n e d s y s t e m of a c t i v i t i e s w h o s e p u r p o s e is to p r o v i d e a q u a l i t y p r o d u c t . "
Conversely, he defines Quality Assurance as, "...a planned system of activities
w h o s e p u r p o s e is to p r o v i d e a s s u r a n c e that the q u a l i t y c o n t r o l p r o g r a m is
actually effective."
Therefore, Quality Control encompasses all of the myriad
r e v i e w , checking and operational procedures routinely used by the laboratory to
m a i n t a i n high analytical quality.
( M a n y of t h e s e are d i s c u s s e d in the
preceeding Chapters 4 and 5.) The following discussions of Quality Assurance
u s e s G a r f i e l d ' s d e f i n i t i o n and c o v e r s t h o s e p r o c e d u r e s u s e d to c o n f i r m t h a t
high quality is being maintained.

7.2

Establishing

a QA

Programme

To be successful, quality assurance must be a formal planned activity which is

designed to fit the needs of the laboratory.
A formal QA p r o g r a m m e is prepared
by establishing:
1.

The acceptable

quality

for a given

2.

A periodic review to confirm this

3.

A system of documentation

4.

Appropriate

laboratory

function.

quality.

to record

the results of the

follow-up to correct any deficiencies

reviews.

found.

The first step is to decide the functions that should have formal review.
Some
s u g g e s t i o n s a r e s t a n d a r d s s t o r a g e and h a n d l i n g , p r e p a r a t i o n of a n a l y s i s
r e p o r t s , i n s t r u m e n t m a i n t e n a n c e and l a b o r a t o r y s a f e t y .
T h e l a b o r a t o r y Head
should carefully examine the entire laboratory operation, by audit review if
n e c e s s a r y , and s e l e c t those f u n c t i o n s w h i c h need i m p r o v e m e n t or w h i c h w o u l d
benefit from periodic monitoring.
A QA p r o g r a m m e should be d y n a m i c and subject
to change when needed. Therefore a detailed QA review could be conducted until
it is felt that the function under review will continue to operate smoothly, at
w h i c h t i m e the r e v i e w could be l e s s e n e d and a n o t h e r f u n c t i o n g i v e n i n - d e p t h
coverage .
T h e r e v i e w i t s e l f is n o r m a l l y l i m i t e d to the c r i t i c a l p a r t s of the f u n c t i o n
under review.
For e x a m p l e , a r e v i e w of s t a n d a r d s t o r a g e and h a n d l i n g c o u l d
include: accounting for all standards by inventory and checking proper storage;
c h e c k i n g t h a t no s t a n d a r d h a s e x c e e d e d its e x p i r a t i o n or d i s p o s a l d a t e ; and
visual,
p h y s i c a l a n d / o r c h e m i c a l c h e c k s to i n d i c a t e
s t a n d a r d s are not
contaminated or decomposed.

46

The "acceptable quality" standard is set by the laboratory.

If some error rate
is acceptable in daily practice, then that rate b e c o m e s the quality standard.
The laboratory will always be striving for perfection, and the QA p r o g r a m m e is
one means to identify those areas which need improvement towards the ideal.
Quality Assurance programmes
are u s u a l l y a l s o r e q u i r e d
for
laboratory
certification.
An e x a m p l e is G u i d e 25 of the I n t e r n a t i o n a l O r g a n i z a t i o n for
S t a n d a r d i z a t i o n ( I S O ) (2).
U n d e r P a r t 4, " Q u a l i t y S y s t e m " it s t a t e s the
following :

1.
The laboratory shall operate an internal quality assurance p r o g r a m m e
a p p r o p r i a t e to the t y p e , r a n g e and v o l u m e of w o r k p e r f o r m e d .
The quality
assurance p r o g r a m m e shall be documented in a quality manual which is available
for u s e b y the l a b o r a t o r y s t a f f .
T h e q u a l i t y m a n u a l s h a l l be m a i n t a i n e d
relevant and current by a responsible m e m b e r of the laboratory staff. A person
or persons having responsibility for q u a l i t y a s s u r a n c e w i t h i n the l a b o r a t o r y
shall be designated by the laboratory m a n a g e m e n t and have direct access to top
management.

2.

The quality manual

shall contain

information

regarding:

a.

The structure of the laboratory

(organizational

charts);

b.

The operational and functional duties and services pertaining to

quality, so that each person concerned will know the extent and
the limits of his responsibility;

c.

General quality assurance

d.

Quality assurance
appropriate ;

e.

Where
appropriate,
m a t e r i a l , etc.;

f.

S a t i s f a c t o r y a r r a n g e m e n t s for f e e d b a c k and c o r r e c t i v e
whenever testing discrepancies are detected;

g.

Procedure

procedures;

procedures

proficiency

specific

testing,

for dealing with technical

for

use

each

of

test,

as

reference

action

complaints.

3.
The quality system shall be systematically and periodically reviewed
by or on b e h a l f of m a n a g e m e n t to e n s u r e the c o n t i n u e d e f f e c t i v e n e s s of the
arrangements, and corrective action initiated.
Such reviews shall be recorded
together with details of any corrective action taken.

This clearly states the importance that m u s t be placed on QA in the analytical

laboratory.
N o t e the key p r o g r a m m e e l e m e n t s are r e v i e w , d o c u m e n t a t i o n and
follow-up.
It
A Quality Assurance p r o g r a m m e must obviously be tailored to specific needs.
c a n be (and o f t e n is) an e x t e n s i v e and c o m p l e x d o c u m e n t w h i c h c o v e r s all
aspects of the laboratory work.
An example is the Quality Manual recommended
for t e s t i n g l a b o r a t o r i e s b y the I L A C (3). T h e v a r i o u s s u b j e c t s i n c l u d e d in a
complete Manual, listed alphabetically, are:

47

DEFINITIONS
Quality Manual
Quality System
Terminology
Testing Laboratory
Test Method
Test Report
ENVIRONMENT
External
Internal

Controls
Controls

E Q U I P M E N T , TESTING AND

MEASURING

Calibration
Identification
Inter laboratory Correlation
P r i o r to U s e
Programmes
U s e of I n - S e r v i c e T e s t E q u i p m e n t
U s e of R e f e r e n c e S t a n d a r d s
External
In-house
O v e r l o a d e d or M i s h a n d l e d
Periodic Maintenance
P u r c h a s i n g and A c c e p t a n c e P r o c e d u r e s
Records
LABORATORY DESCRIPTION
Confidential Information
Employee Responsibility
F i e l d s of A c t i v i t y
Identification
Minimizing Improper Influence
Organizational Structure
Proprietary Rights
Technical Management Personnel
QUALITY MANAGEMENT SYSTEM
Corrective Action
F i e l d s of T e s t i n g A c t i v i t i e s
Obj ec t i v e
P r o f i c i e n c y and I n t e r l a b o r a t o r y C o m p a r i s o n T e s t i n g
Quality Assurance Management
Q u a l i t y M a n u a l - R e v i s i o n and D i s t r i b u t i o n
Quality Policy
Quality System Audit
R e s p o n s i b i l i t y for Q u a l i t y A s s u r a n c e S y s t e m
Reference Materials
Resources Employed
Scope
S u b c o n t r a c ting
Technical Complaints
U p d a t i n g and C o n t r o l of D o c u m e n t s
U s e of E x t e r n a l F a c i l i t i e s
RECORDS
C o n f i d e n t i a l i t y and S e c u r i t y
H i s t o r i c a l F i l e of T e s t M e t h o d s
Maintenance

48

SAMPLES/ITEMS TO BE TESTED
P r o t e c t i o n from Damage
R e c e i p t and D i s p o s a l
Security
STAFF
Deputy Assignments
Job D e s c r i p t i o n s
P e r s o n n e l Records
S u p e r v i s ion
Other Measures
TEST METHODS AND PROCEDURES
I n d e x of Documents
S e l e c t i o n of Test Methods
Use of Non-Standard Test Methods
TEST REPORTS/TEST
Computerized
Format
Revision
Verification

DOCUMENTS
Date

of

Dsta

T h e a b o v e i l l u s t r a t e s h o w c o m p l e x and t h o r o u g h the d o c u m e n t a t i o n f o r a QA
programme can b e .
O b v i o u s l y , not a l l l a b o r a t o r i e s w i l l need such c o m p l e t e n e s s .
H o w e v e r , t h e r e i s a m i n i m u m QA p r o g r a m m e w h i c h s h o u l d be d o n e e v e n in the
s m a l l e s t of food c o n t r o l l a b o r a t o r i e s .
T h i s should i n c l u d e the four key a r e a s
where q u a l i t y c h e c k i n g is needed most.
These are r e f e r e n c e standard m a t e r i a l
used in a n a l y s i s ,
laboratory measuring instruments,
a n a l y s i s r e p o r t s and the
t e c h n i c a l p r o f i c i e n c y of the a n a l y t i c a l s t a f f .
The l a t t e r can be r e v i e w e d in
p a r t by use of a c h e c k s a m p l e a n a l y s i s p r o g r a m m e .
T h e s e f o u r QA c h e c k a r e a s
a r e d i s c u s s e d in d e t a i l in s u c c e e d i n g S e c t i o n s 7 . 3 to 7 . 6 .
O t h e r r e l a t e d QA
a c t i v i t i e s are d i s c u s s e d under S e c t i o n 7 . 7 .

7.3

QA of R e f e r e n c e

Standards

F o r p u r p o s e s of t h i s S e c t i o n , a " R e f e r e n c e S t a n d a r d " i s a p u r e c h e m i c a l or
b i o l o g i c a l s u b s t a n c e w h i c h may be used for c o m p a r i s o n d u r i n g the q u a n t i t a t i v e
a n d / o r q u a l i t a t i v e a n a l y s i s of a c o n s t i t u e n t or a t t r i b u t e of a f o o d .
Of
c o u r s e , " p u r e " is a r e l a t i v e term.
Some m e t a l e l e m e n t s c a n be r o u t i n e l y
o b t a i n e d in 9 9 . 9 9 9 % p u r i t y , w h i l e many o r g a n i c s u b s t a n c e s would be c o n s i d e r e d
" p u r e " at 9 5 % .
The a n a l y s t m u s t j u d g e i f t h e r e f e r e n c e s t a n d a r d u s e d i s
s u f f i c i e n t l y pure for a n a l y s i s p u r p o s e s .
R e f e r e n c e s t a n d a r d s can be d i v i d e d
i n t o three g r o u p s :

1.
Primary:
These are m a t e r i a l s which have been a n a l y z e d and
c e r t i f i e d by a n a t i o n a l s t a n d a r d s o r g a n i z a t i o n or o t h e r a c c e p t a b l e
organization.
2.
Secondary:
S u b s t a n c e s whose p u r i t y is
commercial s u p p l i e r s or o r g a n i z a t i o n s o t h e r than the

certified
above.

by

the p u r i t y
certifying

analysis

by

3.
Other:
This i n c l u d e s a l l r e f e r e n c e s t a n d a r d s w h i c h are c o n s i d e r e d
a c c e p t a b l e by t h e u s e r , b u t w h i c h do n o t f a l l i n t h e a b o v e t w o g r o u p i n g s .
T h e s e can i n c l u d e l o c a l l y o b t a i n e d m a t e r i a l s w h i c h h a v e u n d e r g o n e r e p l i c a t e
a n a l y s i s and have been compared to p r i m a r y or s e c o n d a r y r e f e r e n c e s t a n d a r d s , to
calculate purity.

49

S u b s t a n c e s l a b e l l e d , " p u r e " , " c h e m i c a l l y p u r e " , "c.p.", " p u r i f i e d " or " h i g h e s t

p u r i t y " s h o u l d a l w a y s b e c o n s i d e r e d s u s p e c t as t h e i r a c t u a l p u r i t y o f t e n v a r i e s
widely.
T h e y m u s t be c o m p a r e d to s u i t a b l e r e f e r e n c e s t a n d a r d s b e f o r e u s e as a
standard themselves.
As p r i m a r y and s o m e s e c o n d a r y r e f e r e n c e s t a n d a r d s a r e o f t e n q u i t e e x p e n s i v e , it
c a n b e e c o n o m i c a l to o b t a i n a s u p p l y o f a c h e a p e r p u r e m a t e r i a l a s a w o r k i n g
standard.
It c a n b e a n a l y z e d in c o m p a r i s o n to t h e p r i m a r y ( o r s e c o n d a r y )
r e f e r e n c e s t a n d a r d and the p u r i t y d e t e r m i n e d .
The analyst m u s t be c a r e f u l ,
h o w e v e r , to a v o i d i m p u r i t i e s in the l o c a l m a t e r i a l , w h i c h w i l l c r e a t e p r o b l e m s
during analysis.
T h e f o l l o w i n g is a l i s t o f s o m e s o u r c e s in t h e U n i t e d S t a t e s
s e c o n d a r y r e f e r e n c e s t a n d a r d s of t h e i n d i c a t e d m a t e r i a l s :

Reference

Standards

for p r i m a r y

Source

Number

Alcohols

21

Alkenes

21

Antibiotics

(Chlortetracycline

HC1)

(Erythromycin)

15

(Monensin

14

Sodium)

(Oxytetracycline
(Penicillin

Base)

"G" P r o c a i n e )

(Streptomycin

Sulfate)

(Tylosin)
Atomic

Absorption

Bacterial
Blood

(Metals)

Reference

12
11
12
14
22

Cultures

1, 2 , 3, 4

Group/Typing

Chemicals, Industrial

1 9 , 3 2 , 38

Contaminants, Drinking Water

Drugs

13

1 0 , 34

(Animal)

1 8 , 2 5 , 31

(U.S. Schedules

I, II)

1 6 , 1 7 , 18

(U.S. Schedules

III, IV, V, VI)

18

Ethanol, Absolute

37

Fibers, Synthetic

21

Fuels, Motor

35

Lead

(Alcoholic Beverages)

34

(Blood)

20

(Motor Fuels)

22

50

or

Reference

Standards

Source

Metals (Foods, Feeds, Fertilizers)

Htmber

23, 30, 36

(Fish, Sediments, Fuel Oil)

23

(Sludge)

34
17,

Mycotoxins
Pesticides

21, 24, 25, 26

19, 21, 32, 33

Phenylalanine (PKU)

3, 4

Salmonella Typing & Grouping Antisera

1, 3

Shigella Grouping Antisera

1, 5

Species (Known Fish)

27, 28

(Known Meats)

29

Spirits (Distilled Congeners)

36

Streptococcus

Thallium (Standard 1000 ppm)

19

Trichinosis

Tuleremia

Viral Agent Antisera

1, 6, 7

Wine (Reference)

23

The U.S. sources referred to above, listed by number are:

1.

Department of Health and Human Services

Public Health Service
Centers for Disease Control
Atlanta, GA 30333

2.

American Type Culture Collection

12301 Parklawn Drive
Rockville, MD 20852

3.

Difco Laboratories
P.O. Box 1058
Detroit, MI 48232

4.

BBL Microbiology Systems

P.O. Box 243
Cockeysville, MD 21030

5.

Fisher Scientific
7633 Hull Street Road
Suite 2000D
Richmond, VA 23235

6.

M A Bioproducts
Briggs Ford Road
Building 100
Walkersville, MD 21793
51

7.

Flow Laboratories, Inc.

7655 Old Springhouse Road
McLean, VA 22102

8.

Wellcome Diagnostics
Research Triangle Park
North Carolina 27709

9.

American Dade
P.O. Box 520672
Miami, FL 33152

10

Environmental Resource Associates

5540 Marshall
Arvada, CO 80002

11

ICN Nutritional Biochemicals

P.O. Box 28050
Cleveland, OH 44128

12

Pfizer Laboratories
235 E. 42nd Street
New York, NY 10017

13

Lederle Laboratories
Division of American Cyanamid
One Cyanamid Plaza
Wayne, NJ 07470

14

Eli Lilly and Company

307 E. McCarty Street
Indianapolis, IN 46285

15

Aldrich Chemical Company

Milwaukee, WI 53233

16

U.S. Drug Enforcement Administration

Special Testing Laboratory
7704 Old Springhouse Road
McLean, VA 22102

17

Applied Science
P.O. Box 440
State College, PA 16801

18

United States Pharmacopeia Convention Inc.

12601 Twinbrook Parkway
Rockville, MD 20852

19

Aldrich Chemical Company

P.O. Box 355
Milwaukee, WI 53201

20,

E. S. A. Inc.
45 Wiggins Avenue
Bedford, MA 01730

21,

Supelco Inc.
Supelco Park
Bellefonte , PA 16823

22,

Fisher Scientific Company

711 Forbes Avenue
Pittsburgh, PA 15219

Division

52

(US-DEA)

23.

National Bureau of Standards

Office of Standard -and Reference Materials
Room B 311, Chemistry Building
Washington, DC 20234

24.

The Myco Laboratory Company

P.O. Box 321
Chesterfield, MO 63017

25.

Sigma Chemical Company

P.O. Box 14508
St. Louis, MO 63178

26.

Eureka
215 - 26th Street
Sacramento, CA 95816

27.

U.S. Department of Commerce

National Oceanic and Atmospheric
Northeast Inspection Office
P.O. Box 1188, Emerson Avenue
Gloucester, MA 01930

Admin.

28.

VA Institute of Marine Science

College of William and Mary
Gloucester Point, VA 23062

29.

VA Dept. of Agriculture and Consumer

Division of Animal Health
1 North 14th Street
Richmond, VA 23219

30.

American Dade Division

American Hospital Supply Corp.
Miami, FL 33152

31.

Pfaltz and Bower Inc.

375 Fairfield Avenue
Stamford, CN 06902

32.

U.S. Environmental Protection Agency

Pesticides, Industrial Chemicals Repository
Research Triangle Park, NC 27711

33.

U.S. Environmental Protection Agency

Analytical Chemistry Section
Building 306, Room 101, ARC - East
Beltsville, MD 20705

34.

U.S. Environmental Protection Agency

EMSL - Cincinnati
26 West St. Clair Street
Cincinnati, OH 45268

35.

Phillips Chemical Company

Drawer 0
Borger, TX 79007

36.

J. T. Baker Chemical Company

222 Red School Lane
Phillipsburg, NJ 08865

37.

U.S. Industrial Chemical Company

Tuscola, IL 61953

53

Services

(MD-8)

38.

Chem Service
P.O. Box 194
West Chester, PA

19380

Once a stock of appropriate reference standards has been obtained, they must be
recorded, used and stored properly.
A records book or file cards can be used,
with the following information noted for each standard:
1.

Standard name and date

2.

Source

3.

Code or lot number.

4.

Purity.

5.

Expiration date

(if any).

6.

Special

storage

requirements.

7.

Storage

location.

(from where

received.

obtained).

M a n y laboratories assign a number to the standard container for accountability

purposes.
If the s t a n d a r d is o n e w h i c h m a y d e t e r i o r a t e on s t o r a g e , t h e n the
record should also include dates and results when stability checks were m a d e .
If it is deemed necessary for control, there could be a check-out and - i n sheet
for the s t a n d a r d , w h i c h the a n a l y s t w o u l d d a t e and i n i t i a l w h e n u s i n g the
material.
T h i s is n o t u s u a l l y d o n e e x c e p t for e x t r e m e l y d a n g e r o u s or h i g h l y
sensitive substances which must be accounted for.
It is o f t e n c o n v e n i e n t to s t o r e r e f e r e n c e s t a n d a r d s in a r e a s n e a r w h e r e t h e
a n a l y s e s are b e i n g d o n e (i.e. p e s t i c i d e s t a n d a r d s in the p e s t i c i d e s r e s i d u e
analysis section of a larger food laboratory).
H o w e v e r , the storage area m u s t
be separate from other chemical storage and clearly marked as to its contents.
E x a m p l e s are a marked refrigerator section or cabinet with clear warnings or
i n s t r u c t i o n s that o n l y s p e c i f i c r e f e r e n c e s t a n d a r d s are to be s t o r e d t h e r e .
T h i s p e r m i t s a c c o u n t i n g for a s t a n d a r d l o c a t i o n as w e l l as e n s u r i n g t h a t a
reference standard is not mistakenly used as a non-standard chemical.
If periodic testing is done to check stability, then the test protocol should
be k e p t w i t h the s t a n d a r d r e c o r d .
The r e c o r d w o u l d also c o n t a i n the test
r e s u l t s , d a t e , a n a l y s t n a m e and a n y s u p p o r t i n g d o c u m e n t s s u c h as s p e c t r a or
chromatograms.
W i t h all Quality Control procedures in
would consist of a periodic review of:
1.
Records
c o n d i t i o n of the
correct times?)

for?

the

Quality

Assurance

checking

(Are they complete and current?

Do they reflect the actual
standard?
H a v e a p p r o p r i a t e s t a b i l i t y t e s t s b e e n r u n at

2.
Storage
(is
If not, w h y ? )

3.
review?

place,

the

storage proper?

Are the stored

standards

Physical Condition
( W h e r e w a s the s t a n d a r d at the
Any physical evidence of deterioration or m i s h a n d l i n g ? )

accounted

time

of

the

The t i m i n g of the r e v i e w w o u l d d e p e n d on n e e d .
An i n i t i a l c y c l e of t h r e e
m o n t h s is s u g g e s t e d .
T h i s c a n b e i n c r e a s e d or d e c r e a s e d as c o n d i t i o n s and
review results dictate.

54

M a n a g e m e n t and e a c h a n a l y s t m u s t r e m e m b e r that r e f e r e n c e s t a n d a r d s are

e x t r e m e l y i m p o r t a n t to an a n a l y t i c a l l a b o r a t o r y , a n d m u s t b e
treated
accordingly.
The p e r s o n m a k i n g the QA r e v i e w s h o u l d be a s e n i o r a n a l y s t or
s u p e r v i s o r w h o h a s a k n o w l e d g e and a p p r e c i a t i o n for p r o b l e m s t h a t i m p r o p e r ,
contaminated or deteriorated reference standards can create for the analyst.

7.4

QA of

Instruments

A f t e r r e f e r e n c e s t a n d a r d s , m e a s u r i n g i n s t r u m e n t s are the m o s t s e n s i t i v e and

troublesome items for an a n a l y t i c a l l a b o r a t o r y .
I n s t r u m e n t m a i n t e n a n c e and
r e p a i r are o b v i o u s l y i m p o r t a n t and are d i s c u s s e d e l s e w h e r e .
Of e q u a l (or
possibly greater) importance is an o r g a n i z e d p r o c e d u r e to p e r i o d i c a l l y c h e c k
the instrument performance.
If the performance parameters to be checked are
s e l e c t e d c a r e f u l l y , t h e n the a n a l y s t h a s a r e a s o n a b l e m e a s u r e of w h e t h e r the
i n s t r u m e n t is o p e r a t i n g p r o p e r l y , on a c o n t i n u i n g b a s i s . O n c e a p e r f o r m a n c e
c h e c k i n g p r o t o c o l is d e c i d e d u p o n , an i n d i v i d u a l p e r f o r m a n c e r e c o r d c a n b e
p r e p a r e d for e a c h i n s t r u m e n t .
T h i s can be a s e p a r a t e n o t e b o o k w h i c h is k e p t
p h y s i c a l l y n e a r the i n s t r u m e n t , or c a n be p a r t of the m a i n t e n a n c e and r e p a i r
record kept for each instrument.
The frequency of performance checking varies considerably, again depending on
c i r c u m s t a n c e and p r e v i o u s c h e c k r e s u l t s .
If a c h e c k r e s u l t
indicates
maintenance or repair, then a follow-up check (after the repair, etc.) should
be scheduled before the next routine QA check time.
The routine use of m a n y instruments involves some form of performance checking.
An example is a working standard injection into a gas chromatograph first thing
in the m o r n i n g , to c h e c k i n s t r u m e n t r e s p o n s e .
T h i s is n e c e s s a r y and h a s its
place to assure the analyst that the instrument is operating properly for that
day.
For p u r p o s e s of a QA p e r f o r m a n c e c h e c k , h o w e v e r , t h e r e s h o u l d be a
separate and distinct checking programme.
S o m e l a b o r a t o r i e s m a k e a d i s t i n c t i o n b e t w e e n r o u t i n e i n s t r u m e n t s used by
e s s e n t i a l l y all a n a l y s t s (i.e. b a l a n c e s , s p e c t r o p h o t o m e t e r s , etc.) and t h o s e
used o n l y by h i g h l y t r a i n e d s p e c i a l i s t s (i.e. m a s s s p e c t r o m e t e r s , etc.).
The
p e r f o r m a n c e c h e c k i n g of the f o r m e r c a n b e d o n e b y any a s s i g n e d a n a l y s t .
The
latter, h o w e v e r , should be checked by trained analyst only.
A suggested performance checking protocol
laboratory instruments is as follows:

Analytical

1.

and

schedule

for

some

general

Balances

Sensitivity

(bimonthly)

Check balance sensitivity using three standard weights (10g, lg and

100 mg).
Weight used should be traceable to certified weights of at
l e a s t U.S. C l a s s S.
S e n s i t i v i t y s h o u l d be w i t h i n the
balance
specifications.

2.

Calibration

(annual)

Best done in connection

using standard weights.

with

annual

55

cleaning

and

maintenance,

again

Spectrophotometers

1.

(ultraviolet and

Wavelength

Accuracy

visible)

(bimonthly)

Check by recording over entire UV-visible w a v e l e n g t h range using

H o l m i u m and D i d y m i u m f i l t e r s ( u s u a l l y o b t a i n a b l e f r o m t h e i n s t r u m e n t
m a n u f a c t u r e r or a l a r g e s u p p l y f i r m ) .
Run two spectra
for
comparison.
Results should not differ from published values more
t h a n + 1.0 n m at a n y w a v e l e n g t h .

2.

Photometric

Accuracy

(bimonthly)

P r e p a r e a s o l u t i o n of 60 _+ 0.25 m g p o t a s s i u m d i c h r o m a t e in o n e l i t r e
of 0.01N s u l p h u r i c a c i d .
( T h i s s o l u t i o n is q u i t e s t a b l e a n d o n c e
p r e p a r e d can be used a long time).
S c a n this s o l u t i o n f r o m 2 1 0 to
450 n m .
T h e f o l l o w i n g a b s o r b a n c e s (+ 1% f u l l s c a l e ) s h o u l d o c c u r at
the i n d i c a t e d w a v e l e n g t h s :

Wavelength

(nm)

Absorbance

235
257
313
350

0.747
0.869
0.293
0.644

A l t e r n a t i v e l y , t h e U.S. N a t i o n a l B u r e a u of S t a n d a r d s h a s a v a i l a b l e
for p u r c h a s e S R M 9 3 0 , a g l a s s f i l t e r w h i c h c a n b e u s e d s i m i l a r l y and
which has certified wavelength/absorbance values.

Spectrophotometer

1.

(infrared)

Wavelength Accuracy

(trimonthly)

Scan a standard polystyrene film.

The following peaks
indicated w a v e n u m b e r s w i t h i n the listed a c c u r a c y :

Wavenumber

(cm

1.

Baseline

(atomic

+
_+
+
+

absorption)

(daily when

Absorbance

the

6
6
2
2

used)

U s i n g f l a m e o n l y , the r e c o r d e r b a s e l i n e s h o u l d
.005 a b s o r b a n c e u n i t s in a f i v e m i n u t e p e r i o d .

2.

at

Accuracy

2851
1601
1028
907

Spectrophotometer

occur

(daily when

not vary m o r e

than +

used)

T h r e e c o n s e c u t i v e a b s o r b a n c e c h e c k s of the
v a r y m o r e t h a n _+ .005 a b s o r b a n c e u n i t s .

56

same

solution

should

not

3.

Detection Limit

(monthly)

Prepare a solution of a metal standard sufficiently dilute to give a

response of two times the baseline absorbance under ideal conditions.
T h i s b e c o m e s the ' d e t e c t i o n l i m i t ' s t a n d a r d .
M a k e four r e p l i c a t e
aspirations to check reproducibility.

Gas

Chromatograph

1.

Column Oven

(semiannual)

Check column oven temperature using

2.

Gas Flow Rate

pyrometer.

(monthly)

C h e c k f l o w rates of all c a r r i e r
bubble meter or other device.

3.

a calibrated

Detector Response

(daily when

and

detector

gases

u s e d , using

used)

Compare present detector response with the response obtained when new
or w h e n last c l e a n e d and c a l i b r a t e d .
(in s o m e d e t e c t o r s , n o t a b l y
e l e c t r o n c a p t u r e , a d e t e r i o r a t i n g r e s p o n s e i n d i c a t e s a need for
cleaning).

High Performance Liquid

1.

Chrcmatograph

Column Resolution (daily when

used)

Prepare a solution of two or more substances which the column should

resolve under normal analytical conditions. Use this to check column
performance each time the column is used.

2.

Detector Response (daily when used)

C h e c k d e t e c t o r r e s p o n s e using a k n o w n c o n c e n t r a t i o n standard and
compare to a response previously obtained under ideal conditions.

The above p e r f o r m a n c e c h e c k s are only s u g g e s t i o n s .

The best a p p r o a c h is to
read the o p e r a t i o n s m a n u a l for e a c h i n s t r u m e n t and s e l e c t key o p e r a t i n g
p a r a m e t e r s or s p e c i f i c a t i o n s of i n t e r e s t to p r e p a r e the p r o t o c o l .
Also,
instruments or equipment other than those mentioned above should be considered
for a p e r f o r m a n c e check p r o g r a m m e .
The g o v e r n i n g factor should be the
instrument or equipment importance to the laboratory.
The QA p r o g r a m m e on i n s t r u m e n t p e r f o r m a n c e c h e c k i n g m u s t also include a
p e r i o d i c r e v i e w to i n s u r e the c h e c k s are b e i n g m a d e and that a p p r o p r i a t e
follow-up action is taken if a check discloses a possible performance problem.
This follow-up could be maintenance, cleaning, repair, calibration, etc.
Any
follow-up action should be recorded in the notebook kept with the instrument.

57

7.5

QA of Analytical

Reports

As discussed in preceding Section 5.5, the analytical report is the culmination

of all of the l a b o r a t o r y ' s e f f o r t s .
T h e r e are m a n y t y p e s and f o r m a t s for
analysis reports.
T h e y v a r y from s i m p l e to d e t a i l e d , but all are s u b j e c t to
the same problem, h u m a n error.
A Quality Assurance p r o g r a m m e for analytical
reports is basically an after-the-fact or retrospective review of a document
w h i c h h a s a l r e a d y b e e n t h r o u g h the n o r m a l s u p e r v i s o r y and m a n a g e m e n t r e v i e w
process.
It is d e s i g n e d to d e t e c t r e p o r t w r i t e - u p and r e v i e w e r r o r s so that
appropriate procedures can be instituted to prevent their reoccurrence.
Although report formats m a y vary according to organizational need, the report
m u s t be c o m p l e t e enough to enable the reviewer to reconstruct the analysis and
to c h e c k the a n a l y t i c a l r e a s o n i n g as w e l l as d a t a and c a l c u l a t i o n s .
For
e x a m p l e , in ISO Guide 25 (2) under part 12, "Test Reports", it states:

1.
The work carried out by the testing laboratory shall be covered by a
report w h i c h accurately, clearly and u n a m b i g u o u s l y p r e s e n t s the t e s t r e s u l t s
and all other relevant information.

2.

Each test report

shall

include at least

the following

information:

a.

Name and address of testing

b.

Unique identification of
each page of the report.

c.

Name and address of

d.

Description and identification of the test

e.

D a t e of r e c e i p t of test
tests, as appropriate.

f.

A s t a t e m e n t to the e f f e c t that the test r e s u l t s r e l a t e o n l y to

the items tested.

g.

Identification

h.

Description of sampling

i.

Any d e v i a t i o n s ,
additions
specification, and any other
test .

j.

Disclosure
ut ilized.

k.

M e a s u r e m e n t s , e x a m i n a t i o n s and d e r i v e d r e s u l t s , s u p p o r t e d by
t a b l e s , g r a p h s , s k e t c h e s , p h o t o g r a p h s as a p p r o p r i a t e , and any
failure identified.

1.

A statement on measurement

m.

A s i g n a t u r e a n d t i t l e of p e r s o n ( s ) a c c e p t i n g
technical
responsibility for the test report and date of issue.

n.

A s t a t e m e n t that t h e r e p o r t s h a l l n o t be r e p r o d u c e d
full without the approval of the testing laboratory.

of

report

(such

as serial

number),

and

of

performance

of

client.

of the test

any

company.

item

and

date(s)

of

specification, method

procedure, where

and

procedure.

relevant.

to or e x c l u s i o n s from the test

information relevant to a specific

non-standard

58

item.

test

uncertainty

method

(where

or

procedure

relevant).

except

in

3.
Particular care and attention shall be paid to the arrangement of the
test report, especially with regard to presentation of the test data and ease
of assimilation by the reader.
The format shall be carefully and specifically
a s s i g n e d for e a c h type of test c a r r i e d o u t , but the h e a d i n g s shall be
standardized as far as possible.
The U.S. Food and Drug A d m i n i s t r a t i o n " A n a l y s t W o r k s h e e t "
good example for purposes of discussing an analytical report
is relatively complete and includes space for all pertinent
analytical summary.
The r e v e r s e of the form w o u l d be used
and calculations as the analysis progresses.

(Figure 7.1) is a
QA programme.
It
data including an
for r a w w o r k d a t a

An a n a l y t i c a l r e p o r t QA p r o g r a m m e should i n v o l v e r e v i e w of a p r e d e t e r m i n e d
n u m b e r of c o m p l e t e d r e p o r t s on a m o n t h l y or b i m o n t h l y b a s i s .
The r e p o r t s
should be r e p r e s e n t a t i v e of the k i n d s of w o r k d o n e , w i t h a b o u t as m a n y w h i c h
s h o w law v i o l a t i o n s as are u s u a l l y e n c o u n t e r e d .
An e x a m p l e could be ten
r e p o r t s w i t h t w o b e i n g v i o l a t i v e ( a s s u m i n g the v i o l a t i o n rate is about 20%).
The object is to gain a relatively representative sampling of completed reports
in order to evaluate overall report writing.
If some section of the laboratory
has substandard reports, then their coverage can be selectively increased until
it a p p e a r s that the r e p o r t s are s a t i s f a c t o r y .
T h i s is one of the p r i m e
f u n c t i o n s of QA r e v i e w s ( w h a t e v e r the t y p e ) - to p i n p o i n t p r o b l e m areas and
give them visibility until the problem is solved.
An example of an analytical report review protocol is one which has been used
by the U.S. Food and Drug A d m i n i s t r a t i o n for QA r e v i e w of their A n a l y t i c a l
Worksheets.
Their protocol consists of a listing of performance factors that
their Worksheet (Figure 7.1) must meet, as follows:
1.

2.

Accuracy and

Completeness

a.

Worksheet clearly describes

received by the analyst.

b.

Worksheet fully and accurately reflects continuity and

of sample.

c.

Information on the
Collection Report.

d.

T h e u s e of a p p r o p r i a t e
equipment is described.

e.

C a l c u l a t i o n s are a c c u r a t e , easy to f o l l o w , and are c h e c k e d .

This includes checking of conversion factors, normality factors,
etc., for accuracy of recording.

f.

If m o r e than one p e r s o n p a r t i c i p a t e d in
worksheet clearly indicates who did what.

g.

Sample reserve or disposition is correctly

h.

E r r o r s are noted by s t r i k i n g t h r o u g h the i n c o r r e c t

inserting, initialing and dating the new entry.

i.

Any discarded

Analytical

worksheet

results are

the

sample

and

is compatible

standards,

condition

with

reagents,

the

the

and

when

integrity

Inspection

special

analysis,

the

reported.
entry

and

explained.

Methodology

The a p p r o p r i a t e m e t h o d
is used and is r e f e r e n c e d on the
worksheet.
Analyses performed and methods used are consistent
with appropriate instructions or as directed by the Supervisor.

59

ANALYST WORKSHEET
3. S E A L S

NONE

INTACT

BROKEN

1. P R O D U C T

4. D A T E

REC'D

2. S A M P L E

5. R E C E I V E D

FROM

NUMBER

6. D I S T R I C T O R L A B O R A T O R Y

7. D E S C R I P T I O N O F S A M P L E

8.
NET
CONTENTS

NOT APPLICABLE

DECLARE/UNIT

NOT DETERMINED

AMOUNT

UNITS E X A M I N E D

% OF

10. S U M M A R Y O F

11. R E S E R V E

.ORIGINAL(S)
LABELING

FOUND.

DECLARED

.COPIES

SUBMITTED

SUBMITTED

NONE

ANALYSIS

SAMPLE

1 2 . L. A N A L Y S T S I G N A T U R E (Broke

Seal

)
WORKSHEET
CHECK
14. D A T E

FORM FD 431 (1/77)

P R E V I O U S E D I T I O N IS O B S O L E T E .

Figure
USFDA

Analyst

60

7.1
Worksheet

REPORTED

PAGE

OF

PAGES

3.

4.

b.

Sample is analyzed so
laws or regulations.

c.

Deviations
worksheet.

d.

Any unofficial method

Supervisory

from

the

as

to

permit

referenced

used

application

method

are

of

appriopriate

explained

on

the

is validated.

Review

a.

The a n a l y s i s and m e t h o d o l o g y w a s a p p r o p r i a t e
indicated on the inspection collection report.

b.

L a b o r a t o r y c o n c l u s i o n s and final d e c i s i o n
supported by information on the worksheet.

c.

If the sample is classified

performed (if possible).

Time

Frames

a.

Sample analysis

violative,

to

are

the

problem

accurate

a confirming

analysis

and

is

time frames are met.

Any deviations from the above which are found during the r e v i e w , are recorded
and an a t t e m p t m a d e to d e t e r m i n e h o w they o c c u r r e d .
T h e r e v i e w e r m a y find a
p a t t e r n s u c h as c e r t a i n e r r o r s a r e c o n s i s t e n t l y m a d e , i n d i c a t i n g a n e e d for
specific training.
A l l f o l l o w - u p a c t i v i t i e s and a c t i o n s t a k e n to c o r r e c t
p r o b l e m s , m u s t be detailed and documented to provide laboratory m a n a g e m e n t with
a continuing basis to evaluate improvement.

7.6

Check Sampl

Examination

O n e of the m o s t c o m m o n w a y s to e v a l u a t e o v e r a l l i n d i v i d u a l or l a b o r a t o r y
p e r f o r m a n c e in a g i v e n a n a l y s i s , is b y u s e of k n o w n c h e c k s a m p l e s .
This
i n c l u d e s b o t h i n t r a ( w i t h i n ) the l a b o r a t o r y and i n t e r ( b e t w e e n ) like
laboratories.
The A m e r i c a n Chemical Society (ACS) in their 1980 Guidelines for
Data Quality Evaluation, stated:
"At the o u t s e t , a l a b o r a t o r y s h o u l d d e m o n s t r a t e its p r o f i c i e n c y u s i n g
prototype and non-critical samples, thereby reducing the probability that bad
d a t a w i l l be g e n e r a t e d on c r i t i c a l s a m p l e s , e s p e c i a l l y t h o s e i n v o l v i n g
complicated unknown mixtures.
An i n t r a l a b o r a t o r y q u a l i t y c o n t r o l p r o g r a m
s h o u l d i n c l u d e the use of b l i n d s a m p l e s in a d d i t i o n to c h e c k s a m p l e s w h o s e
v a l u e s are k n o w n to the a n a l y s t s .
A l l a n a l y s t s s h o u l d be m o n i t o r e d b y the
quality control procedures, and any assessment of laboratory performance should
include all of the analysts involved, or at least a random selection of those
analysts.
I n t e r l a b o r a t o r y Q u a l i t y A s s u r a n c e p r o g r a m s s h o u l d also use b l i n d
s a m p l e s in a d d i t i o n to c h e c k s a m p l e s ,
in o r d e r to p r o v i d e a r e a l i s t i c
assessment of the performance of the method that is achievable in the field."
L a t e r , in 1 9 8 2 , the A C S m a d e an a d d i t i o n a l s t a t e m e n t
reliability and acceptability of analysis data:

regarding

improving

" I d e a l l y , for a g i v e n m e t h o d , i n t e r l a b o r a t o r y v a r i a b i l i t y s h o u l d b e the

s a m e as i n t r a l a b o r a t o r y v a r i a b i l i t y :
In real s i t u a t i o n s , h o w e v e r , the
i n t e r l a b o r a t o r y v a r i a b i l i t y is a l m o s t a l w a y s g r e a t e r .
T h e r e f o r e , it is
necessary to determine for a given method the variability of the m e a s u r e m e n t s
( r a n d o m e r r o r ) b e t w e e n l a b o r a t o r i e s in o r d e r to m a k e a l l o w a n c e s for t h o s e
differences
in i n t e r p r e t i n g
the r e s u l t s of a n a l y s e s .
For any p r o p e r l y

61

validated procedure, however, interlaboratory results will be consistent with

i n t r a 1 a b o r a t o r y r e s u l t s / t h a t is, t h e u n c e r t a i n t y i n t e r v a l s
(including
s y s t e m a t i c error b o u n d s ) for all q u a l i f i e d l a b o r a t o r i e s ( i n d i v i d u a l l y and
collectively) will overlap the true value. (This presumes that the measurement
method, itself, has negligible bias.)"
The various

factors

influencing

final

analysis data are shown in Figure 7.2.

DATA

Figure 7.2

During 1984, the U.S. Association of Food and Drug Officials (AFDO) assembled a
listing of proficiency and check sample programs available through various U.S.
a g e n c i e s and o r g a n i z a t i o n s .
The listing is as f o l l o w s , giving c h e c k s a m p l e
type, the product involved and the check sample program sponsor:

Check Sample Type

Program
Sponsor

Product(s)

Aflatoxins

Milk, Corn

Alcohol

Blood

Antibiotics

Meat

Antibiotics

Milk

Arsenic

Meat, Poultry

Filters

Asbestos

(Number of Fibres)

Bacteriology

Milk, General

Bioassay of Antibiotics

Feed s

Cations

Water

Cereal

Water

Cereal

Components

Coliforms

62

Food

6,7

Drinking Water,
Fatty

Prograai
Sponsor

Product(s)

Check Sample Type

Contaminants

Water

Fats and

Acids

Oils

Fertilizers

Frtilizers

13

Fibre

Fibre

11

Flammables

Various

11

Fluoride

Water

Food

Various

Characterization

Components

Herbicides and
Industrial
Lead and

Chemicals

FEP

Medicated
Metals

Organics

Feeds

(Cations)

Metals and

Foods

Urine and

17

Water

10

Fish

Blood

Feed s

Food

Water

Minerals

Microb iology
Microscopic

14

Various
Characterization

Products

18,19

Feed s

15

Mould s

Mycology

Organic

Chemicals

Water

Organic

Solvents

Charcoal

Organics

Semi-Volatile

Organochlorine

Tube

Synthetic

Compounds

PCB's and Chlorinated

14

Organics

Leachate

12

Plasma

10

Fat, Blood
Meats,

Poultry

Phosphatase

Milk

Protein/Moisture/Fat/Salt

Meat

Residues,

Meats,

Pesticide

Poultry

Pesticides/Herbicides

Water

Pesticides/Herbicides

Vegetables,

Smalley Oil

Feed s

Milk

Somatic

Cell

Meals
Count

and Drinking

Sulfonamide s

Meats,

Vitamins

Milk, Feed,

Waste Water

Parameters

Water

63

Foods

Poultry
Foods

Water

9,10,14
6,16

4
1
9

The U . S . s p o n s o r s

for the above c h e c k sample p r o g r a m s

1.

A m e r i c a n A s s o c i a t i o n of C e r e a l
3340 P i l o t K n o b Road
St. P a u l , MN 55121

2.

A m e r i c a n Oil C h e m i s t s Society
508 South Sixth Street
C h a m p a i g n , IL 61820

3.

U . S . D e p a r t m e n t of T r a n s p o r t a t i o n
Transportation Systems Center, Kendall
Cambridge, MA 02142

are

Chemists

Square

4.

U . S . D e p a r t m e n t of A g r i c u l t u r e , FSIS
P . O . Box 5080
S t . L o u i s , MO 63115

5.

N a t i o n a l I n s t i t u t e of O c c u p a t i o n a l Safety and H e a l t h
C h e m i c a l R e f e r e n c e L a b o r a t o r y (PAT) (R-3)
4676 C o l o m b i a P a r k w a y
C i n c i n n a t i , OH 4 5 2 2 6

6.

U . S . Food and D r u g A d m i n i s t r a t i o n
1090 T u s c u l u m A v e n u e
C i n c i n n a t i , OH 4 5 2 2 6

7.

U . S . C e n t e r for D i s e a s e C o n t r o l
Chief, Performance Evaluation Branch, Laboratory
P r o g r a m O f f i c e , A t l a n t a , GA 3 0 3 3 3
Telephone: (404) 329-3847

8.

A m e r i c a n A s s o c i a t i o n of Feed C o n t r o l
c/o L a w and C o m p a n y
P . O . B o x 1558
A t l a n t a , GA 30301

9.

U . S . Environmental Protection
QA B r a n c h , EMSL
C i n c i n n a t i , OH 4 5 2 6 8

10.

U . S . E n v i r o n m e n t a l P r o t e c t i o n A g e n c y , QA D i v i s i o n
E M S L , P . O . Box 15027
Las V e g a s , NV 89114
T e l e p h o n e : (702) 7 9 8 - 2 1 0 0

11.

Forensic Science Foundation

Collaborative Testing Services, Inc.
8343-A Greensboro Drive
M c L e a n , V A 22102

12.

A m e r i c a n S o c i e t y for Testing
1916 R a c e S t r e e t
P h i l a d e l p h i a , PA 19103

13.

A s s o c i a t i o n of A m e r i c a n Plant Food C o n t r o l O f f i c i a l s
c/o W . Penn Z e n t m e y e r
V A D e p a r t m e n t of A g r i c u l t u r e and C o n s u m e r S e r v i c e s
P . O . Box 1163
R i c h m o n d , VA 23201
Telephone: (804) 786-3511

Officials

Agency

Material

64

14.

U.S. Geological Survey

5293 Ward Road
Arvada, CO 80002
Telephone: (303) 234-3975

15.

American Association of Feed

Attn: Mrs. Janet Windsor
1118 Apple Drive
Mechanicsburg, PA 17055

16.

Association of Food and Drug Officials of the Southern States

c/o George Fong
Division of Chemistry
Florida Department of Agriculture and Consumer Services
3125 Connor Boulevard
Tallahassee, FL 32301

17.

National Food Processors Association

1133 20th Street, NW
Washington, DC 20016
Telephone: (202) 331-5955

18.

College of American Pathologists

7400 N. Skokie Boulevard
Skokie, IL 60077
Telephone: (312) 677-3500

19.

American Association of Bioanalysts

Proficiency Testing Service
205 W. Levee Street
Brownsville, TX 78520
Telephone: (512) 546-5315

Microscopists

It is a d v i s a b l e to p a r t i c i p a t e in as m a n y i n t e r - 1 a b o r a t o r y c h e c k s a m p l e
p r o g r a m s as are a v a i l a b l e in the a r e a s of i n t e r e s t to the l a b o r a t o r y .
The
s p o n s o r i n g o r g a n i z a t i o n s u s u a l l y p r o v i d e a s u m m a r y r e p o r t to p a r t i c p a t i n g
l a b o r a t o r i e s , w h i c h g i v e s an e v a l u a t i o n of the l a b o r a t o r y ' s p e r f o r m a n c e as
compared
to o t h e r p a r t i c i p a n t s .
T h e i n t e r - 1 a b o r a t o r y p r o g r a m can be
supplemented by an intra program to highlight specific areas of concern which
W h e n s e l e c t i n g s a m p l e s for an
are n o t c o v e r e d in the inter p a r t i c i p a t i o n .
intra program, the following considerations should be taken into account:
1.

The capability
laboratory.

to analyze

the

sample must be w i d e l y available

2.

The analytical method must be one that

3.

The sample should cover a variety of analytical

identification steps if possible.

4.

The product must be readily available and reasonable

is generally

in the

employed.

techniques,

including

in cost.

A l w a y s keep in mind that the evaluation of check sample results must include
all aspects of the analysis.
In cases where there is a large discrepancy from
the expected or true result, the laboratory must investigate all aspects of the
analysis (as given in Figure 7.2) to d e t e r m i n e w h a t specific analysis area or
areas are suspect.
From this, the laboratory should take appropriate action to
prevent reoccurrence of a similar difficulty.

65

7.7

Other QA Activities

Some important QA review programmes were discussed in the preceding Sections.

Many other areas of laboratory operations would also benefit from QA review.
Keeping in mind the definition for Quality Assurance given in Section 7.1, any
l a b o r a t o r y o p e r a t i o n can be r e v i e w e d to d e t e r m i n e if c o r r e c t p r o c e d u r e s are
being followed and to identify procedural weaknesses.' Examples are:

1.
S a f e t y - The laboratory safety programme can be periodically reviewed
(about every three months) to determine that safety and emergency materials are
on hand and b e i n g used. T h i s w o u l d i n c l u d e a c h e c k of any i n j u r y or a c c i d e n t
records and a review that appropriate follow-up corrective measures were taken.
2.
S u p p l y M a n a g e m e n t - R e f e r e n c e s t a n d a r d h a n d l i n g and s t o r a g e w a s
discussed earlier.
The s a m e g e n e r a l p r i n c i p l e s a p p l y to all l a b o r a t o r y
supplies, such as glassware, chemicals, solvents and others. A QA review would
focus on whether supplies are being ordered, stored and distributed properly.
3.
S a m p l e M a n a g e m e n t - The s a m p l e s r e c e i v e d by the l a b o r a t o r y for
analysis must be accounted for. This is even more critical when the laboratory
is i n v o l v e d in food l a w e n f o r c e m e n t .
An a c c o u n t a b i l i t y s y s t e m s h o u l d be
e s t a b l i s h e d and in o p e r a t i o n (see S e c t i o n s 4.2 and 4.3). The QA r e v i e w w o u l d
determine that the system is working properly and that samples are accounted
for throughout their receipt, storage, analysis and final disposition.
4.
T r a i n i n g - This m a y s e e m an odd area for QA r e v i e w , but it r a n k s in
importance to most other laboratory operations.
A QA review of training could
i n c l u d e c h e c k s of o n g o i n g f o r m a l t r a i n i n g p r o g r a m m e s for n e w a n a l y s t s and
checks of training needs and records for experienced analysts.
The importance
of t r a i n i n g c a n n o t be o v e r e m p h a s i z e d and a QA r e v i e w p r o g r a m m e o f t e n g i v e s
training needed visibility to management.

The above are only examples and laboratory management must select with care the
o p e r a t i o n a l areas n e e d e d for Q u a l i t y A s s u r a n c e r e v i e w .
R e m e m b e r that any
laboratory function can be (and often should be) subject to QA review.

7.8

Text

1.

G A R F I E L D , F.M.,
Laboratories, 2.
VA, U.S.A.

2.

ISO Guide 25, 1982.

General Requirements for the Technical Competence
Testing Laboratories.
International Organization for Standards.

3.

INTERNATIONAL LABORATORY
Report of Task Force D.

Farther

References
1985.
Q u a l i t y A s s u r a n c e P r i n c i p l e s for A n a l y t i c a l
Association of Official Analytical Chemists, Arlington,

ACCREDATION

CONFERENCE,

London.

Oct.

of

1984.

Reading

B E R M A N , G.A. (Ed.) 1980.

Testing Laboratory Performance:
Accreditation, NBS
P u b l i c a t i o n 591, National Bureau
Gaithersburg, MD, U.S.A.

E v a l u a t i o n and
of
Standards,

Chemistry Quality Assurance Handbook, Volume 1, Principles, U.S. Department

Agriculture, Food Safety and Inspection Service, Washington, DC, U.S.A.

66

of

D U N C A N , A.J.
1974.
Q u a l i t y C o n t r o l and I n d u s t r i a l
Richard D. Irwin, Inc., Homewood, IL., U.S.A.

Statistics,

4th

Ed.,

G A R F I E L D , F.M. et al (Ed.) 1980. O p t i m i z i n g C h e m i c a l L a b o r a t o r y P e r f o r m a n c e

T h r o u g h the A p p l i c a t i o n of Q u a l i t y A s s u r a n c e P r i n c i p l e s , A s s o c i a t i o n of
Official Analytical Chemists, Arlington, VA, U.S.A.
H O R W I T Z , W.
1981.
A C S S y m p o s i u m S e r i e s No. 1 6 0 , T h e P e s t i c i d e C h e m i s t and
Modern Toxicology, "Analytical M e a s u r e m e n t s : H o w Do You K n o w Your Results Are
Right". American Chemical Society, Washington, DC, U . S . A .
INHORN, S.L. (Ed.) 1977.
Quality Assurance Practices for Health
American Public Health Association, Washington, DC, U.S.A.
JURAN, J.M. & GRYNA, F.M.
J U R A N , J.M.,
McGraw-Hill.

GRYNA,

1980.

Quality

F.M. & B I N G H A M ,

Planning

B.S.

1974.

and Analysis,
Quality

Laboratories,

McGraw-Hill.

Control

Handbook,

SHERMA, J. (Ed.) 1976.

Manual of Analytical Quality Control for Pesticides in
H u m a n and Environmental Media, U.S. Environmental Protection Agency, Research
Triangle Park, NC, U.S.A.
Y O U D E N , W.J. & S T E I N E R , E.H.
1975.
S t a t i s t i c a l M a n u a l of
Association of Official Analytical Chemists, Arlington, VA, U.S.A.

67

the

AOAC,

F A O T E C H N I C A L PAPERS
F A O F O O D A N D N U T R I T I O N PAPERS
1/1
1/2

R e v i e w of f o o d c o n s u m p t i o n surveys 1 9 7 7 Vol. 1. Europe, N o r t h A m e r i c a , Oceania, 1 9 7 7 (E)

R e v i e w of f o o d c o n s u m p t i o n s u r v e y s 1 9 7 7 V o l . 2 . A f r i c a , Latin A m e r i c a , Near East, Far East,
1 9 7 9 (E)

Report of t h e joint F A O / W H O / U N E P c o n f e r e n c e o n
m y c o t o x i n s , 1 9 7 7 (E F S)

Report o f a j o i n t F A O / W H O expert c o n s u l t a t i o n o n
dietary f a t s and oils in h u m a n nutrition,

JECFA s p e c i f i c a t i o n s for i d e n t i t y and purity of

t h i c k e n i n g a g e n t s , a n t i c a k i n g agents,
a n t i m i c r o b i a l s , a n t i o x i d a n t s and emulsifiers,

18 Rev. 1

Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 8 4 (E)

18 Rev. 2

Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 8 7 (E)

18 Rev. 3

Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 9 0 (E)

19

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of

carrier s o l v e n t s , emulsifiers and stabilizers,
e n z y m e preparations, f l a v o u r i n g a g e n t s , f o o d
colours, s w e e t e n i n g agents and o t h e r f o o d
additives, 1 9 8 1 (E F)

20
21
22

Legumes in h u m a n n u t r i t i o n , 1 9 8 2 (E F S)
M y c o t o x i n surveillance - a guideline, 1 9 8 2 (E)
Guidelines for agricultural t r a i n i n g curricula in
A f r i c a , 1 9 8 2 (E F)

23

M a n a g e m e n t of g r o u p f e e d i n g p r o g r a m m e s ,
1 9 8 2 (E F P S)
Food and n u t r i t i o n in t h e m a n a g e m e n t of g r o u p
feeding p r o g r a m m e s , 1 9 9 3 (E F S)
Evaluation o f n u t r i t i o n i n t e r v e n t i o n s , 1 9 8 2 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
b u f f e r i n g agents, salts; e m u l s i f i e r s , t h i c k e n i n g
a g e n t s , stabilizers; f l a v o u r i n g a g e n t s , f o o d
colours, s w e e t e n i n g agents and m i s c e l l a n e o u s
f o o d additives, 1 9 8 2 (E F)
Food c o m p o s i t i o n tables for t h e Near East,

1 9 7 7 (E F S)

1 9 7 8 (E)
5
5 Rev. 1
5 Rev. 2

JECFA - guide t o s p e c i f i c a t i o n s , 1 9 7 8 (E F)
JECFA - guide t o s p e c i f i c a t i o n s , 1 9 8 3 (E F)
JECFA - guide t o s p e c i f i c a t i o n s , 1 9 9 1 (E)

The f e e d i n g of w o r k e r s in developing countries,

1 9 7 6 (E S)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
f o o d c o l o u r s , e n z y m e preparations and other f o o d
a d d i t i v e s , 1 9 7 8 (E F)

W o m e n in f o o d p r o d u c t i o n , f o o d handling and
n u t r i t i o n , 1 9 7 9 (E F S)

A r s e n i c and t i n in f o o d s : r e v i e w s of c o m m o n l y
u s e d m e t h o d s of analysis, 1 9 7 9 (E)

10
11
12

P r e v e n t i o n of m y c o t o x i n s , 1 9 7 9 (E F S)
The e c o n o m i c value of breast-feeding, 1 9 7 9 (E F)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and purity of
f o o d c o l o u r s , f l a v o u r i n g agents and other f o o d
a d d i t i v e s , 1 9 7 9 (E F)

2 3 Rev. 1
24
25

26
27
28

1 9 8 3 (E)
Review of f o o d c o n s u m p t i o n s u r v e y s 1 9 8 1 ,
1 9 8 3 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
b u f f e r i n g agents, salts, e m u l s i f i e r s , stabilizers,
t h i c k e n i n g agents, e x t r a c t i o n s o l v e n t s , f l a v o u r i n g
agents, s w e e t e n i n g agents and m i s c e l l a n e o u s
f o o d additives, 1 9 8 3 (E F)
Post-harvest losses in quality of f o o d grains,
1 9 8 3 (E F)

13

Perspective o n m y c o t o x i n s , 1 9 7 9 (E F S)

14
14/1
1 4 / 1 Rev.1

Manuals of food quality

control:
Food c o n t r o l l a b o r a t o r y , 1 9 7 9 (Ar E)
The f o o d c o n t r o l laboratory, 1 9 8 6 (E)

14/2

A d d i t i v e s , c o n t a m i n a n t s , t e c h n i q u e s , 1 9 8 0 (E)

14/3
14/4

C o m m o d i t i e s , 1 9 7 9 (E)
M i c r o b i o l o g i c a l analysis, 1 9 7 9 (E F S)

30

F A O / W H O f o o d additives d a t a s y s t e m , 1 9 8 4 (E)

3 0 Rev. 1

14/5
14/6
1 4 / 6 Rev.1
14/7

Food
Food
Food
Food

31/1

F A O / W H O f o o d additives data s y s t e m , 1 9 8 5 (E)

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
f o o d colours, 1 9 8 4 (E F)

c o n t a m i n a n t s and c o m p o s i t i o n , 1 9 8 6 (C E)
Food analysis: q u a l i t y , adulteration and t e s t s of

32

14/8

i d e n t i t y , 1 9 8 6 (E)
I n t r o d u c t i o n t o f o o d s a m p l i n g , 1 9 8 8 (Ar C E F S)
T r a i n i n g in m y c o t o x i n s analysis, 1 9 9 0 (E S)
M a n a g e m e n t of f o o d c o n t r o l p r o g r a m m e s ,

33

14/9
14/10
14/11

1 9 9 1 (E)
Q u a l i t y a s s u r a n c e in the f o o d c o n t r o l
m i c r o b i o l o g i c a l laboratory, 1 9 9 2 (E F S)
Pesticide residue analysis in t h e f o o d c o n t r o l
l a b o r a t o r y , 1 9 9 3 (E F)
Q u a l i t y assurance in t h e f o o d c o n t r o l chemical

35

R e v i e w of f o o d c o n s u m p t i o n s u r v e y s 1 9 8 5 ,
1 9 8 6 (E)

36

Guidelines for c a n m a n u f a c t u r e r s and f o o d

canners, 1 9 8 6 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
certain f o o d additives, 1 9 8 6 (E F)

l a b o r a t o r y , 1 9 9 3 (E)
I m p o r t e d f o o d inspection, 1 9 9 3 (E F)
Radionuclides in f o o d , 1 9 9 4 (E)
C a r b o h y d r a t e s in h u m a n nutrition, 1 9 8 0 (E F S)
A n a l y s i s of f o o d c o n s u m p t i o n s u r v e y data for
d e v e l o p i n g c o u n t r i e s , 1 9 8 0 (E F S)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
s w e e t e n i n g a g e n t s , e m u l s i f y i n g agents, f l a v o u r i n g
a g e n t s and other f o o d additives, 1 9 8 0 (E F)
Bibliography of f o o d c o n s u m p t i o n s u r v e y s ,
1 9 8 1 (E)

38

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of

certain f o o d additives, 1 9 8 8 (E)

39

Quality c o n t r o l in f r u i t and v e g e t a b l e p r o c e s s i n g ,
1 9 8 8 (E F S)
D i r e c t o r y of f o o d and n u t r i t i o n i n s t i t u t i o n s in the
Near East, 1 9 8 7 (E)
Residues of s o m e v e t e r i n a r y d r u g s in animals and
f o o d s , 1 9 8 8 (E)

14/12
14/13
14/14
14/15
14/16
15
16
17

18

inspection, 1981
for e x p o r t , 1 9 7 9
for e x p o r t , 1 9 9 0
analysis: general

(Ar E) (Rev. 1 9 8 4 , E S)
(E S)
(E S)
t e c h n i q u e s , additives,

29

31/2

JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of

f o o d additives, 1 9 8 4 (E F)

34

37

40
41
41/2

Residues of v e t e r i n a r y d r u g s in f o o d s ,
1 9 8 5 (E/F/S)
Nutritional implications of f o o d aid: an a n n o t a t e d
bibliography, 1 9 8 5 (E)
JECFA s p e c i f i c a t i o n s for i d e n t i t y and p u r i t y of
certain f o o d additives, 1 9 8 6 (E F)

Residues of s o m e v e t e r i n a r y d r u g s in animals and

f o o d s . T h i r t y - f o u r t h m e e t i n g of t h e j o i n t
F A O / W H O Expert C o m m i t t e e o n Food A d d i t i v e s ,
1 9 9 0 (E)

41/3

41/4

Residues of s o m e veterinary drugs in animals and

f o o d s . T h i r t y - s i x t h m e e t i n g of the joint F A O / W H O
Expert C o m m i t t e e o n Food A d d i t i v e s , 1 9 9 1 (E)
Residues of s o m e v e t e r i n a r y drugs in animals and

55

Sampling plans for a f l a t o x i n analysis in p e a n u t s

and c o r n , 1 9 9 3 (E)

56

Body m a s s index - A m e a s u r e of c h r o n i c energy

d e f i c i e n c y in adults, 1 9 9 4 (E F S)
Fats and oils in h u m a n n u t r i t i o n , 1 9 9 5 (Ar E F S)

f o o d s . T h i r t y - e i g h t h m e e t i n g of t h e joint
F A O / W H O Expert C o m m i t t e e o n Food A d d i t i v e s ,
1 9 9 1 (E)

57
58

The use of hazard analysis critical c o n t r o l point

(HACCP) principles in f o o d c o n t r o l , 1 9 9 5 (E F S)

41/5

Residues of s o m e veterinary drugs in animals and

59
60

N u t r i t i o n e d u c a t i o n for t h e public, 1 9 9 5 (E F S)
Food f o r t i f i c a t i o n : t e c h n o l o g y and quality c o n t r o l ,
1 9 9 6 (E)

41/6

f o o d s . Fortieth m e e t i n g of t h e J o i n t F A O / W H O
Expert C o m m i t t e e on Food A d d i t i v e s , 1 9 9 3 (E)
Residues of s o m e v e t e r i n a r y drugs in animals and

61
62

B i o t e c h n o l o g y and f o o d s a f e t y , 1 9 9 6 (E)
N u t r i t i o n e d u c a t i o n for t h e public - D i s c u s s i o n
papers of t h e FAO Expert C o n s u l t a t i o n , 1 9 9 6 (E)

63
64

Street f o o d s , 1 9 9 7 (E/F/S)
W o r l d w i d e regulations for m y c o t o x i n s 1 9 9 5 - A
c o m p e n d i u m , 1 9 9 7 (E)
Risk m a n a g e m e n t and f o o d s a f e t y , 1 9 9 7 (E)

f o o d s . F o r t y - s e c o n d m e e t i n g of the J o i n t
F A O / W H O Expert C o m m i t t e e on Food A d d i t i v e s ,
1 9 9 4 (E)
41/7

41/8

Residues of s o m e
f o o d s . Forty-third
Expert C o m m i t t e e
Residues of s o m e

veterinary d r u g s in animals and

m e e t i n g of t h e J o i n t F A O / W H O
o n Food A d d i t i v e s , 1 9 9 4 (E)
veterinary drugs in animals and

41/9

f o o d s . F o r t y - f i f t h m e e t i n g of t h e J o i n t F A O / W H O
Expert C o m m i t t e e o n Food A d d i t i v e s , 1 9 9 6 (E)
Residues of s o m e v e t e r i n a r y drugs in animals and
f o o d s . F o r t y - s e v e n t h m e e t i n g of t h e J o i n t
F A O / W H O Expert C o m m i t t e e o n Food A d d i t i v e s ,
1 9 9 7 (E)

65

Availability: November 1 9 9 7
Ar

Arabic

C
E
F

Chinese
English
French

Multil

Multilingual
Out of print
In preparation

42
42/1

Traditional f o o d plants, 1 9 8 8 (E)

Edible plants of Uganda. The value o f w i l d and

Portuguese

Spanish

43

c u l t i v a t e d plants as f o o d , 1 9 8 9 (E)
Guidelines for agricultural training curricula in A r a b
c o u n t r i e s , 1 9 8 8 (Ar)

44

R e v i e w of f o o d c o n s u m p t i o n s u r v e y s 1 9 8 8 ,

FAO Sales Agents

FAO. Viale delle Terme di Caracalla, 00100Rome,

45
46

1 9 8 8 (E)
Exposure of i n f a n t s and children t o lead, 1 9 8 9 (E)
S t r e e t f o o d s , 1 9 9 0 (E/F/S)

47/1

Utilization of t r o p i c a l f o o d s : cereals, 1 9 8 9 (E F S)

47/2
47/3
47/4

Utilization of t r o p i c a l f o o d s : roots and t u b e r s ,

1 9 8 9 (E F S)
Utilization of t r o p i c a l f o o d s : trees, 1 9 8 9 (E F S)
Utilization o f t r o p i c a l f o o d s : tropical beans,

47/5

1 9 8 9 (E F S)
Utilization of t r o p i c a l f o o d s : t r o p i c a l oil seeds,
1 9 8 9 (E F S)

47/6
47/7
47/8

Utilization of t r o p i c a l f o o d s : sugars, spices and

s t i m u l a n t s , 1 9 8 9 (E F S)
Utilization of t r o p i c a l f o o d s : fruits and leaves,
1 9 9 0 (E F S)
Utilization of t r o p i c a l f o o d s : animal p r o d u c t s ,
1 9 9 0 (E F S)

48

N u m b e r not assigned

49

JECFA s p e c i f i c a t i o n s for i d e n t i t y and purity of

c e r t a i n f o o d additives, 1 9 9 0 (E)

50
51

Traditional f o o d s in the Near East, 1 9 9 1 (E)

Protein quality evaluation. Report of t h e J o i n t
F A O / W H O Expert C o n s u l t a t i o n , 1 9 9 1 (E F)

52/1

C o m p e n d i u m of f o o d additive s p e c i f i c a t i o n s V o l . 1, 1 9 9 3 (E)
C o m p e n d i u m of f o o d additive s p e c i f i c a t i o n s -

52/2

V o l . 2 , 1 9 9 3 (E)
52 Add. 1
52 Add. 2
52 Add. 3
52 Add. 4
52 Add. 5
53
54

C o m p e n d i u m of f o o d additive
A d d e n d u m 1, 1 9 9 2 (E)
C o m p e n d i u m of f o o d additive
A d d e n d u m 2, 1 9 9 3 (E)
C o m p e n d i u m of f o o d additive
A d d e n d u m 3, 1 9 9 5 (E)
C o m p e n d i u m of f o o d additive
A d d e n d u m 4 , 1 9 9 6 (E)

specifications specifications specifications specifications -

C o m p e n d i u m of f o o d additive s p e c i f i c a t i o n s A d d e n d u m 5, 1 9 9 7 (E)
M e a t and m e a t p r o d u c t s in h u m a n n u t r i t i o n in
d e v e l o p i n g c o u n t r i e s , 1 9 9 2 (E)
N u m b e r not assigned

The FAO Technical Papers are available

or directly

through

the

authorized

from Sales and Marketing

Italy

Group,

- --

'

'

'

- - -

'

. .

ISBN 92-5-102489-8

9
M

.87

7 8 9 2 5 1

ISSN 0254-4725

0 2 4 8 9 8
T0432E/2/9.97/500