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AGC

Titration
Book 20%
Excellence
Cyan

34

Application brochure

Titrators
T50
T70
T90

Selected METTLER TOLEDO Methods


for Titration Excellence Line

EDITORAL
Dear Reader
METTLER TOLEDOs business area titration is proud to present the first selected
application methods for the new Titration Excellence line. It consists of the three
models T50, T70 and T90 and offers many advantages such as One Click Titration,
Plug & Play and Method database.
The T50 represents the first level of excellence in titration and offers much more than a
simple titrator: a terminal with brilliant touch screen, expandable with dispensing burette
drives, comprehensive communication connections, and preconfigured system
application packages.
The all-rounder the T70 additionally shows further advantages. It allows the
performance of manual operations, such as burette rinsing, while an analysis is
running. An additional sensor card can be added and it can be upgraded to the highest
model (T90).
The T90 is the most powerful titrator: parallel titrations can be run while up to 6 different
manual operations are running at the same time. It features unlimited flexibility and
expansion possibilities in hardware and software.
No matter which model of the new line you choose method development has never
been easier thanks to the superb, intuitive and consistent graphical user interface using
the color touch screen terminal.
The 38 selected METTLER TOLEDO methods which are pre-programmed in the
standard delivery of every model have been developed and extensively tested on real
samples by the Market Support Group Analytical Chemistry. These methods are readyto-use without modifications, or they can act as excellent starting points for method
development.
Furthermore, 13 application modes have been created in order to find the right control
parameters efficiently. Depending on the indication and the chemistry taking place
during titration, one or more application modes can be selected. Every application
mode shows three sets of control parameters which you can select from (cautious,
normal and fast), depending on the requirements for your specific titration.
This application brochure gives a short introduction into the method development
possibilities of the Titration Excellence instruments, lists the parameters of all
application modes in detail, shows the structures of all method templates and presents
all METTLER TOLEDO methods including procedures, literature references and
results.
We wish you much success titrating with the METTLER TOLEDO Titration Excellence
line.

Mike Treyer
Market Support Manager BA Titration

Rolf Rohner
Marketing Manager BA Titration

METTLER TOLEDO

CONTENT

General Information

Introduction

METTLER TOLEDO Methods

II

Method Templates

IV

EQP Titration

Application Modes

Learn Titrations

VII

38 METTLER TOLEDO Methods

Page 1

21 Method Templates

Page 115

13 Application Modes

Page 125

Figure 1: Excellence in titration: Titration Excellence Line

METTLER TOLEDO

GENERAL INFORMATION
Introduction
No matter what analysis tasks you are challenged with - the process to meet specific
analytical requirements begins with the analysis method.
The Titration Excellence line featuring One Click TitrationTM is designed to be simple,
efficient, modular and secure not only in routine use but also in method
development.
The modular method concept allows customization of methods according to your
specific needs. Methods are made up of method functions which in turn can be flexibly
deleted, edited or inserted at almost every position within the method.

Figure 2: Inserting a method function in the desired place

Not only single method functions can be inserted or deleted, it is possible to add or
remove complete analysis loops at once for more efficient method development.

Figure 3: Removing a complete analysis loop by deleting the method function Sample

METTLER TOLEDO
Secure method development is achieved by assigning user rights which prevent
methods from being changed or deleted by unauthorized personnel. In addition, every
method can be protected by its author. A protected method can only be modified or
removed by an administrator or the author him/herself.

Figure 4: Protecting a method (method function Title)

The following chapters show how simple it is to create methods for your specific
purposes. The main features to achieve this are:

Pre-programmed METTLER TOLEDO Methods


Pre-programmed method templates
Pre-programmed application modes
Learn titration

METTLER TOLEDO Methods


The METTLER TOLEDO method concept is well-known and has been established for
many years. In the first version all Titration Excellence instruments feature 38 different,
pre-programmed METTLER TOLEDO methods which represent a selection of the most
important applications in the field of titration.
One important advantage of these methods is that they are ready-to-use: you simply
select one from the method list and start it. Even the resources such as titrants,
sensors, substances etc. needed to execute the methods are already predefined.
METTLER TOLEDO methods were optimized for the analysis of certain applications.
Your specific application might require a slight adaptation of the method. Simply
change the method as described before and save it under a different method ID.

II

METTLER TOLEDO
Note: Method IDs starting with an M followed by numbers are reserved for METTLER
TOLEDO methods.
Method ID
M400
M401
M402
M403
M404
M405
M406
M407
M408
M409
M410
M411
M412
M413
M414
M415
M416
M417
M418
M419
M420
M421
M422
M423
M424
M425
M426
M427
M428
M429
M430
M431
M432
M433
M434
M435
M436
M437

Title
Acetic acid content in vinegar
Ammonium chloride content
Free fatty acid content
Blank solvent FFA
Chloride content in Ketchup
Total hardness of tap water
Ca + Mg content of tap water
Sulfate content
Barium content conductometric
Copper content
Hydrogen peroxide content
Vitamin C content voltametric
Vitamin C content amperometric
SDS content photometric
SDS content potentiometric
m-Value of tap water (EP)
p-Value of tap water (EP)
Antacid (Stating)
HCl content (EP)
Free SO2 content in wine (EP)
Water content KF (EP)
Titer KF (EP)
Drift KF (EP)
Standby KF (EP)
Bromine number ASTM D1159 (EP)
Blank ASTM D1159 (EP)
Acid number ASTM D664
Blank ASTM D664 (EP)
Base number ASTM D4739
Blank ASTM D4739
Base number ASTM D2896
Blank ASTM D2896
Chloride content in motor oil
Mercaptan sulfur ASTM D3227
SDS content (2-phase)
Titer 0.1 mol/L NaOH
Calibration DG111-SC
HCl content conductometric

Page
1
4
7
10
13
16
19
22
25
28
31
34
37
40
43
46
49
52
55
58
61
64
67
70
73
76
79
82
85
88
91
94
97
100
103
106
109
112

Table 1: METTLER TOLEDO methods

III

METTLER TOLEDO
Method Templates
Another simple and efficient way to obtain your specific method is to use a method
template. Such templates define the structure of a method, namely the sequence of
method functions.
By pressing the New button in the method list which is accessible in the submenu
Home>>Methods, a list of various method templates is displayed. Simply select the
template that best fits the structure of your specific method and edit it according to your
demands.
Title
EQP
EP
Stating
Measure
2-phase
Learn-EQP
Titer with EQP
Titer with EP
Calibration
Calibration segmented
Blank with EQP
Blank with EP
EP / EQP
EQP / EQP
EP / EP
Titer with EQP & EQP
Titer with EP & EP
Calibration & EQP
Calibration & EP
Calibration & Titer with EQP & EQP
Calibration & Titer with EP & EP

Titrator Models
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T50 / T70 / T90
T70 / T90
T70 / T90
T70 / T90
T70 / T90
T70 / T90
T70 / T90

Page
115
115
115
116
116
116
117
117
117
118
118
118
119
119
120
120
121
121
122
123
124

Table 2: Method templates

Note: Multiple-loop methods (and method templates) require a T70 or a T90 titrator. A
method loop characterizes the part of the method which every sample of a sample
series runs through. It starts with a method function Sample and end with the method
function End of sample. A multiple-loop method therefore is nothing else but a
complex method made up of several methods.
Most parameters of a selected method template show default values. After editing
them, the method template has to be saved as a user method using an appropriate
method ID before it can be started. These user methods which can also be developed
from METTLER TOLEDO methods are added to the method list.

IV

METTLER TOLEDO
EQP Titration
The equivalent point (EQP) titration is the most frequently used analysis type in the
field of titration. The control parameters of the method function Titration (EQP)
determine whether the method is suitable for your application or not. The optimal
control parameters for your EQP titration can efficiently be developed either using
application modes or the intelligent Learn Titration.

Application Modes
The parameters of the method subfunction Control define how a titrant is added and
how the measurement points needed for evaluation are taken. Application modes are
predefined sets of control parameters which are optimized for the chemical reaction
involved in titration such as precipitation, complexation etc.
Depending on the sensor type and measurement unit selected in the subfunction
Sensor, one or more application modes are available in the subfunction Control.
Note: all subfunctions mentioned here refer to method function Titration (EQP).
Subfunction Sensor

Sensor type
pH
mV

ISE

Phototrode
Polarized
Temperature

Conductivity

Unit
pH
mV
mV
mV
ppm
pX
pM
mV
%T
A
mV
uA
o
C
o
F
K
mS
uS
mS/cm
uS/cm

Subfunction Control

Application Modes
Acid / base
Acid / base (non aq.)
Precipitation
Precipitation (non aq.)
Redox

Page
125
125
126
126
126

Precipitation

127

Precipitation
Complexation

127
127

Redox
Redox

128
128

Acid / base

129

Acid / base
Precipitation

129
129

Table 3: Application modes for different sensors and measurement units

It is important to note that an application mode shows different control parameters for
different sensors (e.g. Acid / base for a pH sensor does not contain the same
parameters as Acid / base for a conductivity sensor).
V

METTLER TOLEDO
For every application mode there are 3 pre-programmed sets of parameters available.
You select your optimal parameter set from the following options provided under the
parameter Control:

Fast: Parameter set for fast titrations


Normal: Parameter set for the majority of titrations
Cautious: Parameter set for critical titrations

Getting a good starting point on the way to optimal control parameters for your
application is very simple: select Fast, Normal or Cautious and choose an
application mode (if more than one is possible)! In case you would like to view the preprogrammed parameters, just click on the check box Show parameters.
If you wish to change the selected control parameters, simply change the parameter
Control to User (see figure 5). This doesnt change the parameters but enables you
to edit them.

Figure 5: Parameters of subfunction Control of method function Titration (EQP)

VI

METTLER TOLEDO
Learn Titration
Let your Titration Excellence instrument learn the control parameters for optimal
performance of your titration with the Titration (LearnEQP) method function.
In this method function, no control parameters have to be selected they are
determined with the titration of the first sample. After the analysis, the Titration
(LearnEQP) method function turns into a regular method function Titration (EQP),
showing the determined parameters.
When running a series of samples, the parameters determined by sample 1 are applied
to all subsequent samples. There is no need to create another method or to run
another series.
Note: The statistics calculation discards the result of the first sample.

Titration Excellence

Figure 6: Subfunctions of method function Titration (Learn-EQP)

VII

METTLER TOLEDO

Figure 7: Terminal to control the Titration Excellence instruments T50 / T70 / T90

VIII

METTLER TOLEDO

METTLER TOLEDO METHODS


Content
Method ID
M400
M401
M402
M403
M404
M405
M406
M407
M408
M409
M410
M411
M412
M413
M414
M415
M416
M417
M418
M419
M420
M421
M422
M423
M424
M425
M426
M427
M428
M429
M430
M431
M432
M433
M434
M435
M436
M437

Title
Acetic acid content in vinegar
Ammonium chloride content
Free fatty acid content
Blank solvent FFA
Chloride content in Ketchup
Total hardness of tap water
Ca + Mg content of tap water
Sulfate content
Barium content conductometric
Copper content
Hydrogen peroxide content
Vitamin C content voltametric
Vitamin C content amperometric
SDS content photometric
SDS content potentiometric
m-Value of tap water (EP)
p-Value of tap water (EP)
Antacid (Stating)
HCl content (EP)
Free SO2 content in wine (EP)
Water content KF (EP)
Titer KF (EP)
Drift KF (EP)
Standby KF (EP)
Bromine number ASTM D1159 (EP)
Blank ASTM D1159 (EP)
Acid number ASTM D664
Blank ASTM D664 (EP)
Base number ASTM D4739
Blank ASTM D4739
Base number ASTM D2896
Blank ASTM D2896
Chloride content in motor oil
Mercaptan sulfur ASTM D3227
SDS content (2-phase)
Titer 0.1 mol/L NaOH
Calibration DG111-SC
HCl content conductometric

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58
61
64
67
70
73
76
79
82
85
88
91
94
97
100
103
106
109
112

M400

METTLER TOLEDO

Acetic Acid Content in Vinegar


The acetic acid content is determined in vinegar by titration with sodium hydroxide.

Sample

Substance
Chemicals

Vinegar, 0.7-1 g.

Acetic acid, CH3COOH,


M = 60.05 g/mol, z = 1
50 mL deionized water

Preparation and Procedures


Note:
This method allows a fully automated analysis procedure. The
method can be easily modified for manual operation. Select
"Manual stand" in the method function "Titration stand".
1) Adjustment of the DG115-SC pH glass electrode:
The electrode is adjusted using pH buffers 4.01, 7.00, and
9.21before starting the analysis.
2) The titer of sodium hydroxide is determined using potassium
hydrogenphthalate as a primary standard (KHP): 80 mg are
dissolved into 50 ml deion. water and titrated.

Titrant

Sodium hydroxide, NaOH


c(NaOH) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer

Accessories

DV1010 burette
Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DG115-SC

Chemistry

CH3COOH + NaOH =
CH3COONa + H2O

Calculation

R1: Content (%), expressed as w/w

3) Approximately 1 g vinegar is added to 50 mL deionized


water into a titration beaker.
4) In this application, the sample series was analysed using a
Rondolino sample changer in combination with a diaphragm
pump. The rinsing time was defined to 2 s. In this way, the
electrode is cleaned with deionised water before starting the
subsequent sample.

Remarks
1) The method parameters have been developed and optimised
for the above mentioned sample. Since there are different kinds
of vinegar, it may be necessary to slightly adapt the method to
your specific sample.

R1 = Q*C/m,
C = M/(10*z)

Results

Waste
disposal

Neutralization before final disposal as


aqueous solution.

Author

Thomas Hitz

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M400
Vinegar
4.713 %
Vinegar
4.734 %
Vinegar
4.718 %
Vinegar
4.717 %
Vinegar
4.722 %
Vinegar
4.724 %

Method-ID
R1
Samples
Mean
s
srel

M400
Content
6
4.738 %
0.007 %
0.152 %

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

Titration curve

Method
Method
Author

M400
Acetic acid content
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title

General titration
T50 / T70 / T90
M400
Acetic acid content in

Author
Date/Time
Modified
Modified by
Protect
SOP

METTLER TOLEDO
02.08.2006 15:00:00
--No
None

vinegar

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Vinegar
Weight
0.7 g
1.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/m
C=M/(10*z)
M[Acetic acid]
z[Acetic acid]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

004 Stir
Speed
Duration
Condition
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Potential
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

35%
10 s
No

008 End of sample

NaOH
0.1 mol/L
pH
DG115-SC
pH
No
35%
Volume
1 ml
5 s
User
Dynamic
12 mV
0.002 mL
0.5 mL
Equilibrium controlled
0.5 mV
1 s
3 s
30 s
Standard
5 pH/mL
Positive
0
No
10.0 mL
No
No
Yes
1
No

M401

METTLER TOLEDO

Ammonium Chloride Content in Aqueous Solution


Determination of the weak acid ammonium chloride in aqueous solution by titration with sodium hydroxide.

Sample

Ammonium chloride solution,


5 mL 0.1 M NH4Cl solution

Substance

Ammonium chloride, NH4Cl,


M = 53.49 g/mol, z = 1

Chemicals

50 mL deionized water

Preparation and Procedures


1) The titer of sodium hydroxide is determined using potassium
hydrogenphthalate as a primary standard (KHP): 80 mg are
dissolved into 50 ml deion. water and titrated.
2) 5 mL of 0.1 M ammonium chloride solution are added in the
sample beaker. Its concentration is stored as auxiliary value
H[NH4Cl] in g/mL.
3) Dilute the sample with 50 mL deionised water and start the
titration method.

Titrant

Sodium hydroxide, NaOH


c(NaOH) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence T50/T70/T90

Accessories

DV1010 burette
Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DG111-SC

Chemistry

NH4Cl + NaOH = NH4OH + NaCl

4) The content is expressed as % w/w. Since a standard


aqueous solution of ammonium chloride was used, the result in
the calculation function indicates the recovery rate of
ammonium chloride in solution.

Remarks
1) The method parameters have been developed and optimised
for the above mentioned sample. If the composition of your
sample is different, it may be necessary to slightly adapt the
method parameters to your specific sample.
2) The method can be easily modified for automated operation.
Select the appropriate sample changer in the method function
"Titration stand".

Calculation

R1: Content (%), expressed as w/w


R1 = Q*C/m,
C = M/(10*z)

Results

Waste
disposal

Neutralization before final disposal as


aqueous solution.

Author

Maria-Jos Schmid

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M401
Ammonium chloride
101.193 %
Ammonium chloride
101.345 %
Ammonium chloride
101.466 %
Ammonium chloride
101.156 %
Ammonium chloride
101.305 %
Ammonium chloride
101.117 %

Method-ID
R1
Samples
Mean
s
srel

M401
Content
6
101.264 %
0.132
%
0.131
%

solution (1/1)
solution (1/2)
solution (1/3)
solution (1/4)
solution (1/5)
solution (1/6)

Statistics

Table of measured values

Titration curve

Method
Method
Author

M401
Ammonium chloride content
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M401
Ammonium chloride content
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Ammonium chloride solution
Fixed volume
5 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Potential
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
Potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

30%
10 s

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/(m*H[NH4Cl])
C=M/10*z
M[Ammonium chloride]
z[Ammonium chloride]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

NaOH
0.1 mol/L
pH
DG111-SC
mV
No
30%
Potential
- 120 mV
10 s
User
Dynamic
8 mV
0.02 mL
0.2 mL
Equilibrium controlled
1.0 mV
1.0 s
3.0 s
30.0 s
Standard
20 mV/mL
Negative
0
No
10.0 mL
Yes
-300 mV
No
Yes
1
No

M402

METTLER TOLEDO

Free Fatty Acids Content in Edible Oil


Determination of the free fatty acids (FFA) content in edible oil by potentiometric titration with ethanolic
potassium hydroxide in a non-aqueous mixture consisting of ethanol and diethylether (1:1 v/v).
Sample

Olive oil, 2-4 g

Substance

Free fatty acids as mg KOH/g sample,


M=56.1 g/mol, z=1

Chemicals

60 mL ethanol:diethylether 1:1 (v/v)

Titrant

Potassium hydroxide in ethanol, KOH


c(KOH) = 0.02 mol/L

Standard

Potassium hydrogen phthalate, 25 mg

Instruments

Accessories

Titration Excellence T50/T70/T90


Rondolino Sample Changer
1 additional dosing unit
DV1010 and DV1020 glass burettes
Titration beaker ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DG113-SC

Chemistry

R-COOH + KOH = R-COO- + K+ + H2O


R-COOH: Free fatty acids

Calculation

Acid number (mg KOH/g)


R1=(Q-B[FFA])*C/m,
C=M, z=1
FFA in olive oil (g FFA/100g)
R2=(Q-B[FFA])*C/m,
C=M*0.1, z=1
M[Oleic acid], z[Oleic acid]=1

Results

Waste
disposal

Dispose as organic solvent

Preparation and Procedures


Note:
This method allows a fully automated procedure using a
sample changer and an additional dosing unit. The method can
be easily modified for manual operation. Select "Manual stand"
in the method function "Titration stand".
1) The titer is determined using benzoic acid: 25 mg are added
into a glass titration beaker. They are dissolved with it with 60
mL solvent mixture. Since the sample amount is rather small, a
balance having a resolution of at least 0.1 mg is needed.
CAUTION: Benzoic acid is an aggressive substance. Avoid
contact with skin and eyes, particularly.
2) A blank value is determined for every new batch of solvent
mixture (see M403) and stored as B[Solvent FFA].
3) Approx. 2-4 g of olive oil is weighed into a titration beaker.
4) 60 mL solvent mixture are added by an additional dosing
unit (20 mL burette) in two steps to improve sample
dissolution. It can be performed manually with a pipette.
5) After each titration the DG113-SC sensor was rinsed with
solvent by means of the diaphragm pump of the Rondolino
sample changer (Settings: Pos. "1").

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) The free fatty acid content (FFA) is defined as the amount in g
of oleic acid (C18H34O2) in 100 g sample. Depending on the type
of oil, it is also indicated as the amount of lauric or palmitic acid
3) The acid number is a measure of the decomposition by
lipase enzyme in edible oil and fats. The decomposition is
speeded up by heat and light. Rancidity is due to decomposition
and it is accompanied by free fatty acid formation.
4) To ensure hydration of the DG113 glass membrane, the
elelctrode is stored over night in water. Before titration, wash the
electrode with solvent mixture.
5) Some samples can give rather flat titration curve, and noise
can appear. To increase the potential jump, 1 mL 0.05 mol/L
benzoic acid is added to 1 L of solvent mixture. This si also of
help if the blank determination is not possible due to very low
titrant consumption.
Literature:
- METTLER TOLEDO Appl. brochure 24, ME-51 725 054.

Author

Melanie Nijman

Results
All results
Method-ID
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)

M402
Edible oil
(1/1)
0.846807 mg KOH/g
0.426301 g/100g
Edible oil
(1/2)
0.845652 mg KOH/g
0.425720 g/100g
Edible oil
(1/3)
0.847853 mg KOH/g
0.426828 g/100g
Edible oil
(1/4)
0.847045 mg KOH/g
0.426421 g/100g
Edible oil
(1/5)
0.847805 mg KOH/g
0.426804 g/100g
Edible oil
(1/6)
0.842935 mg KOH/g
0.424352 g/100g

Method-ID
R1
Samples
Mean
s
srel
R2
Samples
Mean
s
srel

M402
Content
6
0.846350 mg KOH/g
0.001856 mg KOH/g
0.219
%
Oleic acid content
6
0.426071 g/100g
0.000934 g/100g
0.219
%

Statistics

Table of measured values

Titration curve

Method
Method
Author

M402
Free fatty acid content
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M402
Free fatty acid content
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Edible oil
Weight
0.0 g
5.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Dispense (normal)[1]
Titrant
Concentration
Volume
Dosing rate
Condition

Solvent FFA
1
20.0 mL
60.0 mL/min
No

005 Stir
Speed
Duration
Condition
006 Dispense (normal)[2]
Titrant
Concentration
Volume
Dosing rate
Condition

35 %
10 s
No

Solvent FFA
1
40.0 mL
60.0 mL/min
No

007 Stir
Speed
Duration
Condition
008 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. value acquisition
dE
dt
t(min)
t(max)
Evaluation and recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria

35 %
10 s
No

Termination
At Vmax
At potential
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria
009 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
010 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

10.0 mL
No
No
Yes
1
No

Content
mg KOH/g
R1=(Q-B[Solvent FFA])*C/m
C=M/z
M[Potassium hydroxide]
z[Potassium hydroxide]
6
No
No

Oleic acid content


g/100g
R2=(Q-B[Solvent FFA])*C/m
C=M/(10*z)
M[Oleic oil]
z[Oleic oil]
6
No
No

011 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
012 End of sample

KOH in EtOH
0.02 mol/L
pH
DG113-SC
mV
No
35 %
Volume
1.0 mL
0 s
User
Dynamic
12.0 mV
0.01 mL
0.3 mL
Equilibrium controlled
1.0 mV
2 s
2 s
15 s
Standard
200 mV/mL
Negative
0
No

M403

METTLER TOLEDO

Blank Value of Free Fatty Acids (FFA) Solvent


Determination of the blank value for free fatty acids (FFA) content in edible oil by potentiometric titration with
ethanolic potassium hydroxide in a non-aqueous mixture consisting of ethanol and diethylether (1:1 v/v).
Sample

60 mL ethanol:diethylether 1:1 (v/v)

Substance

Acid components , z=1

Chemicals

--

Titrant

Potassium hydroxide in ethanol, KOH


c(KOH) = 0.02 mol/L

Standard

Potassium hydrogen phthalate, 25 mg

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer
1 additional dosing unit

Accessories

DV1010 and DV1020 glass burettes


Titration beaker ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DG113-SC

Chemistry

R-COOH + KOH = R-COO- + K+ + H2O


R-COOH: Free fatty acids

Calculation

Blank value
R1=Q , mmol

Preparation and Procedures


Note:
This method allows a fully automated procedure using a
sample changer and an additional dosing unit. The method can
be easily modified for manual operation. Select "Manual stand"
in the method function "Titration stand".
1) The titer is determined using benzoic acid: 25 mg are added
into a glass titration beaker. They are dissolved with it with 60
mL solvent mixture. Since the sample amount is rather small, a
balance having a resolution of at least 0.1 mg is needed.
CAUTION: Benzoic acid is an aggressive substance. Avoid
contact with skin and eyes, particularly.
2) A blank value is determined for every new batch of solvent
mixture and stored as B[Solvent FFA].
3) 60 mL solvent mixture are added by an additional dosing
unit (20 mL burette). It can be performed manually with a
pipette.
4) After each titration the DG113-SC sensor was rinsed with
solvent by means of the diaphragm pump of the Rondolino
sample changer (Settings: Pos. "1").

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) To ensure hydration of the DG113 glass membrane, the
elelctrode is stored over nigth in water. Before titration, wash the
electrode with solvent mixture.
3) If needed, the solvent is spiked with 1 mL 0.05 mol/L added
to 1 L of solvent mixture. In this way, the potential jump is more
pronounced.
Literature:
- METTLER TOLEDO Appl. brochure 24, ME-51 725 054.

Results

Waste
disposal

Dispose as organic solvent

Author

Melanie Nijman

10

Results
All results
Method-ID
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)

M403
Solvent FFA
0.002486 mmol
Solvent FFA
0.002612 mmol
Solvent FFA
0.002697 mmol
Solvent FFA
0.002573 mmol
Solvent FFA
0.002638 mmol
Solvent FFA
0.002597 mmol
Solvent FFA
0.002543 mmol

Method-ID
R1
Samples
Mean
s
srel

M403
Consumption
7
0.002592 mmol
0.000068 mmol
2.615
%

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)
(1/7)

Statistics

Table of measured values

Titration curve

11

Method
Method
Author

M403
Blank solvent FFA
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M403
Blank solvent FFA
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

1
Solvent FFA
Fixed volume
60 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Dispense (normal)[1]
Titrant
Concentration
Volume
Dosing rate
Condition
005 Stir
Speed
Duration
Condition
006 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. value acquisition
dE
dt
t(min)
t(max)
Evaluation and recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria

Solvent FFA
1
60.0 mL
60.0 mL/min
No

No

008 Record

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

Consumption
mmol
R=Q
C=1
M[None]
z[None]
6
No

009 End of sample


010 Blank
Name
Value
Units
Limits

35 %
60 s
No

KOH in EtOH
0.02 mol/L
pH
DG113-SC
mV
No
35 %
None
0 s
User
Dynamic
8.0 mV
0.005 mL
0.03 mL
Equilibrium controlled
1.0 mV
1 s
3 s
30 s

011 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Solvent FFA
B=Mean[R1]
mmol
No

Blank Solvent FFA


mmol
R2=Mean[R1]
C=1
M[None]
z[None]
6
No
No

012 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

Standard
200 mV/mL
Negative
0
No
10.0 mL
No
No
Yes
1
No

12

M404

METTLER TOLEDO

Chloride Content in Ketchup


The chloride content in ketchup is determined by precipitation titration with silver nitrate. The content is
expressed as sodium chloride, NaCl (salt).
Sample

Ketchup, 1.4-1.6 g

Substance

Sodium chloride, NaCl,


M = 58.44 g/mol, z = 1

Chemicals

50 mL sulphuric acid, H2SO4


c(H2SO4) = 0.02 mol/L

Titrant

Silver nitrate, AgNO3


c(AgNO3) = 0.1 mol/L

Standard

NaCl, c(NaCl)=0.1 mol/L , 5 mL

Instruments

Titration Excellence T50/T70/T90

Accessories

DV1010 burette
Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DM141-SC

Chemistry

NaCl + AgNO3 = AgCl + NaNO3

Preparation and Procedures


1) The titer determination of silver nitrate is performed using
sodium chloride (NaCl) as a primary standard. Since small
amounts of salt cannot be weighed in exactly, it is
recommended to prepare an aqueous solution of NaCl, and then
to add the standard with a pipette.
2) Approximately 1.5 g ketchup are added in a titration beaker.
Ketchup is dissolved by adding 50 mL 0.02 mol/L H2SO4 .
3) After each sample the DM141-SC electrode, the stirrer and
the titraton dispensing tube are cleaned using a paper tissue
soaked with deionised water to completely remove any AgCl
residue.

Remarks
1) The method parameters have been developed and optimised
for the above mentioned sample. Since there are different
ketchup producers, it may be necessary to slightly adapt the
method to your specific sample.
2) The method can be easily modified for automated operation.
Select the appropriate sample changer in the method function
"Titration stand".

Calculation

R1: Content (%), expressed as w/w


R1 = Q*C/m,
C = M/(10*z)

Results

Waste
disposal

Filtration. The precipitate (AgCl) has to


be classified as special waste. The
liquid phase has to be neutralized to pH
7 before final disposal.

Author

Thomas Hitz

13

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M404
Ketchup
3.287
Ketchup
3.274
Ketchup
3.287
Ketchup
3.290
Ketchup
3.273
Ketchup
3.284

Method-ID
R1
Samples
Mean
s
srel

M404
Content
6
3.282
%
0.007
%
0.220
%

(1/1)
%
(1/2)
%
(1/3)
%
(1/4)
%
(1/5)
%
(1/6)
%

Statistics

Table of measured values

Titration curve

14

Method
Method
Author

M404
Chloride in ketchup
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M404
Chloride content in ketchup
METTLER TOLEDO
02.08.2006 15:00:00
--None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Ketchup
Weight
1.4 g
1.6 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration

35%
15 s

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/m
C=M/(10*z)
M[Sodium chloride]
z[Sodium chloride]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

005 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Potential
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

AgNO3
0.1 mol/L
mV
DM141-SC
mV
No
35%
Volume
1 ml
5 s
User
Dynamic
9 mV
0.008 mL
0.4 mL
Equilibrium controlled
0.5 mV
1.0 s
3.0 s
30.0 s
Standard
250 mV/mL
Positive
0
No
10.0 mL
No
No
Yes
1
No

15

M405

METTLER TOLEDO

Total Hardness of Tap Water by Photometric Titration


The total hardness of water, expressed as CaCO3 content of water is determined by complexometric titration
of calcium and magnesium at pH 10 using EDTA. The color change of the Erio T indicator (violet to blue) at
the equivalence point is sensed by a DP5 PhototrodeTM.
Sample

Tap or surface water, 50 mL

Preparation and Procedures


1) The titer determination is first performed using 0.1 mol/L zinc
sulfate (ZnSO4) standard solution: 5 mL ZnSO4 are added into a
titration beaker and diluted with 50 mL deion. water.

Substance

Magnesium and calcium as CaCO3,


M = 100.09 g/mol, z = 1

Chemicals

10 mL 5% NH3-solution
1 mL 0.1% Eriochrome Black T

Titrant

EDTA, c(EDTA) = 0.1 mol/L

Standard

ZnSO4 , c(ZnSO4)=0.1 mol/L, 5 mL

Instruments

Titration Excellence T50/T70/T90


2 additional dosing units

Accessories

2) 50 mL tap water are added into a beaker with a pipette.


3) 1 mL 0.1% Eriochrome Black T ethanolic solution is added
to the sample beaker.
4) The pH of the sample solution is adjusted by adding 10 mL
5% NH3-solution. Important: Add ammonia solution
immediately before titration and after the ErioT indicator solution.
Note: Instead of ammonia solution it is possible to use borate
buffer pH10. Preparation: Dissolve 40 g sodium hydroxide
(NaOH) in 500 mL water (Caution: solution gets hot!), add 65
g boric acid (H3BO3) and fill up to 1000 mL with deion. water.
4) This method allows a fully automated analysis procedure by
using two additional burette drives. Nevertheless, the method
can be modified for the manual addition of required reagents.
5) Before starting the subsequent sample, electrode and stirrer
are cleaned and dried with a soft tissue.

3 DV1010 glass burettes


Titration beaker ME-101974
Olivetti Printer JobJet 210

Remarks
Indication

DP5 Phototrode , 660 nm

1) After turning on the phototrode, wait for 15-10 minutes before


starting analysis to achieve a stable light intensity.

Chemistry

Ca2+ + EDTA-H22- = Ca_EDTA2- + 2H+


Mg2+ + EDTA-H22- = Mg_EDTA2- + 2H+

2) Subsequently, first check the transmission signal of the


phototrode in deionised water and set it to 1000 mV by turning
the knob on the top of it.

TM

3) Avoid the formation of air bubbles during titration since they


disturb the photometric indication. Thus, select the appropriate
stirring speed.

Calculation

R1: Content (ppm)


R1 = Q*C/m,
C = M*1000/z

4) The wavelength can be also set to 555 nm instead of 660


nm. In this case, the method parameter "Tendency" has to be
set to "Positive".
5) The method parameters have been developed and optimised
for the tap water samples used in this application. It may be
necessary to slightly adapt the method to your specific sample.

Results

Waste
disposal

Neutralization with hydrochloric acid


before final disposal.

Author

Melanie Nijman

6) The method can be easily modified for automated operation.


Select the appropriate sample changer in the method function
"Titration stand".

16

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M405
Tap water
144.574 ppm
Tap water
144.462 ppm
Tap water
144.356 ppm
Tap water
144.216 ppm
Tap water
144.368 ppm
Tap water
144.550 ppm

Method-ID
R1
Samples
Mean
s
srel

M405
Content
6
144.421 ppm
0.135
ppm
0.093
%

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

Titration curve

17

Method
Method
Author

M405
Chloride in ketchup
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M405
Total hardness of tap water
METTLER TOLEDO
02.08.2006
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Water
Fixed volume
50.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Dispense
Titrant
Concentration
Volume
Dosing rate

ErioT
0.1 mol/L
1.0 mL
60.0 mL/min

009 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
ppm
R1=Q*C/m
C=M*1000/z
M[Calcium carbonate]
z[Calcium carbonate]
3
No
No

010 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No
011 End of sample

005 Stir
Speed
Duration
006 Dispense
Titrant
Concentration
Volume
Dosing rate

35%
6 s

5% NH3
0.1 mol/L
10.0 ml
60.0 mL/min

007 Stir
Speed
Duration
008 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

35%
6 s

EDTA
0.1 mol/L
Phototrode
DP5
mV
No
35%
Volume
0.5 ml
5 s
User
Incremental
0.01 mL
Equilibrium controlled
2.0 mV
1.0 s
3.0 s
20.0 s
Standard
1000 mV/mL
Negative
0
No
10.0 mL
No
No
Yes
1
No

18

M406

METTLER TOLEDO

Calcium and Magnesium Content of Tap Water


Method for the determination of calcium and magnesium content of tap water by complexometric titration
with EDTA. The titration is monitored using a calcium selective electrode.
Sample

Substance
Chemicals

80 mL tap water

Ca2+ , M = 40.08 g/mol , z=1


Mg2+ , M = 24.31 g/mol , z=1
6 mL buffer pH 8.5 Acac/THAM:
0.1 mol/L Acetylacetone and 0.2 mol/L THAM
(Tris(hydroxymethyl)-aminomethane)

Titrant

Na2-H2EDTA,
c(EDTA)=0.1 mol/L

Preparation and Procedures


Note: This method allows a fully automated procedure with an
additional dosing unit and a sample changer. The method can
be easily modified for manual operation. Select "Manual stand"
in the method function "Titration stand".
1) The DX240 Ca-ISE and the reference electrodes are installed.
2) A titer determination is run using 5 mL 50 ppm calcium
carbonate solution as a standard.
3) Sample titration: Add 80 mL tap water into the titration beaker
4) 6 mL pH buffer 8.5 Acac/THAM are added to the sample.
This step has been performed using an additional dosing unit. It
can be performed manually using a pipette.
5) The sample is titrated with EDTA.

Standard

Calcium carbonate sol., 50 ppm

Automation:
A Rondolino sample changer with a diaphragm pump was
used. The conditioning time was set to 30 s while the rinsing
time was defined to 2 s (Rondolino settings: 7).

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer
1 additional dosing unit

Buffer pH 8.5
24.228 g THAM (0.20 mol) are added into a 1 L volumetric
flask together with 10.01 g acetylacetone (0.1 mol/L). Deion.
water is added for dissolution and to fill up to 1000 mL.

Accessories

2 DV1010 glass burettes


Titration beakers ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DX240 Ca-ISE, DX200 Ref. electrode


(DX200: Bridge electr. 3 mol/L KCl)

Chemistry

Ca2+ + H2EDTA2- = Ca-EDTA2- + 2H+


Mg(acac)2 + H2EDTA2-=
Mg-EDTA2- + 2 AcAc- + 2 H+
acac: acetylcetone

Calculation

1) Ca content, ppm
R1=Q*C/m, C=M*1000/z
M=M[Calcium], z[Calcium]=1
2) Mg content, ppm
R2=Q2*C2/m, C=M*1000/z
M=M[Magnesium], z[Magnesium]=1

Results

Waste
disposal

Dispose as aqueous solution.

Author

Madeleine Biber

Remarks
1) The method parameters have been optimised for the above
mentioned sample. It may be necessary to slightly adapt the
method to your specific sample.
2) The DX240 Ca-ISE is sensitive to both Ca and Mg ions. The
curve has two equivalence points. The titrant consumption up to
the first equivalence point yields the Ca-content. The additional
titrant volume to the second EQP yields the Mg content.
3) In alkalinic buffered solutions Ca and Mg ions can be titrated
sequentially provided that the complex formation constants have
a ratio of 103-104. With EDTA, the ratio of the constants is about
100. By adding an auxiliary complexing agent such as Acac
which weakly complexes the Mg but not the Ca ion, the ratio of
the constants can be adjusted.
The concentration of acetylacetone significantly influences the
size of the equivalence point jumps. A high concentration of
acetylacetone increases the size of the calcium jump, thereby
masking the magnesium jump. A low concentration will have
the opposite effect.
4) For titer determinations, make sure the pH of the sample after
addition of the Acac/THAM buffer is 8.5. If it is not, an endpoint
titration to pH 8.5 should be performed prior to the EQP titration.

19

Results
All results
Method-ID
Sample
R1 (Ca Content)
R2 (Mg Content)
Sample
R1 (Ca Content)
R2 (Mg Content)
Sample
R1 (Ca Content)
R2 (Mg Content)
Sample
R1 (Ca Content)
R2 (Mg Content)
Sample
R1 (Ca Content)
R2 (Mg Content)
Sample
R1 (Ca Content)
R2 (Mg Content)
Sample
R1 (Ca Content)
R2 (Mg Content)

M406
Tap water
51.443
ppm
4.359
ppm
Tap water
51.009
ppm
4.506
ppm
Tap water
51.022
ppm
4.513
ppm
Tap water
51.004
ppm
4.512
ppm
Tap water
51.243
ppm
4.384
ppm
Tap water
51.054
ppm
4.479
ppm
Tap water
51.117
ppm
4.457
ppm

Method-ID
R1
Samples
Mean
s
srel
R2
Samples
Mean
s
srel

M406
Ca Content
7
51.127
ppm
0.163
ppm
0.318
%
Mg Content
7
4.459
ppm
0.063
ppm
1.417
%

(1/1)
Ca 2+
Mg 2+
(1/2)
Ca 2+
Mg 2+
(1/3)
Ca 2+
Mg 2+
(1/4)
Ca 2+
Mg 2+
(1/5)
Ca 2+
Mg 2+
(1/6)
Ca 2+
Mg 2+
(1/7)
Ca 2+
Mg 2+

Statistics

Table of measured values

Ca 2+
Ca 2+

Mg 2+
Mg 2+

Titration curve

20

Method
Method
Author

M406
Ca and Mg content of tap water
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M406
Ca and Mg content of
tap water
METTLER TOLEDO
02.08.2006
15:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Tap Water
Fixed volume
80 mL
1 g/mL
1.0
25.0C

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
008 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Ca Content
ppm Ca2+
R1=Q*C/m
C=M*1000/z
M[Calcium]
z[Calcium]
3
No
No

Mg Content
ppm Mg2+
R2=Q2*C/m
C=M*1000/z
M[Magnesium]
z[Magnesium]
3
No
No

009 Record
003 Titration stand (Rondolino TTL)
Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

Buffer pH 8.5
1 mol/L
6 mL
60.0 mL/min

005 Stir
Speed
Duration
006 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

50 %
60 s

EDTA
0.1 mol/L
ISE
DX240-Ca2+
mV

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
010 End of sample

No
50%
None
0 s
User
Dynamic
8.0
0.005 mL
0.02 mL
Equilibrium controlled
1.0 mV
1 s
5 s
30 s
Standard
100 mV/mL
Negative
0
No
10.0 mL
No
No
Yes
2
No

21

M407

METTLER TOLEDO

Sulfate Content of Mineral Water


The sulfate content in mineral water is determined by precipitation titration with barium chloride as a titrant.
The titration is monitored potentiometrically using a DX337-Ba2+ barium selective electrode.
Sample

Substance

50 mL mineral water

Sulfate, SO42M=96.06 g/mol, z=1

Chemicals

2 mL Lithium acetate buffer


8 mL 2-propanol

Titrant

Barium chloride, BaCl2


c(BaCl2) = 0.1 mol/L

Standard

Ammonium sulfate sol., 0.1 mol/L

Instruments

Titration Excellence T50/T70/T90


2 additional dosing units
Rondo 60 Sample Changer

Accessories

2 additional burettes DV1010


Titration beakers ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DX337-Ba ISE, DX200 Ref. electrode


(DX200: Bridge electr. 3 mol/L KCl)

Chemistry

Ba2+ + SO42- = BaSO4

Calculation

Content, mg/L:
R1=Q*C/m,
C=M*1000/z
M=M[Sulfate] , z=z[Sulfate]

Results

Waste
disposal

Dispose as heavy metals containing


aqueous solution.

Author

Cosimo De Caro

Preparation and Procedures


Note: This method allows a fully automated procedure with
additional dosing units and a sample changer. The method can
be easily modified for manual operation. Select "Manual stand"
in the method function "Titration stand".
1) Install the DX337-Ba ISE and the reference electrode.
2) Perform a titer determination using 5 mL 0.1 mol/L
ammonium sulfate standard solution.
3) Sample titration: Add 50 mL tap water into the titration beaker
4) Add 8 mL 2-propanol. This step has been performed with an
additional dosing unit. It can be done manually using a pipette.
5) Add 2 mL lithium acetate buffer. This was performed with an
additional dosing unit. It can be done manually using a pipette.
6) The sample is titrated with 0.1 mol/L BaCl2 solution.
7) The electrode is conditioned in deionized water during 60 s.
Automation:
A Rondo 60 sample changer was used. The conditioning time
was set to 60 s.

Remarks
1) The method parameters have been optimised for the above
mentioned sample. It may be necessary to slightly adapt the
method to your specific sample.
2) Ba(II)-ISE:
- Fill the Ba-ISE and the electrode tip with the electrolyte.
- Screw the electrode tip onto the shaft.
- Shake the Ba-ISE 2-3 times to avoid the presence of air
bubbles into the electrode tip. Rinse it with deion. water.
- Condition it in 0.01 mol/L Ba-solution for 20-30 minutes.
3) For optimum precipitation of BaSO4 it is necessary to adjust
the pH with lithium acetate buffer.
4) Lithium acetate buffer solution:
10.2 g lithium acetate dihydrate are dissolved in 500 mL deion.
water in a beaker. Add 5.7 mL glacial acetic acid while stirring.
Transfer to a 1 L volumetric flask and fill up to the mark with
water.
Literature:
- METTLER TOLEDO Appl. brochure 33, ME-51 725 065.
- METTLER TOLEDO Appl. brochure 19, ME-51 725 013

22

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M407
Mineral
882.82
Mineral
884.34
Mineral
883.12
Mineral
884.37
Mineral
886.92
Mineral
886.52
Mineral
883.78

water
mg/L
water
mg/L
water
mg/L
water
mg/L
water
mg/L
water
mg/L
water
mg/L

Method-ID
R1
Samples
Mean
s
srel

M407
Content
7
884.55
1.59
0.180

mg/L
mg/L
%

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)
(1/7)

Statistics

Table of measured values

Titration curve

23

Method
Method
Author

M407
Sulfate content
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M407
Sulfate content
METTLER TOLEDO
02.08.2006
15:00
--None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Mineral water
Fixed volume
50 mL
1.0 g/mL
1.0
25.0C

008 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
009 Conditioning
Type
Interval
Position
Time [s]
Speed [%]

2-Propanol
1 mol/L
8 mL
60.0 mL/min

005 Dispense (Normal)


Titrant
Concentration
Volume
Dosing rate

Li-Acetate buffer
1 mol/L
2 mL
60.0 mL/min

No

Fix
1
Condition beaker
60
30

010 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

003 Titration stand (Rondo60/Tower A)


Type
Rondo60/TowerA
Titration stand
Rondo60/1A
004 Dispense (Normal)
Titrant
Concentration
Volume
Dosing rate

Content
mg/L
R1=Q*C/m
C=M*1000/z
M[Sulfate]
z[Sulfate]
2
No

011 End of sample


006 Stir
Speed
Duration
007 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

30 %
60 s

012 Park
Titration stand
Position

Rondo60/1A
Conditioning beaker

BaCl2
0.1 mol/L
ISE
DX337-Ba2+
mV
No
30%
Volume
3 mL
60 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 mV
2 s
10 s
45 s
Asymmetric
30 mV/mL
Positive
0
No
10.0 mL
No
No
Yes
1
No

24

M408

METTLER TOLEDO

Barium Content of Aqueous Solutions


The barium content of an aqueous solution is determined by precipitation titration with lithium sulfate as a
titrant. The conductivity of the titration is monitored by an InLab717 conductometric sensor.
Sample

2% barium chloride solution,


approx. 3-10 g

Preparation and Procedures

Substance

Barium, Ba2+
M=137.33 g/mol, z=1

2) Perform a titer determination using 5 mL 0.1 mol/L barium


chloride standard solution.

Chemicals

50 mL deionized water

1) Install the InLab717 conductometric sensor by connecting it


to the conductivity board (CB).

3) Sample titration:
Add 3-10 g barium standard solution into the titration beaker
and dilute it with 50 mL deionized water.
4) The sample is titrated with 0.1 mol/L Li2SO4 solution.

Titrant

Lithium sulfate, Li2SO4


c(Li2SO4) = 0.1 mol/L

Standard

Barium chloride, BaCl2 , 0.1 mol/L

Instruments

Titration Excellence T50/T70/T90


1 Conductivity Board ME-51109840

Accessories

Titration beakers ME-101974


XS205 Balance
Olivetti Printer JobJet 210

5) The sensor is cleaned with paper tissue and rinsed with


deionized water after each titration.

Remarks
Indication

InLab717

Chemistry

BaCl2 + Li2SO4 = BaSO4 + 2 LiCl

Calculation

Content, % :
R = Q*C/m
C=M/(z*10)

1) The method parameters have been optimised for the above


mentioned sample. It may be necessary to slightly adapt the
method to your specific sample.
2) For optimum result, the pH value of the sample solution must
be slightly acidic to achieve complete prescipitation of bariums
sulfate. If needed, the sample may be acidified by adding e.g. a
dilute solution of hydrochloric acid.
3) Lithium sulfate is used as a titrant since its molar conductivity
is very low. Therefore, the titration curve shows a more
pronounced segmented profile.
4) 0.1 mol/L Lithium sulfate:
6.295 g LiSO4 * H2O (M = 127.94 g/mol) are dissolved into
150 mL deionized water in a 500 mL volumetric flask. 200 mL
ethanol are added, and the titrant solution is filled up to the mark
with deionized water.

Results

Waste
disposal

Dispose as heavy metals containing


aqueous solution.

Author

Albert Aichert

25

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M408
Barium
2.026
Barium
2.022
Barium
2.019
Barium
2.028
Barium
2.031
Barium
2.017

Method-ID
R1
Samples
Mean
s
srel

M408
Content
6
2.024
0.005
0.261

chloride
%
chloride
%
chloride
%
chloride
%
chloride
%
chloride
%

solution

(1/1)

solution

(1/2)

solution

(1/3)

solution

(1/4)

solution

(1/5)

solution

(1/6)

Statistics

Table of measured values

%
%
%

Titration curve

26

Method
Method
Author

M408
Barium content conductometric
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M408
Barium content conductometric
METTLER TOLEDO
02.08.2006
15:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Barium chloride solution
Weight
4.0 g
10.0 g
1 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

30 %
5 s

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/m
C=M/(10*z)
M[Barium chloride]
z[Barium chloride]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
Last titration function
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

Li2SO4
0.1 mol/L
Conductivity
InLab717
S
No
30%
Volume
3 mL
10 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 S
1 s
3 s
30 s
Segmented
300 S/mL2
0
No
10.0 mL
No
No
Yes
1
No

27

M409

METTLER TOLEDO

Copper Content in Aqueous Solutions


The determination of copper content in aqueous solutions is perfomed by titration of generated iodine with
sodium thiosulfate after addition of potassium iodide to the sample.
Sample

Aqueous copper solution, 3 mL


(approx. conc.: 0.1 mol/L)

Substance

Copper, Cu2+
M = 63.546 g/mol, z = 1

Chemicals

10 mL 0.6 mol/L KI solution


50 mL 0.1 mol/L hydrochloric acid

Titrant

Sodium thiosulfate, Na2S2O3


c(Na2S2O3) = 0.1 mol/L

Standard

Potassium iodate, KIO3 , 20-30 mg

Instruments

Titration Excellence T50/T70/T90


2 additional dosing units
Rondolino Sample Changer

Accessories

2 DV10 and 1 DV1020 burettes


Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DM140-SC redox electrode

Chemistry

2 Cu2+ + 4 I- = 2 CuI + I2
I2 + 2 S2O32- = 2 I- + S4O62-

Calculation

Preparation and Procedures


Note: This method allows a fully automated analysis procedure
by using two additional burette drives. The method can be easily
modified for manual addition of required reagents.
1) A titer determination is first performed by using potassium
iodate (KIO3) as a primary standard: 20-30 mg KIO3 are added
to the sample and dissolved with 50 mL 0.1 mol/L hydrochloric
acid. 10 mL 0.6 mol/L potassium iodide are added before
starting titration.
2) Sample titration: 10 mL 0.6 mol/L (approx. 10%) KI solution
are added to the beaker by an additional dosing unit. This step
can be performed manually by adding 1-2 g KI directly into the
titration beaker if no dosing unit is available.
3) 50 mL 0.1 mol/L HCl are dispensed automatically by a
second additional dosing unit. This step can be performed
manually by adding HCl directly into the beaker with a pipette.
4) Iodine is immediately generated after addition of HCl.
The sample series was analysed using a Rondolino sample
changer. The rinsing time was defined to 2 s: the electrode is
cleaned with deion. water before starting next sample.

Remarks
1) The method parameters have been developed and optimised
for the samples used in this application. Thus, it may be
necessary to slightly adapt the method to your specific sample.
Literature:
1) Applications M509 and M510, see Titration Applications
Brochure 12, "30 Selected Applications", ME-51 724 765.
2) Application M526, see Titration Applications Brochure 18,
"Standaardisation of Titrants", ME-51 724 917.

R1 = Q*C/m, R1: Content (g/L)


C = M/z
R2 = R1*m, R2: Amount (mg)
R3 = Q*C3/m, R3: Concentr. (mol/L)
C3 = 1 /z

Results

Waste
disposal

Disposal as special waste


(heavy metals).

Author

Melanie Nijman

28

Results
All results
Method-ID
Sample
R1 (Content)
R2 (Content)
R3 (Concentration)
Sample
R1 (Content)
R2 (Content)
R3 (Concentration)
Sample
R1 (Content)
R2 (Content)
R3 (Concentration)
Sample
R1 (Content)
R2 (Content)
R3 (Concentration)
Sample
R1 (Content)
R2 (Content)
R3 (Concentration)
Sample
R1 (Content)
R2 (Content)
R3 (Concentration)

M409
Copper solution
6.8860 g/L
20.6580 mg
0.10836 mol/L
Copper solution
6.8828 g/L
20.6484 mg
0.10831 mol/L
Copper solution
6.8854 g/L
20.6562 mg
0.10835 mol/L
Copper solution
6.8785 g/L
20.6355 mg
0.10824 mol/L
Copper solution
6.9070 g/L
20.7210 mg
0.10869 mol/L
Copper solution
6.9244 g/L
20.7732 mg
0.10897 mol/L

Method-ID
R1
Samples
Mean
s
srel
R2
Samples
Mean
s
srel
R3
Samples
Mean
s
srel

M409
Content
6
6.8940 g/L
0.0179 g/L
0.259
%
Content
6
20.6821 mg
0.0536 mg
0.259
%
Concentration
6
0.10850 mol/L
0.00028 mol/L
0.261
%

(1/1)

(1/2)

(1/3)

(1/4)

(1/5)

(1/6)

Statistics

Table of measured values

Titration curve

29

Method
Method
Author

M409
Copper Content
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M409
Copper content
METTLER TOLEDO
02.08.2006
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Copper solution
Fixed volume
3.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Stir
Speed
Duration

25%
4 s

005 Dispense (normal) [1]


Titrant
Concentration
Volume
Dosing rate

KI
0.6 mol/L
10.0 mL
60.0 mL/min

006 Dispense (normal) [2]


Titrant
Concentration
Volume
Dosing rate

HCl
0.1 mol/L
50.0 ml
60.0 mL/min

Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria
009 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
010 Calculation R2
Result
Result unit
Formula
Constant
M
z
Result limits
Add. statistics
functionalities
011 Calculation R3
Result
Result unit
Formula
Constant
M
z
Result limits
Add. statistics
functionalities

7.5 mL
No
No
Yes
1
No

Content
g/L
R1=Q*C/m
C=M/z
M[Copper]
z[Copper]
4
No
No

Content
mg
R2=R1*m
C=1
M[Copper]
z[Copper]
No
No

Content
mol/L
R3=Q*C/m
C=1/z
M[Copper]
z[Copper]
No
No

012 Record

007 Stir
Speed
Duration
008 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria

25%
25 s

Na2S2O3
0.1 mol/L
mV
DM140-SC
mV
No
25%
None
5 s

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
013 End of sample

User
Dynamic
8.0 mV
0.02 mL
0.2 mL
Equilibrium controlled
1.0 mV
2 s
3 s
10 s
Standard
200 mV/mL
Negative
0
No

30

M410

METTLER TOLEDO

Hydrogen Peroxide Content in Aqueous Solutions


The hydrogen peroxide content in aqueous solutions is perfomed by redox titration with potassium
permanganate.
Sample

Substance

1.5 % hydrogen peroxide aqueous


solution, 0.5 mL

Hydrogen peroxide, H2O2


M = 34.01 g/mol, z = 2

Chemicals

60 mL deionized water
1.25 mL 20% sulfuric acid, H2SO4

Titrant

Potassium permanganate, KMnO4


c(1/5 KMnO4) = 0.1 mol/L

Standard

Sodium oxalate, Na2C2O4, 25-40 mg

Instruments

Titration Excellence T50/T70/T90


1 additional dosing unit

Accessories

2 DV1010 burettes
Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DM140-SC redox electrode

Chemistry

2 MnO4- + 5 H2O2 + 6 H+ =
2 Mn2+ + 5 O2 + 8 H2O

Preparation and Procedures


Note:
This method allows a fully automated analysis procedure by
using one additional burette drive for dispensing.The method can
be easily modified for manual operation.
1) A titer determination is first performed by using sodium
oxalate (Na2C2O4) as a primary standard: 25-40 mg Na2C2O4
are added to the sample and dissolved with 60 mL deionized
water. The sample solution is acidified with 1.25 mL 20%
sulfuric acid.
2) Sample titration: 60 mL deionised water are added into the
the titration beaker.
3) Add 0.5 mL hydrogen peroxide solution. This step has been
performed using an additional dosing unit. It can be performed
manually using a pipette.
4) Add 1.25 mL 20% sulfuric acid (H2SO4) to the titration
beaker. This step has been performed using an additional
dosing unit. If this is not possible, this step can be performed
manually using a pipette.

Remarks
1) The method parameters have been developed and optimised
for the sample used in this application. Thus, it may be
necessary to slightly adapt the method to your specific sample.

Literature:

Calculation

R1: Content (%)


R1 = Q*C/m,
C = M/(10*z) ; z = 2

1) Application M527, see Titration Applications Brochure 12,


"30 Selected Applications", ME-51 724 765
.
2) Application M158,
"Determination of Ammonia and Hydrogen Peroxide",
www.mt.com .

Results

Waste
disposal

Disposal as heavy metal containing


aqueous solution.

Author

Claudia Schreiner

31

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M410
Hydrogen peroxide
1.515
%
Hydrogen peroxide
1.516
%
Hydrogen peroxide
1.515
%
Hydrogen peroxide
1.516
%
Hydrogen peroxide
1.525
%
Hydrogen peroxide
1.517
%
Hydrogen peroxide
1.518
%

Method-ID
R1
Samples
Mean
s
srel

M410
Content
7
1.517
%
0.004
%
0.231
%

solution (1/1)
solution (1/2)
solution (1/3)
solution (1/4)
solution (1/5)
solution (1/6)
solution (1/7)

Statistics

Table of measured values

Titration curve

32

Method
Method
Author

M410
Hydrogen peroxide content
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M410
Hydrogen peroxide content
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Hydrogen peroxide solution
Fixed volume
0.5 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

20% H2SO4
1
1.25 ml
60.0 mL/min

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R=Q*C/m
C=M/(10*z)
M[H2O2]
z[H2O2]
3
No
No

008 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
009 End of sample

005 Stir
Speed
Duration
006 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

35%
20 s

1/5 KMnO4
0.1 mol/L
mV
DM140-SC
mV
No
35%
Volume
2 mL
30 s
User
Dynamic
8.0 mV
0.02 mL
0.2 mL
Equilibrium controlled
1.0 mV
1 s
3 s
10 s
Standard
200 mV/mL
Positive
0
No
10 mL
No
No
Yes
1
No

33

M411

METTLER TOLEDO

Vitamin C Content in Orange Juice: Voltametric Indication


Content determination of vitamin C (ascorbic acid) in orange juice by voltametric titration with DPI. The
titration is monitored by a polarized DM143 electrode.
Sample

5 g orange juice

Substance

L(+) ascorbic acid, C6H8O6


M=176.13 g/mol, z=2

Chemicals

50 mL deionized water
2% oxalic acid for adjustment to pH 3

Titrant

2,6-dichlorophenolindophenol, DPI
c(1/2 DPI) = 0.01 mol/L

Standard

Ascorbic acid, 0.01 mol/L

Instruments

Titration Excellence T50/T70/T90

Accessories

One additional DV1010 glass burette


Titration beaker ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DM143-SC

Chemistry

L(+)-ascorbic acid is oxidized by DPI:


C6H6O6-H2 + DPI = C6H6O6 + H2-DPI
Oxidation:
C6H8O6 = C6H6O6 + 2H+ + 2e-

Calculation

R1=Q*C/m; Content (mg/100g)


C=100*M/z
R2=Q*C/m; Content (%)
C=M/(10*z)

Results

Waste
disposal

Neutralize before final disposal as


aqueous solution.

Author

Thomas Hitz

Preparation and Procedures


Note:
- The DPI titrant has to be prepared fresh daily. It has to be
stored in brown glass bottles to protect it from light.
- Ascorbic acid is sensitive to light, temperature and oxygen.
Titration beakers with light protection as well as use of purge
gas are recommended. Keep in the dark.
- Ascorbic acid solution has to be prepared fresh prior to use.
1) Titrant preparation:
0.36 g DPI sodium salt monohydrate (M = 290.08 g/mol) is
weighed in a 250 mL volumetric flask and filled up with deion.
water to obtain a titrant concentration c(1/2 DPI) = 0.01 mol/L.
The flask was placed in an unltrasonic bath during 10 min. to
improve solubility.
2) The titer is determined using L(+) ascorbic acid:
5 mL 0.01 mol/L standard solution are added into a titration
beaker and diluted with 50 mL deionized water. The pH value is
adjusted to pH 3 with 2% oxalic acid by titrating the sample
using an EP titration function.
3) The juice is well homogenized and is weighed directly into
the titration beaker, without special treatment such as filtration.
After addition of 50mL deionised water the sample can be
purged with nitrogen gas to avoit oxidation of Vitamin C.

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) The sample size depends on the amount of vitamin C: 1-15
mg vitamin C correspond 0.5 - 8.5 mL 0.01 mol/L 1/2 DPI.
3) If DPI sodium salt dihydrate (M=308.08 g/mol) is used, an
excess has to be weighed in due to its bad solubility. The titrant
has to be filtrated prior to use.
4) Both DPI titrant and ascorbic acid standard solution are not
stable. To get accurate results, It is recommended to prepare
them fresh before use.
5) Orange juice was stored in the refrigerator when not used.
6) This method describes the voltametric determination of L(+)
ascorbic acid with a polarized sensor DM143-SC. An alternating
current of 10-12 A is applied to the double pin platinum
electrode and the potential is measured.
Literature:
- METTLER TOLEDO Appl. brochure 19, ME-51 725 013.

34

Results
All results
Method-ID
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)

M411
Orange
34.713
0.0347
Orange
34.227
0.0342
Orange
34.887
0.0349
Orange
35.367
0.0354
Orange
34.896
0.0349

Method-ID
R1
Samples
Mean
s
srel
R2
Samples
Mean
s
srel

M411
Content
5
34.816
0.334
0.960
Content
5
0.0348
0.0004
0.960

juice (1/1)
mg/100 g
%
juice (1/2)
mg KOH/g
%
juice (1/3)
mg/100 g
%
juice (1/4)
mg/100 g
%
juice (1/5)
mg/100 g
%

Statistics

Table of measured values

mg/100 g
mg/100 g
%
%
%
%

Titration curve

35

Method
Method
Author

M411
Vitamin C content voltametric
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M411
Vitamin C content
voltametric
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Orange juice
Weight
0.0 g
10.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual Stand 1

007 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R2=Q*C/m
C=M/(10*z)
M[Ascorbic acid]
z[Ascorbic acid]
4
No
Yes

008 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. value acquisition
dE
dt
t(min)
t(max)
Evaluation and recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

35 %
10 s

009 End of sample

1/2 DPI
0.01 mol/L
Polarized
DM143-SC
mV
Voltametric
12 A
No
35 %
Volume
1.0 mL
2 s
User
Incremental
0.05 mL
Equilibrium controlled
2.0 mV
1 s
2 s
30 s
Standard
500 mV/mL
Negative
0
No
10.0 mL
No
No
Yes
1
No

Content
mg/100g
R1=Q*C/m
C=100*M/z
M[Ascorbic acid]
z[Ascorbic acid]
3
No
No

36

M412

METTLER TOLEDO

Vitamin C Content in Orange Juice: Amperometric Indication


Content determination of vitamin C (ascorbic acid) in orange juice by amperometric titration with DPI. The
titration is monitored by a polarized DM143 electrode.
Sample

5 g orange juice

Substance

L(+) ascorbic acid, C6H8O6


M=176.13 g/mol, z=2

Chemicals

50 mL deionized water
2% oxalic acid for adjustment to pH 3

Titrant

2,6-dichlorophenolindophenol, DPI
c(1/2 DPI) = 0.01 mol/L

Standard

Ascorbic acid, 0.01 mol/L

Instruments

Titration Excellence T50/T70/T90

Accessories

One additional DV1010 glass burette


Titration beaker ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DM143-SC

Chemistry

L(+)-ascorbic acid is oxidized by DPI:


C6H6O6-H2 + DPI = C6H6O6 + H2-DPI
Oxidation:
C6H8O6 = C6H6O6 + 2H+ + 2e-

Calculation

R1=Q*C/m; Content (mg/100g)


C=100*M/z
R2=Q*C/m; Content (%)
C=M/(10*z)

Results

Waste
disposal

Neutralize before final disposal as


aqueous solution.

Author

Claudia Schreiner

Preparation and Procedures


Note:
- The DPI titrant has to be prepared fresh daily. It has to be
stored in brown glass bottles to protect it from light.
- Ascorbic acid is sensitive to light, temperature and oxygen.
Titration beakers with light protection as well as use of purge
gas are recommended. Keep in the dark.
- Ascorbic acid solution has to be prepared fresh prior to use.
1) Titrant preparation:
0.36 g DPI sodium salt monohydrate (M = 290.08 g/mol) is
weighed in a 250 mL volumetric flask and filled up with deion.
water to obtain a titrant concentration c(1/2 DPI) = 0.01 mol/L.
The flask was placed in an unltrasonic bath during 10 min. to
improve solubility.
2) The titer is determined using L(+) ascorbic acid:
5 mL 0.01 mol/L standard solution are added into a titration
beaker and diluted with 50 mL deionized water. The pH value is
adjusted to pH 3 with 2% oxalic acid by titrating the sample
using an EP titration function.
3) The juice is well homogenized and is weighed directly into
the titration beaker, without special treatment such as filtration.
After addition of 50mL deionised water the sample can be
purged with nitrogen gas to avoit oxidation of Vitamin C.

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) The sample size depends on the amount of vitamin C: 1-15
mg vitamin C correspond 0.5 - 8.5 mL 0.01 mol/L 1/2 DPI.
3) If DPI sodium salt dihydrate (M=308.08 g/mol) is used, an
excess has to be weighed in due to its bad solubility. The titrant
has to be filtrated prior to use.
4) Both DPI titrant and ascorbic acid standard solution are not
stable. To get accurate results, It is recommended to prepare
them fresh before use.
5) Orange juice was stored in the refrigerator when not used.
6) This method describes the amperometric determination of
L(+) ascorbic acid with a polarized sensor DM143-SC. A
polarization current of 200 mV is applied to the double pin
platinum electrode and the current is monitored during titration.
Literature:
- METTLER TOLEDO Appl. brochure 19, ME-51 725 013.

37

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M412
Orange juice
24.0989
Orange juice
23.9783
Orange juice
24.5614
Orange juice
23.5523
Orange juice
23.5976
Orange juice
24.3256

(1/1)
mg/100
(1/2)
mg/100
(1/3)
mg/100
(1/4)
mg/100
(1/5)
mg/100
(1/6)
mg/100

Method-ID
R1
Samples
Mean
s
srel

M412
Content
6
24.0190
0.3979
1.657

mg/100 g
mg/100 g
%

g
g
g
g
g
g

Statistics

Table of measured values

Titration curve

38

Method
Method
Author

M412
Vitamin C content amperometric
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
amperometric
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M412
Vitamin C content
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Orange juice
Weight
0.0 g
10.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual Stand 1

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
mg/100g
R=Q*C/m
C=100*M/z
M[Ascorbic acid]
z[Ascorbic acid]
4
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
Last titration function
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor Parameters
Type
Sensor
Unit
Indication
Upol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dV
Meas. value acquisition
dE
dt
t(min)
t(max)
Evaluation and recognition
Procedure
Threshold
Ranges
Lower limit
Upper limit
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria

35 %
10 s

009 End of sample

1/2 DPI
0.01 mol/L
Polarized
DM143-SC
A
Amperometric
200 mV
No
30 %
None
0 s
User
Incremental
0.1 mL
Equilibrium controlled
0.3 A
2 s
5 s
30 s
Segmented
1 A/mL2
1
0.6 A
10.0 A
No
10.0 mL
No
No
Yes
1
No

39

M413

METTLER TOLEDO

Anionic Surfactant Content in Liquid Detergents by Turbidimetric Titration


The anionic surfactant content in liquid dish washer as SDS content (sodium dodecyl sulfate, or sodium
lauryl sulfate) is determined by precipitation titration with Hyamine 1622, a cationic surfactant. The turbidity
increase during titration is monitored by the DP5 PhototrodeTMat 550 nm.
Sample

5 mL liquid detergent solution,


approx. 8 g/L

Substance

Sodium dodecyl sulfate, C12H25NaO4S


M = 288.38 g/mol, z = 1

Chemicals

60 mL deionised water

Titrant

Hyamine 1622, C27H42ClNO2


c(Hyamine) = 0.004 mol/L

Standard

SDS, 1 mL 0.01 mol/L, see M549

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer

Accessories

1 DV1010 burette
Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DP5 Phototrode

Chemistry

Simplified scheme:
C27H42NO2+ + C12H25O4S - =
C27H42NO2-C12H25O4S

Calculation

TM

, 550 nm

R1: SDS-Content (%)


R1 = Q*C/m,
C = M/(10*z) ; z = 1

Preparation and Procedures


1) The titer determination is performed by titrating 1 mL 0.01
mol/L SDS, which are diluted with 60 mL deionized water.
2) Sample titration:
5 mL of an aqueous solution of liquid detergent are added into
the titration beaker and diluted with 60 mL deionised water.
3) The concentration of the liquid detergent solution was chosen
to get an approx. titrant consumption of 5 mL. Its value is stored
as auxiliary value H[SDS] in g/mL.
4) Preparation of the liquid detergent solution: Approx. 8 g
liquid detergent are given into 1 L volumetric flask. The flask is
filled up with deionised water (here: 8.5856 g liq. detergent,
which gives a content of 0.0429 g/5 mL)
5) The sample series was analysed using a Rondolino sample
changer. The conditioning time was set to 30 s (Rondolino
settings: 4) to clean the electrode with deionized water before
starting the subsequent sample.

Remarks
1) After turning on the phototrode, wait for 15-10 minutes before
starting analysis to achieve a stable light intensity. Check the
transmission signal of the phototrode in deionised water and set
it to 1000 mV by turning the knob on the top of it.
2) Avoid the formation of air bubbles during titration since they
disturb the photometric indication. Thus, select the appropriate
stirring speed.
3) The method parameters have been developed and optimised
for the sample used in this application. Thus, it may be
necessary to slightly adapt the method to your specific sample.
4) This method allows a fully automated analysis procedure
with a Rondolino sample changer. The method can be easily
modified for manual operation. Select "Manual stand" in the
method function "Titration stand".
Literature:

Results

Waste
disposal

Disposal as aqueous solution; a special


treatment is not necessary

Author

Cosimo De Caro

1) Application M549, see Titration Applications Brochure 18,


"Standardisation of Titrants", ME-51 724 917.
2) Titration Applications Brochure 22,
"Surfactant Titration", ME-51 725 015 .

40

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M413
Liquid
13.91
Liquid
13.89
Liquid
13.83
Liquid
13.91
Liquid
13.90
Liquid
13.83

Method-ID
R1
Samples
Mean
s
srel

M413
Content
6
13.88
%
0.04
%
0.275
%

detergent
%
detergent
%
detergent
%
detergent
%
detergent
%
detergent
%

solution

(1/1)

solution

(1/2)

solution

(1/3)

solution

(1/4)

solution

(1/5)

solution

(1/6)

Statistics

Table of measured values

Titration curve

41

Method
Method
Author

M413
SDS content photometric
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M413
SDS content photometric
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Liquid detergent solution
Fixed volume
5.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

35 %
30 s

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/(m*H[SDS])
C=M/(10*z)
M[Sodium dodecylsulfate]
z[Sodium dodecylsulfate]
2
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

Hyamine 1622
0.004 mol/L
Phototrode
DP5
mV
No
35%
Volume
4.5 mL
15 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 mV
1 s
3 s
10 s
Standard
200 mV/mL
Negative
0
No
10 mL
No
No
Yes
1
No

42

M414

METTLER TOLEDO

Anionic Surfactant Content in Liquid Detergents by Potentiometric Titration


The anionic surfactant content in liquid dish washer as SDS content (sodium dodecyl sulfate, sodium lauryl
sulfate) is determined by precipitation titration with Hyamine 1622, a cationic surfactant. The potential
change during titration is monitored by the DS500 surfactant sensitive electrode.
Sample

5 mL liquid detergent solution,


approx. 8 g/L

Substance

Sodium dodecyl sulfate, C12H25NaO4S


M = 288.38 g/mol, z = 1

Chemicals

60 mL deionised water

Titrant

Hyamine 1622, C27H42ClNO2


c(Hyamine) = 0.004 mol/L

Standard

SDS, 1 mL 0.01 M aliquot, see M610

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer

Accessories

1 DV1010 burette
Titration beaker ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

DS500 Surfactant Sensitive Electrode


DX200 Ref. electrode (1 M KNO3)

Chemistry

Simplified scheme:
C27H42NO2+ + C12H25O4S - =
C27H42NO2-C12H25O4S

Calculation

R1: SDS-Content (%)


R1 = Q*C/m,
C = M/(10*z) ; z = 1

Preparation and Procedures


1) The titer determination is performed by titrating 1 mL 0.01
mol/L SDS, which are diluted with 60 mL deionized water.
2) Sample titration:
5 mL of an aqueous solution of liquid detergent are added into
the titration beaker and diluted with 60 mL deionised water.
3) The concentration of the liquid detergent solution was chosen
to get an approx. titrant consumption of 5 mL. Its value is stored
as auxiliary value H[SDS] in g/mL.
4) Preparation of the liquid detergent solution: Approx. 8 g
liquid detergent are given into 1 L volumetric flask. The flask is
filled up with deionised water (here: 8.0482 g liq. detergent,
which gives a content of 0.0402 g/5 mL)
5) The sample series was analysed using a Rondolino sample
changer. The conditioning time was set to 30 s (Rondolino
settings: 4) to clean the electrode with deionized water before
starting the subsequent sample.
6) Before starting the sample series it is recommended to
condition the DS500 electrode by running a trial titration with
SDS or the liquid detergent.

Remarks
1) The method parameters have been developed and optimised
for the sample used in this application. Thus, it may be
necessary to slightly adapt the method to your specific sample.
2) DS500 surfactant sensitive electrode:
- Fill the DS500-ISE and the electrode tip with the electrolyte.
- Screw the electrode tip onto the shaft.
- Shake the DS500 2-3 times to avoid the presence of air
bubbles into the electrode tip. Rinse it with deion. water.
- Condition it in 0.01 mol/L SDS solution for 20-30 minutes.
3) This method allows a fully automated analysis procedure
with a Rondolino sample changer. The method can be easily
modified for manual operation. Select "Manual stand" in the
method function "Titration stand".
4) The conditioning time was set to 30 s (Rondolino settings: 4)
to clean the electrode with deionized water before starting the
subsequent sample.

Results

Waste
disposal

Disposal as aqueous solution; a special


treatment is not necessary

Author

Cosimo De Caro

Literature:
1) Application M610, Titration Applications Brochure 22,
"Surfactant Titration", ME-51 725 015 .

43

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M414
Liquid
14.10
Liquid
14.14
Liquid
14.16
Liquid
14.23
Liquid
14.20
Liquid
14.19

Method-ID
R1
Samples
Mean
s
srel

M414
Content
6
14.17
%
0.05
%
0.328
%

detergent
%
detergent
%
detergent
%
detergent
%
detergent
%
detergent
%

solution

(1/1)

solution

(1/2)

solution

(1/3)

solution

(1/4)

solution

(1/5)

solution

(1/6)

Statistics

Table of measured values

Titration curve

44

Method
Method
Author

M414
SDS content potentiometric
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M414
SDS content potentiometric
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Liquid detergents olution
Fixed volume
5.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

35 %
60 s

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/(m*H[SDS])
C=M/(10*z)
M[Sodium dodecylsulfate]
z[Sodium dodecylsulfate]
2
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

Hyamine 1622
0.004 mol/L
mV
DS500
mV
No
35%
Volume
2 mL
15 s
User
Dynamic
8.0 mV
0.02 mL
0.2 mL
Equilibrium controlled
1.0 mV
2 s
5 s
30 s
Standard
50 mV/mL
Positive
0
No
10 mL
No
No
Yes
1
No

45

M415

METTLER TOLEDO

m-Value of Tap Water


The m value of water is determined by an endpoint titration to pH 4.30 with hydrochloric acid.

Sample

Substance
Chemicals

50 mL tap water

--

--

Preparation and Procedures


Note: This method allows a fully automated analysis procedure
by using a Rondolinos sample changer. The method can be
easily modified for manual operation. Select "Manual stand" in
the method function "Titration stand".
1) Before the analysis an electrode calibration was performed
using METTLER TOLEDO buffers of pH 4.01, 7.00 and 9.21.
2) Fill a (preferably) PE bottle to the brim with the water to be
analyzed. Keep it closed and at sampling temperature.
3) Pipette 50 mL into the beaker shortly before titration.

Titrant

Hydrochloric acid, HCl


c(HCl) = 0.1 mol/L

Standard

Tris(hydroxymethyl)-aminomethane, 50-100 mg

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer

Accessories

1 DV1010 burette
Titration beakers ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DG115-SC

Chemistry

HCl + NaOH = NaCl + H2O


HCl + CO32- = HCO3- + ClHCl + HCO3- = CO2 + H2O + Cl-

Calculation

Total alkalinity or methyl orange


alkalinity (m-value) is expressed as
mmol/L or mg/L CaCO3

Results

Waste
disposal

Neutralize the slightly acid waste before


disposal.

Author

Madeleine Biber

4) For best results, if the initial pH lies close to the end potential,
use a lower concentration of the corresponding titrant.
5) The samples were analysed using a Rondolino sample
changer. The electrode was rinsed during 2 s and conditioned
during 10 s (Rondolino settings: 6). In this way, the electrode is
cleaned with deionised water before starting the subsequent
sample.

Remarks
1) The method parameters have been optimised for the sample
used in this application. It may be necessary to slightly adapt
the method to your specific sample.
2) The acid capacity allows surface waters to resist sudden pH
changes due to e.g. organic acid waste, groundwater discharge
or industrial waste, or due to sources such as bacteria, Fe 3+,
hydrated Al3+, H2S, fatty acids, proteins, CO2.
3) The acid capacity depends on the equilibrium of free CO 2,
bicarbonate HCO3-, and carbonate CO32- in the corresponding
water and therefore on its temperature.
Mineral weathering buffers groundwaters, e.g. limestone rock
CaCO3 (s) + CO2 (g) = Ca2+ (aq) + 2 HCO3- (aq)
The bicarbonate ion then acts as a base to neutralize acids:
HCO3- (aq) + H+ (aq) = CO2 (g) + H2O (l)
4) The m-value (total alkalinity) represents the acid neutralizing
capacity and is determined in e.g. drinking water. Acidity can
affect corrosion, soil leaching, and aquatic life in general. The
name originates from the methyl orange color indicator (red to
yellow-orange at pH 4.3) formerly used.
References:
http://nas.cl.uh.edu/zhang/3431_04S/05_Acid-Base.ppt

46

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M415
Tap water
(1/1)
3.005
mmol/L
Tap water
(1/2)
2.991
mmol/L
Tap water
(1/3)
2.992
mmol/L
Tap water
(1/4)
2.993
mmol/L
Tap water
(1/5)
2.996
mmol/L
Tap water
(1/6)
2.992
mmol/L

Method-ID
R1
Samples
Mean
s
srel

M415
Content
6
2.995
mmol/L
0.005
mmol/L
0.176
%

Statistics

Table of measured values

Titration curve

47

Method
Method
Author

M415
m-value of tap water
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M415
m-Value of tap water
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Tap water
Fixed volume
100 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
End point type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Tuermination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

50 %
10 s

HCl
0.1 mol/L
pH
DG115
pH
No
50 %
None
0 s
User
Absolute
Negative
4.30 pH
3.0 pH
10 mL/min
10 L/min
Yes
10 s
10.0 mL
Infinity

Content
mmol/L
R1=Q*C/m
C=1000
M[None]
z[None]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

48

M416

METTLER TOLEDO

p-Value of Tap Water


The p-value of water is determined by an endpoint titration to pH 8.20 with sodium hydroxide.

Sample

Substance
Chemicals

100 mL tap water

--

--

Preparation and Procedures


Note: This method allows a fully automated analysis procedure
by using a Rondolino sample changer. The method can be
easily modified for manual operation. Select "Manual stand" in
the method function "Titration stand".
1) Before the analysis an electrode calibration was performed
using METTLER TOLEDO buffers of pH 4.01, 7.00 and 9.21.
2) Fill a (preferably) PE bottle to the brim with the water to be
analyzed. Keep it closed and at sampling temperature.
3) Pipette 50 mL into the beaker shortly before titration.

Titrant

Sodium hydroxide, NaOH


c(HCl) = 0.01 mol/L

Standard

Potassium hydrogen phthalate, 70-120 mg

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer

Accessories

1 DV1010 burette
Titration beakers ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DG115-SC

Chemistry

HCl + NaOH = NaCl + H2O

Calculation

Total acidity or phenolphtalein acidity


(p-value) is expressed as mmol/L or
mg/L CaCO3

4) For best results, if the initial pH lies close to the end potential,
use a lower concentration of the corresponding titrant.
5) The samples were analysed using a Rondolino sample
changer. The electrode was rinsed during 2 s and conditioned
during 10 s (Rondolino settings: 6). In this way, the electrode is
cleaned with deionised water before starting the subsequent
sample.

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) The p-value (total acidity) represents the base neutralizing
capacity of a water and is determined in many different samples,
e.g. drinking water, wastewater, caustic wash solutions.
3) The pH value and the base capacity depend on the
equilibrium of free CO2, bicarbonate HCO3-, and carbonate CO32in the corresponding water and therefore on its temperature.
4) The name p-value originates from the phenolphthalein color
indicator (colorless to pink at pH 8.2 and above) formerly used.
References:
http://nas.cl.uh.edu/zhang/3431_04S/05_Acid-Base.ppt

Results

Waste
disposal

Neutralize the slightly alkaline waste


before disposal.

Author

Madeleine Biber

49

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M416
Tap water
(1/1)
0.229
mmol/L
Tap water
(1/2)
0.220
mmol/L
Tap water
(1/3)
0.234
mmol/L
Tap water
(1/4)
0.217
mmol/L
Tap water
(1/5)
0.237
mmol/L
Tap water
(1/6)
0.214
mmol/L

Method-ID
R1
Samples
Mean
s
srel

M416
Content
6
0.225
mmol/L
0.019
mmol/L
4.190
%

Statistics

Table of measured values

Titration curve

50

Method
Method
Author

M416
p-Value of tap water (EP) 02.08.2006
METTLER TOLEDO

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M416
p-Value of tap water (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Tap water
Fixed volume
100 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
End point type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

50 %
15 s

NaOH
0.01 mol/L
pH
DG115
pH
No
50 %
None
0 s
User
Absolute
Positive
8.20 pH
3.0 pH
10 mL/min
10 L/min
Yes
0 s
10.0 mL
Infinity

Content
mmol/L
R1=Q*C/m
C=1000
M[None]
z[None]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
008 End of sample

51

M417

METTLER TOLEDO

pH-Stat Titration of Antacid at pH 3


The neutralizing capacity in antacid tablet is tested by constantly maintaining the pH value at pH 3.0 using a
pH-Stat titration with HCl as a titrant.
Sample

0.03-0.08 g antacid tablet

Preparation and Procedures


1) The titer is determined by dissolving 50 mg
Tris-(hydroxymethyl)-aminomethane (THAM) as a primary
standard in 50 mL deionized water.

Substance

Acid neutralizing substances


(e.g. CaCO3)

Chemicals

50 mL deionized water

2) Before analysis an electrode calibration is performed using


METTLER TOLEDO buffers of pH 4.01, 7.00 and 9.21.
If there is no automatic temperature compensation, enter the
correct temperature manually.
3) An antacid tablet is crushed and 30-80 mg are added into a
titration beaker. 50 mL deionized water are added to dissolve it.

Titrant

Hydrochloric acid, HCl


c(HCl) = 0.1 mol/L

Standard

THAM, 50-80 mg

Instruments

Titration Excellence T50/T70/T90


Rondolino Sample Changer

Accessories

1 DV1010 Burette
Titration beakers ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DG111-SC

Chemistry

HCl + NaOH = NaCl + H2O


NaOH represents the acid neutralizing
components:

Calculation

4) The electrode is rinsed with deionised water before starting


the subsequent sample.
5) For best results, if the initial pH lies close to the end potential,
use a lower concentration of the corresponding titrant.

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
References:
- METTLER TOLEDO Titration Applications Brochure Nr. 2,
"Various methods", ME-724 557
- METTLER TOLEDO Application M054,
"pH-Stat of Antacids at pH 3"

See method

Results

Waste
disposal

Neutralize the acid waste before


disposal.

Author

Madeleine Biber

52

Results
All results
Method-ID
Sample
R1 (Content)
R2 (Consumption)
R3 (corr. coeff. (0,2))
R4 (% turnover after 2 min.)
R5 (time to 50% titr. conversion)
Sample
R1 (Content)
R2 (Consumption)
R3 (corr. coeff. (0,2))
R4 (% turnover after 2 min.)
R5 (time to 50% titr. conversion)
Sample
R1 (Content)
R2 (Consumption)
R3 (corr. coeff. (0,2))
R4 (% turnover after 2 min.)
R5 (time to 50% titr. conversion)
Sample
R1 (Content)
R2 (Consumption)
R3 (corr. coeff. (0,2))
R4 (% turnover after 2 min.)
R5 (time to 50% titr. conversion)
Sample
R1 (Content)
R2 (Consumption)
R3 (Corr. coeff. (0,2))
R4 (% turnover after 2 min.)
R5 (time to 50% titr. conversion)

M417
Antacid solution (1/1)
1024.911
mg/g
0.213
mL/min
0.980
42.691
%
2.612
min
Antacid solution (1/2)
1016.914
mg/g
0.118
mL/min
0.973
39.445
%
3.668
min
Antacid solution (1/3)
1019.263
mg/g
0.191
mL/min
0.989
40.284
%
2.728
min
Antacid solution (1/4)
1024.219
mg/g
0.133
mL/min
0.981
38.128
%
3.333
min
Antacid solution (1/5)
107.495
mg/g
0.261
mL/min
0.977
42.182
%
2.753
min

Statistics
Method-ID
R1
Samples
Mean
s
srel

Table of measured values

M417
Content
5
1020.560
3.765
0.37

mg/g
mg/g
%

Titration curve

53

Method
Method
Author

M417
Antacid (Stating)
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M417
Antacid (Stating)
METTLER TOLEDO
02.08.2006 15:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Antacid solution
Weight
0.03 g
0.08 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration
005 Stating [1]
Titrant
Titrant
Concentration
Sensor Parameters
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Pretitration
Pretitration
Control band
Predispense
Mode
Wait time
Control
Set potential
Control band
Tendency
Dosing rate (max)
Dosing rate (min)
Monitoring
Monitoring
Termination
At Vmax
From t(min)
At t(max)
t(max)
After stating duration
At minimum rate
dV
dt
Measured value storage
Interval
Start condition
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Additional statistics
functionalities

30 %
15 s

HCl
0.1 mol/L

007 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Additional statistics
functionalities
008 Calculation R3
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Additional statistics
functionalities
009 Calculation R4
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Additional statistics
functionalities
010 Calculation R5
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Additional statistics
functionalities

pH
DG111-SC
pH
No
35 %
Yes
2.0 pH
None
0 s
3.0 pH
0.01 pH
Negative
10 mL/min
10 L/min
No
8.5 mL
No
Yes
20 min
No
Yes
0.01 mL
1 min

Mean consumption
mL/min
R2=CVt(0,tCON(100))
C=1
M[None]
z[None]
3
No
No

Correlation coefficient
-R3=CORRt(0,2)
C=1
M[None]
z[None]
3
No
No

Turnover after 2 minutes


%
R4=CONt(2)
C=1
M[None]
z[None]
3
No
No

Time to 50% titrant


conversion
min
R5=tCON(50)
C=1
M[None]
z[None]
3
No
No

011 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration
Sample data
Per series
Resource data
No
E - V
Last titration
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
No
E - t
Last titration
V - t
Last titration
dV/dt - t
Last titration
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No

function

function

function
function
function

012 End of sample


5 s
After pretitration

Content
mg/g
R1=QStt(tCON(100))*C/m
C=M/z
M[Calcium carbonate]
z[Calcium carbonate]
3
No
No

54

M418

METTLER TOLEDO

Hydrochloric Acid Content by Endpoint Titration


The content of hydrochloric acid in water is determined by potentiometric endpoint titration to pH 8.3 with
sodium hydroxide.
Sample

5 mL hydrochloric acid solution, HCl


c(HCl) = 0.01 mol/L

Substance

Hydrochloric acid, HCl


M = 36.46 g/mol, z = 1

Chemicals

50 mL deionised water

Preparation and Procedures


1) Before analysis an electrode calibration was performed using
METTLER TOLEDO buffers of pH 4.01, 7.00 and 9.21.
2) The titer determination is performed by titrating potassium
hydrogen phthalate (KHP) as a primary standard: 70-120 mg
KHP are dissolved with 50 mL deionized water into a titration
beaker.
3) Sample titration:
5 mL 0.1 mol/L hydrochloric acid solution are transferred into a
titration beaker with a pipette.

Titrant

Sodium hydroxide, NaOH


c(HCl) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 70-120 mg

Instruments

Titration Excellence T50/T70/T90

Accessories

1 DV1010 Burette
Titration beakers ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DG111-SC

Chemistry

HCl + NaOH = NaCl + H2O

Calculation

R1 = Q , consumption, mmol

4) 50 mL deionised water are added into a titration beaker to


dilute the sample.

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.

R2 = Q*C/m , content, g/L


C=M/z

Results

Waste
disposal

Neutralize the slightly alkaline waste


before disposal.

Author

Maria-Jos Schmid

55

Results
All results
Method-ID
Sample
R1 (Consumption)
R2 (Content)
Sample
R1 (Consumption)
R2 (Content)
Sample
R1 (Consumption)
R2 (Content)
Sample
R1 (Consumption)
R2 (Content)
Sample
R1 (Consumption)
R2 (Content)
Sample
R1 (Consumption)
R2 (Content)

M418
HCl content (EP)
0.511
mmol
3.725
g/L
HCl content (EP)
0.509
mmol
3.710
g/L
HCl content (EP)
0.510
mmol
3.717
g/L
HCl content (EP)
0.510
mmol
3.717
g/L
HCl content (EP)
0.508
mmol
3.701
g/L
HCl content (EP)
0.512
mmol
3.730
g/L

Method-ID
R1
Samples
Mean
s
srel

M418
Consumption
6
0.510
mmol
0.001
mmol
0.277
%

Method-ID
R2
Samples
Mean
s
srel

M418
Content
6
3.717
g/L
0.010
g/L
0.279
%

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

Titration curve

56

Method
Method
Author

M418
HCl content (EP)
METTLER TOLEDO

02.08.2006

Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M418
HCl content (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

001 Title

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
HCl solution
Fixed volume
5.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
End point type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

30 %
10 s

007 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
g/L
R2=Q*C/m
C=M/z
M[Hydrochloric acid]
z[Hydrochloric acid]
3
No
No

008 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
009 End of sample

NaOH
0.1 mol/L
pH
DG111-SC
pH
No
30 %
Volume
2.0 mL
10 s
User
Absolute
Positive
8.30 pH
3.0 pH
5 mL/min
5 L/min
Yes
10 s
10.0 mL
Infinity

Consumption
mmol
R1=Q
C=1
M[Hydrochloric acid]
z[Hydrochloric acid]
3
No
No

57

M419

METTLER TOLEDO

Free Sulphur Dioxide (SO2) Content in Wine


The content of free sulphur dioxide (SO2) in wine is determined by redox titration with iodine as a titrant. The
titration is monitored using a Pt double pin electrode DM143 at a fixed polarization current (voltametric
indication)
Sample

50 mL white wine

Preparation and Procedures


Note: This method allows a fully automated analysis procedure
by using two additional burette drives.

Substance

Sulphur dioxide, SO2


M = 64.06 g/mol, z = 2

Chemicals

5 mL 10% potassium iodide, KI


5 mL 20% sulfuric acid, H2SO4

Titrant

Iodine, I2
c(1/2 I2) = 0.02 mol/L

Standard

Ascorbic acid, C6H8O6, M=176.13

Instruments

Titration Excellence T50/T70/T90


Manual stand
Two additional burette drives

Accessories

3 DV1010 Burettes
Titration beakers ME-101974
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DM143-SC

Chemistry

SO2 + I2 + 2 H2O = H2SO4 + 2 HI

Calculation

R = Q*C/m , content, mg/L


C = M*1000/z

1) The titer determination is performed using pure ascorbic acid


as a primary standard.
2) Sample determination: 50 mL wine are transferred into a
titration beaker with a pipette.
3) 5 mL 10% potassium iodide solution are added. This step
has been performed using an additional dosing unit. It can be
performed manually using a pipette.
4) 5 mL 20% sulfuric acid are added to the titration beaker.
This step has been performed using an additional dosing unit. If
not possible, this step can be done manually with a pipette.
Note:
Sodium metabisulfite (Na2S2O5, M = 222.32 g/mol) can be
used as a SO2-Standard (1 Na2S2O5 --> 2 SO2 ).

Remarks
1) The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) In order to avoid loss of SO2, the samples must be taken from
a freshly openend bottle. After opening the bottle, free SO 2 can
evaporate with CO2 or be oxidized while in contact with air
resulting in too low results. Working with the sample changer
leads to SO2 losses from the sample beakers already prepared
on the rack. Therefore it is recommended to work manually.
3) Iodine is also reduced by other wine components. These
competing reactions can partly be delayed by the addition of 5
mL 10% potassium iodide solution.
4) The reaction only takes place in acidic medium. Therefore, 5
mL 20% H2SO4 must be added immediately before titration.

Results

Waste
disposal

Neutralize the acid waste before final


disposal.

Author

Claudia Schreiner

5) If the sample contains ascorbic acid the amount of SO2 will


be higher, because of the reaction from ascorbic acid with
iodine.

58

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M419
White wine
21.222 mg/L
White wine
21.294 mg/L
White wine
21.160 mg/L
White wine
21.114 mg/L
White wine
21.190 mg/L
White wine
21.127 mg/L

Method-ID
R1
Samples
Mean
s
srel

M419
Content
6
21.185 mg/L
0.067
mg/L
0.315
%

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

Titration curve

59

Method
Method
Author

M419
Free SO2 in wine (EP)
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M419
HCl content
METTLER TOLEDO
02.08.200
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
White wine
Fixed volume
50.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

10% KI
1
5.0 mL
60.0 mL/min

005 Dispense (normal) [2]


Titrant
Concentration
Volume
Dosing rate

20% H2SO4
1
5.0 mL
60.0 mL/min

008 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
mg/L
R1=Q*C/m
C=M*1000/z
M[Sulfur dioxide]
z[Sulfur dioxide]
3
No
No

009 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
010 End of sample

006 Stir
Speed
Duration
007 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time

50 %
10 s

1/2 I2
0.02 mol/L
Polarized
DM143
mV
Voltametric
10 A
No
50 %
No
10 s
User
Absolute
Negative
100 mV
30 mV
1.25 mL/min
100 L/min
Yes
5 s
10.0 mL
600 s

60

M420

METTLER TOLEDO

Water Content in Ethanol According to Karl Fischer Reaction


The water content in ethanol is determined by redox titration with one component KF reagent as a titrant. The
titration is monitored using a Pt double pin electrode DM143 at a fixed polarization current (voltametric
indication)
Sample

Preparation and Procedures

0.5-1 g ethanol

1) 50 mL dry methanol are added into the titration cell.

Substance

Water, H2O
M = 18.01 g/mol, z = 1

Chemicals

50 mL dry methanol

2) The method is started to eliminate all moisture present in the


solvent (pretitration). In this case, no sample is added ("dummy
sample titration").
2) A drift determination is started (see application M422) and
the drift value is stored as auxiliary value H[KF Drift].
3) A titer determination is performed using di-sodium tartrate
dihydrate as a primary standard (see application M421).
4) The sample is added with a syringe. The sample size is
determined by back-weighing.

Titrant

KF one component titrant


c = 5 mg H2O/mL

Standard

Disodium tartrate dihydrate, 50 mg

Instruments

Titration Excellence T50/T70/T90


DV705 KF Titration stand

Accessories

1 DV1005 Burette
XS205 Balance
Olivetti JobJet 210 Printer

Remarks
Indication

DM143-SC

Chemistry

1) SO2 + R1N + R2OH = (R1NH)SO3R2


1

1) The method parameters have been optimised for the sample


used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.

2) (R NH)SO3R + I2 + H2O + 2 R N =
(R1NH)SO4R2 + H2SO4 + 2 (R1NH)I

Calculation

Consumption
R1 = VEND; mL
Time
R2 = tUSE ; min
Water content
R3 = (VEND-C)*c*TITER*100/(m*1000)
C = R2*H[KF Drift]/1000 ; %

2) The KF reagent and the solvent must be protected against


intake of air humidity. Drying tubes (ME-23961) filled with
molecular sieve and holders (ME-23915) are used for this
purpose.

Literature:
- METTLER TOLEDO Appl. brochure 26, ME-51 709 855.
- METTLER TOLEDO Appl. brochure 23, ME-51 725 023
- METTLER TOLEDO Appl. brochure 12, ME-51 724 765

Results

Waste
disposal

DIspose as organic solvent.

Author

Albert Aichert

61

Results
All results
Method-ID
Sample
R1 (Consumption)
R2 (Time)
R3 (Content)
Sample
R1 (Consumption)
R2 (Time)
R3 (Content)
Sample
R1 (Consumption)
R2 (Time)
R3 (Content)
Sample
R1 (Consumption)
R2 (Time)
R3 (Content)
Sample
R1 (Consumption)
R2 (Time)
R3 (Content)
Sample
R1 (Consumption)
R2 (Time)
R3 (Content)

M420
Ethanol
2.18625
4.880
1.756
Ethanol
1.89925
4.130
1.752
Ethanol
2.17125
5.400
1.757
Ethanol
2.11675
4.420
1.749
Ethanol
2.01850
3.720
1.744
Ethanol
2.20400
4.320
1.755

(1/1)
mL
min
%
(1/2)
mL
min
%
(1/3)
mL
min
%
(1/4)
mL
min
%
(1/5)
mL
min
%
(1/6)
mL
min
%

Method-ID
R3
Samples
Mean
s
srel

M420
Content
6
1.752
0.005
0.283

%
%
%

Statistics

Table of measured values

Titration curve

62

Method
Method
Author

M420
Water content KF (EP) 02.08.2006
METTLER TOLEDO

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M420
Water content KF (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature

004 Stir

005 Titration (EP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

008 Calculation R3
Result
Result unit
Formula

1
Ethanol
Weight
0.5 g
1.0 g
1.0 g/mL
1.0
25.0C

003 Titration stand (External stand)


Type
External stand
Titration stand
External Stand 1

Speed
Duration

007 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

30 %
10 s

One comp. titrant 5


5 mol/L
Polarized
DM143-SC
mV
Voltametric
24 A
No
30 %

Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Time
min
R2=tUSE
C=1
M[None]
z[None]
3
No
No

Content
%
R3=(VEND-C)*c*TITER*
*100/(m*1000)
C=R2*H[KF Drift]/1000
M[None]
z[None]
3
No
No

009 Record
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2E/dV2 - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Calibration curve
Method
Series data
Condition

Per series
Per series
Last titration
Per series
No
Last titration
No
No
No
Last titration
Last titration
No
No
No
No
No
No
No
No

function

function

function
function

010 End of sample

Volume
1.5 mL
10 s
User
Absolute
Negative
150 mV
5 mV
2 mL/min
150 L/min
Yes
10 s
10.0 mL
1200 s

Consumption
mL
R1=VEND
C=1
M[None]
z[None]
5
No
No

63

M421

METTLER TOLEDO

Titer of 5 mg H2O/mL Karl Fischer One Component Reagent


The titer of one component KF reagent is determined by redox titration with disodium tartrate dihydrate. The
titration is monitored using a Pt double pin electrode DM143 at a fixed polarization current (voltametric
indication)
Sample

Preparation and Procedures

Disodium-tartrate dihydrate,
0.03-0.07 g

Substance

Water, H2O
M = 18.01 g/mol, z = 1

Chemicals

50 mL dry methanol

1) 50 mL dry methanol are added into the titration cell.


2) The general KF method M420 is started to eliminate all
moisture present in the solvent (pretitration). In this case, no
sample is added ("dummy sample titration").
3) The method M422 is started and the drift value in L/min is
stored as auxiliary value H[KF Drift].
4) The sample is added with a weighing boat. The sample size
is determined by back-weighing.

Titrant

KF one component titrant


c = 5 mg H2O/mL

Standard

--

Instruments

Titration Excellence T50/T70/T90


DV705 KF Titration stand

Accessories

1 DV1005 Burette
XS205 Balance
Olivetti JobJet 210 Printer

5) It is recommended to replace the solvent after 3 samples, as


its dissolving capacity is exhausted.

Remarks
Indication

DM143-SC

Chemistry

1) SO2 + R1N + R2OH = (R1NH)SO3R2


1

1) The method parameters have been optimised for the sample


used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.

2) (R NH)SO3R + I2 + H2O + 2 R N =
(R1NH)SO4R2 + H2SO4 + 2 (R1NH)I

Calculation

Consumption
R1 = VEND ; mL
Time
R2 = tUSE ; min
Titer
R3 = (15.66*10*m+C)/(VEND/c)
C = R2*H[KF Drift]/1000

2) The KF reagent and the solvent must be protected against


intake of air humidity. Drying tubes (ME-23961) filled with
molecular sieve and holders (ME-23915) are used for this
purpose.
3) The mean value of the titer is automatically stored as part of
the setup data by means of the function "Titer".
4) The concentration of the KF titrant must be set to 5 mol/L
since the concentration can not be defined as mg/mL.
5) If the titer value is lower than 0.8, it is recommended to
replace the titrant with fresh one.

Results

Waste
disposal

DIspose as organic solvent.

Author

Albert Aichert

Literature:
- METTLER TOLEDO Appl. brochure 26, ME-51 709 855.
- METTLER TOLEDO Appl. brochure 23, ME-51 725 023
- METTLER TOLEDO Appl. brochure 12, ME-51 724 765

64

Results
All results
Method-ID
Sample
R1 (Consumption)
R2 (Time)
R3 (Titer)
Sample
R1 (Consumption)
R2 (Time)
R3 (Titer)
Sample
R1 (Consumption)
R2 (Time)
R3 (Titer)
Sample
R1 (Consumption)
R2 (Time)
R3 (Titer)
Sample
R1 (Consumption)
R2 (Time)
R3 (Titer)
Sample
R1 (Consumption)
R2 (Time)
R3 (Titer)

M421
Disodium
1.64925
5.600
1.023759
Disodium
1.60550
5.020
1.032610
Disodium
1.87650
4.950
1.024185
Disodium
1.89275
5.600
1.028735
Disodium
1.91725
5.400
1.028331
Disodium
1.91600
5.520
1.029002

Method-ID
R3
Samples
Mean
s
srel

M421
Titer
6
1.027770
0.003
0.323

tartrate (1/1)
mL
min
tartrate (1/2)
mL
min
tartrate (1/3)
mL
min
tartrate (1/4)
mL
min
tartrate (1/5)
mL
min
tartrate (1/6)
mL
min

Statistics

Table of measured values

Titration curve

65

Method
Method
Author

M421
Titer KF (EP) 02.08.2006
METTLER TOLEDO

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample (Titer)
Titrant
Concentration
Standard
Type of standard
Entry type
Lower limit
Upper limit
Correction factor
Temperature
Entry

General titration
T50 / T70 / T90
M421
Titer KF (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

One comp. titrant 5


5 mol/L
Disodium tartrate
Solid
Weight
0.03 g
0.07 g
1.0
25.0C
Arbitrary

007 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
008 Calculation R3
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2E/dV2 - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Calibration curve
Method
Series data

004 Stir

005 Titration (EP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

30 %
60 s

One comp. titrant 5


5 mol/L
Polarized
DM143-SC
mV
Voltametric
24 A
No

User
Absolute
Negative
150 mV
5 mV
2 mL/min
150 L/min
Yes
10 s
10.0 mL
1200 s

Consumption
mL
R1=VEND
C=1
M[Disodium tartrate]
z[Disodium tartrate]
5
No

Titer
R3=(15.66*10*m+C)/(VEND/c)

C=R2*H[KF Drift]/1000
M[Disodium tartrate]
z[Disodium tartrate]
6
No
No

Per series
Per series
Last titration
Per series
No
Last titration
No
No
No
Last titration
Last titration
No
No
No
No
No
No
No

function

function

function
function

010 End of sample


011 Titer
Titrant
Concentration
Titer=
Result limits

30 %
Volume
0.5 mL
10 s

No

009 Record

003 Titration stand (External stand)


Type
External stand
Titration stand
External Stand 1

Speed
Duration

Time
min
R2=tUSE
C=1
M[Disodium tartrate]
z[Disodium tartrate]
3
No

012 Calculation R4
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

One comp. titrant 5


5 mol/L
Mean[R3]
No

Mean Titer
No
R4=Mean[R3]
C=1
M[Disodium tartrate]
z[Disodium tartrate]
5
No
No

013 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

No

66

M422

METTLER TOLEDO

Drift Determination for The Karl Fischer Titration


The drift of the KF titration vessel is determined by redox titration. The titration is monitored using a Pt double
pin electrode DM143 at a fixed polarization current (voltametric indication)
Sample

Preparation and Procedures

--

1) 50 mL dry methanol are added into the titration cell.

Substance

Water, H2O
M = 18.01 g/mol, z = 1

Chemicals

50 mL dry methanol

Titrant

KF one component titrant


c = 5 mg H2O/mL

Standard

--

Instruments

Titration Excellence T50/T70/T90


DV705 KF Titration stand

Accessories

1 DV1005 Burette
Olivetti JobJet 210 Printer

2) The general KF method M420 is started to eliminate all


moisture present in the solvent (pretitration). In this case, no
sample is added ("dummy sample titration").
3) The method M422 is started and the drift value in L/min is
stored as auxiliary value H[KF Drift].
4) To achieve an accurate drift determination it is recommended
to perform it immediately after pretitration of the solvent, or after
the standby titration. A series of 2-3 drift determination is
recommended.

Remarks
Indication

DM143-SC

Chemistry

1) SO2 + R1N + R2OH = (R1NH)SO3R2


1

1) The method parameters have been optimised for the solvent


used in this application. Thus, it may be necessary to slightly
adapt the method to your specific solvent or solvent mixture.

2) (R NH)SO3R + I2 + H2O + 2 R N =
(R1NH)SO4R2 + H2SO4 + 2 (R1NH)I

Calculation

Consumption
R1 = VEND *1000; L
Time
R2 = t*60 ; sec
Drift
R3 = 60*R1/R2 ; g/min

Results

Waste
disposal

DIspose as organic solvent.

Author

Albert Aichert

2) The KF reagent and the solvent must be protected against


intake of air humidity. Drying tubes (ME-23961) filled with
molecular sieve and holders (ME-23915) are used for this
purpose.

Literature:
- METTLER TOLEDO Appl. brochure 26, ME-51 709 855.
- METTLER TOLEDO Appl. brochure 23, ME-51 725 023
- METTLER TOLEDO Appl. brochure 12, ME-51 724 765

67

Results
All results
Method-ID
Sample
R1 (Consumption)
R2 (Time)
R3 (Drift KF)
Sample
R1 (Consumption)
R2 (Time)
R3 (Drift)
Sample
R1 (Consumption)
R2 (Time)
R3 (Drift KF)
Sample
R1 (Consumption)
R2 (Time)
R3 (Drift KF)
Sample
R1 (Consumption)
R2 (Time)
R3 (Drift)
Sample
R1 (Consumption)
R2 (Time)
R3 (Drift KF)

M422
KF Solvent
(1/1)
6.250
L
604.200
s
0.625
L/min
KF Solvent
(1/2)
6.000
L
604.200
s
0.600
L/min
KF Solvent
(1/3)
5.750
L
604.200
s
0.575
L/min
KF Solvent
(1/4)
5.000
L
604.200
s
0.500
L/min
KF Solvent
(1/5)
6.750
L
604.200
s
0.675
L/min
KF Solvent
(1/6)
5.250
L
604.200
s
0.525
L/min

Method-ID
R3
Samples
Mean
s
srel

M422
Drift KF
6
0.583
0.065
11.066

Statistics

Table of measured values

L/min
L/min
%

Titration curve

68

Method
Method
Author

M423
Drift KF (EP)
METTLER TOLEDO

02.08.2006

Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M422
KF Drift determination
METTLER TOLEDO
02.08.2006 15:00
--No
None

001 Title

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature
003 Titration stand (Auto stand)
Type
Titration stand

1
KF Solvent
Fixed volume
50.0 mL
1.0 g/mL
1.0
25.0C

007 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
008 Calculation R3
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Auto stand
Auto Stand 1

009 Auxiliary value


Titrant
Formula
Result limits

30 %
5 s

010 Record

Time
sec
R2=t*60
C=1
M[None]
z[None]
3
No
No

Drift
L/min
R3=60*R1/R2
C=1
M[None]
z[None]
3
No
No

KF Drift
H=R3
No

004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2E/dV2 - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Calibration curve
Method
Series data

One comp. titrant 5


5 mol/L
Polarized
DM143-SC
mV
Voltametric
24 A
No
30 %
None
0 s

Per series
Per series
Last titration
Per series
Per series
Last titration
No
No
No
Last titration
Last titration
No
No
No
No
No
No
No

function

function

function
function

011 End of sample


User
Absolute
Negative
150 mV
2000 mV
0.002 mL/min
1 L/min
Yes
600 s
10.0 mL
600 s

012 Calculation R4
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

KF Drift
L/min
R4=R3
C=1
M[None]
z[None]
3
No
No

013 Record
Consumption
L
R1=VEND*1000
C=1
M[None]
z[None]
3
No

Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

No

69

M423

METTLER TOLEDO

Standby Titration the Karl Fischer Reaction


The KF titration vessel is kept anhydrous by continuously titrating the solvent with one component KF
reagent. The titration is monitored using a Pt double pin electrode DM143 at a fixed polarization current
(voltametric indication)
Sample

--

Preparation and Procedures


1) 50 mL dry methanol are added into the titration cell and the
method is started to eliminate all moisture present in the solvent.

Substance

Water, H2O
M = 18.01 g/mol, z = 1

Chemicals

50 mL dry methanol

Titrant

KF one component titrant


c = 5 mg H2O/mL

Standard

Disodium tartrate dihydrate, 50 mg

Instruments

Titration Excellence T50/T70/T90


DV705 KF Titration stand

Accessories

1 DV1005 Burette
XS205 Balance
Olivetti JobJet 210 Printer

Remarks
Indication

DM143-SC

Chemistry

1) SO2 + R1N + R2OH = (R1NH)SO3R2

1) The KF reagent and the solvent must be protected against


intake of air humidity. Drying tubes (ME-23961) filled with
molecular sieve and holders (ME-23915) are used for this
purpose.

2) (R1NH)SO3R2 + I2 + H2O + 2 R1N =


(R1NH)SO4R2 + H2SO4 + 2 (R1NH)I

Calculation

--

Literature:
- METTLER TOLEDO Appl. brochure 26, ME-51 709 855
- METTLER TOLEDO Appl. brochure 23, ME-51 725 023
- METTLER TOLEDO Appl. brochure 12, ME-51 724 765

Results

Waste
disposal

DIspose as organic solvent.

Author

Albert Aichert

70

Results
------

Table of measured values

Titration curve

71

Method
Method
Author

M423
Standby KF (EP)
METTLER TOLEDO

02.08.2006

Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M423
Standby KF (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

001 Title

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Standby
Fixed volume
50.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (External stand)


Type
External stand
Titration stand
External Stand 1
004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time

30 %
5 s

One comp. titrant 5


5 mol/L
Polarized
DM143-SC
mV
Voltametric
24 A
No
30 %
None
0 s
User
Absolute
Negative
150 mV
2000 mV
0.002 mL/min
1 L/min
Yes
100000000 s
20.0 mL
infinity

005 End of sample

72

M424

METTLER TOLEDO

Bromine Number in Petrol According to ASTM D1159-01


Method for the determination of the bromine number in petrol by titration with a bromide-bromate solution.
The titration is monitored using a Pt double pin electrode DM143 at a fixed polarization current (voltametric
indication)
Sample

Substance
Chemicals

0.01-0.6 g petrol;
Also for: petroleum distillates and
aliphatic alkenes with 1-200g Br2/100g
"C-C double bonds", expressed as g
Br2/100g sample , M=159.81, z=1
50 mL bromine nr. solvent
(see Preparation and procedures)

Titrant

Bromide-bromate solution, Br-/BrO3c(Br2) = 0.05 mol/L

Standard

--

Instruments

Titration Excellence T50/T70/T90


1 additional dosing unit
1 peristaltic pump (waste pump)

Accessories

DV1010 and DV1020 Burettes


Thermostatable beaker ME-23517
DT1000 Temperature sensor
XS205 Balance

Indication

DM143-SC

Chemistry

BrO3- + 5 Br- + 6 H+ = 3 Br2 + 3 H2O


R1-CH=CH-R2+Br2 = R1-CHBr-CHBr-R2
By maintaining a temperature between 0C and
5C only the bromine addition reaction takes
place. Substitution and oxidation are avoided.

Calculation

Bromine number, g Br2 /100 g


R = (QEND-B[ASTM D1159])*C/m
C = M/(10*z)

Results

Waste
disposal

Dispose the waste as halogenated


organic solvent.

Author

Melanie Nijman

Preparation and Procedures


1) Bromine Nr. solvent preparation:
714 mL glacial acetic acid, 134 mL 1,1,1,-trichloroethane, 134
mL methanol and 18 mL H2SO4 (16% v/v) are mixed in 1 L
volumetric flask.
2) A blank value is determined accordind to application M425
and stored as blank value B[ASTM D1159]. It is determined for
every new batch of solvent mixture.
3) Titrant preparation:
Dissolve 10.2 g KBr and 2.78 g of KBrO3 with deionized water
into a 1 L volumetric flask and fill up to the mark. The salts are
dried at 105C (220 F) during 30 minutes. The titrant can also
be bought commercially. The commercially available product
can be used without further standardization.
4) The Br2-number is an indication of the quantity of brominereactive constituents. It represents the amount (g) of Br 2 which
reacts with 100 g sample under the condition of the standard
test method.
5) The method parameters have been optimised for the sample
used in this application. It may be necessary to slightly adapt
the method to your specific sample. This application does not
replace the ASTM standard.

Remarks
1) Sample size for bromine number < 50: Direct titration
Depending on the Br2-number, the appropriate amount has to be
weighed in (back-weighing) and filled directly into the vessel
with 50 mL of the bromine number solvent.
Bromine Number
1-5
5 - 10
10 - 20
20 - 50

Sample size/g
6.0 - 1.2
1.0 - 0.6
0.5 - 0.3
0.25 - 0.1

2) Sample size for bromine number > 50: Dilution


- 10 mL of 1,1,1-trichloroethane are placed in a 50 mL flask
and a test specimen is added as indicated below:
Bromine Number Sample size/g
50 - 100
1.0 - 0.6
100 - 200
0.5 - 0.4
200 - 500
0.35 - 0.15
-The sample mass (m') is obtained by back-weighing
(accuracy: +/- 1 mg)
- Fill the flask to the mark with 1,1,1-trichloroethane and mix.
- A 5 mL aliquot of this solution has to be filled into the
thermostatable beaker together with 50 mL of the solvent.
4- Take care to enter m'/10 as sample mass.

73

Results
All results
Method-ID
Sample
R1 (Bromine
Sample
R1 (Bromine
Sample
R1 (Bromine
Sample
R1 (Bromine
Sample
R1 (Bromine
Sample
R1 (Bromine

number)
number)
number)
number)
number)
number)

M424
Petrol
19.62059
Petrol
19.65058
Petrol
19.60262
Petrol
19.82843
Petrol
19.69236
Petrol
19.71195

(1/1)
g/100 g
(1/2)
g/100 g
(1/3)
g/100 g
(1/4)
g/100 g
(1/5)
g/100 g
(1/6)
g/100 g

Statistics
Method-ID
R1
Samples
Mean
s
srel

Table of measured values

M424
Bromine number
6
19.68382 g/100 g
0.08055
g/100 g
0.409
%

Titration curve

74

Method
Method
Author

M424
Bromine number ASTM D1159 (EP) 02.08.2006
METTLER TOLEDO

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M424
Bromine number
ASTM D1159 (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Bromine number
g/100 g
R=(QEND-B[ASTM D1159])*C/m
C=M/(10*z)
M[Bromine]
z[Bromine]
5
No
No

008 Drain
Drain pump
Drain volume

SP250
80.0 mL

009 Record
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Petrol
Weight
0.01 g
6.00 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual Stand
Titration stand
Manual Stand 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

Bromine nr. solvent


1
50.0 mL
60.0 mL/min

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
No
E - t
Last titration function
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No
010 End of sample

005 Stir
Speed
Duration
006 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Temperature sensor
Unit
Stir
Speed
Predispense
Mode
Wait time
Control
Control
End point type
Tendency
End point value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time

20 %
300 s

Bromide-Bromate
0.05 mol/L
Polarized
DM143-SC
mV
Voltametric
10 A
Yes
DT1000
C
25 %
None
0 s
Mettler
Absolute
Negative
150 mV
0.1 mV
1.0 mL/min
350 L/min
Yes
15.0 s
10.0 mL
infinity

75

M425

METTLER TOLEDO

Blank Value for Bromine Number Solvent According to ASTM D1159-01


Method for the determination of the blank value of the bromine number solvent by titration with a
bromide-bromate solution. The titration is monitored using a Pt double pin electrode DM143 at a fixed
polarization current (voltametric indication)
Sample

Substance

50 mL bromine nr. solvent

"C-C double bonds", expressed as g


Br2/100g sample , M=159.81, z=1

Chemicals

--

Titrant

Bromide-bromate, Br-/BrO3c(Br2) = 0.05 mol/L

Standard

--

Instruments

Titration Excellence T50/T70/T90


1 additional dosing unit
1 peristaltic pump (waste pump)

Accessories

DV1010 and DV1020 Burettes


Thermostatable beaker ME-23517
DT1000 Temperature sensor
XS205 Balance

Preparation and Procedures


1) Bromine Nr. solvent preparation:
714 mL glacial acetic acid, 134 mL 1,1,1,-trichloroethane, 134
mL methanol and 18 mL H2SO4 (16% v/v) are mixed in 1 L
volumetric flask.
2) Titrant preparation:
Dissolve 10.2 g KBr and 2.78 g of KBrO3 with deionized water
into a 1 L volumetric flask and fill up to the mark. The salts are
dried at 105C (220 F) during 30 minutes. The titrant can also
be bought commercially. The commercially available product
can be used without further standardization.
3) Determination of blank value:
50 mL of bromine nr. solvent are dispensed using an additional
dosing unit. This step can be dispensed manually by using a
pipette. The titration is started and the titrant consumption in
mmol to the endpoint is stored as B[ASTM D1159] by means of
the method function Blank.
4) With sample having a bromine number smaller than
50 g Br2/100g the blank is performed by analysing 50 mL of
solvent. For blank determination of samples with bromine
number larger than 50 gr Br2/100 g, 5 mL 1,1,1-trichloroethane
are added to 50 mL of the solvent.

Remarks

Indication

DM143-SC

1) This application does not replace the ASTM standard.

Chemistry

BrO3- + 5 Br- + 6 H+ = 3 Br2 + 3 H2O

2) The magnitude of the bromine number is an indication of the


quantity of bromine-reactive constituents. It represents the
amount (g) of bromine which reacts with 100 g of the sample
under the condition of the standard test method.

R1-CH=CH-R2+Br2 = R1-CHBr-CHBr-R2

3) By maintaining a temperature between 0C and 5C only the


bromine addition reaction takes place. Substitution and
oxidation are avoided.

Calculation

Blank value for bromine number


R = QEND
R is stored as blank value
B[ASTM D1159].

Results

Waste
disposal

Dispose the waste as halogenated


organic solvent.

Author

Melanie Nijman

4) According to the standard the blank titration of 110 mL


solvent should use less than 0.1 mL of titrant, otherwise the
solvent should be disposed and a fresh batch produced. In this
application we have not disposed the solvent to reduce the
waste amount.
Literature:
1) ASTM D1159-01, see www.astm.org
2) Memory Card Application Package,
"Determination in the Petroleum Industry",
METTLER TOLEDO Application brochure 20, ME-51 725 020.

76

Results
All results
Method-ID
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)

M425
Bromine
0.01695
Bromine
0.01713
Bromine
0.01690
Bromine
0.01688
Bromine
0.01663
Bromine
0.01685

Method-ID
R1
Samples
Mean
s
srel

M425
Bromine nr. solvent
6
0.01689 mmol
0.00016 mmol
0.958
%

nr. solvent
mmol
nr. solvent
mmol
nr. solvent
mmol
nr. solvent
mmol
nr. solvent
mmol
nr. solvent
mmol

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

Titration curve

77

Method
Method
Author

M425
Blank ASTM D1159 (EP)
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M425
Blank ASTM D1159 (EP)
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
No
E - t
Last titration function
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No

1
Bromine nr. solvent
Fixed volume
50.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual Stand
Titration stand
Manual Stand 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

Bromine nr. solvent


1
50.0 mL
60.0 mL/min

009 Drain
Drain pump
Drain volume

005 Stir
Speed
Duration
006 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor Parameters
Type
Sensor
Unit
Indication
Ipol
Temperature acquisition
Temperature acquisition
Temperature sensor
Unit
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time

20 %
300 s

No

008 Record

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

Consumption
mmol
R=QEND
C=1
M[None]
z[None]
5
No

SP250
80.0 mL

010 End of sample


011 Blank

Bromide-Bromate
0.05 mol/L
Polarized
DM143
mV
Voltametric
10 A
Yes
DT1000
C
25 %
None
0 s
User
Absolute
Negative
150 mV
0.1 mV
1.0 mL/min
350 L/min

Name
Formula
Unit
Limits
012 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
013 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

ASTM D1159
B=Mean[R1]
mmol
No

Mean consumption
mmol
R2=Mean[R1]
C=1
M[None]
z[None]
5
No
No
Yes
No
No
No
No
No

Yes
15.0 s
10.0 mL
infinity

78

M426

METTLER TOLEDO

Acid Number in Motor Oil According to ASTM D664-04


Method for the determination of the acid number (AN) in motor oil by potentiometric titration with potassium
hydroxide in 2-propanol.
Sample

Motor oil, approx. 5 g for AN 1-5

Preparation and Procedures


1) The titer is determined using potassium hydrogen phthalate
(KHP): add approx. 80 mg KHP into a glass titration beaker
and dissolve it with 60 mL deion. water.

Substance

Acid components as mg KOH/g


sample, M=56.1 g/mol, z=1

Chemicals

60 mL ASTM D664-04 solvent:


Toluene:2-propanol:deion. water
500 mL : 495 mL : 5 mL

Titrant

Potassium hydroxide in 2-Propanol


KOH, c(KOH) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence T50/T70/T90

Accessories

DV1010 Burette
Titration glass beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

2) The buffer potential 1 (pH 4) and the buffer potential 2


(pH 11) are determined using aqueous pH buffers. These
values are stored as auxiliary values H{Buffer pH4] and
H[Buffer pH11].
3) A blank value is determined for every new batch of solvent
mixture (see M427) and stored as B[ASTM664].
4) Depending on the AN of the sample, different sample
amounts are requested:
AN
0.05 - <1.0
20.0 +/- 2.0
1.0 - <5.0
5.0 +/- 0.5
5
- <20
1.0 +/- 0.1
20 - <100
0.25 +/- 0.02
100 - <260
0.1 +/- 0.01
5) After each sample titration the DG113-SC sensor has to be
rinsed and conditioned in deion. water during 5 minutes.
Subsequently, the electrode is rinsed with solvent before starting
next titration.

Remarks

Indication

DG113-SC

1) This application does not replace the ASTM standard.

Chemistry

KOH + HA = KA + H2O

2) The method parameters have been optimised for the sample


used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.

HA: Acid components

Calculation

R1=(Q-B[ASTM664])*C/m, C=M
AN (mg KOH/g) at EQP
R2=QE(H[pH11]-B[ASTM664])*C/m,
C=M
KOH cons. (mmol) at buffer pot. 2

Results

Waste
disposal

Dispose as aromatic organic solvent


(toluene)

3) The acid number indicates the amount of base as mg KOH/g


sample needed to titrate the acidic constituents in a sample
under specific conditions, i.e. specified solvent and endpoint.
4) The sample is titrated using an EQP method function. If no
inflection point is detected, endpoints are taken at meter
readings corresponding to those found for aqueous acidic and
basic buffer solutions i.e. pH 4 and 11:
4.1. Acidic buffer pH 4 :
Strong Acid Number (SAN), titration with HCl in 2-propanol
4.2. Basic buffer pH 11:
Acid Number (AN), titration with KOH in 2-Propanol
5) In this application the SAN at pH 4 could not be calculated
since the initial potential was already below buffer potential 1
(pH 4).
Literature:
- ASTM D664-04, see www.astm.org
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Author

Thomas Hitz

79

Results
All results
Method-ID
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)

M426
Motor
2.053
2.177
Motor
2.075
2.247
Motor
----2.262
Motor
----2.262
Motor
----0.294
Motor
2.147
2.471

Method-ID
R1
Samples
Mean
s
srel
R2
Samples
Mean
s
srel

M426
Content
3
2.092
0.040
1.919
Content
6
2.286
0.090
3.947

oil
oil
oil
oil
oil
oil

(1/1)
mg KOH/g
mg KOH/g
(1/2)
mg KOH/g
mg KOH/g
(1/3)
mg KOH/g
mg KOH/g
(1/4)
mg KOH/g
mg KOH/g
(1/5)
mg KOH/g
mg KOH/g
(1/6)
mg KOH/g
mg KOH/g

Statistics

Table of measured values

mg KOH/g
mg KOH/g
%
mg KOH/g
mg KOH/g
%

Titration curve

80

Method
Method
Author

M426
Acid number ASTM D664
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M426
Acid number ASTM D664
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities
007 Calculation R2
Result
Result unit
Formula

1
Motor oil
Weight
0.0 g
10.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
mg KOH/g
R1=(Q-B[ASTM664])*C/m
C=M/z
M[Potassium hydroxide]
z[Potassium hydroxide]
3
No
No

Content
mmol
R2=(QE(H[Buffer pH11]B[ASTM664])*C/m
C=M
M[KOH]
z[KOH]
3
No
No

008 Record
003 Titration stand (Manual stand)
Type
Manual Stand
Titration stand
Manual Stand 1
004 Stir
Speed
Duration
005 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. value acquisition
dE
dt
t(min)
t(max)
Evaluation and recognition
Procedure
Threshold
Tendency
Ranges
Lower limit
Upper limit
Add. EQP criteria
Termination
At Vmax
At potential
Potential
Termination tendency
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria

35 %
15 s

KOH in 2-Propanol
0.1 mol/L
pH
DG113-SC
mV
No
35 %

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
009 End of sample

None
0 s
User
Dynamic
15.0 mV
0.01 mL
0.5 mL
Equilibrium controlled
1.0 mV
1 s
5 s
40 s
Standard
50 mV/mL
Negative
1
- 300 mV
50 mV
No
10.0 mL
Yes
- 240
None
No
No
No
No

81

M427

METTLER TOLEDO

Blank Value of Acid Number Solvent According to ASTM D664-04


Method for the blank value determination of the acid number (AN) solvent by potentiometric titration with
potassium hydroxide in 2-propanol in non aqueous solvent according to ASTM D664-04
Sample

60 mL ASTM D664-04 solvent:


Toluene:2-propanol: deion. water
500 mL : 495 mL : 5 mL

Substance

Acid components as mg KOH/g


sample, M=56.1 g/mol, z=1

Chemicals

--

Preparation and Procedures


1) The titer is determined using potassium hydrogen phthalate
(KHP): add approx. 80 mg KHP into a glass titration beaker
and dissolve it with 60 mL deionized water.
2) The buffer potential 1 (pH 4) and the buffer potential 2
(pH 11) are determined using aqueous pH buffers. These
values are stored as H{Buffer pH4] and H[Buffer pH11].
3) Since no inflection point was detected, the endpoint potential
was determined using buffer pH 11 (evaluation at pH 11).

Titrant

Potassium hydroxide in 2-Propanol


KOH, c(KOH) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence T50/T70/T90

Accessories

1 DV1010 Burette
Titration glass beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

4) After each sample the electrode was cleaned with 2-propanol


and conditioned for 300 s in deionized water. The potential at
pH 11.0 was determined again and compared with the initial
potential (first determination). If the potential difference was less
or equal 2 mV, then the next sample for blank determination
was started.

Remarks

Indication

DG113-SC

1) This application does not replace the ASTM standard.

Chemistry

KOH + HA = KA + H2O

2) The method parameters have been optimised for the sample


used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.

HA: Acid components

Calculation

R1 = Q ; mmol
R2 = QE(H[pH11]) ; mmol

3) The acid number indicates the amount of base as mg KOH/g


sample needed to titrate the acidic constituents in a sample
under specific conditions, i.e. specified solvent and endpoint.
4) The sample is titrated using an EQP method function. If no
inflection point is detected, endpoints are taken at meter
readings corresponding to those found for aqueous acidic and
basic buffer solutions i.e. pH 4 and 11:
4.1. Acidic buffer pH 4 :
Strong Acid Number (SAN), titration with HCl in 2-propanol
4.2. Basic buffer pH 11:
Acid Number (AN), titration with KOH in 2-Propanol

Results

Waste
disposal

Dispose as aromatic organic solvent


(toluene)

Author

Thomas Hitz

Literature:
- ASTM D664-04, see www.astm.org
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

82

Results
All results
Method-ID
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)

M427
Blank ASTM
0.00570
Blank ASTM
0.00550
Blank ASTM
0.00560
Blank ASTM
0.00530
Blank ASTM
0.00550
Blank ASTM
0.00560

Method-ID
R1
Samples
Mean
s
srel

M427
Consumption
6
0.00553
mmol
0.00014
mmol
2.469
%

D664 (EP)
mmol
D664 (EP)
mmol
D664 (EP)
mmol
D664 (EP)
mmol
D664 (EP)
mmol
D664 (EP)
mmol

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

Titration curve

83

Method
Method
Author

M427
Blank ASTM D664
METTLER TOLEDO

02.08.2006

Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M427
Blank ASTM D664
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
No
E - t
Last titration function
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

001 Title

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Solvent ASTM D664
Fixed volume
60.0 mL
1.0 g/mL
1.0
25.0C

008 End of sample


009 Blank
Name
Value
Units
Limits

003 Titration stand (Manual stand)


Type
Manual Stand
Titration stand
Manual Stand 1
004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor Parameters
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Endpoint type
Tendency
Endpoint value
Control band
Dosing rate (max)
Dosing rate (min)
Termination
At EP
Termination delay
At Vmax
Max. time
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

35 %
15 s

KOH in 2-Propanol
0.1 mol/L
pH
DG113-SC
mV
No
35 %
None
0 s

010 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

ASTM664
B=Mean[R1]
mmol
No

Mean consumption
mmol
R2=Mean[R1]
C=1
M[None]
z[None]
5
No
No

011 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

User
Absolute
Negative
H[Buffer pH11] mV
300 mV
0.1 mL/min
10 L/min
Yes
0 s
2.0 mL
infinity

Consumption
mmol
R1=Q
C=1
M[None]
z[None]
5
No
No

84

M428

METTLER TOLEDO

Base Number According to ASTM D4739-05


Method for the determination of the base number BN in oil by titration with hydrochloric acid in 2-propanol
according to ASTM D4739-05.
Sample

Substance
Chemicals

Cutting oil, 0.1-10 g

Alkaline components in oil expressed


as KOH, M=56.1 g/mol , z=1
60 mL ASTM D4739-05 solvent
(see Preparation and Procedures)

Titrant

HCl in 2-propanol, c(HCl)=0.1 mol/L


KOH in 2-propanol, c(HCl)=0.1 mol/L

Standard

KOH in 2-propanol 0.1 mol/L / KHP

Instruments

Titration Excellence T50/T70/T90


Rondo 60 Sample changer
1 additional dosing unit (20 mL)

Accessories

DV1010 and DV1020 Burettes


Glass beaker ME-101446
XS205 Balance, SP250
Olivetti Printer JobJet 210

Indication

DG113-SC

Chemistry

HCl + NaOH = Cl- + Na+ + H2O


NaOH represents the alkaline
components.

Calculation

Base number mg KOH/g:


R1=(Q-B[ASTM D4739])*C/m, C=M/z
Base number mg KOH/g at acidic potential:
R2=
(QE(H[Buffer pH3])-B[ASTM D4739])*C/m;

C=M/z

Results

Waste
disposal

Disposal as halogenated organic waste

Author

Claudia Schreiner

Preparation and Procedures


1) Solvent preparation:
ASTM D4739-05 solvent is prepared by mixing 2-propanol,
toluene, chloroform and water in the following ratio:
10 : 10 : 10 : 0.3 (v/v).
2) The titer is determined by titration of standardized KOH in
2-propanol solution. The latter is standardized using potassium
hydrogen phthalate (KHP).
3) The acidic and the alkaline aqueous buffers are measured
and stored as auxiliary values pH3 (BN) and pH10 (SBN).
4) Blank value determinations for the base number are
determined for every new batch of solvent mixture by titration
with HCl in 2-propanol to pH 3 buffer potential value (M429).
The result is stored as blank value B[ASTM D4739]. For SBN,
the solvent is titrated with KOH in 2-propanol to pH 10 pot.
value.
5) Add the oil sample into the titration beaker. The appropriate
sample size is calculated according to the following formula:
sample size (g) = 7/expected BN
6) 60 mL ASTM D4739-05 solvent are added using an
additional dosing unit. This step can be performed manually
using a dispenser or a graduated cylinder.

Remarks
This method allows a fully automated procedure using a
sample changer and an additional dosing unit. It can be
modified for manual operation. Select "Manual stand" in the
method function "Titration stand".
1) This application does not replace the ASTM standard.
The method parameters have been optimised for the sample
used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.
2) The base number BN is defined as the consumption of
hydrochloric acid to a specific endpoint to neutralize the alkaline
components of the oil. It is expressed as mg KOH/g sample:
- If an EQP is found between the acidic buffer potential value and
a point 100 mV past this potential, then this will be the BN.
- If no EQP is found in this region, then the result is evaluated a
the potential value of the acidic buffer.
3) Between each sample it is necessary to condition the
electrode under stirring during 300 s in deion. water. The
electrode is parked in buffer pH 4 (Rinse beaker).
Literature:
1) ASTM D4739-05 and 4739-04 Draft , see www.astm.org
2) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

85

Results
All results
Method-ID
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)
Sample
R1 (Content)
R2 (Content)

M428
Cutting
19.48
17.15
Cutting
19.70
15.33
Cutting
19.84
15.38
Cutting
19.15
15.91
Cutting
19.34
15.86

Method-ID
R1
Samples
Mean
s
srel
R2
Samples
Mean
s
srel

M428
Cutting oil
5
19.50
mg
0.27
mg
1.404
%
Cutting oil
5
15.93
mg
0.74
mg
4.620
%

oil
mg
mg
oil
mg
mg
oil
mg
mg
oil
mg
mg
oil
mg
mg

(1/1)
KOH/g
KOH/g
(1/2)
KOH/g
KOH/g
(1/3)
KOH/g
KOH/g
(1/4)
KOH/g
KOH/g
(1/5)
KOH/g
KOH/g

Statistics

Table of measured values

KOH/g
KOH/g

KOH/g
KOH/g

Titration curve

86

Method
Method
Author

M428
Base number ASTM D4739
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M428
Base number ASTM D4739
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

008 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

1
Cutting oil
Weight
0.0 g
10.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondo60/TowerA)


Type
Rondo60/TowerA
Titration stand
Rondo60/1A
004 Dispense (normal)[1]
Titrant
Concentration
Volume
Dosing rate

Auxiliary reagent
Rinse cycles
Vol. per cycle
Position
Drain
Drain pump
010 Conditioning
Typ
Interval
Position
Time [s]
Speed [%]

006 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dt
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Combined termination
criteria
007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Fix
1
Conditioning
300 s
30%

Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

ASTM D4739 solvent


1
60.0 mL
60.0 mL/min

35%
60 s

HCl in 2-Propanol
0.1 mol/L
pH
DG113-SC
mV

ASTM D4739
3
20 mL
Actual position
Yes
SP250

011 Record

005 Stir
Speed
Duration

No

009 Rinse

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

Content
mg KOH/g
R2=(QE(H[Buffer pH3]B[ASTM D4739])*C/m
C=M/z
M[Potassium hydroxide]
z[Potassium hydroxide]
2
No

012 End of sample

No
013 Park
35%

Titration Stand
Position

Rondo60/1A
Rinse beaker

Volume
0.5 mL
30 s
User
Incremental
0.1 mL
Fixed time
90.0 s
Standard
5 mV/mL
Positive
0
No
3.0 mL
No
No
No
No

Content
mg KOH/g
R1=(Q-B[ASTM D4739])*C/m
C=M/z
M[Potassium hydroxide]
z[Potassium hydroxide]
2
No
No

87

M429

METTLER TOLEDO

Blank Value of Base Number Solvent According to ASTM D4739-05


Blank value determination of the base number BN solvent by titration with hydrochloric acid and potassium
hydroxide in 2-propanol according to ASTM D4739-05.
Sample

Substance

60 mL solvent ASTM D4739-05

--

Preparation and Procedures


1) Solvent preparation:
ASTM D4739-05 solvent is prepared by mixing 2-propanol,
toluene, chloroform and water in the following ratio:
10 : 10 : 10 : 0.3 (v/v).

--

2) The titer is determined by titration of standardized KOH in


2-propanol solution. The latter is standardized using potassium
hydrogen phthalate (KHP).

HCl in 2-propanol, c(HCl)=0.1 mol/L


KOH in 2-propanol, c(HCl)=0.1 mol/L

3) The acidic and the alkaline aqueous buffers are measured


and stored as auxiliary values H[pH3] (BN) and H[pH10]
(SBN, Strong Base Number). The values are then used in the
parameter "Termination at potential" of the method function
"Titration EQP".

Standard

KOH in 2-propanol 0.1 mol/L / KHP

4) 60 mL ASTM D4739-05 solvent are added using an


additional dosing unit. This step can be performed manually
using a dispenser or a graduated cylinder.

Instruments

Titration Excellence T50/T70/T90


Rondo 60 Sample changer
1 additional dosing unit (20 mL)

Accessories

DV1010 and DV1020 Burettes


Glass beaker ME-101446
XS205 Balance
Olivetti Printer JobJet 210

Chemicals

Titrant

Indication

DG113-SC

Chemistry

--

5) Blank value determinations are determined for every new


batch of solvent by titration with HCl in 2-propanol to pH 3
potential value. The result is stored as blank B[ASTM D4739].
6) For SBN, the solvent is titrated with KOH in 2-propanol to pH
10 buffer potential value and stored as B[ASTM D4739 pH10].

Remarks
This method allows a fully automated procedure using a sample
changer and an additional dosing unit. It can be modified for
manual operation. Select "Manual stand" in the method function
"Titration stand".
1) This application does not replace the ASTM standard.

Calculation

BN blank: Consumption of HCl/ 2Propanol


up to acidic potential value:
R1=QEND, mmol
SBN blank: Consumption of KOH/2-Prop. up
to alkaline potential value:
R1=QEND, mmol

Results

Waste
disposal

Disposal as halogenated organic waste

Author

Claudia Schreiner

2) The base number BN is defined as the consumption of


hydrochloric acid to a specific endpoint to neutralize the alkaline
components of the oil. It is expressed as mg KOH/g sample:
- If an EQP is found between the acidic buffer potential value and
a point 100 mV past this potential, then this will be the BN.
- If no EQP is found in this region, then the result is evaluated a
the potential value of the acidic buffer.
3) Between each sample it is necessary to condition the
electrode under stirring during 300 s in deion. water. The
electrode is subsequently cleaned in a beaker containing
solvent.
Literature:
1) ASTM D4739-05 and 4739-04 Draft , see www.astm.org
2) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

88

Results
All results
Method-ID
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)

M429
ASTM D4739
0.00199
ASTM D4739
0.00186
ASTM D4739
0.00193
ASTM D4739
0.00170
ASTM D4739
0.00195

Method-ID
R1
Samples
Mean
s
srel

M429
ASTM D4739 solvent
5
0.00189
mmol
0.00111
mmol
6.301
%

solvent
mmol
solvent
mmol
solvent
mmol
solvent
mmol
solvent
mmol

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)

Statistics

Table of measured values

Titration curve

89

Method
Method
Author

M429
Blank BN ASTM D4739
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M429
Blank ASTM D4739
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
ASTM D4739 solvent
Fixed volume
60.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Rondo60/TowerA)


Type
Rondo60/TowerA
Titration stand
Rondo60/Tower1A
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

Solvent ASTM D4739


1 mol/L
60.0 mL
60.0 mL/min

005 Stir
Speed
Duration
006 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dt
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
Potential
At slope
After number
of recognized EQPs
Combined termination
criteria
007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

30%
10 s

HCl in 2-Propanol
0.1 mol/L
pH
DG113-SC
mV
No
30%

008 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
009 End of sample
010 Park
Titration Stand
Position

Rondo60/1A
Rinse beaker

Name
Value
Units
Limits

ASTM D4739
B=Mean[R1]
mmol
No

(pH 4)

011 Blank

012 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Mean consumption
mmol
R2=Mean[R1]
C=1
M[None]
z[None]
5
No
No

013 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

None
0 s
Acidic buffer potential value:
User
Dynamic
2.0 mV
0.002 mL
0.05 mL
Fixed time
90.0 s
Standard
10000 mV/mL
Positive
0
No
1.0 mL
Yes
228.6 mV
No
No
No

Consummption
mmol
R1=QEND
C=1
M[None]
z[None]
5
No

228.6 mV

----------------------------------------------

Strong Base Number, SBN


....
Titrant
Titrant
Concentration
....
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
Potential
At slope
Alkaline buffer potential value:

KOH in 2-Propanol
0.1 mol/L

Standard
10000 mV/mL
Negative
0
No
1.0 mL
Yes
- 185.1 mV
No
-185.1 mV

No

90

M430

METTLER TOLEDO

Base Number in Cutting Oil According to ASTM D2896-05


Method for the determination of the base number BN in cutting oil by titration with perchloric acid solution in
non aqueous solvent according to ASTM D2896-05.
Sample

Substance
Chemicals

Cutting oil, 0.5 g

Alkaline components in oil, expressed


as mg KOH/g sample, M=56.1, z=1
60 mL ASTM D2896-05 solvent
(see Preparation and Procedures)

Titrant

Perchloric acid in acetic acid, HClO4


c(HClO4) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Accessories

Titration Excellence T50/T70/T90


1 additional dosing unit (20 mL)

DV1010 and DV1020 Burettes


Glass beaker ME-101446
XS205 Balance
Olivetti Printer JobJet 210

Preparation and Procedures


1) Solvent preparation:
ASTM D2896-05 solvent is prepared by mixing one volume part
of glacial acetic acid with two volume parts of chlorobenzene
(acetic acid:chlorobenzene 1:2 v/v)
2) The titer is determined by titrating potassium
hydrogenphthalate (KHP) as a primary standard: approx. 80
mg are dissolved in deonized water in a titration beaker.
3) A blank value is determined for every new batch of solvent
mixture (see application M431) and stored as blank value
B[ASTM D2896].
4) The appropriate sample size for 60 mL solvent is calculated
accorrding to the following formula:
Sample size (g) = 10/expected BN
5) The sample is titrated with perchloric acid in acetic acid
using an EQP titration method.
6) 60 mL ASTM D2896-05 solvent are added using an
additional dosing unit. It can be performed manually using a
pipette.

Remarks

Indication

DG113-SC with saturated NaClO4 in


acetic acid as electrolyte

1) This application does not replace the ASTM standard.

Chemistry

HClO4 + NaOH = ClO4- + Na+ + H2O

2) The method parameters have been optimised for the sample


used in this application. Thus, it may be necessary to slightly
adapt the method to your specific sample.

NaOH represents the alkaline


components.

Calculation

Base number (mg KOH/g)


R = (Q-B[ASTM D2896])*C/m,
C = 56.1

3) The method can be easily modified for automated operation.


Select the appropriate sample changer in the method function
"Titration stand".
4) The base number is defined as the consumption of perchloric
acid to the first equivalence point for one g of sample in order to
neutralize the alkaline components of the oil. It is expressed as
mg KOH/g sample.
Literature:
1) ASTM D2896-05, see www.astm.org
2) Memory Card Application Package,
"Determination in the Petroleum Industry",
METTLER TOLEDO Application brochure 20, ME-51 725 020.

Results

Waste
disposal

Disposal as halogenated organic waste

Author

Maria-Jos Schmid

91

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M430
Cutting
20.24
Cutting
20.31
Cutting
20.14
Cutting
20.36
Cutting
20.15
Cutting
20.16

Method-ID
R1
Samples
Mean
s
srel

M430
Cutting oil
6
20.23
mg KOH/g
0.09
mg KOH/g
0.458
%

oil
mg
oil
mg
oil
mg
oil
mg
oil
mg
oil
mg

(1/1)
KOH/g
(1/2)
KOH/g
(1/3)
KOH/g
(1/4)
KOH/g
(1/5)
KOH/g
(1/6)
KOH/g

Statistics

-------------------------------------------------------------Results with fixed titrant increments:


Statistics
Method-ID
R1
Samples
Mean
s
srel

Table of measured values

INC / BN oil ASTM 2896


Oil
6
20.372
mg KOH/g
0.166
mg KOH/g
0.814
%

Titration curve

92

Method
Method
Author

M430
Base number ASTM D2896
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M430
Base number ASTM D2896
METTLER TOLEDO
02.08.2006
--None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Cutting oil
Weight
0.1 g
10.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

ASTM 2896 solvent


1
60.0 mL
60.0 mL/min

007 Calculation
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
mg KOH/g
R=(Q-B[ASTM D2896])*C/m
C=56.1
M[None]
z[None]
2
No
No

008 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No
009 End of sample

005 Stir
Speed
Duration
006 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
Potential
Termination tendency
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

50%
120 s

HClO4
0.1 mol/L
pH
DG113-SC
mV
No
40%
Volume
0.5 mL
15 s

----------------------------------------------Additional test: fixed titrant increments / fixed time


Control
Control
Show parameters
Titrant addition
dV
Meas. val. acquisition
dt

Mettler
Yes
Incremental
0.05 mL
Fixed time
7.0 s

User
Dynamic
15 mV
0.01 mL
0.2 mL
Equilibrium controlled
1.0 mV
1 s
3 s
30 s
Standard
200 mV/mL
Positive
0
No
10.0 mL
Yes
850 mV
None
No
Yes
1
No

93

M431

METTLER TOLEDO

Blank Value of Base Number Solvent According to ASTM D2896-05


Method for the determination of the blank value of the base number solvent by titration with perchloric acid
solution in non aqueous solvent according to ASTM D2896-05.
Sample

Substance
Chemicals

60 mL solvent ASTM D2896-05

Alkaline components, expressed as


mmol HClO4 consumption
--

Preparation and Procedures


1) Solvent preparation:
ASTM D12896-05 solvent is a prepared by mixing one volume
part of glacial acetic acid with two volume parts of
chlorobenzene (acetic acid:chlorobenzene 1:2 v/v)
2) 60 mL ASTM D2896-05 solvent are added using an
additional dosing unit. It can be performed manually using a
pipette
3) The sample is titrated with perchloric acid in acetic acid
using an EQP titration method.

Titrant

Perchloric acid in acetic acid, HClO4


c(HClO4) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence T50/T70/T90


1 additional dosing unit (20 mL)

Accessories

DV1010 and DV1020 Burettes


Glass beaker ME-101446
XS205 Balance
Olivetti Printer JobJet 210

4) A blank value is determined for every new batch of solvent


mixture and stored as blank value B[ASTM D2896].

Remarks

Indication

DG113-SC with saturated NaClO4 in


acetic acid as electrolyte

1) This application does not replace the ASTM standard.

Chemistry

HClO4 + NaOH = ClO4- + Na+ + H2O

2) The method can be easily modified for automated operation.


Select the appropriate sample changer in the method function
"Titration stand".

NaOH represents the alkaline


components.

Calculation

Blank value (mmol):

Literature:
1) ASTM D2896-05, see www.astm.org
2) Memory Card Application Package,
"Determination in the Petroleum Industry",
METTLER TOLEDO Application brochure 20, ME-51 725 020.

R = Q, mmol
C=1

Results

Waste
disposal

Disposal as halogenated organic waste

Author

Maria-Jos Schmid

94

Results
All results
Method-ID
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)
Sample
R1 (Consumption)

M431
ASTM D2896 solvent
0.0006
mmol
ASTM D2896 solvent
0.0006
mmol
ASTM D2896 solvent
0.0004
mmol
ASTM D2896 solvent
0.0005
mmol
ASTM D2896 solvent
0.0005
mmol
ASTM D2896 solvent
0.0010
mmol
ASTM D2896 solvent
0.0005
mmol

Method-ID
R1
Samples
Mean
s
srel

M431
Consumption
6
0.0005
mmol (*)
0.0001
mmol (*)
14.570
%

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6) (-)
(1/7)

Statistics

Sample 1/6 deleted

Table of measured values

Titration curve

95

Method
Method
Author

M431
Blank ASTM D2896
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M431
Blank ASTM D2896
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Consumption
mmol
R1=Q
C=1
M[None]
z[None]
4
No
No

008 End of sample


009 Blank

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
ASTM D2896 solvent
Fixed volume
60.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Dispense
Titrant
Concentration
Volume
Dosing rate

ASTM D2896 solvent


1
60.0 mL
60.0 mL/min

005 Stir
Speed
Duration
006 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Show parameters
Titrant addition
dV
Meas. val. acquisition
dt
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
Potential
Termination tendency
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

50%
10 s

Name
Value
Unit
Limits
010 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

ASTM D2896
B=Mean[R1]
mmol
No

Mean consumption
mmol
R2=Mean[R1]
C=1
M[None]
z[None]
4
No
No

011 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

HClO4
0.1 mol/L
pH
DG113-SC
mV
No
35%
None
0 s
Mettler
Yes
Incremental
0.001 mL
Fixed time
7 s
Standard
500 mV/mL
Positive
0
No
2.0 mL
Yes
850 mV
None
No
Yes
1
No

96

M432

METTLER TOLEDO

Chloride Content in Motor Oil


Inorganic chloride content in fresh motor oil is determined by precipitation titration in non aqueous solvent
with silver nitrate. The content is expressed as chloride, Cl-.
Sample

Substance
Chemicals

Motor oil, approx. 0.6 g

Chloride, Cl-,
M = 35.45 g/mol, z = 1
40 mL solvent ASTM D3227-04a
20 mL NaCl in 2-propanol solution
(see remarks)

Titrant

Silver nitrate, AgNO3 , in 2-Propanol


c(AgNO3) = 0.01 mol/L

Standard

NaCl, c(NaCl) = 0.01 M , 5 mL

Instruments

Titration Excellence T50/T70/T90


2 additional dosing units (10 and 20 mL)
Rondolino Sample Changer

Accessories

2 DV1010 and 1 DV1020 Burettes


Glass titration beaker ME-101446
XS205 Balance
Olivetti Printer JobJet 210

Indication

DM141-SC

Chemistry

NaCl + AgNO3 = AgCl + NaNO3

Calculation

R1: Content (ppm)


R1 = (Q-B[Chloride ASTM D3227])*C/m,
C = M*1000/z

Results

Waste
disposal

Filtration. The precipitate (AgCl) has to


be classified as special waste. The
liquid phase has to be disposed as
aqueous waste.

Author

Cosimo De Caro

Preparation and Procedures


1) A sodium chloride standard solution is used for the titer
determination. Since small amounts of salt cannot be weighed
in exactly, it is recommended to prepare an aqueous solution of
NaCl, and then add the standard with a pipette.
2) Before sample determination a blank value titration of the
solvent spiked with a NaCl standard solution (see 4). The result
is taken into account as B[Chloride ASTM D3227].
3) 0.6 g of sample is added into the titration beaker.
4) 20 mL approx. 50 mg/L NaCl standard solution are added to
spike the sample since the chloride content is too low. This step
has been performed using an additional dosing unit. It can be
performed manually using a pipette.
5) Add 40 mL solvent ASTM D3227-04a. This step has been
performed using an additional dosing unit. It can be performed
manually using a pipette.
6) The sample series were analysed using a Rondolino sample
changer. The conditioning time was set to 30 s (Rondolino
settings: 4). In this way, the electrode was condiitoned in the
sample solvent before starting the next titration.

Remarks
1) The method parameters have been developed and optimised
for the above mentioned sample. It may be necessary to slightly
adapt the method to your specific sample.
2) A fully automated analysis procedure is performed by using
two additional burette drives and a sample changer. The method
can be easily modified for manual operation. Select "Manual
stand" in the method function "Titration stand".
3) ASTM D3227-04a alkaline solvent:
Dissolve 1.6 g anhydrous sodium acetate (NaC2H3O2) in 25 mL
of deion. water and pour into 1 L flask. Fill up to the mark with
2-propanol. This solvent allows a good dissolution of the oil.
4) The NaCl standard solution is prepared by dissolving approx.
50 mg NaCl in few mL water, adding it into a 1 L volumetric
flask, and then by filling up with the ASTM D3227 solvent.
5) Sulfides interfere with the analysis. If necessary, they have to
be oxidised to sulfates by adding 10 mL 30% H2O2 previous to
the analysis. In this application, this was not the case.
Literature:
1) METTLER TOLEDO Application brochure 20, ME-51 725 020.
2) ASTM D3227-04a, D4929-04, see www.astm.org

97

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M432
Motor oil (1/1)
675.23 ppm
Motor oil (1/2)
666.66 ppm
Motor oil (1/3)
676.89 ppm
Motor oil (1/4)
681.68 ppm
Motor oil (1/5)
682.10 ppm
Motor oil (1/6)
885.16 ppm

Method-ID
R1
Samples
Mean
s
srel

M432
Content
6
677.95 ppm
6.62
ppm
0.977
%

Statistics

Table of measured values

Titration curve

98

Method
Method
Author

M432
Chloride content in motor oil
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M432
Chloride in motor oil
METTLER TOLEDO
02.08.2006
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
Motor oil
Weight
0.5 g
0.7 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

NaCl standard
0.00009
20.0 mL
60.0 mL/min

008 Calculation R1
Result
Result unit
Formula
D3227])*
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
ppm
R=(Q-B[Chloride ASTM
*C/m
C=M*1000/z
M[Chloride]
z[Chloride]
2
No
No

009 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
010 End of sample

005 Dispense (normal) [2]


Titrant
Concentration
Volume
Dosing rate

ASTM D3227 solvent


1
40.0 mL
60.0 mL/min

006 Stir
Speed
Duration
007 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Potential
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Lower limit 1
Upper limit
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

40%
120 s

AgNO3
0.01 mol/L
mV
DM141-SC
mV
No
40%
Volume
1.5 ml
15 s
Mettler
Incremental
0.1 mL
Equilibrium controlled
1.0 mV
3 s
5 s
15 s
Standard
30 mV/mL
Positive
1
-50 mV
500 mV
No
10.0 mL
No
No
Yes
1
No

99

M433

METTLER TOLEDO

Mercaptan Sulfur Content in Kerosine According to ASTM D3227-04a


The content of (thiol mercaptan) sulfur in kerosine is determined by precipitation titration in non aqueous
solvent using silver nitrate in 2-propanol. The content is expressed as sulfur, S2-.
Sample

30 mL, kerosine

Preparation and Procedures


1) Dissolved oxygen is removed by purging the solvent and the
titrant solutions with nitrogen gas for at least 10 min prior to
use. The solutions must be kept protected from atmosphere.

Substance

Mercaptan sulfur, R-S-,


M = 32.06 g/mol, z = 1

Chemicals

20 mL solvent ASTM D3227-04a


2 mL Ethyl mercaptan standard sol.
(see remarks)

Titrant

Silver nitrate, AgNO3 , in 2-Propanol


c(AgNO3) = 0.01 mol/L

Standard

NaCl, c(NaCl) = 0.01 mol/L , 5 mL

Instruments

Titration Excellence T50/T70/T90


2 additional dosing units (10+20 mL)
Rondolino Sample Changer

Accessories

2 DV1010 and 1 DV1020 Burettes


Glass titration beaker ME-101446
XS205 Balance
Olivetti Printer JobJet 210

Indication

Sensor input: InLab201 glass electrode


Ref. input: Sulfidized Ag850 electr.

Chemistry

R-SH + AgNO3 = R-S-Ag + HNO3

Calculation

R1: Mercaptan content (mg/kg)


R1 = (Q-B[ASTM D 3227])*C/(m*d),
C = M*1000/z

2) Before sample analysis a blank value titration is determined


(result is stored as B[ASTM D 3227]).
3) Reagents addition:
- 20 mL solvent ASTM D3227-04a are added into the beaker.
- 2 mL approx. 360 mg/L ethyl mercaptan standard solution are
added to spike the sample since the content is too low.
These steps have been performed using an additional dosing
unit. They can be performed manually using a pipette.
4) A Rondolino sample changer with a diaphragm pump was
used. The conditioning time was set to 30 s while the rinsing
time was defined to 2 s (Rondolino settings: 7). The electrode is
cleaned with solvent before starting the subsequent sample.
5) For accurate sampling, kerosine was added with a pipette
instead of weighing (volatility). Thus, its density must be taken
into account. The density of flight petrol was measured using a
METTLER TOLEDO DR45 density meter (d = 0.7905 g/cm 3 ,
25C)

Remarks
1) The method parameters have been optimised for the above
mentioned sample. It may be necessary to slightly adapt the
method to your specific sample.
2) A fully automated procedure is performed by using two
additional burette drives and a sample changer. It can be easily
modified for manual operation. Select "Manual stand" in the
method function "Titration stand".
3) ASTM D3227-04a alkaline solvent:
Dissolve 1.6 g anhydrous sodium acetate (NaC2H3O2) in 25 mL
of deion. water and pour into 1 L flask. Fill up to the mark with
2-propanol. This solvent allows a good dissolution of the oil.

B[ASTM D3227]: Blank value of


mercaptan standard solution

4) Sulfidation of the Ag850 electrode:


Place the electrode during 10 minutes in an 2% aqueous
sodium sulfide solution. Subsequently, place it in a 10%
aqueous sodium sulfide solution during 12 h (over night).

Waste
disposal

Filtration. The precipitate has to be


classified as special waste. The liquid
phase has to be disposed as organic
waste.

5) The 0.02 mol/L mercaptan standard is prepared by


dissolving approx. 1.24 g ethyl mercaptan in a 1 L volumetric
flask and filling up with the ASTM D3227 solvent.
Literature:
1) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
2) ASTM D3227-04a, see www.astm.org

Author

Claudia Schreiner

Results

100

Results
Flight petrol 57354
Addition of 2 mL 0.02 mol/L ethyl mercaptan standard solution
Consumption: approx. 2.8 mL
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M433
Kerosine
15.07
mg/kg
Kerosine
14.31
mg/kg
Kerosine
14.28
mg/kg
Kerosine
14.75
mg/kg
Kerosine
13.48
mg/kg

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)

Statistics
Method-ID
M433
R1
Content
Samples
5
Mean
14.34
mg/kg
s
0.60
mg/kg
srel
4.172
%
----------------------------------------------------------------------Without addition of ethyl mercaptan standard solution
Consumption: approx. 1 mL
All results
Method-ID
M433
Sample
Kerosine
R1 (Content)
15.07
mg/kg
...............................
Sample
Kerosine
R1 (Content)
14.33
mg/kg
Sample
Kerosine
R1 (Content)
12.85
mg/kg

(1/1)
(1/8)
(1/9)

Statistics
Method-ID
R1
Samples
Mean
s
srel

Table of measured values

M433
Content
9
14.04
mg/kg
1.23
mg/kg
8.741
%

Titration curve

101

Method
Method
Author

M433
Mercaptan sulfur ASTM D3227
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title

General titration
T50 / T70 / T90
M433
Mercaptan sulfur ASTM D3227

Author
Date/Time
Modified
Modified by
Protect
SOP

METTLER TOLEDO
02.08.2006 15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Kerosine
Fixed volume
30.0 mL
0.7905 g/mL
1.0
25.0C

003 Titration stand (Rondolino TTL)


Type
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

ASTM D3227 solvent


1
20.0 mL
60.0 mL/min

005 Dispense (normal) [2]


Titrant
Concentration
Volume
Dosing rate

Mercaptan Standard
0.019
2.0 mL
60.0 mL/min

006 Stir
Speed
Duration
007 Titration (EQP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stirrer
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Steepest jump

40%
300 s

Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria
008 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

10.0 mL
No
No
Yes
1
No

Content
mg/kg
R1=(Q-B[ASTM D3227])*C/(m*d)
C=M*1000/z
M[Mercaptan sulfur]
z[Mercaptan sulfur]
2
No
No

009 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration functions
dE/dV - V
Last titration functions
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
010 End of sample

AgNO3 in 2-Propanol
0.01 mol/L
mV
InLab201
mV
No
40%
Volume
0.5 ml
10 s
User
Dynamic
8.0
0.05 mL
0.4 mL
Equilibrium controlled
1.0 mV
2 s
10 s
30 s
Standard
200 mV/mL
Negative
0
Steepest jump
1

102

M434

METTLER TOLEDO

Anionic Surfactant Content in Liquid Detergents by Two-Phase Titration


The anionic surfactant content in liquid dish washer as SDS (sodium dodecyl sulfate) is determined by
precipitation titration with Hyamine 1622, a cationic surfactant. The content is determined by colorimetric
two-phase titration with the DP5 Phototrode (automated Epton titration).
Sample

5 mL liquid detergent solution,


approx. 8 g/L

Substance

Sodium dodecyl sulfate, C12H25NaO4S


M = 288.38 g/mol, z = 1

Chemicals

10 mL deionised water
10 mL mixed indicator*
60 mL chloroform
*see Preparation and Procedures

Titrant

Hyamine 1622, C27H42ClNO2


c(Hyamine) = 0.004 mol/L

Standard

SDS, 1 mL 0.01 mol/L aliquot

Instruments

Titration Excellence T50/T70/T90


1 additional dosing unit (20 mL)

Accessories

1 DV1010 and 1 DV1020 Burettes


Two-phase titr. beaker ME-51107655
XS205 Balance
Olivetti Printer JobJet 210

Indication

DP5 Phototrode , 520 nm

Chemistry

Simplified scheme:
C27H42NO2+ + C12H25O4S - =
C27H42NO2-C12H25O4S

Calculation

TM

R1: SDS-Content (%)


R1 = Q*C/m,
C = M/(10*z) ; z = 1

Results

Waste
disposal

Separation of chloroform and final


disposal as halogenated organic
waste. Neutralization of the aqueous
phase.

Author

Cosimo De Caro

Preparation and Procedures


CAUTION:
Chloroform is toxic. Work in a fume hood
1) Add 10 mL of deionised water into the titration beaker.
2) Add 10 mL of mixed indicator solution.
3) Add 60 mL of chloroform. This step was performed wiht an
additional dosing unit. It can be done manually with a pipette.
4) Add 5 mL of an liquid detergent solution.
Liquid detergent solution:
The concentration was chosen to get an approx. titrant
consumption of 5 mL. Its value is stored as auxiliary value
H[SDS] in g/mL.
Preparation: Dissolve ca. 8 g into a 1 L volumetric flask and fill
up with deionised water (here: 8.5856 g liquid detergent,
0.0429 g/5 mL.).
DP5 PhototrodeTM:
After turning on the PhototrodeTM, wait for 15-10 minutes before
starting analysis to achieve a stable light intensity. Check the
transmission signal of the phototrode in deionised water and
set it to 1000 mV by turning the knob on the top of it.
Literature:
Application M606, Titration Applications Brochure 22,
"Surfactant Titration", ME-51 725 015 .

Remarks
1) The method parameters have been developed and optimised
for the sample used in this application. Thus, it may be
necessary to slightly adapt the method to your specific sample.
2) Avoid the formation of air bubbles during the separation time
since they disturb the photometric indication. Thus, select the
appropriate stirring speed.
3) Mixed indicator solution:
3.1. Dimidium bromide: Weigh accurately 0.2 g into a 100 mL
volumetric flask and dissolve the dye with 10% (v/v) ethanol. If
necessary, warm gently to achieve complete dissolution. After
cooling, fill with 10% (v/v) ethanol to the mark. CAUTION:
Dimidium bromide is toxic. Work under appropriate conditions
e.g. wear gloves.
3.2. Disulfine Blue VN: Weigh accurately 0.1 g into a
second100 mL volumetric flask and dissolve the dye with 10%
(v/v) ethanol. If necessary, warm gently. After cooling, fill with
10% (v/v) ethanol to the mark.
3.3. MIxed indicator solution: 10 dimidium bromide solution,
10 mL disulfine blue solution and 10 mL 2.5 mol/L (245 g/L)
sulfuric acid solution (be careful: the solution can become hot)
are poured into a 250 mL volumetric flask. The solution is
diluted to the mark with deionised water. Store in the dark.

103

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M434
Liquid
13.59
Liquid
13.53
Liquid
13.45
Liquid
13.59
Liquid
13.60
Liquid
13.57

Method-ID
R1
Samples
Mean
s
srel

M434
Content
6
13.56
%
0.06
%
0.422
%

detergent
%
detergent
%
detergent
%
detergent
%
detergent
%
detergent
%

solution

(1/1)

solution

(1/2)

solution

(1/3)

solution

(1/4)

solution

(1/5)

solution

(1/6)

Statistics

Table of measured values

Titration curve

104

Method
Method
Author

M434
SDS content (2-phase)
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M434
SDS content (2-phase)
METTLER TOLEDO
02.08.2006
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature

1
Liquid detergent solution
Fixed volume
5.0 mL
1.0 g/mL
1.0
25.0C

003 Titration stand (Manual stand)


Type
Manual Stand
Titration stand
Manual Stand 1
004 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate

Chloroform
1
60 mL
60.0 mL/min

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/(m*H[SDS])
C=M/(10*z)
M[Sodium dodecylsulfate]
z[Sodium dodecylsulfate]
2
No
No

008 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No
End of sample

005 Stir
Speed
Duration
006 Titration (2-phase) [1]
Titrant
Titrant
Concentration
Sensor Parameters
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
Mix time
Separation time
Stir speed (S. time)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Lower limit 1
Upper limit 1
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Combined termination
criteria

60 %
60 s

Hyamine 1622
0.004 mol/L
Phototrode
DP5
mV
No
60%
Volume
2.5 mL
5 s
User
Incremental
0.15 mL
Fixed time
5 s
40 s
20 %
Standard
8 mV/mL
Positive
1
120 mV
500 mV
No
6.0 mL
No
No
No
No

105

M435

METTLER TOLEDO

Titer Determination of NaOH 0.1mol/L


Method for the standardization of 0.1 mol/L sodium hydroxide. The method can be used with minor changes
for the titer determination of most aqueous strong base titrants.
Sample

Primary standard
Potassium hydrogen phthalate
70 - 120 mg

Substance

Potassium hydrogen phthalate, KHP


M = 204.23; z = 1

Chemicals

50 mL deionized water

Preparation and Procedures


1) The DG111-SC electrode is calibrated before analysis using
METTLER TOLEDO buffers pH 4.01, 7.00 and 9.21.
2) Approximately 0.1 g potassium hydrogen phthalate are
added to the titration beaker.
3) 50 mL deionized water are added to the beaker.
4) The titration method is started.

Titrant

Sodium hydroxide, NaOH


c(NaOH) = 0.1 mol/L

Standard

--

Instruments

Titration Excellence T50/T70/T90


1 DV1010 Burette
XS205 Balance

Accessories

Glass titration beaker ME-101446


Drying tube ME-23961
Drying tube holder ME-23915
Olivetti Printer JobJet 210

Remarks

Indication

DG111-SC

1) Glass beakers are recommended in order to avoid any


interference during weighing due to electrostatic effects.

Chemistry

NaOH + HOOC-C6H4-COOK =
Na+ + K+ + -OOC-C6H4-COO-

2) To keep the titer of the sodium hydroxide constant, it is


important to avoid intake CO2 from the air which leads to the
formation of carbonate. This is achieved by using a suitable
adsorbing medium i.e. sodium hydroxide on support. It is filled
in a drying tube (cup ME-23961, holder ME-23915) on top of
the burette holder.

Calculation

Titer :

3) The mean value of the titer is automatically stored as part of


the setup data by the function TITER.

R1=m/(VEQ*c*C)
C=M/(10*p*z)

Results

Waste
disposal

Neutralization before final disposal as


aqueous solution.

Author

Thomas Hitz

106

Results
All results
Method-ID
Sample
R1 (Titer)
Sample
R1 (Titer)
Sample
R1 (Titer)
Sample
R1 (Titer)

M435
Potassium
0.99714
Potassium
0.99372
Potassium
0.99240
Potassium
0.99240

Method-ID
R1
Samples
Mean
s
srel

M435
Potassium hydrogen phthalate
4
0.99392
0.00224
0.225
%

hydrogen phthalate

(1/1)

hydrogen phthalate

(1/2)

hydrogen phthalate

(1/3)

hydrogen phthalate

(1/4)

Statistics

Table of measured values

Titration curve

107

Method
Method
Author

M435
Titer 0.1 mol/L NaOH
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample (Titer)
Titrant
Concentration
Standard
Type of standard
Entry type
Lower limit
Lower limit
Correction factor
Temperature
Entry

General titration
T50 / T70 / T90
M435
Titer 0.1 mol/L NaOH
METTLER TOLEDO
02.08.2006
15:00:00
--No
None

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Titer
-R1=m/(VEQ*c*C)
C=M/(10*p*z)
M[Potassium hydrogen phthalate ]
z[Potassium hydrogen phthalate ]
5
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
Last titration function
log dE/dV - V
No
d2E/dV2 - V
No
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No

NaOH
0.1 mol/L
Potassium hydrogen phthalate
Solid
Weight
0.08 g
0.12 g
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration

35 %
60 s

008 End of sample


009 Titer

005 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Wait time
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

Titrant
Concentration
Titer=
Result limits

NaOH
0.1 mol/L
pH
DG111-SC
pH
No
35%
None
0 s
User
Dynamic
12.0 mV
0.002 mL
0.5 mL
Equilibrium controlled
1.0 mV
1 s
5 s
30 s

010 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

NaOH
0.1 mol/L
Mean[R1]
No

Mean Titer
-R2=Mean[R1]
C=1
M[Potassium hydrogen phthalate ]
z[Potassium hydrogen phthalate ]
5
No
Yes

011 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data

Yes
No
No
No
No
No

Standard
5 pH/mL
Positive
0
No
10.0 mL
No
No
Yes
1
No

108

M436

METTLER TOLEDO

Calibration of a pH Electrode
A general purpose pH sensor adjustment (calibration) method.

Sample

Substance
Chemicals

60 mL METTLER TOLEDO Buffers


pH 4.01 / pH 7.00 / pH 9.21

--

--

Preparation and Procedures


1) Three titration beakers are filled with 60 mL of each pH
buffers solutions i.e. pH 4.01, 7.00 and 9.21 .
The pH buffer solutions are defined as a pH buffer list "METTLER
TOLEDO (Ref. 25C) pH".
2) Connect the first beaker to the titration stand and start the
method.
3) After measurement of each pH buffer solution the electrode is
cleaned with deionized water before starting the next sample.

Titrant

--

Standard

--

Instruments

Titration Excellence T50/T70/T90

Accessories

Titration beaker ME-101974

Remarks
Indication

DG111-SC

Chemistry

--

Calculation

R1=E ; mV
Potential measurement of the buffer
solutions

1) The calibration data are automatically stored in the setup


data of the titrator. They are assigned to the sensor used in the
method and are only valid for this sensor.
2) The reference data (temperature table) of the METTLER
TOLEDO buffers are stored into the titrator. These buffers can be
selected from the menu and stored in a buffer list, if frequent use
is requested.
3) If the sensor is used at a different temperature at a later time,
the titrator corrects the slope of the sensor according to the
Nernst equation by manual entry or temperature measurement
with a T-sensor.
4) More details can be found in "Fundamentals of
Titration"(ME-704153) and in the T50/T70/t90 operating
instructions.

Results

Waste
disposal

Neutralization before final disposal

Author

Madeleine Biber

109

Results
All results
Method
R1
R1
R1

M436
(Potential)
(Potential)
(Potential)

174.5
0.0
-129.5

mV
mV
mV

(1/1)
(1/2)
(1/3)

pH 4.01
pH 7.00
pH 9.21

Calibration
Sensor
Buffer list

DG111-SC
METTLER TOLEDO (Ref. 25C) pH

Calibration temperature
Number of segments

25.0C
1

Slope (TCalib)
Zero point

-58.80 mV/pH
7.027 pH

Table of measured values

Titration curve

110

Method
Method
Author

M436
Calibration DG111-SC
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample (Calib)
Sensor type
Sensor
Unit
Automatic buffer
recognition
pH buffer list
Calibration
Buffer 1
Buffer 2
Buffer 3
Temperature

General titration
T50 / T70 / T90
M436
Calibration DG111-SC
METTLER TOLEDO
02.08.2006 15:00:00
--No
None

pH
DG111-SC
pH
No
METTLER TOLEDO (Ref. 25C)pH
Linear
4.01
7.00
9.21
25.0C

003 Titration stand (Manual Stand)


Type
Manual stand
Titration stand
Manual Stand 1
004 Stir
Speed
Duration
005 Measure (normal)[1]
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Acquisition of measured values
Acquisition
dE
dt
t(min)
t(max)
Mean value
006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

30 %
60 s

pH
DG111-SC
mV
No
30 %
Equilibrium controlled
0.5 mV
1 s
3 s
30 s
No

Potential
mV
R1=E
C=1
M[None]
z[None]
2
No
No

007 End of sample


008 Calibration
Sensor
Limits

DG111-SC
No

009 Record
Results
Raw results
Resource data
Calibration curve
Method
Series data
Condition

Yes
Yes
No
Yes
No
No
No

111

M437

METTLER TOLEDO

Hydrochloric Acid Content by Conductometric Titration


The hydrochloric acid content is determined by neutralization titration with sodium hydroxide as a titrant. The
conductivity of the titration is monitored by an InLab717 conductometric sensor.
Sample

0.4% hydrochloric acid,


approx. 3-10 g

Substance

Hydrochloric acid, HCl


M=36.46 g/mol, z=1

Chemicals

50 mL deionized water

Preparation and Procedures


1) Install the InLab717 conductometric sensor by connecting it
to the conductivity board (CB).
2) Perform a titer determination using potassium hydrogen
phthalate (KHP) as a primary standard: 70-120 mg KHP are
dissolved into 50 mL deionized water in a titration beaker.
3) Sample titration:
Add 3-10 g hydrochloric acid solution into the titration beaker
and dilute it with 50 mL deionized water.
4) The sample is titrated with 0.1 mol/L NaOH solution.

Titrant

Sodium hydroxide, NaOH


c(NaOH) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, KHP, 70-120 mg

Instruments

Titration Excellence T50/T70/T90


1 Conductivity Board ME-51109840

Accessories

DV1010 Burette
Titration beakers ME-101974
XS205 Balance
Olivetti Printer JobJet 210

Indication

InLab717

Chemistry

HCl + NaOH = NaCl + H2O

Calculation

Content (%) :

5) The sensor is rinsed with deionized water after each titration.

Remarks
1) The method parameters have been optimised for the above
mentioned sample. It may be necessary to slightly adapt the
method to your specific sample.

R1 = Q*C/m
C=M/(z*10)

Results

Waste
disposal

Neutralize before final disposal as


aqueous solution.

Author

Albert Aichert

112

Results
All results
Method-ID
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)
Sample
R1 (Content)

M437
HCl solution
0.364
%
HCl solution
0.362
%
HCl solution
0.364
%
HCl solution
0.364
%
HCl solution
0.362
%
HCl solution
0.363
%

Method-ID
R1
Samples
Mean
s
srel

M437
Content
6
0.363
0.001
0.235

(1/1)
(1/2)
(1/3)
(1/4)
(1/5)
(1/6)

Statistics

Table of measured values

%
%
%

Titration curve

113

Method
Method
Author

M437
HCl content conductometric
METTLER TOLEDO

02.08.2006

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP

General titration
T50 / T70 / T90
M437
HCl content conductometric
METTLER TOLEDO
02.08.2006
15:00:00
--No
None

002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

1
HCl solution
Weight
3.0 g
10.0 g
1 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Manual stand)


Type
Manual stand
Titration stand
Manual stand 1
004 Stir
Speed
Duration

30 %
5 s

006 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Add. statistics
functionalities

Content
%
R1=Q*C/m
C=M/(10*z)
M[Hydrochloric acid]
z[Hydrochloric acid]
3
No
No

007 Record
Results
Per series
Raw results
Per series
Table of measured values Last titration function
Sample data
Per series
Resource data
No
E - V
Last titration function
dE/dV - V
No
log dE/dV - V
No
d2E/dV2 - V
Last titration function
E - t
No
V - t
No
dV/dt - t
No
T - t
No
E - V & dE/dV - V
No
V - t & dV/dt - t
No
Calibration curve
No
Method
No
Series data
No
Condition
No
008 End of sample

005 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Predispense
Mode
Volume
Wait time
Control
Control
Titrant addition
dV
Meas. val. acquisition
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

NaOH
0.1 mol/L
Conductivity
InLab717
S
No
30%
Volume
3 mL
10 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 S
2 s
3 s
30 s
Segmented
500 S/mL2
0
No
10.0 mL
No
No
Yes
1
No

114

METTLER TOLEDO

METHOD TEMPLATES

Method template EQP


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

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Calculation R2
Calculation R3
Record
End of sample

Method template EP
Nr.
1
2
3
4
5
6
7
8
9
10

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Calculation R2
Calculation R3
Record
End of sample

Method template Stating


Nr.
1
2
3
4
5
6
7
8
9
10
11
12

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Stating [1]
Calculation R1
Calculation R2
Calculation R3
Calculation R4
Calculation R5
Record
End of sample

115

METTLER TOLEDO
Method template Measure
Nr.
1
2
3
4
5
6
11
12

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Calculation R1
Record
End of sample

Method template 2-phase


Nr.
1
2
3
4
5
6
7
8
11
12

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (2-phase) [1]
Calculation R1
Calculation R2
Calculation R3
Record
End of sample

Method template Learn-EQP


Nr.
1
2
3
4
5
6
7
8
11
12

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (Learn-EQP) [1]
Calculation R1
Calculation R2
Calculation R3
Record
End of sample

116

METTLER TOLEDO
Method template Titer with EQP
Nr.
1
2
3
4
5
6
7
8
9
10
11

Method Function
Title
Sample (Titer)
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Record
End of sample
Titer
Calculation R2
Record

Method template Titer with EP


Nr.
1
2
3
4
5
6
7
8
9
10
11

Method Function
Title
Sample (Titer)
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Record
End of sample
Titer
Calculation R2
Record

Method template Calibration


Nr.
1
2
3
4
5
6
7
8
9

Method Function
Title
Sample (Calib)
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Record
End of sample
Calibration
Record

117

METTLER TOLEDO
Method template Calibration segmented
Nr.
1
2
3
4
5
6
7
8
9

Method Function
Title
Sample (Calib)
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Record
End of sample
Calibration
Record

Method template Blank with EQP


Nr.
1
2
3
4
5
6
7
8
9
10
11

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Record
End of sample
Blank
Calculation R2
Record

Method template Blank with EP


Nr.
1
2
3
4
5
6
7
8
9
10
11

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Record
End of sample
Blank
Calculation R2
Record

118

METTLER TOLEDO
Method template EP / EQP
Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Stir
Titration (EQP) [2]
Calculation R2
Calculation R3
Calculation R4
Record
End of sample

Method template EQP / EQP


Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Calculation R2
Calculation R3
Stir
Titration (EQP) [2]
Calculation R4
Calculation R5
Calculation R6
Record
End of sample

119

METTLER TOLEDO
Method template EP / EP
Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

Method Function
Title
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Calculation R2
Calculation R3
Stir
Titration (EP) [2]
Calculation R4
Calculation R5
Calculation R6
Record
End of sample

Method template Titer with EQP & EQP


Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Method Function
Title
Sample (Titer)
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Record
End of sample
Titer
Calculation R2
Record
Sample
Titration stand (Manual stand)
Stir
Titration (EQP) [2]
Calculation R3
Calculation R4
Calculation R5
Record
End of sample

120

METTLER TOLEDO
Method template Titer with EP & EP
Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Method Function
Title
Sample (Titer)
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Record
End of sample
Titer
Calculation R2
Record
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [2]
Calculation R3
Calculation R4
Calculation R5
Record
End of sample

Method template Calibration & EQP


Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18

Method Function
Title
Sample (Calib)
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Record
End of sample
Calibration
Record
Sample
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Calculation R2
Calculation R3
Record
End of sample

121

METTLER TOLEDO
Method template Calibration & EP
Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18

Method Function
Title
Sample (Calib)
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Record
End of sample
Calibration
Record
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Calculation R2
Calculation R3
Record
End of sample

122

METTLER TOLEDO
Method template Calibration & Titer with EQP & EQP
Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28

Method Function
Title
Sample (Calib)
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Record
End of sample
Calibration
Record
Sample (Titer)
Titration stand (Manual stand)
Stir
Titration (EQP) [1]
Calculation R1
Record
End of sample
Titer
Calculation R2
Record
Sample
Titration stand (Manual stand)
Stir
Titration (EQP) [2]
Calculation R3
Calculation R4
Calculation R5
Record
End of sample

123

METTLER TOLEDO
Method template Calibration & Titer with EP & EP
Nr.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28

Method Function
Title
Sample (Calib)
Titration stand (Manual stand)
Stir
Measure (normal) [1]
Record
End of sample
Calibration
Record
Sample (Titer)
Titration stand (Manual stand)
Stir
Titration (EP) [1]
Calculation R1
Record
End of sample
Titer
Calculation R2
Record
Sample
Titration stand (Manual stand)
Stir
Titration (EP) [2]
Calculation R3
Calculation R4
Calculation R5
Record
End of sample

124

METTLER TOLEDO

APPLICATION MODES

Sensor type pH
Units pH and mV
Application mode Acid / base
Control
Mode
Show parameters
Titrant addition
dE(set value) [mV]
dV(min) [mL]
dV(max) [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious

Normal
Acid / base
Yes
Dynamic
10.0
12.0
0.002
0.002
0.2
0.5
Equilibrium controlled
0.5
0.5
2
1
3
3
30
30

Fast

18.0
0.002
0.75
1.0
1
2
20

Application mode Acid / base (non aq.)


Control
Mode
Show parameters
Titrant addition
dE(set value) [mV]
dV(min) [mL]
dV(max) [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious
Normal
Acid / base (non aq.)
Yes
Dynamic
10.0
12.0
0.05
0.01
0.5
0.3
Equilibrium controlled
1.0
1.0
3
2
5
2
30
15

Fast

12.0
0.05
0.5
1.0
1
2
10

125

METTLER TOLEDO
Sensor type mV
Unit mV
Application mode Precipitation
Control
Mode
Show parameters
Titrant addition
dE(set value) [mV]
dV(min) [mL]
dV(max) [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious

Normal
Precipitation
Yes
Dynamic
5.0
9.0
0.004
0.008
0.2
0.4
Equilibrium controlled
0.5
0.5
2
1
3
3
30
30

Fast

12.0
0.01
0.5
1.0
1
3
20

Application mode Precipitation (non aq.)


Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious
Normal
Precipitation (non aq.)
Yes
Incremental
0.075
0.1
Equilibrium controlled
1.0
1.0
5
3
5
5
20
15

Fast

Cautious

Fast

0.15
1.0
1
3
10

Application mode Redox


Control
Mode
Show parameters
Titrant addition
dE(set value) [mV]
dV(min) [mL]
dV(max) [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Normal
Redox
Yes
Dynamic
6.0
8.0
0.005
0.02
0.1
0.2
Equilibrium controlled
0.5
1
2
2
5
3
15
10

18.0
0.03
0.3
5.0
1
1
10

126

METTLER TOLEDO
Sensor type ISE
Units mV, ppm, pX, pM
Application mode Precipitation
Control
Mode
Show parameters
Titrant addition
dE(set value) [mV]
dV(min) [mL]
dV(max) [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious

Normal
Precipitation
Yes
Dynamic
8.0
8.0
0.005
0.02
0.15
0.2
Equilibrium controlled
0.5
1.0
2
2
8
5
45
30

Fast

8.0
0.05
0.5
1.0
1
4
15

Sensor type Phototrode


Units mV, %T, A
Application mode Precipitation
Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious

0.05
0.5
1
6
30

Normal
Precipitation
Yes
Incremental
0.1
Equilibrium controlled
1.0
1
5
15

Fast

Normal
Complexation
Yes
Incremental
0.01
Equilibrium controlled
2.0
1
3
20

Fast

0.15
3.0
1
3
6

Application mode Complexation


Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious

0.01
0.5
2
5
40

0.04
8.0
1
1
15

127

METTLER TOLEDO
Sensor type Polarized
Unit mV
Application mode Redox
Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [mV]
dt [s]
t(min) [s]
t(max) [s]

Cautious

0.04
1.0
1
3
30

Normal
Redox
Yes
Incremental
0.05
Equilibrium controlled
2.0
1
2
30

Fast

Normal
Redox
Yes
Incremental
0.1
Equilibrium controlled
0.3
2
5
30

Fast

0.08
2.0
1
2
20

Sensor type Polarized


Unit A
Application mode Redox
Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [uA]
dt [s]
t(min) [s]
t(max) [s]

Cautious

0.1
0.1
2
10
30

0.2
0.5
1
3
15

128

METTLER TOLEDO
Sensor type Temperature
Units oC, K, oF
Application mode Acid / base
Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dT [oC] / [K] / [oF]
dt [s]
t(min) [s]
t(max) [s]

Cautious

Normal
Acid / base
Yes
Incremental
0.1
0.15
Equilibrium controlled
0.5 / 0.5 / 1.0
1.0 / 1.0 / 2.0
1
1
6
3
30
20

Fast

0.2
2.0 / 2.0 / 4.0
1
2
10

Sensor type Conductivity


Units mS, mS/cm, S, S/cm
Application mode Acid / base
Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [S] bzw. [S/cm]
dE [mS] bzw. [mS/cm]
dt [s]
t(min) [s]
t(max) [s]

Cautious

0.05
1.0
0.01
1
3
30

Normal
Acid / base
Yes
Incremental
0.1
Equilibrium controlled
1.0
0.01
1
3
30

Fast

Normal
Precipitation
Yes
Incremental
0.1
Equilibrium controlled
1.0
0.01
1
3
30

Fast

0.2
3.0
0.01
1
2
20

Application mode Precipitation


Control
Mode
Show parameters
Titrant addition
dV [mL]
Meas. val. acquisition
dE [S] bzw. [S/cm]
dE [mS] bzw. [mS/cm]
dt [s]
t(min) [s]
t(max) [s]

Cautious

0.05
0.2
0.01
1
3
30

0.2
3.0
0.01
1
2
10

129

The methods in this brochure represent selected, possible application examples.


These have been tested with all possible care with the analytical instruments
mentioned in the brochure. The experiments were conducted and the resulting
data evaluated based on our current state of knowledge.
However, the applications do not absolve you from personally testing their
suitability for your intended methods, instruments and purposes. As the use and
transfer of an application example are beyond our control, we cannot accept
responsibility therefore.
When chemicals and solvents are used, the general safety rules and the
directions of the manufacturer must be observed.

Application Brochure 34
Selected METTLER TOLEDO Methods
for Titration Excellence Line
This application brochure is the first to cover the Titration Excellence
instruments T50, T70 and T90. It describes the unique possibilities these
titrators offer in order to find the optimal method for your purposes.
How easily methods can be created and edited is briefly described in the
introduction chapter. The concept of ready-to-use METTLER TOLEDO methods is explained in the following. Further features that support efficient
method development such as method templates and application modes
are described in addition.
All METTLER TOLEDO methods (including procedures, literature references
and results) which are available in every model are shown in detail. Furthermore, the structure of all pre-programmed method templates is listed
and the parameters of all available application modes are specified.
Enjoy an easy and efficient method development in all models of the
Titration Excellence line.

T50A Terminal

T70 with Terminal and two


additional dosing units

www.mt.com
For more information

Mettler-Toledo AG, Analytical


Sonnenbergstrasse 74
CH-8606 Schwerzenbach, Switzerland
Tel. +41-44 806 77 11
Fax +41-44 806 73 50

Subject to technical changes.


11/2006 Mettler-Toledo AG
Printed in Switzerland, ME-51725066A
Markt Support AnaChem

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