Lab Automation & QC

ICPS 2002

Laboratory
Automation
&
Quality Control
1

FLS Automation June 2002

 Sampling
Sample

transport
Sample preparation
Sample Analysis
Control Actions
Storage of data

Lab Automation & QC

What is lab automation?

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FLS Automation June 2002

 Do

you want to have a consistent and

maybe an improved QC, which will also
give you an improved product?
z

Different operators do things differently. This

results in shifts in analytical level from one
operator to another. Have you seen that?
Do you know if your sampling is
representative? Continous sampling
theoretically the preferred nmethod. Continous
sampling is easier done by an automatic
sampler than by manual sampling.

Lab Automation & QC

Why automate?

3
FLS Automation June 2002

 Do

you want to have a consistent and

maybe an improved QC, which will also
give you an improved product?
z

Some preparation/analytical methods are not

suited for some materials. The right method
may be difficult in manual operation, but easy
to automate.
Would it be of value to you to increase the
analytical schedule? So you would gain more
knowledge of your process? An automatic
system may be able to process an increased
number of samples compared to an operator
Is it easy for you to retrieve data for evaluation
purposes. Automatic systems helps you store
and distribute valuable data.

Lab Automation & QC

Why automate?

4
FLS Automation June 2002

 Do

you want to tighten the quality

control? Do you want to avoid producing
low quality product, but to save fuel and
energy?
z

You would need frequent and fast capture of

analyses and production data. This is not easy
to do manually.
It may be obtained by moving the analytical
instruments into the process thereby saving
sampling and sample transport time,
preparation time and analysis time

Lab Automation & QC

Why automate?

5
FLS Automation June 2002

 Do

you want to save construction and/or

operational costs?
z

Tight quality control allows for optimisation of

process lay-out, i.e. reduced blending
facilities and controlled use of
difficult/expensive raw materials

Lab Automation & QC

Why automate?

6
FLS Automation June 2002

 Lastly,

you may also want to save labour

cost.
z

This may be done by exchanging the

operator/lab tecnician with automated
equipment from sampling to analysis

Lab Automation & QC

Why automate?

7
FLS Automation June 2002

 Tight

quality
control during
production
z On-stream, Inline analysers
etc
z Automated Lab
system

Quality

requirements from
customers on
(end) product
z Automated Lab
systems

Lab Automation & QC

Main Purposes of Lab Automation

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FLS Automation June 2002

Laboratory Automation and On-line Analysis

On-line Analysis:
PGNAA

Central
laboratory
automation
FLS Automation June 2002

Lab Automation & QC

or PGNAA

XRF
FCaO/PSZ
9

 Based

on very accurate analytical

instruments, correct sample preparation
methods, reliable sampling and sample
transport systems
Various suppliers (FLSA, Polysius, Pfaff,
Herzog, Iteca )
Possible FLSA solutions will be discussed
in details, competitor solution mentioned!

Lab Automation & QC

Automated Lab Systems

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FLS Automation June 2002

 FLS Automation June 2002

Lab Automation & QC

FLS Automation lab systems

11

QCX/RoboLab

integrates manual or semi-automatic analysis &

sample prep equipment
high flexibility in equipment selection
high to very high capacity
built in manual back-up
modular design allows for easy integration of
additional equipment

QCX/AutoPrep

automated equipment units

well suited for small powder prep only
applications
small to medium capacity
built in manual back-up

Lab Automation & QC

FLS Automation lab systems

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FLS Automation June 2002

13
Raw meal
Silo

Cement
Silos

Raw mill

Clinker
storage
Kiln

Manual production lab

QCX
Scalability: Small
Laboratory Automation and On-line Analysis
FLS Automation June 2002

Cement
mill

Lab Automation & QC

Quarry
& Piles

14
Raw meal
Silo

Cement
Silos

Raw mill

Clinker
storage

Cement
mill

Kiln

Automated production lab

QCX Scalability: Medium size

FLS Automation June 2002

Lab Automation & QC

Quarry
& Piles

 FLS Automation June 2002

Lab Automation & QC

ASIA Cement, Thailand

15

QCX Scalability: Large

Raw meal
Silo

Cement
Silos

Raw mill

Clinker
storage

Cement
mill

Kiln

AAS

Fully automated production lab

FLS Automation June 2002

CST

Plant wide LIMS for

ALL analysis & test data

Lab Automation & QC

Quarry
& Piles

16

17
Mill

X-ray room

Sample
prep room

Press

Mill

XRF

Composites

Sample
transport
Colour

XRD
Dosing/
cleaning

Lab Automation & QC

QCX/RoboLab

Particle Size
Fusion

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FLS Automation June 2002

 Sample

receipt

Identification & registration

Sample splitting & dosing
Individual preparation recipes
Priority management
Alternative routing in
failure situations
Integrated control and
dynamic supervision of :
- Robot
- Prep eqp & Analysis instrms
( - Sample transport PLC )
FLS Automation June 2002

Lab Automation & QC

QCX/RoboLab - General features

18

18

19

AUT
LAB

AUT
LAB

AUT
LAB

AUT
LAB

FLS Automation June 2002

Lab Automation & QC

QCX/RoboLab Configurations

 Allow

your self time to study your needs

carefully
Discuss your needs with qualified
suppliers, who knows the process and the
problems most often seen
If any doubt, have a pre-study made on
your materials to ensure the correct
choice of equipment
Balance your investments between
sampling and lab equipment. Where do
you gain the most?

Lab Automation & QC

Recommendation

20

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FLS Automation June 2002

Laboratory Automation and On-line Analysis

On-line Analysis:
PGNAA

Central
laboratory
automation
FLS Automation June 2002

Lab Automation & QC

or PGNAA

21

XRF
FCaO/PSZ
21

On-line analysis

On-line analysis

Central laboratory
automation

Main objective : quality control

Applied on more and more sampling points

Central laboratory
Main objectives : quality control and quality
assurance
manpower savings, correct sample
preparation, ...

Lab Automation & QC

Competing technologies ?

22

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FLS Automation June 2002

Process flow
Analysis data

Limestone

Accounting
Control loop
(manual or auto)

Clay

Feed
proportions

PGNAA

QCX/
BlendExpert
OLA

Lab Automation & QC

QCX & On-Line StockPile Control

23

QCX/Laboratory
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FLS Automation June 2002

 Circular

stockpiles: accounting in
accordance with circular coordinates
of stacker and reclaimer, if coordinates
are provided from the PLC.
If not, accounting is simple endless
integration

Lab Automation & QC

QCX/BlendExpert & Pile Cntrl

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FLS Automation June 2002

 Longitudinal

stockpiles: the accounting

provides one total average composition
of the stockpile section currently being
stacked = simple batch integration.
After completion status changes to
reclaimed and later historic pile

Lab Automation & QC

QCX/BlendExpert & Pile Cntrl

25

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FLS Automation June 2002

Sand

Process flow
Analysis data

Pyrite

Limestone

Accounting
Control loop
(manual or auto)

PGNAA

QCX/
BlendExpert
OLA

Lab Automation & QC

Raw mix on the stockpile

26

QCX/Laboratory
Control scheme for producing raw mix on the pile
FLS Automation June 2002

26

Before:

Manual stockpile control

4 component mix cntrl before mill
(Polab)
LSF std devs out of mill = 4-5

Now:

Two stockpiles (one circular, one

longitudinal) equipped with PGNAA
analysers (ASYS FSA)
Manual feed to pile control including
additives
100 % feed from both piles to raw mills,
thus no mixing before raw mills
LSF std devs out mill = 1.7-1.9

Future:

Automation of additive feed

Lab Automation & QC

Raw mix on the stockpile

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FLS Automation June 2002

Raw materials

Raw mill
Feeder
set
points

PGNAA

QCX/
BlendExpert

Fast
OLA

QCX/
OnStream
Fast

Process flow
Sample
Analysis data
Control loop

FLS Automation June 2002

Average
sample

28

Lab Automation & QC

QCX & On-Line Raw Mix Control

Slow

QCX/Laboratory
Control can be based solely on on-line analysis or
in a redundant set-up incorporating lab XRF analysis

28

29

Compact and robust

cabinet (IP65) with local
control panel
Analyses all 4 main
elements:
Fe, Ca, Al, Si
Analysis time 2-5 minutes
(EDXRF)
Lower investment required
than for PGNAA-based
alternatives

Lab Automation & QC

QCX/OnStream

Combines traditional and on-line techniques.

Tighter quality control at lowest possible cost.
29
FLS Automation June 2002

Process
flow

OnStream air slide sampler

OnStream
screw sampler

Process flow

Dosing device

Analyzer cabinet
Blower

Excess
material
return

30

Lab Automation & QC

QCX/OnStream

alternative

QCX/OnStream cabinet
30

FLS Automation June 2002

Process
flow

OnStream air slide sampler

OnStream
screw sampler

Process flow

Dosing device

Screw
sampler
Air slide
sampler

Analyzer cabinet
Blower

Excess
material
return

31

Lab Automation & QC

QCX/OnStream

alternative

Dosing device
31

FLS Automation June 2002

Process
flow

OnStream air slide sampler

OnStream
screw sampler

Process flow

Dosing device

OSCA3000 analyzer
Analyzer cabinet
Blower

Excess
material
return

32

Lab Automation & QC

QCX/OnStream :

alternative

Calibration
sample outlet
32

FLS Automation June 2002

130

LSF
120
110
100
90
80

Before QCX/OnStream

With QCX/OnStream

US Plant
1999

70

High frequency sampling and analysis

Fast control response
Reduced kiln feed variations with small (or poor) silos
Reduced work load for sampling, preparation & analysis
Robust installation

Lab Automation & QC

QCX/OnStream Control performance

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FLS Automation June 2002

Static

Dynamic

SiO2

Results
0.078

Results
0.111

Al2O

0.072

0.096

CaO

0.065

0.126

Fe2O3

0.008

0.022

LSF

0.57

0.72

Lab Automation & QC

OnStream test results

34

Results achieved with 30 secs integration

time for all elements.
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FLS Automation June 2002

Lab
WDXRF

On-line
EDXRF

On-line
PGNAA

( 20 sec )

( 100 sec )

( 10 min )

SiO2

0.05

0.10-0.20

0.15-0.30

Al2O3

0.015

0.10-0.15

0.12-0.20

CaO

0.025

0.10-0.20

0.25-0.40
( 0.15-0.20 )

Fe2O3

0.004

0.03-0.05

0.03-0.06

ASYS

Precision ( = repeatability) data incl sample prep for

Lab WDXRF & sample presentation for On-line EDXRF
FLS Automation June 2002

Lab Automation & QC

Online Analytical Performance

35

20

11

13

14

12

if this is Lab WDXRF

then this is
on-line EDXRF
18

16

10

15

Lab Automation & QC

Precision

36

and this is
on-line PGNAA

17

19

36
FLS Automation June 2002

C3S / LSF S.dev

4
: sampling

On-line
PGNAA

: sample preparation

(10 min)

: analysis

Traditional
Lab WDXRF

On-line
EDXRF
OSCA3000
(100 sec)

(20 sec)

FLS Automation June 2002

S
Y
S

Lab Automation & QC

Error on Dynamic Precision

37

C3S / LSF S.dev

12

Including time for filling of flow cell, compacting,

emptying etc, one OnStream cycle is 5 min.
so this would be the fair value to compare with

----- On-line PGNAA -----

(5 min)

4
(10 min)

On-line EDXRF
3

OSCA3000
(5 min)

A
FLS Automation June 2002

S
Y
S

S
Y
S

Lab Automation & QC

Error on Dynamic Precision

38

39

12 8

Manual/
off-line
control
+
Lab-XRF

Based on hourly average

samples taken at raw mill
outlet and measured on Lab
WDXRF ( = true value)

Lab-XRF
Lab-XRF
6

manual
sample prep automatic
sample prep
(1 sample/hr)
(RoboLab)
(2 samples/hr)

On-line
PGNAA

On-line
EDXRF

2
: Advanced computerized raw mix blending control

FLS Automation June 2002

Lab Automation & QC

C3S/LSF S.dev

Traditional

OnStream

QCX/OnStream combines the high freq. of

the OnStream analyser with the high precision and high accuracy of lab analyser

QCX/OnStream monitors the process dynamics; the lab analyser

establish the accurate
chemical levels

The redundant structure is tolerant to errors in one of the instr

instruments

Sampling
error

Sampling
error

Analytical
& sample
presentation

error
Preparation
error
Analytical error
FLS Automation June 2002

Lab Automation & QC

Traditional Vs OnStream analysis

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-EDXRF or PGNAA for raw mix control

(Choice to some extent pending process lay-out details)
EXDRF has the potential for lowest LSF std.dev. Out of
mill
-PGNAA for stock pile control
where requirements to analysis precision are less
stringent, and for raw mix control when long transport
delays in the material department exists (e.g. Surge
bins)
QCX supports interfacing og all PGNAA models on the market

On-line EDXRF/PGNAA does not eliminate the need

for the traditional lab analyser (WDXRF)

Lab Automation & QC

FLSA recommendations

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FLS Automation June 2002

 On-line

instrumentation for control of

material properties (chemical analysis,
fineness ) will increase to support JustIn-Time production:
z
z
z
z

z
z

Reduce material storage's

Recipe control
Special products and qualities
Fast change of production to
reduce waste
Utilise difficult raw materials
Power savings

Lab Automation & QC

Future Trends

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FLS Automation June 2002

 Increased

demand for documentation and

accountability from both customers (Total
Quality Control) and from authorities on
environmental impact:
z

System must handle large amount

of data in a safe way
Laboratory procedures will be very
stringent and automation will be
wide-spread in other areas of the
cement analysis (physical testing,
fuel, )

Lab Automation & QC

Future Trends

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FLS Automation June 2002

EDXRF
FCaO
FSA
LIMS
PGNAA
PSZ
QCX
WDXRF
XRF
XRD

Energy Dispersive X-Ray Fluorescence

Free Lime
Full Stream Analyser
Laboratory Information Management System
Prompt Gamma Neutron Activation Analysis
Particle Size Measurement
Quality Control by Computer and X-ray
Wavelength Dispersive X-Ray Fluorescence
X-Ray Fluorescence
X-Ray Diffraction

Lab Automation & QC

Abbreviations

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FLS Automation June 2002