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Method Validation: Potentiometric Surfactant Titration

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 Method Validation:
Titration Application Note
Potentiometric Surfactant Titration

The quality of products depends on the measurements, determinations and analyzes performed
in quality control. By validating the analytical methods, an important step is taken in achieving
this goal. Validation is a requisite of any regulated environment and the foundation of quality
in the laboratory. A well-defined and correctly documented validation process serves as
evidence for the regulatory agencies that the chemical analysis is suitable for its intended use.
As an example, the complete method validation procedure is illustrated for the potentiometric
two-phase titration of surfactants using surfactant sensitive electrodes.
 Introduction
Motivation
The goal of all titrations is to get accurate and precise
Titration Application Note
results to ensure reliable analytical data for q­ uality
monitoring in the production process of the most
­different products such as pharmaceuticals products.
Reliable analytical information is crucial to achieve
high quality products.
The validation of an analytical method represents a
key step in this direction i.e. it determines if the devel-
oped method fulfills the requirements for the specific
analytical application. Method validation is required
by most regulations and standards such as the United
States Pharmacopoeia (USP) and the International
Council on Harmonization (ICH).
Various parameters have to be considered when
­validating analytical methods, namely accuracy,
­precision, specificity, linearity, limit of detection, limit
of quantitation, range and robustness [1, 2]. Both
the USP and ICH guidelines are universal and apply
to any analytical procedure and technique used in
a ­regulated environment.
Figure 1: Setup.
This application note provides a detailed explanation
on method validation in titration [3]. In particular, the
validation parameters are investigate for the anionic
surfactant content determination by potentiometric
two-phase titration [4–6].
Surfactant content determination
Anionic surfactants are present in e.g. personal hygiene
and cosmetic products, as well as in pharmaceuticals.
These products mainly consist of complex formulations,
and the surfactant content is generally determined using
sophisticated techniques such as chromatography or
NIR spectroscopy.
However, such techniques are time consuming, may
require a long sample preparation and calibration of the
instruments, and should be performed by well-trained
and skilled operators.
Titration analysis with surfactant sensitive electrodes
(SSEs) represents a valuable alternative to these
­analytical techniques since it is less expensive, easier
to perform and it does not require a high degree of
knowledge from the operators.
METTLER TOLEDO Titration Application Note 2
 Sample Preparation
and Procedures
Titration Application Note
Sample handling
• Place the empty PP titration beakers on the InMotion
sample rack.
• Place one beaker with deionized water in the con-
ditioning beaker position (pos. 18) to condition the
sensors after each titration, and to park them at the
end of the sample series.
• The sample solution is dispensed with a burette
when the method is started.
pH electrode calibration
• Calibrate the DGi111-SC pH electrode with buffers
pH 4.01, 7.00 and 9.21.
Content determination
• The surfactant content is determined automatically
by potentiometric two-phase titration [4, 5] of so-
dium dodecyl sulfate (SDS) solution with Hyamine®
1622 (Benzethonium chloride) as titrant in a mixed
two-phase system with the DS800-TwoPhase SSE.
• Titration analysis:
1. 40 mL water is automatically added by means
of the PowerShower rinsing unit.
2. The pH value is adjusted to pH = 3 with 0.1 M
hydrochloric acid (EP titration).
3. 20 mL MIBK:EtOH 1:1 v/v solvent is added by
a burette.
4. Stir at a high speed (80%) to get a homogeneous
emulsion.
5. The sample is titrated with Hyamine®.
Chemistry
Precipitation reaction of the anionic surfactant SDS
with the cationic surfactant Hyamine® 1622:
SDS− + Hyamine+ → SDS-Hyamine (↓)
The SDS-Hyamine complex formed during t­itration
is extracted in the organic phase consisting of
MIBK:Ethanol (Two-phase titration) [4–6].
Solutions
Titrant
Hyamine® 1622 (Benzethonium chloride),
C27H42ClNO2
c(Hyamine) = 0.004 mol/L
Standard
SDS (Sodium dodecyl sulfate),
C12H25NaO4S,
c(SDS) = 0.004 mol/L
Chemicals
Methyl isobutyl ketone (MIBK)
Ethanol (EtOH), Buffer pH 4, 7 and 9.21
Hydrochloric acid, HCl, c(HCl) = 0.1 mol/L
Solvent mixture for two-phase titration
Methyl isobutyl ketone:Ethanol, MIBK:EtOH 1:1 v/v
To extract the complex SDS-Hyamine in the organic
phase, the MIBK:EtOH organic mixture is added to
the sample forming two liquid phases separated by
a clear boundary.
Substance
SDS, M = 288.38 g/mol, z = 1
Instruments and Accessories
• 1 × Titration Excellence T9 (30252676)
(­other ­titrators: T5, T7)
• 1 × Autotitration Kit (51109221)
• 4 × Burette DV1020 20 mL (51107502)
• 3 × additional DU Dosing Unit (51109030)
• 3 × Dispensing Tube InMotion 1.35 m w/tip
(51108070)
• 1 × Autosampler InMotion Flex 100 mL (30094120)
• 1 × DGi111-SC pH combined electrode (51109500)
• 1 × DS800-TwoPhase surfactant electrode
(51109540)
• 1 × InLab Reference half-cell (51343190)
• 1 × NS14.5/15-12 PE conical sensor adapter
(51340024)
• 1 × additional SC-LEMO cable 160 cm (51108034)
• 1 × 4 mm banana reference cable for InLab
Reference half-cell (30281922)
• PP titration beakers 100 mL, 1400 pcs (00101974)
• Analytical balance e.g. XPR204 (30355419)
• LabX software
METTLER TOLEDO Titration Application Note 3
 Validation of a Titration Method
Overview
Titration Application Note

Validation parameter Definition

Accuracy Closeness of agreement between the true value and the value found.

Precision Closeness of agreement among a series of measurements obtained from multiple

sampling of the same homogeneous sample:
• Repeatability:
Precision under identical operating conditions over a short time interval.
• Intermediate precision:
Variations in laboratory e.g. different days or operators, or equipment.
• Reproducibility:
Precision among different laboratories involved in collaborative studies.

Specificity Ability to measure unequivocally the analyte in the presence of components, which
(Selectivity) may be expected to be present in the sample. It is demonstrated by the ability to
discriminate between other compounds in the sample or by comparison to reference
substances. The term “selectivity” is also used for the same meaning.
Interferences that may be caused by the sample matrix should also be evaluated, e.g.
other acids for acid base titration, or similar ions when using ion selective sensor, etc.
The absence of matrix interferences for a given method should be demonstrated by the
analysis of several independent sources of the control matrix.

Linearity and Linearity is the ability of the analytical method to obtain test results that are directly
systematic error proportional to the analyte concentration within a given range.
Systematic errors of a titration are for example disturbing influences due to the method
itself or to solvent blank values.

Limit of detection LOD The limit of detection (LOD) is defined as the lowest concentration of analyte in the
sample that can be detected but not necessarily quantified as an exact value.

Limit of quantitation Limit of quantitation (LOQ) is defined as the minimum concentration of the analyte
LOQ in the sample that produces quantitative measurements with acceptable precision
and accuracy.

Range Interval between upper and lower concentration of the analyte in the sample for
which it has been demonstrated that the analytical procedure has a suitable level
of precision, accuracy and linearity.

Robustness Robustness describes whether a titration method is sensitive to small, but deliberate
variations in procedural parameters listed in the documentation such as pH, sample
size, cleaning and conditioning procedures of the sensor, ambient conditions, etc.
Robustness provides an indication of the method’s suitability and reliability during
normal use.

METTLER TOLEDO Titration Application Note 4

 Potentiometric two-phase surfactant titrations with standard solutions:
Selected parameters for method validation

Validation parameter Definition

Titration Application Note

Accuracy Titration of multiple series of standard or samples with known concentration:

• Sample number: at least 6
• Sample size: random
• Titrant consumption: 20–90% of burette volume, no burette refilling
Accuracy: Difference between the mean value of a series and the true value.

Precision • Repeatability:
- Multiple series of a sample are titrated.
- The sample size is varied for a titrant consumption of 20–90% burette vol.
- The relative standard deviation (srel) is calculated for each series.
- The srel-value expresses the repeatability of the method.
• Intermediate precision:
- Multiple series are titrated e.g. on different days.
- Sample size variation for a consumption of 20–90% burette vol.
- The relative standard deviation (srel) is calculated.
- The srel-value expresses the intermediate precision of the method.
• Reproducibility: Not tested.

Specificity Not relevant: The sample is a standard solution of pure SDS.

Linearity and The linearity is tested in the range of interest by varying the sample size, and it is
systematic error reported as the variance of the slope b of the regression line y = a + b·x.
The range of interest is between 20–90% of the burette volume since the refilling must
be avoided to eliminate the additional uncertainty.
Systematic errors show up as a significant deviation of the y-axis intercept the zero
point coordinates i.e. the value of a is clearly different from zero.
• Verification of the linearity:
- The determination coefficient (R2) of the linear regression (VEQ vs. sample size)
must be greater than the recommended limit, e.g. R2 > 0.995.
- A significant positive (negative) slope b (resp. ΔR/ΔV) of the regression line
(concentration vs. sample size) indicates a non-linearity.

Limit of detection LOD The LOD can be tested by titrating decreasing amounts of sample.
Not relevant – The SDS sample has a constant concentration of 0.004 M.

Limit of quantitation The LOQ is determined by titrating several sample series with decreasing sample size
LOQ are titrated, e.g. 18, 10 and 5 mL 0.004 M SDS, and the srel calculated.
The srel of all sample series are plotted against the amount of analyte (mmol).
The amount of analyte that corresponds to the required precision is the LOQ.

Range In titration, it is recommended that the analyte size should correspond to a titrant
consumption of 20% up to 90% of the burette volume.

Robustness Selected changes in the automated titrator method, e.g. titrant predispensing before
titration, different stirring speed, titrant increments and solvent amounts for dilution.

METTLER TOLEDO Titration Application Note 5

 Potentiometric two-phase surfactant titrations with standard solutions:
Results of method validation

Validation parameter Results

Titration Application Note

Accuracy and 4.500 105.0

Content: 4.006 ± 0.016 mmol/L srel = 0.391%
Repeatability Nom. value: 4.011 mmol/L 104.0
4.400 Accuracy: −0.005 mmol/L (−0.135%)
103.0

Concentration [mmol/L]
102.0
4.300

Recovery [%]
101.0
4.200 100.0

99.0
4.100 Nominal value: 98.0
4.011 mmol/L
97.0
4.000
96.0
3.900 95.0
0 5 10 15 20
Sample size [mL]
Figure 2: Accuracy.

Sample Sample size Concentration Recovery

No. (mL) (mmol/L) (%)
1 5.8 4.005 99.85
2 6.5 3.977 99.16
3 8.3 4.012 100.03
4 10.1 4.010 99.98
5 9.0 4.007 99.90
6 18.0 4.031 100.49
7 15.0 4.023 100.29
8 16.5 4.020 100.22
9 8.0 3.970 98.98
10 12.5 4.014 100.07
11 11.1 4.015 100.09
12 7.5 3.983 99.31
Comments: Average 4.006 99.86
Sample sizes smaller than 5 mL consistently s 0.019 0.47
show a smaller recovery of 98%.
Thus, only sample sizes equal or larger than srel (%) 0.474 0.470
5 mL are used. Nominal value 4.011 100.00
Deviation −0.005 −0.14
Rel. deviation (%) −0.135 −0.140

• The accuracy of the method shows a deviation of 0.135% from the nominal value,
and this is below the recommended limit of 0.3% [3].
• The precision (expressed as repeatability) is with srel = 0.474% slightly higher than
the recommended value of max. 0.3% [3].

METTLER TOLEDO Titration Application Note 6

 Validation parameter Results

Additional Titration of multiple sample series

measurements
n Sample size (mL) Nominal value (mmol/L) SDS Content (mmol/L) srel (%) Comments
Titration Application Note

6 5 4.016 3.981 ± 0.030 0.756

Precision
4.015 ± 0.016 0.411
• Repeatability
4.007 ± 0.038 0.963
4.038 ± 0.016 0.404
4.023 ± 0.017 0.420
4.009 ± 0.006 0.140
3.997 ± 0.013 0.319 3 mL predispensing
6 10 4.016 3.954 ± 0.022 0.559
3.953 ± 0.013 0.331
4.035 ± 0.011 0.279
4.020 ± 0.002 0.060
4.011 ± 0.006 0.155 8 mL predispensing
6 15 4.016 3.947 ± 0.003 0.085
3.955 ± 0.005 0.119
4.027 ± 0.005 0.124
4.029 ± 0.007 0.186
4.018 ± 0.002 0.047 12 mL predispensing
6 18 4.016 3.980 ± 0.018 0.465
4.010 ± 0.060 0.149
4.031 ± 0.004 0.089
4.030 ± 0.003 0.082
4.037 ± 0.004 0.110
4.026 ± 0.006 0.159 15 mL predispensing

• The relative standard deviations srel of multiple sample series vary from 0.060 up
to 0.963%. More than 60% of all srel values are below the recommended value of
0.3% [3], whereas up to 40% are above it.
• The larger deviation can be attributed to the performance of the surfactant sensitive
electrode. This is strongly dependent on appropriate conditioning before titration start,
as well as on conditioning during the analysis itself. In fact, the performance of a
surfactant sensitive electrode is improved with increasing number of titrations.

Precision Titration of series with various sample sizes on different days – Start: Day 1
• Intermediate
precision 4.200
Concentration [mmol/L]

Nominal value:
4.100 4.016 mmol/L
5 mL SDS
10 mL SDS
4.000
15 mL SDS
18 mL SDS
3.900
0 1 2 3 4 5 6 7 8
Day
Figure 3: Intermediate precision (different days).

• The results are closely distributed around the nominal value of 4.016 mmol/L.
• The average content of all measured series is 4.006 ± 0.029 mmol/L i.e. the
accuracy corresponds to −0.010 mmol/L (0.249%).
This is below the recommended value of ± 0.3% [3] for the accuracy.

METTLER TOLEDO Titration Application Note 7

 Validation parameter Results

Linearity and Linearity

systematic error • Determination coefficient R2 = 1.0000:
Titration Application Note

20.0

Titrant consumption VEQ [mL]

15.0

10.0

y = 1.0007 x − 0.1054
5.0 R² = 1.0000

0.0
0.0 5.0 10.0 15.0 20.0
Sample size [mL]
Figure 4 A: Linearity and systematic error I: VEQ vs. sample size.

4.300

4.200
Concentration [mmol/L]

4.100

4.000

3.900 y = 0.0036 x + 3.9673

3.800

3.700
0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0
Sample size [mL]
Figure 4 B: Linearity and systematic error II: concentration vs. sample size.

- The titrant consumption VEQ is linearly increasing with increasing sample size.
- Hence, the method is linear, as given by the coefficient of determination R2 = 1.

• Non-linearity ΔR/ΔV (slope) = 0.0036 mmol/L / L (0.36%):

- The slope over 12 sample series is higher than the recommended value of
max. 0.1% [3]. The slope is mainly caused by the three results between 6 and
8 mL sample size.
- The three slightly lower results can be partially explained by insufficient conditioning
of the DS800 sensor since these were the first series measured.

Systematic error: −105.4 µL

• The offset (105.4 µL) is larger than the recommended value of 15 µL [3].
• Thus, the offset has to be taken into account in the method calculation to
compensate for it.

METTLER TOLEDO Titration Application Note 8

 Validation parameter Results

Limit of quantitation Multiple series with different sample amounts:

LOQ
2.5
Titration Application Note

y = 3.8809 x−0.795
2

Rel. std. deviation srel [%]

1.5

1
LOQ for srel ≤0.3%

0.5

0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80
Sample amount [mmoL]
Figure 5: Limit of Quantitation (LOQ); relative std. deviation vs. sample amount.

• The smallest amount of analyte that can be determined with a recommended relative
standard deviation srel of ≤0.3% [3] is 25 mmol SDS. This corresponds to a sample
size of 6.25 mL 0.004 M SDS, and thus to a titrant consumption of 31.25% burette
volume for a 20 mL glass burette.
• Hence, to achieve a repeatability better or equal 0.3%, the minimum sample size
should be 6.25 mL 0.004 M SDS.

Range Multiple series with different sample sizes:

• Recommendation:
Select the sample size to achieve a titrant consumption of 20–90% of the burette
volume [3].
• In this range, the result should be constant and accurate, independently of the
sample size:
Burette volume [%]
0 10 20 30 40 50 60 70 80 90 100
4.100
Nominal value:
4.016 mmol/L
4.050
Concentration [mmol/L]

4.000

3.950

3.900

3.850

3.800
0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0
Sample size [mL]
Figure 6: Range: 20–90% burette volume (20 mL burette).

• Between 20 and 90% burette volume, the average content is 4.005 ± 0.012 mmol/L,
i.e. the deviation from the nominal value is −0.011 mmol/L, i.e. a relative deviation
of −0.273% which is below the recommended value of ±0.3% [3].
• Note that the content is constant even for a titrant consumption of 10% burette volume.

METTLER TOLEDO Titration Application Note 9

 Validation parameter Results

Robustness Modification of the titration method parameter “Predispensing”:

• The titration method is modified by defining a titrant predispensing in order to test the
robustness of the method:
Titration Application Note

4.100 Titration method with ( ) and without predispensing ( )

Nominal value:
4.016 mmol/L
4.050

Concentration [mmol/L]
4.000

3.950

3.900

3.850

3.800
0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0
Sample size [mL]
Figure 7: Robustness.

• The average content of all series in the graphics is 4.006 ± 0.029 mmol/L (n = 23,
srel = 0.736%). The average is −0.010 mmol/L lower than the nominal value, which
corresponds to a deviation of −0.249%. This is within the range of the recommended
value ±0.3% [3].
• The definition of a predispensing in the titration method does not affect the results,
and therefore the method can be considered as robust against titrant predispensing.

METTLER TOLEDO Titration Application Note 10

 Results Remarks
Method validation • This application has been developed for the men-
tioned sample. Hence, it is necessary to optimize
Recommended
Titration Application Note

Result values [3]
the method for your specific sample.
Accuracy Deviation = −0.135% Deviation = ±0.3% • The application has been developed based on the
Precision procedure according to DIN EN 14480 standard.
• Repeatability • srel = 0.474% • srel ≤0.3%
However, this application note does not replace
• Intermediate • Deviation = −0.249% • Deviation = ±0.3%
precision (6 days Tests) the DIN EN 14480 standard.
• Reproducibility • N/A • Deviation = ±0.3% • The sample aliquots of the SDS standard solution
srel ≤0.3%
were dispensed automatically by a burette. If this is
Specificity N/A
Linearity R2 = 1.0000 R2 > 0.995 not desired, the manual addition of the sample solu-
R , ΔR/ΔV
2
ΔR/ΔV = 0.36% ΔR/ΔV < 0.1% tion can be performed before titration.
Systematic a = −105.4 µL a < 15 µL
error a
Limit of N/A
detection LOD Waste Disposal and
Limit of 25 mmol SDS for Analyte amount for
quantitation LOQ srel ≤0.3% srel ≤0.3% Safety Measures
Range Over the whole range 20–90% burette
of 20–90% burette volume
volume • Use gloves, safety goggles and a lab coat.
Deviation = −0.273% Deviation = ±0.3%
Robustness Deviation = −0.249% Deviation = ±0.3% • MIBK is an intensive smelling organic solvent. It is
Modified titration recommended to work in a fume hood.
method (predispensing)
• Neutralize the titrated solutions before final disposal
as organic solvents.
• The method validation for the potentiometric
two-phase titration is in good agreement with
the r­ecommended values in Titration Application References
Brochure 16 [3].
• The discrepancies in the repeatability, systematic [1] United States Pharmacopeia 38, National
error and non-linearity are mainly due to the dif- Formulary 33, USA, The United States
ferent kind of sensor and chemical analysis in this Pharmacopeial Convention, Inc., 2015.
application. [2] International Conference on Harmonization,
• The recommended values [3] have to be considered Validation of Analytical Procedures: Text and
as an estimation for a method validation. In fact, Methodology, Geneva (2005).
they have been estimated by running a very large [3] Titration Applications Brochure No. 16, “Validation
number of potentiometric acid / base, precipita- of Titration Methods”, ME-51724912C, March 2017.
tion and redox titrations. Thus, they should not be [4] “Anionics Content in Shower Gels by Potentiometric
considered as an absolute limit for the acceptance Two-Phase Titration”, Titration Application M376,
of the validation for any other titration method, but 2007.
rather as indicative values. [5] “Titer Determination of Hyamine by Potentiometric
• A suitable conditioning of the electrode before the Two-Phase Titration”, Titration Application M378,
analysis is crucial for accurate results. The sensitive 2007.
membrane is strongly dependent on it. [6] “Good Titration Practice™ in Surfactant Titration”,
• After each sample, the electrode is first rinsed and GTP® Brochure 51725279B, March 2014.
conditioned 60 s in deionized water. Good Titration Practice™ in Surfactant Titration –
• The sensor performance is increasing with increas- METTLER TOLEDO (mt.com)
ing number of titrated samples. In fact, the first
series show a slightly higher deviation and relative
standard deviation. Further information
• Multiple sample series show that the relative
­standard deviation varies from srel = 0.060 up Modular Titrators For Your Titration Applications,
to 0.963%. This can be mainly attributed to the and Compliance Needs (mt.com)
­conditioning of the DS800 sensor.

METTLER TOLEDO Titration Application Note 11

 dE/dV E
[mV/mL] [mV]
200.0
100.0
180.0
Titration Application Note

80.0
160.0

60.0 140.0

E
40.0 120.0
dE/dV

100.0
20.0

80.0
0.0
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0
V [mL]
Figure 8: Measured values.

Titration and first derivative curves (below: table of measured values) of 5.8 mL 0.004 M SDS with 0.004 M
Hyamine (sample 1/12).

t [s] V [mL] E [mV] dE/dV [mV/mL] T [°C] EQP

0 0.000 74.6 25.0
6 0.020 75.0 25.0
12 0.040 74.7 25.0
17 0.090 75.6 25.0
… … … …
146 5.015 111.0 22.11 25.0
151 5.215 115.7 35.20 25.0
156 5.415 122.6 58.22 25.0
162 5.615 135.3 91.28 25.0
167 5.695 147.7 98.52 25.0
174 5.716 150.1 102.91 25.0
5.739085 153.1 108.89 EQP
181 5.768 156.9 108.67 25.0
187 5.819 162.6 92.57 25.0
192 5.905 172.3 83.79 25.0
198 5.975 177.2 70.01 25.0
203 6.150 184.1 25.0
208 6.350 190.6 25.0
213 6.550 195.0 25.0
218 6.750 198.0 25.0
224 6.950 200.6 25.0

METTLER TOLEDO Titration Application Note 12

 Method Sensor
Type pH
001 Title Sensor DGi111-A
Type General titration Unit pH
Compatible with T5/T7/T9
Titration Application Note

Temperature acquisition
ID M867 Temperature measurement No
Title SDS content by pot. 2P-titration Stir
… Speed 35%
Predispense
002 Sample Mode None
Number of IDs 1 Wait time 0s
ID 1 0.004 M SDS Control
Entry type Volume Endpoint type Absolute
Lower limit 0.0 mL Tendency Negative
Upper limit 20.0 mL Endpoint value [pH] 3
Volume 5 mL Control band [pH] 2.0
Density 1 g/mL Dosing rate (max) 10 mL/min
Number of sample factors 0 Dosing rate (min) 500 µL/min
Correction factor 1.0 Termination
Temperature 25.0°C At EP Yes
Entry Arbitrary Termination delay 0s
InMotion reader None At Vmax 10.0 mL
Max. time infinite Yes
003 Titration stand (InMotion T / Tower A) Max. time ∞
Type InMotion T / Tower A Accompanying stating
Titration stand InMotion T / 1A Accompanying stating No
Titration head position Sample Condition
Lid handling Condition No

004 Pump 008 Dispense (normal) [2]

Auxiliary reagent Water-A Titrant MIBK:EtOH
Volume 40 mL Concentration 1 mol/L
Pump property 1-way Volume 20 mL
Condition No Dosing rate 60.0 mL/min
Condition No
005 Dispense (normal) [1]
Titrant SDS 009 Stir
Concentration 0.004 mol/L Speed 80%
Volume m mL Duration 60 s
Dosing rate 60.0 mL/min Condition No
Condition No
010 Titration (EQP) [2]
006 Stir Titrant
Speed 35% Titrant Hyamine
Duration 15 s Concentration 0.004 mol/L
Condition No Sensor
Type mV
007 Titration (EP) [1] Sensor DS800-SC
Titrant Unit mV
Titrant HCl-A Temperature acquisition
Concentration 0.1 mol/L Temperature measurement No

METTLER TOLEDO Titration Application Note 13

 Stir Extra statistical func. No
Speed 80% Send to buffer No
Predispense Write to Smart Tag None
Mode None Condition No
Titration Application Note

Wait time 0s
Control 012 Calculation R2
Control User Result Concentration
Titrant addition Dynamic Result unit mmol/L
dE(set) 8.0 mV Formula R2 = Q[2]*C/m
dV(min) 0.02 mL Constant C = 1000
dV(max) 0.2 mL M M[none]
Meas. val. acquisition Equilibrium controlled z z[none]
dE 1 mV Decimal places 3
dt 2s Result limits No
t(min) 5s Record statistics Yes
t(max) 30 s Extra statistical func. No
Evaluation and recognition Send to buffer No
Procedure Standard Write to Smart Tag None
Threshold 15 mV/mL Condition No
Tendency Positive
Ranges 0 013 Calculation R3
Add. EQP criteria No Result Recovery
Termination Result unit %
At Vmax 20.0 mL Formula R3 = Q[2]*C/QENDDi
At potential No Constant C = 100
At slope No M M[SDS]
After number of recognized Yes z z[SDS]
EQPs Decimal places 2
Number of EQPs 1 Result limits No
Combined termination criteria No Record statistics Yes
Accompanying stating Extra statistical func. No
Accompanying stating No Send to buffer No
Condition Write to Smart Tag None
Condition No Condition No

011 Calculation R1 014 Conditioning

Result Consumption Interval 1
Result unit mL Position Conditioning beaker
Formula R1 = VEQ[2] Time 60 s
Constant C=1 Speed 30%
M M[none] Lid handling No
z z[none] Condition No
Decimal places 3
Result limits No 015 End of sample
Record statistics Yes

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