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Selected Applications

35
Application Brochure

Excellence Line Titrators

Selected Applications
for METTLER TOLEDO Titration Excellence Line

METTLER TOLEDO

Contents
Method

Electrode

Title

M361

DGi112-Pro

Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl

M362

DGi112-Pro

Buffer Capacity of Coca Cola

M363-A

DGi116-

Acid Number in Used Motor Oil According to ASTM D664-07

Page

Solvent

M363-B

M363-C

M363-D

M363-E

M363-F

DGi116-

Blank Value of Acid Number Solvent

Solvent

According to ASTM D664-07

DGi116-

Blank Value for Strong Acid Number According to ASTM D664-

Solvent

07

DGi116-

Buffer Value pH 11 for Acid Number

Solvent

According to ASTM D664-07

DGi116-

Buffer Value pH 4 for Acid Number

Solvent

According to ASTM D664-07

DGi116-

10

13

16

19

Titer Determination of 0.1 mol/L KOH in 2-Propanol

22

Base Number in Used Motor Oil According to ASTM D4739-06a

25

DGi116-

Blank Value of Base Number Solvent

28

Solvent

According to ASTM D4739-06a

Solvent

M364-A

DGi116Solvent

M364-B

M364-C

DGi116-

Titer Determination of 0.1 mol/L HCl in 2-Propanol

31

Titer Determination of 0.1 mol/L KOH in 2-Propanol

34

m-Value of Tap Water with Automatic Temperature

37

Solvent

M364-D

DGi116Solvent

M365

DG117-Water

Compensation

M366

DX202-SC

Na2O and SiO2 in Waterglass

40

Chloride Content in Used Motor Oil

43

Sb850-S7

M367

DMi145-SC

METTLER TOLEDO
M368

DMi145-SC

Titer Determination of 0.01 mol/L AgNO3 in 2-Propanol

46

M369

DMi147-SC

Peroxide Value of edible Oils and Fats

49

M370

DMi147-SC

Titer Determination of 0.01 mol/L Na2S2O3

52

M371

DMi148-SC

Chloride Determination in Ethanol

55

M372

DMi148-SC

Titer Determination of 0,001 mol/L AgNO3

58

M373

DM405-SC

Mercaptan Sulfur Content in Kerosine

61

According to ASTM D3227-04a

M374-A

InLab718

Base Number Determination in Fresh Oils

64

by Conductometric Titration According to IP400-1994

M374-B

InLab718

Base Number Determination in Used Oils

67

by Conductometric Titration According to IP400-1994

M375

InLab718

Titer Determination of 0.1 mol/L HCl in 2-Propanol

70

by Conductometric Titration

M376

M377

M378

M379

DS800 -

Anionic Content in Shower Gels by Potentiometric Two-Phase

TwoPhase

Titration According to DIN EN 14480

DS800-

Anionic Content in Cutting Oils by Potentiometric Two-Phase

TwoPhase

Titration According to DIN EN 14480

DS800-

Titer Determination of 0.004 mol/L Hyamine by Potentiometric

TwoPhase

Two-Phase Titration According to DIN EN 14480

DGi102-Mini

Acid and Chloride Content in Wine

DMi102-Mini

II

73

76

79

81

Titration Probes: An Overview

DGi101-SC

DGi102-Mini

DGi111-SC

DGi113-SC

DGi116-Solvent

DGi112-Pro

DGi114-SC

DGi115-SC

DGi117-Water

DG300-SC

DX200

DX202-SC

Half-Cell pH sensor

Glass reference sensor

Plastic reference sensor

III

DMi102-SC

DMi141-SC

DMi145-SC

DMi101-SC

DMi140-SC

DMi147-SC

DMi144-SC
Sensor for Rondo 20
COD set 149.5 mm

IV

DMi148-SC

DM143-SC

DM405-SC

Sb850S7/120

InLab717

InLab718

DS500

DS800-TwoPhase

Conductometric
titration

Conductometric
titration

Surfactant
Titration

Surfactant
Titration

Conductivity range:

Conductivity range:

10 S/cm 500 mS/cm

0.1 200 S/cm

Medium::

Medium:

Aqueous solutions

Mixed two-phase
system
(water, MIBK)

pH electrodes for aqueous media

Product name

Combined micro pH electrode for direct pH measurements and


acid/base titrations in aqueous solutions:
-

For very small sample volumes


(min. volume 1 mL)

pH range: 0-14

Temperature range: 0-100C

3 mm shaft

ceramic junction

ARGENTHALTM reference system


(increased life span and heat resistance)

Silver ion trap


(avoid precipitation of e.g. silver sulfide at the ceramic junction)

U glass bulb

Electrolyte
3 mol/L KCl

DGi101-SC

Combined semi micro pH electrode for direct pH measurements and


acid/base titrations in aqueous solutions
-

For small sample volumes


1) 10-25 mL, suitable for micro-titration beaker ME-23516
2) Automation with Rondo 30 and Rondo 60 plus

pH range: 0-14

Temperature range: 0-100C

6 mm shaft

Ceramic junction

ARGENTHALTM reference system


(increased life span and heat resistance)

Silver ion trap


(avoid precipitation of e.g. silver sulfide at the ceramic frit)

U glass bulb

3 mol/L KCl

DGi102-Mini

3 mol/L KCl
saturated
with AgCl

Combined pH electrode for general direct pH measurements and


acid/base titrations:
-

Standard aqueous solutions

pH range: 0-14

Temperature range: 0-80C

Ceramic junction

Ag/AgCl reference element

Large U cone glass membrane:


Large surface area and low membrane resistance
allow for a fast and stable electrode response

DGi111-SC

VI

Reference
electrolyte:

Professional, combined pH electrode with movable sleeve junction for


direct pH measurements and acid/base titrations
-

Difficult, aqueous matrices


(e.g. suitable to avoid contamination with chloride in water
samples with very low chloride content)

pH range: 0-14

Temperature range: 0-60C

Movable PTFE-sleeve junction

ARGENTHALTM reference system

Double junction with refillable reference and bridge electrolyte

Tubular HA glass membrane with low alkali error

3 mol/L KCl

DGi112-Pro

(standard
delivery :
3 mol/L KCl)

3 mol/L KCl

Combined pH electrode for direct pH measurements and acid/base


titrations:
-

Dirty aqueous matrices

Protein containing samples such as milk and yoghurt

Sulfide containing samples


(e.g. white and green liquors in pulp and paper industry, tall oil)

pH range: 0-14

Temperature range: 0-60C

Movable PTFE-sleeve junction

ARGENTHALTM reference system

Tubular HA glass membrane

DGi114-SC

3 mol/L KCl

Combined pH electrode for direct pH measurements and acid/base


titrations:
-

Low ionic strength media


(e.g. pure water, organic solvents such as alcohols)

pH range: 0-14

Temperature range: 0-100C

Fixed ground glass sleeve junction (higher electrolyte flow)

ARGENTHALTM reference system

Silver ion trap

Large tubular HA glass membrane


excellent response, stable signal

Bridge
electrolyte:
selectable

DGi115-SC

Bridge
electrolyte:

Combined pH electrode and integrated temperature sensor for direct pH


measurements and acid/base titrations
-

Simultaneous temperature measurement in aqueous solutions


(Integrated Pt1000 T-sensor)

Low ionic strength aqueous media (e.g. pure and rain water)

pH range: 1-11, temperature range: 0-100C

ARGENTHALTM reference system, gold shielding

Double junction with 3 M KCl-based reference gel electrolyte

Fixed ground glass sleeve junction (higher electrolyte flow)

Spherical LoT glass membrane with low resistance

1 mol/L KCl

DGi117-Water

VII

pH electrodes for non-aqueous media

Product name

1 mol/L LiCl
in ethanol

Combined glass pH electrode for non-aqueous media with moderate


electrostatic effects
-

Acid/base titrations in standard organic solvents such as


alcohols and acetic acid

pH range: 0-12

Temperature range: 0-60C

ARGENTHALTM reference system

Movable PTFE-sleeve junction

Tubular A41 glass membrane with low resistance


(Membrane glass with excellent chemical resistance)

Electrolyte

DGi113-SC

1 mol/L LiCl
in ethanol

Combined glass pH electrode for non-aqueous matrices with strong


electrostatic effects
-

High performance titrations that require fast response times and


quick equilibration of measured values

Applications:
1. TAN/TBN determinations in oil products according to oil
standards
2. Perchloric acid titrations
3. Cyclohexylamine and alcoholic HCl as titrants
4. Titrations using alcoholic KOH, NaOH, TBAOH and NaMethylate as titrants,
5. Epoxy number in epoxy resins
6. Acid value and numbers (AN) in polymers
7. Free fatty acids (FFA) in oil or fat
8. Saponification number in resins

pH range: 0-12

Temperature range: 0-60C

Gold shielding for efficient electrical and static shielding

ARGENTHALTM reference system

Movable glass sleeve junction

Spherical A41 glass membrane of low resistance for fast and


sensitive pH response and chemical resistance

DGi116Solvent

Silver ring electrodes


1 mol/L KNO3

Combined semi micro silver ring electrode for argentometric precipitation


titration in aqueous media
-

For small sample volumes:


1) 10-25 mL, suitable for micro-titration beaker ME-23516
2) Automation with Rondo 30 and Rondo 60 plus

Determination of e.g. chlorides, bromides, iodides, cyanides and


thiocyanides

Sulfidation is possible: titration of sulfides, hydrogen sulfides and


mercaptans, in particular in petroleum and oil products

Temperature range: 0-80C

6 mm shaft

Ceramic junction, Ag/AgCl reference system

VIII

DMi102-SC

1 mol/L KNO3

Combined silver ring electrode for argentometric precipitation titration in


aqueous media
-

Determination of e.g. chlorides, bromides, iodides, cyanides and


thiocyanides

Sulfidation is possible:
argentometric titration of sulfides, hydrogen sulfides and
mercaptans

Temperature range: 0-80C

Ceramic junction

Ag/AgCl reference system

DMi141-SC

1 mol/L KNO3

Combined silver ring electrode for argentometric precipitation titration in


aqueous and non-aqueous media
-

Dirty or viscous samples (e.g. chloride in used oils)

Determination of e.g. chlorides, bromides, iodides, cyanides and


thiocyanides

Low level chloride determinations (e.g. 0.1 ppm Cl- in ethanol)

Sulfidation is possible:
argentometric titration of sulfides, hydrogen sulfides and
mercaptans

Temperature range: 0-80C

Movable sleeve junction

Ag/AgCl reference system

DMi145-SC

--

Combined silver ring electrode for argentometric precipitation titration in


aqueous and non-aqueous media
-

Without change of the pH value

Application examples:
1. Chloride, bromide, iodide and cyanide

2. Chloride, sulfide, hydrogen sulfide, mercaptans in mineral oil

3. Chloride in physiological solutions for dialysis or infusions

4. Chloride in bioethanol

Temperature range: 0-80C

Junction-free bulb pH glass reference, no electrolyte

DMi148-SC

1 mol/L KNO3

Combined Ag2S-sulfidized silver billet electrode for argentometric


precipitation titrations
-

Chloride in physiological solutions with low concentration

Chloride, bromide, iodide, cyanide and thiocyanides in e.g.


electroplating baths

Sulfur containing compounds


(hydrogen sulfide, mercaptans, sulfides)

Temperature range: 0-80C

Annular ceramic junction


Faster response than bulb pH glass reference of DMi148

DM405-SC

IX

Platinum ring electrode


3 mol/L KCl
saturated with
AgCl

Combined semi micro platinum ring electrode for redox titration in


aqueous media
-

For small sample volumes:


1) 10-25 mL, suitable for micro-titration beaker ME-23516
2) Automation with Rondo 30 and Rondo 60 plus

Oxidation with potassium permanganate

Cerium sulfate (e.g. gold determination)

Iodine (e.g. copper determination)

Reduction with sodium thiosulfate (back titration reagent for


iodometric determinations)

Ammonium ferrous sulfate (back titration reagent for a variety of


oxidation reactions)

Temperature range: 0-80C

6 mm shaft

Ceramic junction, Ag/AgCl reference system

DMi101-Mini

3 mol/L KCl
saturated with
AgCl

Combined platinum ring electrode for redox titration in aqueous media


-

Oxidation with potassium permanganate

Cerium sulfate (e.g. gold determination)

Iodine (e.g. copper determination)

Reduction with sodium thiosulfate (back titration reagent for


iodometric determinations)

Ammonium ferrous sulfate (back titration reagent)

Temperature range: 0-80C

Ceramic junction

Ag/AgCl reference system

DMi140-SC

3 mol/L KCl
saturated with
AgCl

Combined platinum ring electrode for redox titration in aqueous media


-

Dedicated electrode for automatic COD determinations on the


Rondo 20 COD rack

Temperature range: 0-80C

Ceramic junction

Ag/AgCl reference system

DMi144-SC

Combined platinum ring electrode for redox titrations

--

For very dirty samples and in oils

Without change of the pH value

Application examples:
1. Chloride, bromide, iodide and cyanide
2. Chloride, sulfide, hydrogen sulfide and mercaptans in mineral
oils and petroleum products
3. Chloride in physiological solutions for dialysis or infusions
4. Chloride in bioethanol

Temperature range: 0-80C

Junction-free bulb pH glass reference, no electrolyte

DMi147-SC

Double pin platinum electrode


-

--

Voltametric titration
1. Karl Fischer titration
2. Vitamin C determination (Voltam. det. with DPI as a titrant)
3. Sulphur dioxide in wine
4. Bromine number and Bromine index (Petroleum products)

Amperometric titration
1. Vitamin C determination (Amperom. det. with DPI as a titrant)

No junction, no reference electrolyte

DM143-SC

Half-cell electrodes
Reference
electrolyte:
3 mol/L KCl
saturated with
AgCl

Double junction glass half-cell reference electrode


-

Ion selective measurements with ISE half-cell

In combination with pH half cell electrodes in aqueous or non


aqueous media

In combination with metal half cell electrodes in aqueous or non


aqueous media

Temperature range: 0-80C

pH range: 0-14

Fixed 4 mm banana plug cable

Ag/AgCl reference system

Movable glass sleeve junction

DX200

Standard
delivery:
3 mol/L KCl
1 mol/L KNO3
0.9 mol/L
Al2(SO4)3
Internal
Ag/AgCl
reference
system
(not refillable)

Plastic reference half-cell electrode


-

Especially suitable for applications in hydrofluoric acid


containing samples (in combination with Sb850-S7/120
antimony half-cell measuring electrode)

Ion selective measurements (in particular, fluoride)

In combination with pH or metal half cell electrodes in aqueous


media

Temperature range: 0-80C

pH range: 0-14

S7-screw cap connection

Internal Ag/AgCl reference system

Porous plastic junction

Bridge
electrolyte:
selectable

DX202-SC

Bridge
electrolyte:
selectable
Standard
delivery:
3 mol/L KCl
1 mol/L KNO3

--

Half cell pH electrode


-

for direct pH measurements and acid/base titrations

for difficult aqueous and non-aqueous matrices in conjunction


with reference electrode DX200

Temperature range: 0-100C

pH range: 0-13

S7-Screw cap connection

DG300-SC

XI

M361

METTLER TOLEDO

Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl


Titration Excellence Line: The buffer capacity of the acidic mixture HCl, CH3COOH and NH4Cl and the
concentration of each acid was determined by potentiometric titration with the DG112-Pro electrode.
Sample

Substance
Chemicals

3 mL acidic mixture (1 mL of each


acid)

Preparation and Procedures


1) The electrode is calibrated using METTLER TOLEDO pH 4, 7
and 9 buffer solutions.

Ammonium chloride (NH 4Cl), all approx. 0.1 mol/L

2) The acidic mixture is prepared by adding 1 mL of each acid


solution into the titration beaker.

40 mL deionized water
pH 4, 7 and 9 buffer solutions

3) The mixture is diluted with 40 mL deionized water before


titration. Since 3 mL acidic mixture is used , the total sample
volume is 43 mL.

Hydrochloric acid (HCl), Acetic acid (HOAc),

4) After each sample, the electrode is rinsed with water during 2


s and conditioned during 10 s (Rondolino mode: 6).

Titrant

Sodium hydroxide (NaOH)


c(NaOH) = 0.1 mol/L

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence Line T70/T90


Rondolino Sample Changer with
PowerShowe and pump

Accessories

Titration beaker ME-101974


LabX Titration Software

Indication

DGi112-Pro

Chemistry

pH 2.8-5.0:
+
HCl+NaOH = Na +Cl +H 2O
pH 5.0-9.0:
+
HOAc+NaOH = OAc+Na +H 2O
pH 9.0-11.5:
NH4Cl+NaOH = Na ++Cl- +NH 3+H 2O

Remarks

Calculation

Results

R1=Q1*C/1, C=1/z (HCl in mol/L)


R2=Q2*C/1, C=1/z (HOAc in mol/L)
R3=Q3*C/1, C=1/z (NH 4Cl in mol/L)
R4=BETAHNV1, unit: mmol/(L*pH)
R5=BETAHNV2, unit: mmol/(L*pH)
R6=BETAHNV3, unit: mmol/(L*pH)
R7=BETAHNV1+BETAHNV2, unit: mmol/(L*pH)
R8=BETAHNV1+BETAHNV2+BETAHNV3, unit:
mmol/(L*pH)

Waste
Waste
disposal
disposal

Neutralize the sample before final


disposal as aqueous solution

Author

Thomas Hitz

A mixture of three different acids (HCl, HOAc, NH4Cl) with clearly


different pKa values (HCl: -7, HOAc: 4.75, NH4Cl: 9.25) is
titrated with 0.1 mol/L NaOH. The buffer capacity is used to
describe this complex mixture. Since three EQPs are found three
different half neutralization values can be calculated (HNV1HNV3, see titration curve).
Three different series (6 samples) have been performed. The
statistics of one series is shown below:
R1
R2
R3
R4
R5
R6
R7
R8

HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+2
BETAHNV1+2+3

0.1088
0.08263
0.09374
3.47
1.18667
1.21333
4.65667
5.87

mol/L
0.00143
mol/L
0.00151
mol/L
0.00084
mmol/(L*pH) 0.15824
mmol/(L*pH) 0.00516
mmol/(L*pH) 0.01033
mmol/(L*pH) 0.15908
mmol/(L*pH) 0.15849

1.318
1.827
0.896
4.56
0.435
0.851
3.416
2.7

In the following the mean value range and the srel-range


obtained for these three different series are shown:
R1:
R2:
R3:
R4:
R5:
R6:
R7:
R8:

0.1081 - 0.10939
0.08263 - 0.08344
0.09374 - 0.09455
3.47 - 3.53833
1.175 - 1.195
1.21333 - 1.225
4.65667 - 4.73333
5.87 - 5.95833

0.7 - 2.4
1.8 - 3.3
0.9 - 1.5
3.0 - 8.8
0.4 - 3.2
0.8 - 3.0
1.7 - 6.2
1.5 - 4.8

Results
No.
1/6

Comment / ID
--

Rx
R1
R2
R3
R4
R5
R6
R7
R8

=
=
=
=
=
=
=
=

Result
0.109
0.07941
0.09244
3.71
1.15
1.19
4.86
6.05

Unit
mol/L
mol/L
mol/L
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

Name
HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+BETAHNV2
BETAHNV1+BETAHNV2+BETAHNV3

2/6

--

R1
R2
R3
R4
R5
R6
R7
R8

=
=
=
=
=
=
=
=

0.10712
0.08107
0.09558
3.52
1.17
1.24
4.69
5.93

mol/L
mol/L
mol/L
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+BETAHNV2
BETAHNV1+BETAHNV2+BETAHNV3

3/6

--

R1
R2
R3
R4
R5
R6
R7
R8

=
=
=
=
=
=
=
=

0.10798
0.08468
0.09327
3.4
1.26
1.22
4.66
5.88

mol/L
mol/L
mol/L
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+BETAHNV2
BETAHNV1+BETAHNV2+BETAHNV3

4/6

--

R1
R2
R3
R4
R5
R6
R7
R8

=
=
=
=
=
=
=
=

0.10756
0.08358
0.0955
3.47
1.19
1.21
4.66
5.87

mol/L
mol/L
mol/L
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+BETAHNV2
BETAHNV1+BETAHNV2+BETAHNV3

5/6

--

R1
R2
R3
R4
R5
R6
R7
R8

=
=
=
=
=
=
=
=

0.10756
0.0863
0.09445
3.53
1.19
1.2
4.72
5.92

mol/L
mol/L
mol/L
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+BETAHNV2
BETAHNV1+BETAHNV2+BETAHNV3

6/6

--

R1
R2
R3
R4
R5
R6
R7
R8

=
=
=
=
=
=
=
=

0.10886
0.08557
0.09606
3.6
1.21
1.29
4.81
6.1

mol/L
mol/L
mol/L
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

HCl
HOAc
NH4Cl
BETAHNV1
BETAHNV2
BETAHNV3
BETAHNV1+BETAHNV2
BETAHNV1+BETAHNV2+BETAHNV3

Table of measured values

Titration curve

HNV1

HNV2

HNV3

Method
Method:
User:

m361
Buffer Capacity
Thomas Hitz

001 Title
Typ
Compatible with
ID
Titel
Author
Date / Time
Modified at
Protect
SOP
002 Sample
Number of IDs
ID 1
Entry Type
Volume [mL]
Density [g/ml]
Correction factor
Temperature [C]
003 Titration stand (Rondolino TTL)
Typ
Titration stand
004 Stir
Speed
Duration
Condition
005 Titration (EQP) [1]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Control
Mode
Show parameters
Titrant addition
dE(set value)
dV(min) [mL]
dV(max) [mL]
Mode
dE
dt [s]
t(min)[s]
t(max)[s]
Evaluation and recognition
Procedure
Threshold [pH/mL]
Tendency
Ranges
Add. EQP criteria
Buffer capacity
Termination
At Vmax [mL]
At potential
At Slope
After numbered of recognized EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
006 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition
007 Calculation R2
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

08.01.2008

008 Calculation R3
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical
Send to buffer
Condition
009 Calculation R4
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical
Send to buffer
Condition
010 Calculation R5
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical
Send to buffer
Condition
011 Calculation R6
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical
Send to buffer
Condition
012 Calculation R7
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical
Send to buffer
Condition
013 Calculation R8
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical
Send to buffer
Condition
014 Record
Summary
Results
Raw results
Table of measured
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2 E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition

General titration
T70/T90
m361
Buffer Capacity
Thomas Hitz
08.01.2008
08.01.2008
No
None
1
-Fixed volume
43
1
1.0
25.0C
Rondolino TTL
Rondolino TTL 1
50 %
20 s
No

NaOH
0.1
pH
DG112-SC
pH
No
30
None
0
Normal
Acid/base
Yes
Dynamic
10
0.005
0.2
Equilibrium controlled
0.5
2.0
3.0
30.0
Standard
1.5
None
0
No
Yes
5
No
No
No
No
No
No
HCl
mol/L
R1=Q1*C/1
1/z
M[Hydrochloric acid]
z[Hydrochloric acid]
5
No
Yes
No
No
No
HOAc
mol/L
R2=Q2*C/1
1/z
M[Acetic acid]
z[Acetic acid]
5
No
Yes
No
No
No

functions

functions

functions

functions

functions

functions

values

NH4 Cl
mol/L
R3=Q3*C/1
1/z
M[Ammonium chloride]
z[Ammonium chloride]
5
No
Yes
No
No
No
Buffer capacity HCl
mmol/(L*pH)
R4=BETAHNV1
1
M[None]
z[None]
5
No
Yes
No
No
No
Buffer capacity HOAc
mmol/(L*pH)
R5=BETAHNV2
1
M[None]
z[None]
5
No
Yes
No
No
No
Buffer capacity NH4 Cl
mmol/(L*pH)
R6=BETAHNV3
1
M[None]
z[None]
5
No
Yes
No
No
No
Buffer capacity sum1
mmol/(L*pH)
R7=BETAHNV1+BETAHNV2
1
M[None]
z[None]
5
No
Yes
No
No
No
Buffer capacity sum2
mmol/(L*pH)
R8=BETAHNV1+BETAHNV2+BETAHNV3
1
M[None]
z[None]
5
No
Yes
No
No
No
No
Per sample
Per sample
No
No
No
Last titration function
Last titration function
No
No
Last titration function
No
No
No
No
No
No
No
No
No

M362

METTLER TOLEDO

Buffer Capacity of Coca Cola


Titration Excellence Line: The buffer capacity of Coca Cola is determined by titration with sodium hydroxide

Sample

Substance

Coca Cola, 50 mL

Acidic components

Chemicals

pH 4, 7 and 9 buffer solutions

Titrant

Sodium hydroxide, NaOH


c(NaOH) = 0.1 mol/L

Preparation and Procedures

- 1 L of Coca Cola is added to an Erlenmeyer flask and


degassed by stirring and while heating for 1 hour.
- The degassed Coca Cola is stored in a sealed bottle, which is
only opened for sample aliquotation.

2) 50 mL of degassed Coca Cola are dispensed into a titration


beaker.

Standard

Potassium hydrogen phthalate (KHP)

Instruments

Titration Excellence Line T70/T90


Rondolino Sample Changer with
PowerShower and pump

Accessories

Olivetti JobJet 210 Printer


LabX Titration Software

Indication

DGi112-Pro

The determination of the buffer capacity represents an alternative


way to analyze the general behaviour of e.g. an acid solution.

Chemistry

HX + NaOH = NaX + H2O

In particular, it can be used to describe complex acid/base


mixtures that can be found in electroplating baths, in beverages
as well as in saliva.

3) The titration is started.


4) After each sample, the electrode is rinsed with water during 2
s and conditioned during 10 s (Rondolino mode: 6).

Remarks

Calculation

R1 = BETAHNV1
R2 = BETAHNV2
R3 = BETAHNV1+BETAHNV2
Units: mmol/(L*pH)

Remarks to the graph:


- HNV stands for half neutralization value.
- HNV1 indicates the half neutralization value of the 1 EQP
(EQP1).
- HNV2 indicates the half neutralization value of the second EQP
(EQP2).
- The dashed line represents the buffer capacity curve (unit:
mmol/(L*pH)).

Results

Waste
Waste
disposal
disposal

Neutralization before final disposal as


aqueous solution.

Author

Thomas Hitz

Results
No.

Comment / ID

Start time

1/5

CocaCola

10.09.2007 15:54:43

2/5

CocaCola

3/5

Rx

Result

Unit

R1 =
R2 =
R3 =

5.24
3.62
8.86

mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

10.09.2007 16:00:04

R1 =
R2 =
R3 =

5.17
3.64
8.81

mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

CocaCola

10.09.2007 16:05:15

R1 =
R2 =
R3 =

5.22
3.63
8.85

mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

4/5

CocaCola

10.09.2007 16:10:22

R1 =
R2 =
R3 =

5.16
3.51
8.67

mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

5/5

CocaCola

10.09.2007 16:15:35

R1 =
R2 =
R3 =

5.16
3.46
8.62

mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

Statistics
Rx

Mean value

Unit

srel[%]

R1
R2
R3

5
5
5

5.19000
3.57200
8.76200

mmol/(L*pH)
mmol/(L*pH)
mmol/(L*pH)

0.03742
0.08167
0.10986

0.721
2.286
1.254

Table of measured values

Titration curve

HNV1

HNV2

Method
Method:
User:

m362
Buffer Capacity Coca Cola
Thomas Hitz

001 Title
Typ
Compatible with
ID
Titel
Author
Date / Time
Modified at
Protect
SOP
002 Sample
Number of IDs
ID 1
Entry Type
Volume
Density
Correction factor
Temperature [C]

10.09.2007

General titration
T50/T70/T90
m362
Buffer Capacity Coca Cola
Thomas Hitz
01.09.2007
10.09.2007
No
None

1
Coca Cola
Fixed volume
50 mL
1.0 g/mL
1.0
25.0

003 Titration stand (Rondolino TTL)


Typ
Rondolino TTL
Titration stand
Rondolino TTL 1
004 Stir
Speed
Duration
Condition
005 Titration (EQP)
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Control
Titrant addition
dE (set value)
dV (min)
dV (max)
Mode
dE
dt [s]
t(min) [s]
t(max) [s]
Evaluation and recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Buffer capacity
Termination
At Vmax
At potential
At Slope
After number
of recognized EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
006 Calculation
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions

30 %
10 s
No

NaOH
0.1 mol/L
pH
DG112-SC
pH
No
30
None
0
User
Dynamic
12
0.005
0.5
Equilibrium controlled
0.5
1
3
30

007 Calculation
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition

BufferCapacity
mmol/(L*pH)
R2 = BETAHNV2
1
M[None]
z[None]
5
No
Yes
No
No

008 Calculation
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition

BufferCapacity
mmol/(L*pH)
R3 = BETAHNV1+BETAHNV2
1
M[None]
z[None]
5
No
Yes
No
No

009 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2E/dV2 - V
Beta-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

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

010 End of sample

Standard
0.7 pH/mL
Positive
0
No
Yes
15 mL
No
No
No
No
No
No
BufferCapacity
mmol/(L*pH)
R1 = BETAHNV1
1
M[None]
z[None]
5
No
Yes
No

function

functions
functions

function

M363-A

METTLER TOLEDO

Acid Number in Used Motor Oil According to ASTM D664-07


Titration Excellence Line: Method for the determination of the Acid Number (AN) and Strong Acid Number
(SAN) in used motor oil by potentiometric titration with potassium hydroxide in 2-propanol according to
ASTM D664-07.
Sample

Used motor oil,


approx. 3 g for AN 5 -10

Substance

Acid components as mg KOH/g


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

Chemicals

60 mL ASTM D664-07 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

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 (See M363-F).
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]. See M363-D (pH 11) and M363-E (pH 4).
3) A blank value is determined for every new batch of solvent
mixture and stored as B[ASTM 664 AN] and B[ASTM 664 SAN]
See applications M363-B for AN and M363-C for SAN.
4) Depending on the AN of the sample, different sample
amounts are requested:
AN / mg KOH/g
Sample size/g
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

Standard

Potassium hydrogen phthalate, 80 mg

Instruments

Titration Excellence T50/T70/T90


Rondo20 with two membrane pumps
LabX Titration Software

Accessories

DV1010 Burette
Glass titration beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DGi116-Solvent

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

Results

R1= (Q-B[ASTM 664 AN])*C/m


C = M/z
R2= QE(H[Buffer pH11])
R3= (R2-B[ASTM 664 AN])*C/m
C = M/z
R4 = QE(H[Buffer pH4])
R5= (R4+B[ASTM 664 SAN])*C/m
C = M/z

Waste
Waste
disposal
disposal

Dispose as aromatic organic solvent


(toluene)

Author

Albert Aichert

5) After each sample titration the DG116-Solvent electrode is


rinsed and conditioned in a chloroform/toluene 1:1 mixture
during 5 minutes. Subsequently, it is conditioned in deionized
water during additional 5 minutes.

Remarks

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 for SAN at pH 4 and AN at pH 11
5) Calculations
R1 = AN to EQP in mg KOH/g
R2 = mmol consumption to buffer potential pH 11
R3 = AN to buffer potential pH 11 in mg KOH/g
R4 = mmol consumption to buffer potential pH 4
R5 = SAN to buffer potential pH 4 in mg KOH/g
Literature:
- ASTM D664-07, see www.astm.org
- METTLER TOLEDO Appl. brochure 34, ME-51 725 066
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020

Results
Method-ID

Summary
Sample
No.
ID
1
Used oil

m363A

Sample size and


3.04742 g
R1 (TAN EQP)
R2 (Consumption
R3 (TAN BP)
R4 (Consumption
R5 (SAN BP)
3.31062 g
R1 (TAN EQP)
R2 (Consumption
R3 (TAN BP)
R4 (Consumption
R5 (SAN BP)
3.27543 g
R1 (TAN EQP)
R2 (Consumption
R3 (TAN BP)
R4 (Consumption
R5 (SAN BP)
3.09854 g
R1 (TAN EQP)
R2 (Consumption
R3 (TAN BP)
R4 (Consumption
R5 (SAN BP)
3.16791 g
R1 (TAN EQP)
R2 (Consumption
R3 (TAN BP)
R4 (Consumption
R5 (SAN BP)
3.27816 g
R1 (TAN EQP)
R2 (Consumption
R3 (TAN BP)
R4 (Consumption
R5 (SAN BP)

Used oil

Used oil

Used oil

Used oil

Used oil

results

BP)
SAN)

BP)
SAN)

BP)
SAN)

BP)
SAN)

BP)
SAN)

BP)
SAN)

----0.376
6.849
0.011
0.312

mg KOH/g
mmol
mg KOH/g
mmol
mg KOH/g

----0.405
6.796
0.015
0.355

mg KOH/g
mmol
mg KOH/g
mmol
mg KOH/g

----0.402
6.817
0.015
0.359

mg KOH/g
mmol
mg KOH/g
mmol
mg KOH/g

----0.381
6.826
0.015
0.379

mg KOH/g
mmol
mg KOH/g
mmol
mg KOH/g

----0.388
6.801
0.016
0.389

mg KOH/g
mmol
mg KOH/g
mmol
mg KOH/g

----0.401
6.794
0.015
0.358

mg KOH/g
mmol
mg KOH/g
mmol
mg KOH/g

Statistics
R3
Samples
Mean
s
srel
R5
Samples
Mean
s
srel

TAN BP
6
6.814
0.021311
0.313
SAN BP
6
0.359
0.026553
7.403

mg KOH/g
mg KOH/g
%

mg KOH/g
mg KOH/g
%

Table of measured values


Volume
mL
0
0.05
0.1
0.153
0.214
0.278
0.337
0.4
0.46
0.521
0.578
0.639
0.692
0.754
0.806
0.865
0.916
0.972
1.023
1.08
1.144
1.204
1.266
1.336
1.399
1.476
1.538
1.616
1.693
1.764
1.844
1.914
1.987
2.08
2.149
2.232
2.334
2.4
2.484
2.57
2.67
2.75
2.86
2.952
3.059
3.164
3.257
3.39
3.488
3.614
3.717
3.845
3.957
4.098
4.21
4.39
4.536
4.686
4.886
5.051
5.251
5.451
5.651
5.851
6.051
6.251
6.451
6.651
6.851
7.051

Increment Signal
Change
mL
mV
mV
NaN
187 NaN
0.05
181.1
-5.9
0.05
174.4
-6.7
0.053
167.3
-7.1
0.061
159.5
-7.8
0.064
151
-8.5
0.059
143.4
-7.6
0.063
135
-8.4
0.06
127.3
-7.7
0.061
118.9
-8.4
0.057
111.3
-7.6
0.061
102.6
-8.7
0.053
95.5
-7.1
0.062
86.5
-9
0.052
79.2
-7.3
0.059
70.5
-8.7
0.051
63
-7.5
0.056
54.7
-8.3
0.051
47.2
-7.5
0.057
39.5
-7.7
0.064
30.8
-8.7
0.06
23
-7.8
0.062
15.4
-7.6
0.07
6.7
-8.7
0.063
-0.6
-7.3
0.077
-9.8
-9.2
0.062
-16.7
-6.9
0.078
-25.2
-8.5
0.077
-33.6
-8.4
0.071
-41.1
-7.5
0.08
-49.8
-8.7
0.07
-57.5
-7.7
0.073
-64.6
-7.1
0.093
-74.3
-9.7
0.069
-81.4
-7.1
0.083
-88.7
-7.3
0.102
-99.4
-10.7
0.066
-105.9
-6.5
0.084
-114
-8.1
0.086
-121.5
-7.5
0.1
-131
-9.5
0.08
-137.5
-6.5
0.11
-146.8
-9.3
0.092
-154.2
-7.4
0.107
-162.5
-8.3
0.105
-171.1
-8.6
0.093
-177.6
-6.5
0.133
-187.7
-10.1
0.098
-194.5
-6.8
0.126
-203.7
-9.2
0.103
-210.7
-7
0.128
-219.5
-8.8
0.112
-226.6
-7.1
0.141
-236.1
-9.5
0.112
-242.2
-6.1
0.18
-252
-9.8
0.146
-259.9
-7.9
0.15
-266.7
-6.8
0.2
-276
-9.3
0.165
-282.3
-6.3
0.2
-289.7
-7.4
0.2
-295.5
-5.8
0.2
-301.3
-5.8
0.2
-306.1
-4.8
0.2
-310.4
-4.3
0.2
-314.3
-3.9
0.2
-317.7
-3.4
0.2
-320.9
-3.2
0.2
-323.6
-2.7
0.2
-326.2
-2.6

Titration curve
1st deriv. Time
Temperature
mV/mL
s
C
NaN
0
25
NaN
5
25
NaN
10
25
NaN
15
25
NaN
20
25
-131.19
25
25
-130.39
30
25
-131.91
36
25
-133.33
41
25
-135.08
46
25
-137.04
51
25
-138.96
56
25
-140.91
61
25
-142.71
66
25
-145.46
71
25
-146.73
76
25
-147.09
81
25
-145.08
86
25
-141.58
91
25
-137.1
97
25
-131.48
102
25
-127.32
108
25
-124.03
114
25
-120.47
119
25
-117.37
124
25
-113.94
130
25
-111.36
136
25
-109.72
142
25
-108.28
147
25
-106.87
152
25
-106.95
157
25
-104.32
163
25
-102.22
169
25
-100.26
174
25
-99.8
179
25
-98.69
184
25
-97.91
189
25
-96.27
194
25
-94.33
200
25
-91.47
205
25
-86.83
210
25
-85.12
215
25
-82.14
220
25
-80.26
225
25
-77.69
230
25
-76.36
235
25
-74.67
240
25
-73.03
245
25
-71.37
250
25
-70.21
255
25
-69.31
260
25
-66.44
266
25
-64.23
271
25
-60.27
276
25
-57.67
282
25
-53.15
288
25
-49.99
294
25
-46.27
300
25
-41.8
305
25
-37.81
310
25
-33.28
315
25
-29.4
320
25
-25.75
325
25
-23
330
25
-20.38
336
25
NaN
341
25
NaN
346
25
NaN
351
25
NaN
356
25
NaN
361
25

Method
Method
Author

m363
SAN & AN ASTM D664
Albert Aichert

29.01.2008

No

008 Conditioning
Type
Interval
Position
Time
Speed
Condition
009 Calculation R1
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
010 Calculation R2
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
011 Calculation R3
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
012 Calculation R4
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
013 Calculation R5
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
014 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition
015 End of sample

No

016 Park

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

General titration
T50 / T70 / T90
m363
SAN & AN ASTM D664
Albert Aichert
29.01.2008 10:12:42
--No
None

1
Used oil
Weight
1.0 g
10.0 g
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A
004 Pump
Auxiliary reagent
Volume
Condition

ASTM 664 solvent


60 mL
No

Speed
Duration
Condition

35 %
60 s
No

005 Stir

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
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
Accompanying stating
Accompanying stating
Condition
Condition
007 Conditioning
Type
Interval
Position
Time
Speed
Condition

KOH in 2-Propanol
0.1 mol/L
pH
DG116-SC
mV
No
30 %
None
0 s
User
Dynamic
8.0 mV
0.05 mL
0.2 mL
Equilibrium controlled
0.5 mV
1 s
5 s
60 s
Standard
150 mV/mL
None
1
-400.0 mV
0.0 mV
No
15.0 mL
Yes
H[Buffer pH11]-100 mV
None
No
No
No
No

Titration stand
Position
Condition
014 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition

Fix
1
Special beaker 1
180 s
100 %
no

Fix
1
Conditioning beaker
300 s
30 %
no
TAN (EQP)
mg KOH/g
R1=(Q-B[ASTM 664 AN])*C/m
z/M
M[Potassium hydroxid]
z[Potassium hydroxid]
3
No
Yes
No
No
No
Consumption EP
mmol
R2=QE(H[Buffer pH11])
1
M[none]
z[none]
3
No
No
No
No
No
TAN (BP)
mg KOH/g
R3=(R2-B[ASTM 664 AN])*C/m
z/M
M[Potassium hydroxid]
z[Potassium hydroxid]
3
No
Yes
No
No
No
Consumption SAN
mmol
R4=QE(H[Buffer pH4])
1
M[none]
z[none]
3
No
No
No
No
No
SAN (BP)
mg KOH/g
R5=(R4+B[ASTM 664 SAN])*C/m
z/M
M[Potassium hydroxid]
z[Potassium hydroxid]
3
No
Yes
No
No
No
No
Per sample
Per sample
No
Last titration function
Last titration function
No

Rondo60/1A
Conditioning beaker
No
Yes
No
No
No
No
No
No

M363-B

METTLER TOLEDO

Blank Value for Acid Number According to ASTM D664-07


Titration Excellence Line: Method for the blank value determination to pH 11 of the acid number in the
solvent ASTM D664-07 with potassium hydroxide in 2-propanol.
60 mL solvent ASTM 664-07
mixture of 2-propanol/toluene/water in
the ratio 495 mL : 500 mL : 5 mL

Preparation and Procedures

Substance

--

Chemicals

--

2) For the blank determination, an EQP titration is used and the


result is calculated at the potential value obtained for pH 11
buffer, i.e. QE(H[Buffer pH11]).
This value was previously determined with application M363-D
and stored as auxiliary value H[Buffer pH11].

Sample

1) Use the empty beaker for the blank determination. Add the
solvent by means of the first membrane pump of Rondo 20.

3) Finally, the result QE(H[Buffer pH11]) in mmol is stored as


blank value B[ASTM 664 AN]

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


Rondo20 with two membrane pumps
LabX Titration Software

Accessories

DV1010 Burette
Glass titration beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DGi116-Solvent

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= QE(H[Buffer pH11])

Remarks

3) The titrant has to be protected against the uptake of CO2 from


the air. NaOH on carrier (e.g. "Sodium hydroxide on support",
MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKA
Nr. 03350) is an effective medium to avoid such formation of
carbonate.
Literature:
- ASTM D664-07, see www.astm.org
- METTLER TOLEDO Appl. brochure 34, ME-51 725 066
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Results

Waste
Waste
disposal
disposal

Dispose as aromatic organic solvent


(toluene)

Author

Albert Aichert

10

Results
Method-ID
T202
Summary
Sample
No. ID
Sample size and results
1
Solvent 664
60 mL
R1 (Blank pH11)
0.003970
2
Solvent 664
60 mL
R1 (Blank pH11)
0.003941
3
Solvent 664
60 mL
R1 (Blank pH11)
0.004210
Statistics
R1
Blank pH11
Samples
3
Mean
0.004040 mmol
s
0.000148 mg KOH/g
srel
3.654
%

Table of measured values


Volume
mL
0
0.002
0.004
0.009
0.019
0.029
0.039
0.044

Increment
Signal
Change
1st deriv.
mL
mV
mV
mV/mL
NaN
-189.2 NaN
NaN
0.002
-177.9
11.3 NaN
0.002
-171.9
6 NaN
0.005
-169
2.9 NaN
0.01
-168.7
0.3 NaN
0.01
-172.8
-4.1 NaN
0.01
-189.4
-16.6 NaN
0.005
-256.5
-67.1 NaN

Titration curve
Time
s
0
10
20
31
41
52
62
87

Temperature
C
25
25
25
25
25
25
25
25

11

Method
Method
Author

T202
Blank AN pH11 ASTM D664
Albert Aichert

07.12.2007

008 Calculation R1
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
009 Blank
Name
Value B=
Unit
Limits
Condition
010 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition
011 End of sample

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature
Entry

General titration
T50 / T70 / T90
T202
Blank AN pH11 ASTM D664
Albert Aichert
07.12.2007 10:12:42
--No
None

1
Solvent 664
Fixed volume
60 mL
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A

Blank pH11
mmol
R1=QE(H[Buffer pH11])
1
M[None]
z[None]
6
No
Yes
No
No
No
ASTM 664 AN
Mean[R1]
mmol
No
No
No
Per sample
Per sample
No
Last titration function
Last titration function
No

004 Pump
Auxiliary reagent
Volume
Condition

ASTM 664 solvent


60 mL
No

Speed
Duration
Condition

35 %
60 s
No

012 Park
Titration stand
Position
Condition
013 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition

005 Stir

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
Potential
Termination tendency
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria
Accompanying stating
Accompanying stating
Condition
Condition
007 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle
Position
Drain
Condition

KOH in 2-Propanol
0.1 mol/L
pH
DG116-SC
mV
No
30 %
None
0 s
User
Dynamic
12.0 mV
0.002 mL
0.01 mL
Equilibrium controlled
0.5 mV
1 s
10 s
60 s
Standard
200 mV/mL
Negative
0
No
15.0 mL
Yes
H[Buffer pH11]-30 mV
None
No
No
No
No
No
No
ASTM 664 solvent
1
15 mL
Actual sample
No
No

12

Rondo60/1A
Conditioning beaker
No
Yes
No
No
No
No
No
No

M363-C

METTLER TOLEDO

Blank Value for Strong Acid Number According to ASTM D664-07


Titration Excellence Line: Method for the blank value determination to pH 4 in the solvent ASTM D664-07
with hydrochloric acid in 2-propanol.
60 mL solvent ASTM 664-07
mixture of 2-propanol/toluene/water in
the ratio 495 mL : 500 mL : 5 mL

Preparation and Procedures

Substance

--

Chemicals

--

2) For the blank determination, an EQP titration is used and the


result is calculated at the potential value obtained for pH 4
buffer, i.e. QE(H[Buffer pH4]).
This value was previously determined with application M363-E
and stored as auxiliary value H[Buffer pH4]

Sample

1) Use the empty beaker for the blank determinaton. Add the
solvent by means of the first membrane pump of Rondo 20.

3) Finally, the result QE(H[Buffer pH4]) in mmol is stored as


blank value B[ASTM 664 SAN].

Titrant

Hydrochloric acid in 2-Propanol


HCl, c(HCl) = 0.1 mol/L

Standard

Tris-(hydroxymethyl)-aminomethane, 80 mg

Instruments

Titration Excellence T50/T70/T90


Rondo20 with two membrane pumps
LabX Titration Software

Accessories

DV1010 Burette
Glass titration beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DGi116-Solvent

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.

Remarks

HA: Acid components

Calculation

R1= QE(H[Buffer pH4])

Literature:
- ASTM D664-07, see www.astm.org
- METTLER TOLEDO Appl. brochure 34, ME-51 725 066
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Results

Waste
Waste
disposal
disposal

Dispose as aromatic organic solvent


(toluene)

Author

Albert Aichert

13

Results
Method-ID
T212
Summary
Sample
No. ID
Sample size and results
1
solvent 664
60 mL
R1 (Blank pH4)
0.006157
2
solvent 664
60 mL
R1 (Blank pH4)
0.005933
3
solvent 664
60 mL
R1 (Blank pH4)
0.005929
4
solvent 664
60 mL
R1 (Blank pH4)
0.005733
Statistics
R1
Blank pH4
Samples
4
Mean
0.005938 mmol
s
0.000173 mg KOH/g
srel
2.918
%

Table of measured values


Volume
mL
0
0.002
0.004
0.008
0.016
0.026
0.036
0.046
0.054
0.06
0.062
0.064
0.066
0.068

Increment
Signal
Change
1st deriv.
Time
mL
mV
mV
mV/mL
s
NaN
44.5 NaN
NaN
0.002
67.8
23.3 NaN
0.002
80
12.2 NaN
0.004
92.6
12.6 NaN
0.008
107.1
14.5 NaN
0.01
120.8
13.7
997.3
0.01
133.2
12.4
1010.34
0.01
146.5
13.3
1673.72
0.008
161.2
14.7
2863.48
0.006
175.6
14.4 NaN
0.002
187.1
11.5 NaN
0.002
197.4
10.3 NaN
0.002
210.7
13.3 NaN
0.002
227.6
16.9 NaN

Titration curve
0
10
20
30
41
51
62
72
82
92
103
113
124
134

Temperature
C
25
25
25
25
25
25
25
25
25
25
25
25
25
25

14

Method
Method
Author

T212
Blank SAN pH4 ASTM D664
Albert Aichert

17.01.2008

008 Calculation R1
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
009 Blank
Name
Value B=
Unit
Limits
Condition
010 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition
011 End of sample

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample
Number of IDs
ID 1
Entry type
Volume
Density
Correction factor
Temperature
Entry

General titration
T50 / T70 / T90
T212
Blank SAN pH4 ASTM D664
Albert Aichert
17.01.2008 10:12:42
--No
None

1
Solvent 664
Fixed volume
60 mL
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A

Blank pH4
mmol
R1=QE(H[Buffer pH4])
1
M[None]
z[None]
6
No
Yes
No
No
No
ASTM 664 SAN
Mean[R1]
mmol
No
No
No
Per sample
Per sample
No
Last titration function
Last titration function
No

004 Pump
Auxiliary reagent
Volume
Condition

ASTM 664 solvent


60 mL
No

Speed
Duration
Condition

35 %
60 s
No

012 Park
Titration stand
Position
Condition
013 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition

005 Stir

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
Potential
Termination tendency
At slope
After number of
recognized EQPs
Number of EQPs
Combined termination
criteria
Accompanying stating
Accompanying stating
Condition
Condition

HCl in 2-propanol
0.1 mol/L
pH
DG116-SC
mV
No
30 %
None
0 s
User
Dynamic
12.0 mV
0.002 mL
0.01 mL
Equilibrium controlled
0.5 mV
1 s
10 s
60 s
Standard
200 mV/mL
Positive
0
No
15.0 mL
Yes
H[Buffer pH4]+50 mV
None
No
No
No
No
No
No

007 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle
Position
Drain
Condition

ASTM 664 solvent


1
15 mL
Actual sample
No
No

15

Rondo60/1A
Conditioning beaker
No
Yes
No
No
No
No
No
No

M363-D

METTLER TOLEDO

Buffer Value pH 11 for Acid Number According to ASTM D664-07


Titration Excellence Line: Determination of the potential value for pH 11 buffer (AN, Acid Number) acccording
to ASTM D 664-07.
Sample

50 mL pH 11 buffer solution

Preparation and Procedures


1) Always use fresh pH 11 buffer solution. The buffer pH 11 is
not stable when exposed to air.

Substance

--

2) 50 mL pH 11 buffer solution are added into a titration


beaker.

Chemicals

--

3) Before measure the buffer potential, the electrode should


conditioned in aquous media (water pH 5-6) for 3 - 5 minutes.
4) The measured potential value for buffer pH 11 is stored as
auxilliary value H[Buffer pH11].

Titrant

--

Standard

--

Instruments

Titration Excellence T50/T70/T90


Rondo20 with two membrane pumps
LabX Titration Software

Accessories

DV1010 Burette
Glass titration beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DGi116-Solvent

Chemistry

--

Calculation

R1= E

5) Finally, the electrode is parked in the condioning beaker


containing slightly acidic water (pH 5-6).

Remarks
1) This application does not replace the ASTM standard.
2) The buffer pH 11 is not stable when exposed to air. In fact,
due to the high alkaline pH value, the absorption of CO2 from the
air is strongly improved.
For instance, the potential value (mV) in an open beaker with
buffer pH 11.can change of 0.1 mV/min
The potential value of an opened bottle of pH 11 buffer solution
can rapidly change.
Thus, it is very important to use fresh pH 11 buffer solution every
time a new value has to be determined

Literature:
- ASTM D664-07, see www.astm.org
- METTLER TOLEDO Appl. brochure 34, ME-51 725 066
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Results

Waste
Waste
disposal
disposal

Neutralize before final disposal as


queous solution.

Author

Albert Aichert

16

Results
Method-ID

T102

Data / Time

07.01.2008 03:12:05 pm

All results
Sample 1/1
R1(Buffer pH11)

Buffer pH11
-222.400 mV

Table of measured values

Titration curve

17

Method
Method
Author

T102 Buffer value AN pH11 ASTM D664


Albert Aichert

17.12.2007

001 Title
Type
Compatible with
ID
Title

General titration
T50 / T70 / T90
T102
Buffer value AN pH11 ASTM

Author
Date/Time
Modified
Modified by
Protect
SOP

Albert Aichert
17.12.2007 10:12:42
--No
None

D664

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

1
Buffer pH11
Fixed volume
50 mL
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A
004 Stir
Speed
Duration
Condition
005 Measure (normal) [1]
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Acquisition of the measured
Acquisition
Time
Mean value
t(min)
t(max)
Condition
Condition
006 Calculation R1
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition

35 %
300 s
No

pH
DG116-SC
mV
No
30 %
value
Fix
30 s
No
10 s
60 s
No

Buffer pH11
mV
R1=E
1
M[None]
z[None]
3
No
No
No
No
No

007 Auxiliary value


Name
Value B=
Unit
Limits
Condition

Buffer pH11
R1
mV
No
No

008 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition

No
Per sample
Per sample
No
No
No
No

009 End of sample


010 Park
Titration stand
Position
Condition

Rondo60/1A
Conditioning beaker
No

18

M363-E

METTLER TOLEDO

Buffer Value pH4 for Strong Acid Number According to ASTM D664-07
Titration Excellence Line: Determination of the potential value for pH 4 buffer (SAN, Strong Acid Number)
acccording to ASTM D 664-07.
Sample

50 mL pH 4 buffer solution

Preparation and Procedures


1) Always use fresh pH 4 buffer solution.
2) 50 mL pH 4 buffer solution are added into a titration beaker.

Substance

--

Chemicals

--

3) Before measure the buffer potential, the electrode should


conditioned in aquous media (water pH 5-6) for 3 - 5 minutes.
4) The measured potential value for buffer pH 4 is stored as
auxilliary value H[Buffer pH4].
5) Finally, the electrode is parked in the condioning beaker
containing slightly acidic water (pH 5-6).

Titrant

--

Standard

--

Instruments

Titration Excellence T50/T70/T90


Rondo20 with two membrane pumps
LabX Titration Software

Accessories

DV1010 Burette
Glass titration beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DGi116-Solvent

1) This application does not replace the ASTM standard.

Chemistry

--

2) Before measure the buffer potential, the electrode should


conditioned in aqueous media (water pH 5-6) for 3 - 5
minutes.

Calculation

R1= E

Remarks

Literature:
- ASTM D664-07, see www.astm.org
- METTLER TOLEDO Appl. brochure 34, ME-51 725 066
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Results

Waste
Waste
disposal
disposal

Neutralize before final disposal as


queous solution.

Author

Albert Aichert

19

Results
Method-ID

T112

Data / Time

17.01.2008 11:12:05 pm

All results
Sample 1/1
R1(Buffer pH4)

Buffer pH4
169.200 mV

Table of measured values

Titration curve

20

Method
Method
Author

T112 Buffer value SAN pH4 ASTM D664


Albert Aichert

16.01.2008

001 Title
Type
Compatible with
ID
Title

General titration
T70 / T90
T112
Buffer value SAN pH4 ASTM

Author
Date/Time
Modified
Modified by
Protect
SOP

Albert Aichert
16.01.2008 10:12:42
--No
None

D664

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

1
Buffer pH4
Fixed volume
50 mL
1.0 g/mL
1.0
25.0C
Arbitrary

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A
004 Stir
Speed
Duration
Condition
005 Measure (normal) [1]
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Stir
Speed
Acquisition of the measured
Acquisition
Time
Mean value
t(min)
t(max)
Condition
Condition
006 Calculation R1
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition

35 %
300 s
No

pH
DG116-SC
mV
No
30 %
value
Fix
30 s
No
10 s
60 s
No

Buffer pH4
mV
R1=E
1
M[None]
z[None]
3
No
No
No
No
No

007 Auxiliary value


Name
Value B=
Unit
Limits
Condition

Buffer pH4
R1
mV
No
No

008 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition

No
Per sample
Per sample
No
No
No
No

009 End of sample


010 Park
Titration stand
Position
Condition

Rondo60/1A
Conditioning beaker
No

21

M363-F

METTLER TOLEDO

Titer Determination of 0.1 mol/L KOH in 2-Propanol (ASTM D664-07)


Titration Excellence Line:
Method for the titer determination of 0.1 mol/L KOH in 2-Propanol according to ASTM D664-07.
Sample

Substance

Primary standard
Potassium hydrogen phthalate,
70 - 100 mg

Preparation and Procedures

Potassium hydrogen phthalate


M=204.23 g/mol z=1

2) Add 50 mL CO 2-free deionized water to dissolve the sample.

Chemicals

50 mL CO 2-free, deionized water

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


Rondo20 with two membrane pumps
LabX Titration Software

Accessories

DV1010 Burette
Glass titration beaker ME-101446
XS205 Balance
Olivetti JobJet 210 Printer

Indication

DGi116-Solvent

Chemistry

KOH + K2HPO3 = H2O + 3K+ + PO43-

Calculation

R1= m/(VEQ*c*C)
C=(10*p*z)

1) Weigh the primary standard into the glass titration beaker to


avoid electrostatic influence.

3) After each sample titration, the eelctrode is rinsed with water


4) At the end of the titration, the electrode is parked in the
condioning beaker containing slightly acidic water (pH 5-6).

Remarks
1) This application does not replace the ASTM standard.
2) The titrant has to be protected against the uptake of CO2 from
the air. NaOH on carrier (e.g. "Sodium hydroxide on support",
MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKA
Nr. 03350) is an effective medium to avoid such formation of
carbonate.

Literature:
- ASTM D664-07, see www.astm.org
- METTLER TOLEDO Appl. brochure 34, ME-51 725 066
- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

p: purity of standard

Results

Waste
Waste
disposal
disposal

Neutralize before final disposal as


aqueous solution.

Author

Albert Aichert

22

Results
Summary

Sample
No.
1

Method-ID

ID
KHP

KHP

KHP

KHP

T001

Sample size and results


0.11936 g
R1 (Titer)
0.961720
0.12372 g
R1 (Titer)
0.961095
0.11054 g
R1 (Titer)
0.960251
0.11502 g
R1 (Titer)
0.960945

Statistics
R1
Samples
Mean
s
srel

Titer
4
0.961003
0.000603
0.063 %

Titer
Titrant
New titer

KOH in 2-Propanol
0.96100

Table of measured values

Titration curve

23

Method
Method
Author

m363F Titer of KOH in 2-propanol


Albert Aichert

02.10.2007

008 Calculation R1
Result
Result unit
Formula
Constant C
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition

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
Density
Correction factor
Temperature
Entry

General titration
T50 / T70 / T90
m363F
Titer of KOH in 2-propanol
Albert Aichert
02.10.2007 10:51:42
--No
None

009 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition
010 End of sample

KOH in 2-Propanol
0.1 mol/L
KHP
solid
Weight
0.07 g
0.12 g
1.0 g/mL
1.0
25.0C
Arbitrary

Titer
-R1=(m/(VEQ*c*C)
M/(10*p*z)
M[Potassium hydroxid]
z[Potassium hydroxid]
6
No
Yes
No
No
No

No
Per sample
Per sample
No
Last titration function
Last titration function
No

011 Titer

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A
004 Pump

Titrant
Concentration
TITER=
Limits
Condition

KOH in 2-Propanol
0.1 mol/L
Mean[R1]
No
No

Titration stand
Position
Condition

Rondo60/1A
Conditioning beaker
No

012 Park
Auxiliary reagent
Volume
Condition

Water
60 mL
No

Speed
Duration
Condition

60 %
60 s
No

005 Stir

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. value acquisition
dE
dt
t(min)
t(max)
Evaluation and recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax
At potential
Tendency
At slope
After number of
recognized EQPs
Number of EQP's
Number of EQPs
Combined termination
criteria
Accompanying stating
Accompanying stating
Condition
Condition

013 Record
Summary
Results
Raw results
Table of meas. value
E - V
dE/dV - V
Condition

KOH in 2-Propanol
0.1 mol/L
pH
DG116-SC
mV
No
30 %
Volume
1.0 mL
5 s
User
Dynamic
8.0 mV
0.005 mL
0.5 mL
Equilibrium controlled
1.0 mV
1 s
3 s
60 s
Standard
3.0 pH/mL
Positive
0
No
10.0 mL
No
None
No
Yes
1
No
No
No
No

007 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle
Position
Drain
Condition

Water
1
15 mL
Actual sample
No
No

24

Yes
No
No
No
No
No
No

M364-A

METTLER TOLEDO

Base Number in Used Motor Oil According to ASTM D4739-06a


Titration Excellence Line: Method for the determination of the base number (BN) in oil by titration with
hydrochloric acid in 2-propanol according to ASTM D4739-06a.
Sample

Used Motor oil, ~2.5 g

Preparation and Procedures


1) Solvent preparation: ASTM D4739-06a solvent is prepared
by mixing 2-propanol, toluene, chloroform and water in the
following ratio: 10:10:10:0.3 (v/v).

Substance

Alkaline components in oil expressed


as KOH, M=56.1 g/mol , z=1

Chemicals

60 mL ASTM D4739-06a solvent


(see Preparation and Procedures)
pH 3 and pH 10 buffer solutions

2) The titer is determined by titration of previously standardized


KOH in 2-propanol solution. The latter has been standardized
using potassium hydrogen phthalate (KHP), see M364-D.
3) The acidic (pH 3) and the alkaline (pH 10) aqueous buffer
potentials are measured and stored as auxiliary values pH 3 (H
[Buffer pH3] ) and ( H[Buffer pH10] ).

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 T70/T90


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

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

Accessories

DV1010 and DV1020 Burettes


Titration beakers ME-101974
XS205 Balance, SP250 pump
PC with LabX Software

6) 60 mL ASTM D4739-06a solvent are added using an


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

Indication

DGi116-Solvent

Chemistry

HCl + KOH = Cl - + K+ + H 2O
KOH 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
Waste
disposal
disposal

Dispose of as halogenated organic


waste

Author

Melanie Nijman

4) Blank values for the base number (BN) are determined for
every new batch of solvent mixture by titration with HCl in 2propanol to the buffer pH 3 potential.
For strong base number (SBN), the solvent is titrated with KOH
in 2-propanol to pH 10 pot. value. The result is stored as blank
value ASTM D4739 (M364-B).

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 at
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 D4739-06a and draft next version, see www.astm.org
2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.
3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

25

Results
Mettler Toledo T90

Titrator

Method

Base Number According to ASTM D4739-06a

M364_A

Mettler Toledo AG
Market Support Laboratory
17.01.2008

RESULTS with DG116-Solvent electrode


No.
ID
Sample size and results
1
Used Motor Oil
2.54656 g
R1 =
3.50
mg KOH/g
R2 =
1.87
mg KOH/g
2
Used Motor Oil
2.67162 g
R1 =
3.48
mg KOH/g
R2 =
1.80
mg KOH/g
3
Used Motor Oil
2.48459 g
R1 =
3.46
mg KOH/g
R2 =
1.80
mg KOH/g
4
Used Motor Oil
2.54055 g
R1 =
3.49
mg KOH/g
R2 =
1.84
mg KOH/g
5
Used Motor Oil
2.4121
g
R1 =
3.45
mg KOH/g
R2 =
1.81
mg KOH/g
6
Used Motor Oil
2.53271 g
R1 =
3.44
mg KOH/g
R2 =
1.83
mg KOH/g
STATISTICS
Number results
Mean value
Standard deviation
Relative standard deviation
Number results
Mean value
Standard deviation
Relative standard deviation

R1

R2

Content (EQP)
Content (Buffer Potential)
Content (EQP)
Content (Buffer Potential)
Content (EQP)
Content (Buffer Potential)
Content (EQP)
Content (Buffer Potential)
Content (EQP)
Content (Buffer Potential)
Content (EQP)
Content (Buffer Potential)

n =
x =
s =
srel =

6
3.47
0.02
0.682

mg KOH/g Content (EQP)


mg KOH/g Content (EQP)
%

n =
x =
s =
srel =

6
1.82
0.03
1.501

mg KOH/g Content (Buffer Potential)


mg KOH/g Content (Buffer Potential)
%

n =
x =
s =
srel =

6
3.46
0.06
1.659

mg KOH/g Content (EQP)


mg KOH/g Content (EQP)
%

n =
x =
s =
srel =

6
1.71
0.05
3.072

mg KOH/g Content (Buffer Potential)


mg KOH/g Content (Buffer Potential)
%

RESULTS with DG113-SC electrode


STATISTICS
Number results
Mean value
Standard deviation
Relative standard deviation
Number results
Mean value
Standard deviation
Relative standard deviation

R1

R2

Table of measured values

Titration curve

26

Method
Method:
User:

m364A Base number ASTM D4739


Melanie Nijman

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

General titration
T70/ T90
m364A
Base number ASTM D4739
Melanie Nijman
17.01.2008
11.01.2008
Administrator
No
None
None

002 Conditioning
Titration stand
Position
Time [s]
Speed [%]
Condition

Rondo60/1A
Conditioning beaker
20
30
No

003 Sample
Number of IDs
ID 1
Entry Type
Lower limit [g]
Upper limit [g]
Density [g/mL]
Correction factor
Temperature [C]
Entry

1
Motor Oil
Weight
0.0
10.0
1.0
1.0
25.0
Arbitrary

004 Titration stand


Type
Titration stand
Lid handling

Rondo/Tower A
Rondo60/1A
No

005 Dispense (normal) [1]


Titrant
Concentration [mol/L]
Volume [mL]
Dosing rate [mL/min]
Condition

ASTM D4739 solvent


1
60
60.0
No

006 Stir
Speed [%]
Duration [s]
Condition

35
60
No

007 Titration (EQP) [1]


Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Volume
Wait time [s]
Predispense
Mode
Volume [mL]
Wait time [s]
Control
Control
Titrant addition
dV (mL)
Mode
dt [s]
Evaluation and Recognition
Procedure
Threshold [mV/mL]
Tendency
Ranges
Lower limit 1 [mV]
Upper limit 1 [mV]
Add. EQP criteria
Termination
At Vmax [mL]
At potential
Potential
Termination tendency
At Slope
After number of recognized EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition

008 Calculation R1
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

17.01.2008

009 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

HCl in 2-Propanol
0.1
pH
DG116-Solvent
mV
No
35
Volume
0.5
60

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

Content (Buffer Potential)


mg KOH/g
R1=(QE(H[Buffer pH3])
-B[ASTM D4739])*C/m
M/z
M[Potassium hydroxide]
z[Potassium hydroxide]
2
No
Yes
No
No
No

010 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Drain pump
Condition

ASTM D4739
3
20.0
Actual position
Yes
SP250
No

011 Conditioning
Type
Interval
Position
Time [s]
Speed [%]
Condition

Fix
1
Conditioning beaker
300
30
No

012 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2 E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition

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

013 End of sample

Volume
0.2
5

014 Park
Titration stand
Position

User
Incremental
0.1
Fixed time
90

Condition

Standard
80.0
None
1
H[Buffer pH3]
H[Buffer pH3]+100
No
5.0
Yes
H[Buffer pH3]+140
Positive
No
No
No
No
No

27

Rondo60/1A
Rinse beaker
No

M364-B

METTLER TOLEDO

Blank Value of Base Number Solvent According to ASTM D4739-06a


Titration Excellence Line: Blank value determination of the base number BN solvent by titration with
hydrochloric acid or potassium hydroxide in 2-propanol according to ASTM D4739-06a.
Sample

Substance
Chemicals

Titrant

60 mL solvent ASTM D4739-06a

--

pH 3 and pH 10 buffer solutions

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 T70/T90


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

Accessories

DV1010 and DV1020 Burettes


Titration beakers ME-101974
XS205 Balance, SP250
PC with LabX Software

Indication

DGi116-Solvent

Chemistry

--

Preparation and Procedures


1) Solvent preparation:
ASTM D4739-06a 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 2propanol 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 H[Buffer pH3] (BN) and H[Bufffer
pH10] (SBN, Strong Base Number). The values are then used
for the EQP termination and the calculation R1.
4) 60 mL ASTM D4739-06a solvent are added using an
additional dosing unit. This step can be performed manually
using a dispenser or a graduated cylinder.
5) Blank value determinations are performed 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

Results

Consumption of HCl in 2-Propanol up to


EQP or acidic potential value:
R1=Q (mmol) or
R1=QE(H[Buffer pH3])
SBN blank: Consumption of KOH in 2Propanol up to EQP/potential value:
R1=Q (mmol) or
R1=QE(H[Buffer pH10])

Waste
Waste
disposal
disposal

Dispose of as halogenated organic


waste

Author

Melanie Nijman

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 at
the potential value of the acidic buffer pH3.
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 D4739-06a and draft next version, see www.astm.org
2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.
3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

28

Results
Mettler Toledo T90

Titrator

Mettler Toledo AG
Market Support Laboratory
17.01.2008

Method

m364B

Blank Base Number According to ASTM D4739-06a

Measured

17.01.2007

RESULTS
No.
1

ID
ASTM D4739 Solvent

ASTM D4739 Solvent

ASTM D4739 Solvent

ASTM D4739 Solvent

ASTM D4739 Solvent

STATISTICS
Number results
Mean value
Standard deviation
Relative standard deviation
Number results
Mean value
Standard deviation
Relative standard deviation

R1

R3

Sample size and results


60.0
mL
R1 =
0.00478 mmol
R3 =
0.00469 mmol
60.0
mL
R1 =
0.00487 mmol
R3 =
0.00478 mmol
60.0
mL
R1 =
0.00484 mmol
R3 =
0.00474 mmol
60.0
mL
R1 =
0.00481 mmol
R3 =
0.00472 mmol
60.0
mL
R1 =
0.00482 mmol
R3 =
0.00474 mmol

Consumption (Buffer potential)


Consumption (EQP)
Consumption (Buffer potential)
Consumption (EQP)
Consumption (Buffer potential)
Consumption (EQP)
Consumption (Buffer potential)
Consumption (EQP)
Consumption (Buffer potential)
Consumption (EQP)

n =
x =
s =
srel =

5
0.00482 mmol
0.00003 mmol
0.697
%

Consumption (Buffer potential)


Consumption (Buffer potential)

n =
x =
s =
srel =

5
0.00473 mmol
0.00003 mmol
0.694
%

Consumption (EQP)
Consumption (EQP)

Table of measured values

Titration curve

29

Method
Method:
User:

m364B Blank BN According to ASTM


Nijman

001 Title
Type
Compatible with
ID
Title
Author
Date / Time
Modified at
Modified by
Protect
SOP
LabX SOP
002 Conditioning
Titration stand
Position
Time [s]
Speed [%]
Condition
003 Sample
Number of IDs
ID 1
Entry Type
Volume [mL]
Density [g/mL]
Correction factor
Temperature [C]
004 Titration stand
Type
Titration stand
Lid handling
005 Dispense (normal) [1]
Titrant
Concentration [mol/L]
Volume [mL]
Dosing rate [mL/min]
Condition
006 Stir
Speed [%]
Duration [s]
Condition
007 Titration (EQP) [1]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Volume
Wait time [s]
Predispense
Mode
Volume [mL]
Wait time [s]
Control
Control
Titrant addition
dV (mL)
Mode
dt [s]
Evaluation and Recognition
Procedure
Threshold [mV/mL]
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
Potential
Termination tendency
At Slope
After number of recognized EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
008 Calculation R1
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer

009 Calculation R3
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition
010 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2 E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition
011 Conditioning
Type
Interval
Position
Time [s]
Speed [%]
Condition
012 End of sample
013 Park
Titration stand
Position

17.01.2008

General titration
T70/ T90
M364_B
Blank ASTM D4739
Mettler Toledo
17.01.2008
17.01.2008
Administrator
No
None

Rondo60/1A
Conditioning beaker
20
30
No
1
ASTM D4739 Solvent
Fixed volume
60.0
1.0
1.0
25.0
Rondo/Tower A
Rondo60/1A
No
ASTM D4739 solvent
1
60
60.0
No
30
10
No

HCl in 2-Propanol
0.1
pH
DG116-Solvent
mV
No
30
Volume
0.02
10
Volume
0.2
5
User
Incremental
0.002
Fixed time
30
Standard
7500.0
Positive
0
No
1.0
Yes
H[Buffer pH3]+100
Positive
No
No
No
No
No
Consumption (Buffer potential)
mmol
R1=QE(H[Buffer pH3])
1
M[None]
z[None]
5
No
Yes
No
No

30

Consumption (EQP)
mmol
R3=Q
1
M[None]
z[None]
5
No
Yes
No
No
No
No
Per series
Per series
Last titration function
Per series
No
Last titration function
Last titration function
No
No
No
No
No
No
No
No
No
No
No
No
Fix
1
Conditioning beaker
300
30
No

Rondo60/1A
Rinse beaker

Condition
014 Blank
Name
Value B=
Unit
Limits
Condition

No

Formula
015 Blank
Name
Value B=
Unit
Limits
Condition
Formula
016 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Send to buffer
Condition
017 Calculation R4
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Send to buffer
Condition
018 Record
Summary
Results
Raw results
Resource data
Calibration curve
Method
Series data
Condition

Mean[R1]>0

ASTM D4739
Mean[R1]
mmol
No
Yes

ASTM D4739
Mean[R3]
mmol
No
Yes
Mean[R3]>0
Mean Consumption (Buffer potential)
mmol
R2=Mean[R1]
1
M[None]
z[None]
5
No
Yes
No
No
Mean Consumption (EQP)
mmol
R4=Mean[R3]
1
M[None]
z[None]
5
No
Yes
No
No
No
Yes
No
No
No
No
No
No

M364-C

METTLER TOLEDO

Titer Determination of 0.1 mol/L HCl in 2-Propanol (ASTM D4739-06a)


Titration Excellence Line: Method for the titer determination of hydrochloric acid in 2-propanol according to
ASTM D4739-06a.
Sample

Standardized KOH in 2-Propanol


c(KOH) = 0.1 mol/L, 8.00 mL

Substance

Potassium hydroxide, KOH


M(KOH)=56.1 g/mol, z=1

Chemicals

50 mL deionized water

Titrant

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

Standard

KOH in 2-propanol 0.1 mol/L(via KHP)

Instruments

Titration Excellence T50/T70/T90


Rondo 20 Sample changer
1 additional dosing unit

Accessories

DV1010 Burettes
Titration beakers ME-101974
PC with LabX Software

Indication

DGi111-SC

Chemistry

HCl + KOH = Cl - + K+ + H 2O

Calculation

Titer HCl:

Preparation and Procedures


1) Add 50 ml deionized into the titration beaker
2) 8 mL KOH in 2-propanol are added automaticlayy by menas
ot an additional dosing unit. If this is not available, the sample
can be added manaully using a pipette.
3) The mean value of the titer determinations is saved
automatically as the titer for the titrant by means of the function
TITER in the method.

Remarks
Literature:
1) ASTM D4739-06a and draft next version, see www.astm.org
2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.
3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

R1=VENDDi/(VEQ*c*C)
C=1/(cst*H[KOH Titer]*z)

Results

The real value for the KOH concentration


determined in M364_D is used for the titer
determination of HCl in 2-Propanol.

Waste
Waste
disposal
disposal

Disposal as halogenated organic waste

Author

Melanie Nijman

31

Results
Mettler Toledo T90

Method
Measured

Titrator
Mettler Toledo AG
Market Support Laboratory
07.03.2008

m364C
Titer HCl in 2-Propanol
07.03.2008

RESULTS
No.
1
2
3
4
5
6
7

ID
Sample size and
KOH in 2-Propanol 8.0
mL
R1 =
0.99689 -KOH in 2-Propanol 8.0
mL
R1 =
0.99622 -KOH in 2-Propanol 8.0
mL
R1 =
0.99649 -KOH in 2-Propanol 8.0
mL
R1 =
0.99674 -KOH in 2-Propanol 8.0
mL
R1 =
0.99613 -KOH in 2-Propanol 8.0
mL
R1 =
0.99626 -KOH in 2-Propanol 8.0
mL
R1 =
0.99694 --

STATISTICS
Number results
Mean value
Standard deviation
Relative standard deviation

R1
x =
s =
srel =

results
Titer HCl
Titer HCl
Titer HCl
Titer HCl
Titer HCl
Titer HCl
Titer HCl

n = 7
0.99652 -0.00033 -0.034
%

Titer HCl
Titer HCl

Table of measured values

Titration curve

32

Method
Method:
User:

m364C Titer of HCl in 2-Propanol


Melanie Nijman

001 Title
Type
Compatible with
ID
Title
Author
Date / Time
Modified at
Modified by
Protect
SOP
LabX SOP
002 Sample (Titer)
Titrant
Concentration
Standard
Type of standard
Entry type
Volume [mL]
Correction factor
Temperature [C]
003 Titration stand
Type
Titration stand
Lid handling
004 Dispense (normal) [1]
Titrant
Concentration [mol/L]
Volume [mL]
Dosing rate [mL/min]
Condition
005 Stir
Speed [%]
Duration [s]
Condition
006 Titration (EQP) [1]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Control
Titrant addition
dE (set value)
dV(min) [mL]
dV(max) [mL]
Mode
dE
dt [s]
t(min) [s]
t(max) [s]
Evaluation and Recognition
Procedure
Threshold [pH/mL]
Tendency
Ranges
Add. EQP criteria
Buffer capacity
Termination
At Vmax [mL]
At potential
At Slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
007 Calculation R1
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions

008 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2 E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition

07.03.2008

Titer determination
T50 / T70 / T90
M364_C
Titer of HCl in 2-Propanol
melanie Nijman
26.02.2008
07.03.2008
Administrator
No
None

HCl in 2-Propanol
0.1
KOH in 2-Propanol
liquid
Fixed volume
8.0
1.0
25.0

No
Per sample
Per sample
Last titration function
No
No
Last titration function
Last titration function
No
No
No
No
No
No
No
No
No
No
No
No

009 End of sample


010 Titer
Titrant
Concentration [mol/L]
TITER=
Limits

Rondo/Tower A
Rondo60/1A
No

Condition

KOH in 2-Propanol
0.1
8.0
60.0
No

30
10
No

HCl in 2-Propanol
0.1
pH
DG111-SC
pH
No
30
None
0

Standard
3.0
None
0
No
No
10.0
No
No
Yes
1
No
No
No

Titer
-R1=VENDDi/(VEQ*c*C)
1/(cst*H[KOH Titer]*z)
M[None]
z[None]
5
No
Yes
No

33

No

011 Park
Titration stand
Position
Condition

Rondo60/1A
Conditioning beaker
No

012 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Send to buffer
Condition

Mean Titer
-R2=Mean[R1]
1
M[None]
z[None]
5
No
Yes
No
No

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

No
Yes
No
No
No
No
No

Condition

User
Dynamic
8.0
0.01
0.5
Equilibrium controlled
0.5
1
3
30

HCl in 2-Propanol
0.1
Mean[R1]
No

No

M364-D

METTLER TOLEDO

Titer Determination of 0.1 mol/L KOH in 2-Propanol (ASTM D4739-06a)


Titration Excellence Line: Method for the titer determination of potassium hydroxide in 2-propanol according
to ASTM D4739-06a.
Sample

Substance

Primary standard KHP


m = ~ 0.11 g

Preparation and Procedures

Potassium hydrogen phthalate


M = 204.23 g/mol; z=1

2) Add 50 ml deionized into the titration beaker.

Chemicals

50 mL deionized water

Titrant

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

Standard

--

Instruments

Titration Excellence T50/T70/T90


Rondo 20 Sample changer

Accessories

DV1010 Burettes
Titration beakers ME-101974
PC with LabX Software

Indication

DGi111-SC

Chemistry

KHC8H4O4 + KOH = H20 + K 2C 8H4O4

1) weigh the standard into the glass titration beaker in order to


avoid electrostatic interferences.

3) The mean value of the titer determinations is saved


automatically as the titer for the titrant by means of the function
TITER in the method.

Remarks

Calculation

Titer KOH:

1) The titrant has to be protected against the uptake of CO2 from


the air.
NaOH on carrier (e.g. "Sodium hydroxide on support", MERCK
no. 101564, or "Sodium hydroxide on carrier", FLUKA Nr.
03350) is an effective medium to avoid such formation of
carbonate.

Literature:
1) ASTM D4739-06a and draft next version, see www.astm.org
2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.
3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

R1=m/(VEQ*c*C)
C=M/(10*p*z)

Results

Waste
Waste
disposal
disposal

Disposal as halogenated organic waste

Author

Melanie Nijman

34

Results
Mettler Toledo T90

Method
Measured

Titrator Mettler Toledo AG


Market Support Laboratory
28.02.2008

m364D
Titer of KOH in 2-propanol
28.02.2008

RESULTS
No.
1

ID
KHP

KHP

KHP

KHP

KHP

KHP

Sample size and results


0.1057
g
R1 =
0.9870
-0.1030
g
R1 =
0.9920
-0.1018
g
R1 =
0.9960
-0.1209
g
R1 =
0.9900
-0.1183
g
R1 =
0.9920
-0.1205
g
R1 =
0.9930
--

STATISTICS
Number results
Mean value
Standard deviation
Relative standard deviation

R1
x =
s =
srel =

n = 6
0.992
0.003
0.304

Titer KOH
Titer KOH
Titer KOH
Titer KOH
Titer KOH
Titer KOH

--%

Titer KOH
Titer KOH

Table of measured values

Titration curve

35

Method
Method:
User:

m364D Titer of KOH in 2-Propanol


Melanie Nijman

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

Titer determination
T50 / T70 / T90
M364_D
Titer of KOH in 2-Propanol
Melanie Nijman
26.02.2008
28.02.2008
Administrator
No
None

002 Sample (Titer)


Titrant
Concentration
Standard
Type of standard
Entry type
Lower limit
Upper limit
Correction factor
Temperature [C]
Input

KOH in 2-Propanol
0.1
Potassium hydrogen phthalate
solid
Weight
0.0
0.5
1.0
25.0
Arbitrary

003 Titration stand


Type
Titration stand
Lid handling

Rondo/Tower A
Rondo60/1A
No

004 Stir
Speed [%]
Duration [s]
Condition
005 Titration (EQP) [1]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Control
Titrant addition
dE (set value)
dV(min) [mL]
dV(max) [mL]
Mode
dE
dt [s]
t(min) [s]
t(max) [s]
Evaluation and Recognition
Procedure
Threshold [pH/mL]
Tendency
Ranges
Add. EQP criteria
Buffer capacity
Termination
At Vmax [mL]
At potential
At Slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
006 Calculation R1
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

007 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d2 E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition

28.02.2008

No
Per sample
Per sample
Last titration function
No
No
Last titration function
Last titration function
No
No
No
No
No
No
No
No
No
No
No
No

008 End of sample


009 Titer
Titrant
Concentration [mol/L]
TITER=
Limits
Condition

30
30
No

KOH in 2-Propanol
0.1
pH
DG111-SC
pH
No
30
None
0
User
Dynamic
8.0
0.01
0.5
Equilibrium controlled
0.5
1
3
30

10.0
No
No
Yes
1
No
No
No

Titer
-R1=m/(VEQ*c*C)
M/(10*p*z)
M[Potassium hydrogen phthalate]
z[Potassium hydrogen phthalate]
3
No
Yes
No
No
No

36

No

010 Park
Titration stand
Position
Condition

Rondo60/1A
Conditioning beaker
No

011 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Send to buffer
Condition

Mean Titer
-R2=Mean[R1]
1
M[None]
z[None]
3
No
Yes
No
No

012 Auxiliary value


Name
Formula H=
Limits
Condition

KOH Titer
R2
No
No

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

No
Yes
No
No
No
No
No

Condition

Standard
3.0
None
0
No
No

KOH in 2-Propanol
0.1
Mean[R1]
No

No

M365

METTLER TOLEDO

m-Value of Tap Water with Automatic Temperature Compensation


Titration Excellence Line: The m-value of tap water is determined by endpoint titration to pH 4.3 with the
DG117-SC sensor, which allows automatic temperature compensation during titration.
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.

Titrant

3) Pipette 50 mL into the beaker shortly before titration.

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

LabX Titration Software


1 DV1010 burette
Titration beakers ME-101974
Cable MultiPinTM-Lemo/Pt1000

Indication

DGi117-SC with internal temperature


sensor Pt1000

Chemistry

HCl + NaOH = NaCl + H2O


HCl + CO32- = HCO3- + ClHCl + HCO3- = CO2 + H 2O + Cl-

Calculation

Total alkalinity or methyl orange


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

Results

Waste
Waste
disposal
disposal

Neutralization of the acidic waste before


final disposal.

Author

Thomas Hitz

4) 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.
5) The automatic temperature compensation was achieved
using the new DG117-SC titration electrode with the
MultiPinTM-Lemo/Pt1000 cable, connected to the analogue
board of the T50.
See also: Application M415, Brochure 34, ME-51 725 066

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) Automatic temperature compensation during titration
increases the accuracy of the analysis (smaller limit of error),
since temperature fluctuations are taken into consideration.
3) Comparison with the DG115-SC (no internal T-sensor).
The following result was obtained from 8 samples:
m-value: 2.650 +/- 0.005 mmol/L , srel: 0.188%.
The slightly higher value probably arises from the missing
temperature correction. However the obtained m-values
determined with both sensors are, as expected, rather similar.
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. The acid capacity
depends on the equilibrium of free CO2, bicarbonate HCO3 , and
2carbonate CO3 in the on its temperature.
Mineral weathering buffers groundwaters, e.g. limestone rock
2+
CaCO3 (s) + CO2 (g) = Ca (aq) + 2 HCO3 (aq)
The bicarbonate ion then acts as a base to neutralize acids:
+
HCO3 (aq) + H (aq) = CO2 (g) + H2O (l)

37

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)
Sample
R1 (Content)

m365
Tap water
2.62200
Tap water
2.61534
Tap water
2.61600
Tap water
2.61250
Tap water
2.62000
Tap water
2.61800
Tap water
2.61600
Tap water
2.63200

Method-ID

m365
Content R1
8
2.61898
mmol/L
0.00602
mmol/L
0.230 %

(1/8)
mmol/L
(2/8)
mmol/L
(3/8)
mmol/L
(4/8)
mmol/L
(5/8)
mmol/L
(6/8)
mmol/L
(7/8)
mmol/L
(8/8)
mmol/L

Statistics
Samples
Mean
s
srel

Table of measured values

Titration curve
EP-titraion (m-value of tap water)

9
8

pH-value

7
6
5
4
3
0

0.2

0.4

0.6

0.8
Volume (mL)

38

1.2

1.4

1.6

Method
Method
Author

m365
m-Value of tap water
Thomas Hitz

10.08.2007

007 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

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

General titration
T50 / T70 / T90
m365
m-Value of tap water
Thomas Hitz
10.08.2007 10:00:00
--No
None

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

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

003 Titration stand (Rondolino TTL)


Type
Titration stand

Rondolino TTL
Rondolino TTL 1

008 End of sample

004 Stir
Speed
Duration
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature acquisition
Temerature sensor
Unit
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

50 %
10 s

HCl
0.1 mol/L
pH
DG117
pH
Yes
interner Sensor 1
C
50 %
None
0 s
User
Absolute
Negative
4.30 pH
3.0 pH
10 mL/min
10 mL/min
Yes
10 s
10.0 mL
Infinity

006 Calculation R1
Result
Content
Result unit
mmol/L
Formula
R1=Q*C/m
Constant
C=1000
M
M[None]
z
z[None]
Decimal places
5
Result limits
No
Record statistics
Yes
Extra statistical functions No
Send to buffer
No
Condition
No

39

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

M366

METTLER TOLEDO

Na2O and SiO2 in Waterglass


Titration Excellence Line: Method for the determination of Na2O and SiO2 in waterglass

Sample

Waterglass ~1.0 g

Preparation and Procedures


Determination of Na2O with HCl in Titration (EQP) [1]:
Na2SiO3 + 2 HCl -> 2 NaCl + SiO2 + H2O

Substance

Na2O, SiO2

Add excess KF to form NaOH from SiO2:


SiO2 + 6 KF + 2 H2O -> Na2SiF6 + 4 NaOH

Chemicals

KF solution, 25%

Neutralise NaOH formed with excess HCl, back-titrate remaining


HCl with NaOH in Titration (EQP) [2]:
HCl + NaOH -> NaCl + H2O

Titrant

HCl, 2.0 mol/L (hydrochloric acid)


NaOH, 1.0 mol/L (sodium hydroxide)

Standard

TRIS/THAM for HCl, KHP for NaOH

Instruments

Titration Excellence T70/T90


2 additional dosing units

Accessories

Titration beakers ME-101974


LabX Titration Software
Rondo 20 Sample Changer

Indication

Sb850-S7/120 (pH sensor input)


DX202-SC (ref. electrode)

Chemistry

Na2SiO3 + 2HCl -> 2NaCl + SiO2 + H 2O


SiO2+6KF+2H2O -> Na2SiF 6 + 4NaOH
HCl + NaOH -> NaCl + H2O

1) Because of the high fluoride content in acidic environment


glass electrodes and titration beakers cannot be used for the
determination of Na2O and SiO2 in waterglass.
2) For this reason only the polypropylene titration beakers can
be used. Care needs to be taken when weighing in the
waterglass samples in the polypropylene beakers that static
electricity is avoided as much as possible.
3) Also, no glass sensors may be used for this determination as
these will be the corroded as well.
All fluoride solutions should be kept in plastic bottles.

Remarks
The titration curve for the first EQP titration shows clearly that
more than one site is present for the alkali metal oxide (mainly
Na2O) component of waterglass.
Waterglass is used in a wide variety of application areas as e.g.,
filler, additive, flame retardant, etc.
Order number for Sb850-S7/120:
Available from MT-PRO, old Ingold no. 10 850 3074

Calculation

R1: Na2O content (%)


R2: SiO2 content (%)
R3: Relative amounts Na2O/SiO2 (-)

Order no. for DX202 ref. electrode: ME-51 109 295

Results

Waste
Waste
disposal
disposal

Dilute and non-acidic fluoride solutions


do not have to be treated as special
waste.

Author

Melanie Nijman

40

Results
Method

m366

Na2O and SiO2 in waterglass

No.

ID

Sample size and results

Waterglass
R1
R2
R3
Waterglass
R1
R2
R3
Waterglass
R1
R2
R3
Waterglass
R1
R2
R3
Waterglass
R1
R2
R3
Waterglass
R1
R2
R3
Waterglass
R1
R2
R3

RESULTS

0.9365
49.91661
44.05010
1.13318
0.9843
49.92277
44.32853
1.12620
0.9806
49.85243
44.21881
1.12740
0.9521
49.90093
44.02595
1.13344
0.9843
49.88776
44.25015
1.12740
1.0449
49.89149
44.35087
1.12493
1.0130
49.95810
44.25864
1.12878

g
%
%

STATISTICS
Number results
R1
Mean value
Standard deviation
Relative standard deviation

n =
x =
s =
srel =

7
49.9043 %
0.03298
0.066
%

Content
Content

Number results
R2
Mean value
Standard deviation
Relative standard deviation

n =
x =
s =
srel =

7
44.21186 %
0.12739
0.288
%

Content
Content

Number results
R3
Mean value
Standard deviation
Relative standard deviation

n =
x =
s =
srel =

7
1.12876
0.00333
0.295
%

=
=
=
=
=
=
=
=
=
=
=
=
=
=
=
=
=
=
=
=
=

g
%
%
g
%
%
g
%
%
g
%
%
g
%
%
g
%
%

Content
Content
Content
Content
Content
Content
Content
Content
Content
Content
Content
Content
Content
Content
-

Table of measured values

Titration curve

41

Method
Method:
User:

m366
Na2O and SiO2 in waterglass
Melanie Nijman

001 Title
Type
Compatible with
ID
Titel
Author
Date / Time
Modified at
Protect
SOP
LabX SOP
002 Sample
Number of IDs
ID 1
Entry Type
Lower limit [g]
Upper limit [g]
Density [g/mL]
Correction factor
Temperature [C]
Entry
003 Titration stand
Type
Titration stand
Lid handling
004 Stir
Speed [%]
Duration [s]
Condition
005 Titration (EQP)
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Control
Titrant addition
dE (set value)
dV (min)
dV (max)
Mode
dE
dt [s]
t(min) [s]
t(max) [s]
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
At Slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
006 Calculation R1
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition
007 Dispense (normal)
Titrant
Concentration [mol/L]
Volume [mL]
Dosing rate [mL/min]
Condition
008 Dispense (normal)
Titrant
Concentration [mol/L]
Volume [mL]
Dosing rate [mL/min]
Condition

009 Stir
Speed [%]
Duration [s]
Condition
010 Titration (EQP)
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Control
Titrant addition
dE (set value)
dV (min)
dV (max)
Mode
dE
dt [s]
t(min) [s]
t(max) [s]
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
At Slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
011 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition
012 Calculation R3
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition
013 Conditioning
Type
Interval
Position
Time [s]
Speed [%]
Condition
014 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - 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
015 End of sample

08.08.2007

General titration
T70/ T90
m366
Na2O/SiO2 in Waterglass
Melanie Nijman
03.08.2007
08.08.2007
No
None

1
Waterglass
Weight
0.8
1.2
1.0
1.0
25.0
Arbitrary
Rondo60/Tower A
Rondo60/1A
No
50
60
No

HCl
2.0
mV
Sb-850
mV
No
30
None
0
User
Dynamic
9.0
0.008
0.4
Equilibrium controlled
0.5
1
3
30
Standard
1500
None
0
No
10
No
No
Yes
1
No
No
No
Na2O Content
%
R1=Q*C/m
M/(10*z)
M[Sodium oxide]
z[Sodium oxide]
5
No
Yes
No
No
25% KF
25
10.0
60.0
No
HCl
2.0
16.0
60.0
No

42

30
30
No

NaOH
1.0
mV
Sb-850
mV
No
30
None
0
User
Dynamic
5
0.002
0.4
Equilibrium controlled
1
1.0
3
30
Standard
150
None
0
No
15
No
No
Yes
1
No
No
No
SiO2 Content
%
R2=(QEX[1]+QENDDi[2]-Q[2])*C/m
M/(10*z)
M[Silicon dioxide]
z[Silicon dioxide]
5
No
Yes
No
No
Na2O/SiO2
R2=R1/R2
1
M[None]
z[None]
5
No
Yes
No
No
Fix
1
Conditioning beaker
20
50
No
No
Per
Per
No
No
No
All
All
No
No
No
No
No
No
No
No
No
No

sample
sample

titration functions
titration functions

M367

METTLER TOLEDO

Chloride Content in Used Motor Oil


Titration Excellence Line: Inorganic chloride content in used motor oil is determined by precipitation titration
in non aqueous solvent with silver nitrate. The content is expressed as chloride, Cl .
Sample

Used motor oil, approx. 10 g

Preparation and Procedures


1) 10 g of sample is added into a glass titration beaker.

Substance
Chemicals

Chloride, Cl -,
M = 35.45 g/mol, z = 1
50 mL Solvent (ASTM 3227)
2-Propanol p.a.
Toluene p.a.
Sodium acetate (anhydrous)

Titrant

Silver nitrate (AgNO 3) in 2-Propanol


c(AgNO 3) = 0.01 mol/L

Standard

c(NaCl) = 0.01 mol/L, 2.5 mL

Instruments

Titration Excellence T70/T90


Rondo 20 Sample Changer with
PowerShowerTM

Accessories

1 DV1005 Burette
Glass titration beaker ME-101446
XS205 Balance
LabX Titration Software

Indication

DMi145-SC (with 1 mol/L KNO3)

Chemistry

NaCl + AgNO 3 = AgCl + NaNO3

2) 2.5 mL 0.01mol/L NaCl standard solution are added to


spike the sample since the chloride content is too low
(Standard-Addition).
3) 50 mL Solvent ASTM 3227 will be added automatically with
the Rondo membrane pump.
4) The sample serie is analysed using a Rondo 20 sample
changer. Special beaker 1 and 2 are filled with toluene and
the condition beaker with solvent ASTM 3227.
Preparation of 0.01 mol/L NaCl
- Dissolve 0.2922 g NaCl p.a. in deionized water
- transfer quantitatively in a 500 volumetric flask and fill up to the
mark with deionized water
Preparation of Solvent ASTM 3227
- Dissolve 1.6 g sodium acetate anhydrous (NaC2H3O2) in
25 mL of deionized water and pour into 1 L flask
- Fill up to the mark with 2-Propanol
Preparation of 0.01 mol/L AgNO3
- Dissolve 8.494 g AgNO3 p.a. in 50 mL deionized water
- transfer it quantitatively into a 500 mL volumetric flask and fill
up to the mark with 2-Propanol (c=0.1 mol/L)
- take 100.0 mL of this solution and dilute it with 2- Propanol
to 1L in a volumetric flask (c=0.01 mol/L)

Remarks
- 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. The weight
of the sample can vary from 0.5 to 30 g (depending on the
kind of oil).
- 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.

Calculation

R1: Content (mg/L Chloride)


R1 = (Q-H[NaCl Std])*C/m,
C = M*1000/z

Results

Literature:
1) METTLER TOLEDO Application brochure 20, ME-51 725 020
2) METTLER TOLEDO Application brochure 34, ME-51 725 066

1 mL AgNO 3 (0.01 mol/l) is equal to


0.354 mg Chloride

Waste
Waste
disposal
disposal

Filtration. The precipitate (AgCl) has to


be classified as special waste. The
liquid phase has to be disposed as
organic waste.

Author

Claudia Schreiner

43

Results
Start time:

04.12.2007

Sample Data
No. 1/6
No. 2/6
No. 3/6
No. 4/6
No. 5/6
No. 6/6

Note / ID
Motor Oil
Motor Oil
Motor Oil
Motor Oil
Motor Oil
Motor Oil

Sample size
10.0318 g
10.1953 g
10.0720 g
10.1120 g
10.1386 g
10.1322 g

Results
No. 1/6
No. 2/6
No. 3/6
No. 4/6
No. 5/6
No. 6/6

Note / ID
Motor Oil
Motor Oil
Motor Oil
Motor Oil
Motor Oil
Motor Oil

Rx
R1=
R1=
R1=
R1=
R1=
R1=

Statistics
Rx
R1

Name
Chloride

Result
28.25
27.80
26.33
27.35
27.28
26.38

n
6

Unit
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L

Mean Value
27.23

Table of measured values

Unit
mg/L

Titration curve

44

s
0.76

srel[%]
2.8

Method
Method
Author

367 Chloride content in motor oil


Claudia Schreiner

04.12.2007

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition

001 Title
Type
Compatible with
ID
Title
Author
Date/Time
Modified
Modified by
Protect
SOP
002 Sample
Number of IDs
ID 1
Entry type
Lower limit
Upper limit
Density
Correction factor
Temperature
Entry

General titration
T70 / T90
367
Chloride in motor oil
Claudia Schreiner
04.12.2007
--No
None

No
No
No

008 Rinse
1
Motor oil
Weight
0 g
15 g
1.0 g/mL
1.0
25.0C
Arbitrary

Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A
004 Pump
Auxiliary reagent
Volume

ASTM D3227 solvent


50.0 mL

Speed
Duration

60%
120 s

005 Stir

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
dV
Mode
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

Chloride
mg/L
R=(Q-H[Std NaCl])*C/m
C= M*1000/z
M[Chloride]
z[Chloride]
3
No
Yes

AgNO 3
0.01 mol/L
mV
DMi145-SC
mV

009 Conditioning
Type
Interval
Position
Time
Speed

Fix
1
Special beaker 1
120s
60%

010 Conditioning
Type
Interval
Position
Time
Speed

Fix
1
Special beaker 2
300s
60%

011 Conditioning
Type
Interval
Position
Time
Speed

Fix
1
Conditioning beaker
120s
60%

012 End of sample

No
40%
None
0 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 mV
3 s
5 s
30 s
Standard
100 mV/mL
Positive
0
No
5 mL
No
No
Yes
1
No

45

ASTM D3227 solvent


1
15
Actual position
No
No

M368

METTLER TOLEDO

Titer Determination of 0.01 mol/L AgNO3 in 2-Propanol


Titration Excellence Line: Method for the titer determination of 0.01 mol/L AgNO 3 by precipitation titration with
sodium chloride as a primary standard.
Primary standard
Sodium chloride solution (0.01 mol/L),
2.5 mL

Preparation and Procedures

Substance

Chloride, Cl -,
M = 35.45 g/mol, z = 1

2) 50 mL Solvent ASTM 3227 will be added automatically with


the Rondo membrane pump.

Chemicals

50 mL Solvent (ASTM 3227)


2-Propanol p.a.
Toluene p.a.
Sodium acetate (anhydrous)

Sample

Titrant

Silver nitrate (AgNO 3) in 2-Propanol


c(AgNO 3) = 0.01 mol/L

Standard

c(NaCl) = 0.01 mol/L, 2.5 mL

Instruments

Titration Excellence T50/T70/T90


Rondo 20 Sample Changer with
PowerShowerTM

Accessories

1 DV1005 Burette
Glass titration beaker ME-101446
XS205 Balance
LabX Titration Software

Indication

DMi145-SC (with 1 mol/L KNO3)

Chemistry

NaCl + AgNO 3 = AgCl + NaNO3

Calculation

R1: Titer

1) Pipette 2.5 mL 0.01mol/L NaCl standard solution in a


titration beaker

3) The sample serie is analysed using a Rondo 20 sample


changer. The condition beaker is filled with solvent ASTM
3227.
Preparation of 0.01 mol/L NaCl
- Dissolve 0.2922 g NaCl p.a. in deionized water
- transfer quantitatively in a 500 volumetric flask and fill up to the
mark with deionized water
Preparation of Solvent ASTM 3227
- Dissolve 1.6 g sodium acetate anhydrous (NaC2H3O2) in
25 mL of deionized water and pour into 1 L flask
- Fill up to the mark with 2-Propanol
Preparation of 0.01 mol/L AgNO3
- Dissolve 8.494 g AgNO3 p.a. in 50 mL deionized water
- transfer it quantitatively into a 500 mL volumetric flask and fill
up to the mark with 2-Propanol (c=0.1 mol/L)
- take 100.0 mL of this solution and dilute it with 2- Propanol
to 1L in a volumetric flask (c=0.01 mol/L)

Remarks
- This method is used to standardize the silver nitrate solution
which is used in the method M367 (Chloride in motor oil).

R1 = m/(VEQ*c*C)
C = 1/(cst*z)

Results

1 mL AgNO 3 (0.01 mol/l) is equal to


0.584 mg sodium chloride

Waste
Waste
disposal
disposal

Filtration. The precipitate (AgCl) has to


be classified as special waste. The
liquid phase has to be disposed as
organic waste.

Author

Claudia Schreiner

46

Results
Start time:

04.12.2007

Sample Data
No. 1/6
No. 2/6
No. 3/6
No. 4/6
No. 5/6
No. 6/6

Note
NaCl
NaCl
NaCl
NaCl
NaCl
NaCl

/ ID
solution
solution
solution
solution
solution
solution

Sample size
2.5 mL
2.5 mL
2.5 mL
2.5 mL
2.5 mL
2.5 mL

Results
No. 1/6
No. 2/6
No. 3/6
No. 4/6
No. 5/6
No. 6/6

Note
NaCl
NaCl
NaCl
NaCl
NaCl
NaCl

/ ID
solution
solution
solution
solution
solution
solution

Rx
R1=
R1=
R1=
R1=
R1=
R1=

Statistics
Rx
R1

Name
Titer

Result
0.9694
0.9684
0.9704
0.9690
0.9708
0.9711

n
6

Unit
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L

Mean Value
0.9698

Table of measured values

Unit
mg/L

Titration curve

47

s
0.0011

srel[%]
0.11

Method
Method
Author

368 Titer 0.01 mol/L AgNO 3


Claudia Schreiner

04.12.2007

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition

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
Volume
Correction factor
Temperature

General titration
T50 / T70 / T90
368
Titer 0.01 mol/L AgNO3
Claudia Schreiner
04.12.2007
--No
None

Titer
--R= m/(VEQ*c*C)
C= 1/(cst*z)
M[Sodium chloride]
z[Sodium chloride]
5
No
Yes
No
No
No

008 Rinse
AgNO 3
0.01 mol/L
NaCl
liquid
Fixed volume
2.5 mL
1.0
25.0C

Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition
009 Conditioning
Type
Interval
Position
Time
Speed

003 Titration stand (Rondo/Tower A)


Type
Rondo/Tower A
Titration stand
Rondo60/1A

ASTM D3227 solvent


1
15
Actual position
No
No

Fix
1
Conditioning beaker
120s
60%

004 Pump
Auxiliary reagent
Volume

ASTM D3227 solvent


50.0 mL

010 End of sample


011 Titer
Titrant
Concentration
Titer =
Limits

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
dV
Mode
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

40%
120 s

AgNO 3
0.01 mol/L
mV
DMi145-SC
mV
No
40%
Volume
1.5 mL
15 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 mV
3 s
5 s
30 s
Standard
100 mV/mL
Positive
0
No
5 mL
No
No
Yes
1
No

48

AgNO3
0.01 mol/L
Mean[R1]
No

M369

METTLER TOLEDO

Peroxide Value of Edible Oils and Fats


Titration Excellence Line: Method for the determination of the peroxide value in oil, fat and margarine by
iodometric titration with sodium thiosulphate of released iodine.
Sunflower oil, 4-5 g
Olive oil, 1 g
Margarine, 2 g

Preparation and Procedures

Substance

Peroxide functional group, R-OOH

2) About 3 g of sample were dissolved in 20 mL of acetic acid/


chloroform (3:2) The acetic acid/chloroform mixture was added
by the function DISPENSE.

Chemicals

20 mL acetic acid/chloroform (3:2)


1 mL saturated KI solution
50 mL deion. water

3) 1 mL saturated KI solution is added by an additional burette.


The reaction takes place and iodine is formed.

Sample

Titrant

1) Beakers have to be cleaned very well. Invisible fat residues or


metal traces can strongly affect the result.

4) 50 mL deionized water are added by the membrane pump of


Rondo 20.

Sodium thiosulfate, Na2S2O3


c(Na2S2O3)= 0.01mol/L

5) Iodine is titrated with sodium thiosulphate.

Standard

Potassium iodate, KIO 3

127 g KI were dissolved in 100 mL water to obtain the


saturated KI solution. The solution has to be kept in the dark.

Instruments

Titration Excellence T70/T90


Rondo 20 Sample Changer with
PowerShowerTM

Accessories

2 additional dosing units


1 DV1020 and 2 DV1010 Burettes
Glass titration beaker ME-101446
XS205 Balance, LabX 2.6

Indication

DMi147-SC

Chemistry

R-OOH + 2 I- + 2 H3O+ =
R-OH + I2 + 3 H2O
I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6

Calculation

R = (Q-B[1])*C/m
C = 1000, meq/kg
B[1]: Solvent blank value, mmol

Results

Waste
Waste
disposal
disposal

The waste contains halogenated


organic solvents and has to be
disposed of accordingly.

Author

Maria-Jos Schmid

Impurities of the solvent are taken into account by a blank value


determination. The blank value determination is done under the
same conditions as the peroxide value determination itself. The
value is stored under B[1].

Remarks
1) Fats and oils undergo changes during storage due to
oxidation with air (oxidative rancidity). The compounds formed
react as peroxides. Their content is commonly expressed as the
"peroxide value" in milliequivalents peroxidic oxygen per kg of
sample.
2) Peroxide values higher than 10 to 20 meq O2/kg are
commonly interpreted as rancidity. Unrefined oils have higher
peroxide values. They are usually in the range between 5 to 20
meq O2/kg.

1) Exactly 60 seconds were allowed for the generation of iodine,


as is requested by the official method (AOAC No. 28.022).
2) Earlier studies, however, had indicated that the generation is
not complete yet at this time. 200 to 300 seconds were found
to yield the highest results. Longer generation times resulted in
low results (secondary reactions between iodine and the oil).
3) The duration of the generation time (time between 'adding the
KI solution' and 'adding the water + starting the titration') is the
critical point for repeatable results.

49

Results
Method:
DM1471
Peroxide number
10/25/2007 11:27:34 AM
Start time:
25.10.2007 1:53:24 PM
___________________________________________________________________________________________
Sample Data
No. 1/5
No. 2/5
No. 3/5
No. 4/5
No. 5/5
Results
No.
1/5

Comment / ID
Olive oil
Olive oil
Olive oil
Olive oil
Olive oil

Sample size
0.8164 g
0.8523 g
0.815 g
0.8149 g
0.8235 g

Comment / ID
Olive oil

Start time
10/25/2007 1:53:25 PM

2/5

Olive oil

10/25/2007 2:05:29 PM

3/5

Olive oil

10/25/2007 2:17:32 PM

4/5

Olive oil

10/25/2007 2:29:19 PM

5/5

Olive oil

10/25/2007 2:41:10 PM

Rx
R1=
R2=
R1=
R2=
R1=
R2=
R1=
R2=
R1=
R2=

Result
0.024
25.601
0.025
25.795
0.024
26.013
0.024
25.888
0.024
26.074

Unit
mmol
meq/kg
mmol
meq/kg
mmol
meq/kg
mmol
meq/kg
mmol
meq/kg

Name
Consumption
Content
Consumption
Content
Consumption
Content
Consumption
Content
Consumption
Content

SQC/Statistics
Rx
Name
n
Mean Value
Unit
s
srel[%]
____________________________________________________________________________________________
R1
R2

Consumption
Content

5
5

0.024
25.874

mmol
meq/kg

0.000
0.187

1.848
0.724

Additional results
Sample
Size
n
Mean value
Unit
s
srel[%]
____________________________________________________________________________________________
Sunflower oil

4-5 g

0.028
5.583

mmol
meq/kg

0.000
0.044

1.609
0.791

Margarine

2 g

0.022
11.759

mmol
meq/kg

0.001
0.578

4.624
4.918

Mais oil

4-5 g

0.021
3.980

mmol
meq/kg

0.000
0.043

2.150
1.087

Table of measured values

EQP1

Volume
mL
0
0.057
0.086
0.1
0.135
0.222
0.322
0.422
0.522
0.622
0.722
0.822
0.922
1.022
1.122
1.222
1.322
1.422
1.522
1.622
1.722
1.822
1.922
2.022
2.122
2.222
2.322
2.422
2.522
2.622
2.642
2.648
2.654
2.661
2.666
2.671
2.671216
2.676
2.681
2.686
2.694
2.704
2.728
2.772
2.872
2.972

Increment
mL
NaN
0.057
0.029
0.014
0.035
0.087
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.02
0.006
0.006
0.007
0.005
0.005
NaN
0.005
0.005
0.005
0.008
0.01
0.024
0.044
0.1
0.1

Signal
mV
-16.7
-8
-11.3
-11.2
-10.9
-10.4
-10.1
-9.6
-9.1
-8.6
-8.1
-7.3
-6.7
-6
-5.3
-4.5
-3.6
-2.7
-1.8
-0.9
0.2
1.7
3.1
4.7
6.8
8.9
12.2
15.7
21.7
35.3
42.2
46.4
50
57.2
66.2
78.3
78.8
89.8
97.7
104
109.9
114.2
120.3
125.3
130
132.5

Titration curve
Change
mV
NaN
8.7
-3.3
0.1
0.3
0.5
0.3
0.5
0.5
0.5
0.5
0.8
0.6
0.7
0.7
0.8
0.9
0.9
0.9
0.9
1.1
1.5
1.4
1.6
2.1
2.1
3.3
3.5
6
13.6
6.9
4.2
3.6
7.2
9
12.1
NaN
11.5
7.9
6.3
5.9
4.3
6.1
5
4.7
2.5

1st deriv.
mV/mL
NaN
NaN
NaN
NaN
NaN
5.85
4.51
4.57
4.98
5.57
6.12
6.4
6.84
7.31
7.76
8.08
8.42
8.92
9.72
10.58
12.06
13.44
15.57
17.35
16.96
22.42
36.29
64.9
129.96
311.23
520.27
822.53
1165.65
1330.43
1635.55
1915.47
1916.21
1536.17
1263.43
1191.38
774.71
NaN
NaN
NaN
NaN
NaN

Time
s
0
3
8
13
18
23
28
33
38
43
48
53
58
64
69
74
79
84
89
94
99
104
109
114
120
125
130
135
142
158
169
180
190
202
217
232
NaN
247
262
277
292
303
318
330
342
351

Temperature
C
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
NaN
25
25
25
25
25
25
25
25
25

50

Method
Method
Author

DM1471 Peroxide number


schmid

25.10.2007

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
Accompanying stating
Accompanying stating
Condition
Condition
011 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
012 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
013 Record
......
014 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition
015 Conditioning
Type
Interval
Position
Time
Speed
Condition
016 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition
017 Conditioning
Type
Interval
Position
Time
Speed
Condition
018 End of sample
019 Park
Titration stand
Position
Condition

001 Title
Type
General titration
Compatible with
T70 / T90
ID
DM1471
Title
Peroxide number
Author
schmid
Date/Time
10/16/2007 12:37:42 pm
Modified
10/25/2007 11.27:34 am
Modified by
Administrator
Protect
No
SOP
None
002 Sample
Number of IDs
1
ID 1
Olive oil
Entry type
Weight
Lower limit
0.5 g
Upper limit
20 g
Density
1.0 g/mL
Correction factor
1.0
Temperature
25.0C
Entry
Arbitrary
003 Titration stand (Rondo/Tower A)
Type
Rondo/Tower A
Titration stand
Rondo60/1A
Lid handling
No
004 Dispense (normal) [1]
Titrant
AA/Chloroform
Concentration
32
Volume
20 mL
Dosing rate
60.0 mL/min
Condition
No
005 Stir
Speed
40 %
Duration
30 s
Condition
No
006 Dispense (normal) [2]
Titrant
KI
Concentration
63.5
Volume
1 mL
Dosing rate
60.0 mL/min
Condition
No
007 Stir
Speed
30 %
Duration
30 s
Condition
No
008 Stir
Speed
0 %
Duration
60 s
Condition
No
009 Pump
Auxiliary reagent
Water
Volume
50.0 mL
Condition
No
010 Titration (EQP) [1]
Titrant
Titrant
Na 2S 2O 3
Concentration
0.01 mol/L
Sensor
Type
mV
Sensor
DM147
Unit
mV
Temperature acquisition
Temperature acquisition No
Stir
Speed
30%
Predispense
Mode
Volume
Volume
0.1 mL
Wait time
0 s
Control
Control
Cautious
Mode
Redox
Show parameters
Yes
Titrant addition
Dynamic
dE(set value)
6.0 mV
dV(min)
0.005 mL
dV(max)
0.1 mL
Meas. val. acquisition Equilibrium controlled
dE
0.5 mV
dt
2.0 s
t(min)
5.0 s
t(max)
15.0 s

51

Standard
200.0 mV/mL
Positive
0
No
20 mL
No
No
Yes
1
No
No
No
Consumption
mmol
R1=Q
1
M[None]
z[None]
3
No
Yes
No
No
No
Content
meq/kg
R2=(Q-B[1])*C/m
1000
M[None]
z[None]
3
No
Yes
No
No
No

Water
1
10 mL
Actual position
No
No
Fix
1
According to interval
60 s
30%
No
Water
1
10 mL
Actual position
No
No
Fix
1
Conditioning beaker
10 s
30 %
No

Rondo60/1A
Conditioning beaker
No

M370

METTLER TOLEDO

Titer Determination of 0.01 mol/L Na 2S2O3


Titration Excellence Line: Method for the titer determination of 0.01 mol/L Na2S 2O3 by redox titration with
potassium iodate as a primary standard.
1 mL potassium iodate standard
solution, KIO 3
c(KIO3) = 0.01 mol/L

Preparation and Procedures

Substance

Potassium iodate, KIO 3


M=213.99 g/mol ; z = 6

2) About 3 g of sample were dissolved in 20 mL of acetic acid/


chloroform (3:2) The acetic acid/chloroform mixture was added
by the function DISPENSE.

Chemicals

40 mL HCl 0.1 mol/L


1 mL saturated KI solution

3) 1 mL saturated KI solution is added by an additional burette.


The reaction takes place and iodine is formed.

Sample

Titrant

1) Beakers have to be cleaned very well. Fat residues or metal


traces can strongly affect the result.

4) 50 mL deionized water are added by the membrane pump of


Rondo 20.

Sodium thiosulfate, Na2S2O3


c(Na2S2O3)= 0.01mol/L

5) Iodine is titrated with sodium thiosulphate.

Standard

---

127 g KI were dissolved in 100 mL water to obtain the


saturated KI solution. The solution has to be kept in the dark.

Instruments

Titration Excellence T70/T90


Rondo 20 Sample Changer with
PowerShowerTM

Accessories

2 additional dosing units


1 DV1020 and 2 DV1010 Burettes
Glass titration beaker ME-101446
XS205 Balance, LabX 2.6

Indication

DMi147-SC

Chemistry

IO3- + 5 I- + 6 H+ = 3 I2 + 3 H2O
I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6

Calculation

R1=m/(VEQ*c*C)
C=1/(cst*z)
cst = concentration of standard solution

Results

Waste
Waste
disposal
disposal

Inorganic salt solution

Author

Maria-Jos Schmid

Impurities of the solvent are taken into account by a blank value


determination. The blank value determination is done under the
same conditions as the peroxide value determination itself. The
value is stored under B[1].

Remarks
1) Fats and oils undergo changes during storage due to
oxidation with air (oxidative rancidity). The compounds formed
react as peroxides. Their content is commonly expressed as the
"peroxide value" in milliequivalents peroxidic oxygen per kg of
sample.
2) Peroxide values higher than 10 to 20 meq O2/kg are
commonly interpreted as rancidity. Unrefined oils have higher
peroxide values. They are usually in the range between 5 to 20
meq O2/kg.

1) Exactly 60 seconds were allowed for the generation of iodine,


as is requested by the official method (AOAC No. 28.022).
2) Earlier studies, however, had indicated that the generation is
not complete yet at this time. 200 to 300 seconds were found
to yield the highest results. Longer generation times resulted in
low results (secondary reactions between iodine and the oil).
3) The duration of the generation time (time between 'adding the
KI solution' and 'adding the water + starting the titration') is the
critical point for repeatable results.

52

Results
Method:
T147
Titer Na2S2O3
09.10.2007 13:39:16
Start time:
09.10.2007 13:42:03
___________________________________________________________________________________________

Results
No.
1/5
2/5
3/5
4/5
5/5

Comment /
Potassium
Potassium
Potassium
Potassium
Potassium

ID
iodate
iodate
iodate
iodate
iodate

Start time
09.10.2007
09.10.2007
09.10.2007
09.10.2007
09.10.2007

Rx
R1=
R1=
R1=
R1=
R1=

13:42:03
13:55:31
14:08:40
14:21:55
14:35:14

Result
0.901
0.909
0.910
0.908
0.908

Unit
------

Name
Titer
Titer
Titer
Titer
Titer

SQC/Statistics
Rx
Name
n
Mean Value
Unit
s
srel[%]
____________________________________________________________________________________________
R1

Titer

0.906

--

Table of measured values

EQP1

Volume
mL
0
1.143
1.714
2
2.1
2.2
2.3
2.4
2.5
2.6
2.7
2.8
2.9
3
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8
3.9
4
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9
5
5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8
5.9
6
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.79
6.815
6.822
6.829
6.836
6.841
6.846
6.846215
6.851
6.856
6.861
6.866
6.875
6.892
6.919
6.981
7.081

Increment
mL
NaN
1.143
0.571
0.286
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.09
0.025
0.007
0.007
0.007
0.005
0.005
NaN
0.005
0.005
0.005
0.005
0.009
0.017
0.027
0.062
0.1

Signal
mV
18.4
19.6
20.6
21.1
21.3
21.4
21.6
21.8
22
22.2
22.4
22.7
22.9
23.1
23.4
23.7
23.9
24.2
24.5
24.8
25.1
25.4
25.8
26.1
26.5
26.9
27.3
27.7
28.2
28.6
29.1
29.7
30.2
30.8
31.4
32.1
32.8
33.6
34.4
35.3
36.3
37.3
38.5
39.8
41.3
43
45
47.3
50.2
54.1
60.4
71.4
79.3
83.3
87.6
95.1
103.2
111.9
112.3
120.2
127.6
134.1
139.3
144.3
150.4
155.5
161
165.3

0.004

Titration curve
Change
mV
NaN
1.2
1
0.5
0.2
0.1
0.2
0.2
0.2
0.2
0.2
0.3
0.2
0.2
0.3
0.3
0.2
0.3
0.3
0.3
0.3
0.3
0.4
0.3
0.4
0.4
0.4
0.4
0.5
0.4
0.5
0.6
0.5
0.6
0.6
0.7
0.7
0.8
0.8
0.9
1
1
1.2
1.3
1.5
1.7
2
2.3
2.9
3.9
6.3
11
7.9
4
4.3
7.5
8.1
8.7
NaN
8.3
7.4
6.5
5.2
5
6.1
5.1
5.5
4.3

1st deriv.
mV/mL
NaN
NaN
NaN
NaN
NaN
1.86
1.83
1.89
2.1
2.2
2.2
2.36
2.44
2.5
2.56
2.64
2.8
2.8
2.9
3.05
3.2
3.3
3.5
3.64
3.86
4
4.08
4.36
4.54
4.84
5.1
5.4
5.69
6.1
6.44
6.88
7.5
7.99
8.58
9.23
10.07
11.05
12.35
13.82
15.51
17.1
18.16
23.2
36.4
64.74
131.13
293.52
480.39
710.68
987.73
1151.71
1337.28
1610.88
1611.06
1474.04
1174.26
1070.14
881.97
NaN
NaN
NaN
NaN
NaN

Time
s
0
6
11
16
21
26
31
36
41
46
51
56
62
67
72
77
82
87
92
97
102
107
112
117
122
128
133
138
143
148
153
158
163
168
173
178
183
188
194
199
204
209
214
219
224
229
234
239
244
250
258
272
285
294
304
319
334
349
NaN
364
379
394
408
420
434
445
456
466

Temperature
C
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
NaN
25
25
25
25
25
25
25
25
25

53

0.437

Method
Method
Author

T147
Titer Na2S 2O 3
schmid

09.10.2007

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
Accompanying stating
Accompanying stating
Condition
Condition
009 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition
010 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
011 Record
Summary
Results
Raw results
Table of meas. values
Sample data
...............
Method
Series data
Condition
012 End of sample
013 Titer
Titrant
Concentration
TITER=
Limits
Condition
014 Park
Titration stand
Position
Condition
015 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
016 Record
Summary
Results
Raw results
Resource data
Calibration curve
Method
Series data
Condition

001 Title
Type
Titer determination
Compatible with
T70 / T90
ID
T147
Title
Titer Na2S 2O 3
Author
schmid
Date/Time
09.10.2007 13:39:16
Modified
09.10.2007 13:39:16
Modified by
Administrator
Protect
No
SOP
None
LabX SOP
002 Sample (Titer)
Titrant
Na 2S 2O 3
Concentration [mol/L]
0.01
Standard
Potassium iodate
Type of standard
liquid
Entry type
Fixed weight
Volume
1.0 mL
Correction factor
1.0
Temperature
25.0C
003 Titration stand (Rondo/Tower A)
Type
Rondo/Tower A
Titration stand
Rondo60/1A
Lid handling
No
004 Dispense (normal) [1]
Titrant
HCl
Concentration
0.1 mol/L
Volume
40.0 mL
Dosing rate
60.0 mL/min
Condition
No
005 Dispense (normal) [2]
Titrant
KI
Concentration
63.5 mol/L
Volume
1.0 mL
Dosing rate
60.0 mL/min
Condition
No
006 Stir
Speed
30 %
Duration
30 s
Condition
No
007 Stir
Speed [%]
0 %
Duration [s]
60 s
Condition
No
008 Titration (EQP) [1]
Titrant
Titrant
Na 2S 2O 3
Concentration
0.01 mol/L
Sensor
Type
mV
Sensor
DM147
Unit
mV
Temperature acquisition
Temperature acquisition No
Stir
Speed
30 %
Predispense
Mode
Volume
Volume
2.0 mL
Wait time
0 s
Control
Control
Cautious
Mode
Redox
Show parameters
Yes
Titrant addition
Dynamic
dE(set value)
6.0 mV
dV(min)
0.005 mL
dV(max)
0.1 mL
Meas. val. acquisition Equilibrium controlled
dE
0.5 mV
dt
2.0 s
t(min)
5.0 s
t(max)
15.0 s

54

Standard
200.0 mV/mL
Positive
0
No
10 mL
No
No
Yes
1
No
No
No
Water
1
10 mL
Actual position
No
No
Titer
-R1=m/(VEQ*c*C)
1/(cst*z)
M[Potassium iodate]
z[Potassium iodate]
3
No
Yes
No
No
No
No
Per sample
Per sample
Last titration function
No
No
No
No

Na2S 2O 3
0.01 mol/L
Mean[R1]
No
No
Rondo60/1A
Conditioning beaker
No
Mean Titer
-R2=Mean[R1]
1
M[None]
z[None]
3
No
Yes
No
No
No
No
Yes
No
No
No
No
No
No

M371

METTLER TOLEDO

Chloride Determination in Ethanol


Titration Excellence Line: Method for the determination of the chloride content in ethanol by precipitation
titration with silver nitrate.
Sample

Ethanol, 40 g
(approx. 60 mL)

Preparation and Procedures


The samples have been prepared by spiking high purity ethanol
with NaCl solution in order to achieve different choride
concentrations. In this way, several NaCl ethanolic solutions
have been prepared.
General procedure:
1) Weigh accurately ethanolic NaCl solution into the beaker.
2) Add 1 mL 0.001 mol/L NaCl standard solution to spike the
sample.
3) The sample is acidified by adding 1 mL 0.1 mol/L HClO4
using an additional dosing unit. If this is not available,
perchloric acid is added with a manual pipette.
4) Place the beaker on the Rondo sample rack and start the
determination.

Substance

Chloride ions, ClM(Cl) = 35.45 g/mol, z = 1

Chemicals

Perchloric acid, HClO4 (0.1 mol/L)


Sodium chloride, NaCl (0.001 mol/L)

Titrant

Silver nitrate, AgNO 3


c(AgNO 3)= 0.001mol/L

Standard

NaCl solution, 1 mL 0.001 mol/L

Instruments

Titration Excellence T50/T70/T90


Rondo 20 Sample Changer with
PowerShowerTM

Accessories

1 additional dosing unit


2 DV1010 Burettes
Titration beaker ME-101974
XS205 Balance, LabX 2.6

Indication

DMi148-SC

Literature:

Chemistry

NaCl + AgNO 3 = AgCl + NaNO3

1. "Standard Tests Methods for Chloride Ion in Water"


ASTM D512-04

1) Weigh accurately 40 g ethanol into the titration beaker.


2) Add 1 mL 0.001 mol/L NaCl standard solution to spike the
blank sample.
3) 1 mL 0.1 mol/L HClO 4 is added to the blank solution using
an additional dosing unit. if this is not available, perchloric acid
is added using a manual pipette.
4) Place the beaker on the Rondo sample rack and start the
blank value determination.

Remarks

2. METTLER TOLEDO Titration Application M359,


"Chloride content determination in ethanol based on ASTM D512
-04".

Calculation

R = (Q-B[Blank EtOH])*C/m
C = M*100/z, mg/kg

3. "Selected METTLER TOLEDO Methods for Biofuel Analysis"


Application Brochure 36, May 2007, ME-51725070

B[Blank EtOH]:
Solvent blank value, mmol
Results

Waste
Waste
disposal
disposal

Neutralization before final disposal as


heavy metal aqueous solutions.

Author

Maria-Jos Schmid

55

Results
Method:
148
Chloride content in EtOH
12/18/2007 12:17:35 PM
Start time:
12/18/2007 12:17:35 AM
___________________________________________________________________________________________
Sample Data
No. 1/5
No. 2/5
No. 3/5
No. 4/5
No. 5/5
Results
No.
1/5

Comment / ID
Ethanol
Ethanol
Ethanol
Ethanol
Ethanol

Sample size
38.672 g
38.4992 g
38.791 g
38.983 g
38.9095 g

Comment / ID
Ethanol

Start time
12/18/2007 12:17:35 PM

Rx
R1=

Result
0.45

Unit
mg/kg

Name
Content

2/5

Ethanol

12/18/2007 12:17:35 PM

R1=

0.48

mg/kg

Content

3/5

Ethanol

12/18/2007 12:17:35 PM

R1=

0.45

mg/kg

Content

4/5

Ethanol

12/18/2007 12:17:35 PM

R1=

0.45

mg/kg

Content

5/5

Ethanol

12/18/2007 12:17:35 PM

R1=

0.45

mg/kg

Content

SQC/Statistics
Rx
Name
n
Mean Value
Unit
s
srel[%]
____________________________________________________________________________________________
R1

Content

0.46

mg/kg

0.01

2.942

Additional results
Rx
Name
n
Mean Value
Unit
s
srel[%]
____________________________________________________________________________________________
R1
R1
R1

Content
Content
Content

3
5
5

4.61
12.15
23.60

mg/kg
mg/kg
mg/kg

0.06
0.04
0.08

1.253
0.291
0.318

DM140 electrode results


Rx
Name
n
Mean Value
Unit
s
srel[%]
____________________________________________________________________________________________
R1
R1

Content
Content

3
3

0.43
5.60

mg/kg
mg/kg

Table of measured values

EQP1

Volume
mL
0
0.057
0.086
0.1
0.135
0.222
0.422
0.622
0.822
0.943
1.032
1.135
1.213
1.269
1.314
1.355
1.388
1.415
1.435
1.452
1.466
1.479
1.49
1.497
1.504
1.51
1.514
1.519
1.523
1.527
1.531
1.533123
1.535
1.539
1.543
1.548
1.552
1.557
1.568
1.574
1.582
1.592

Increment
mL
NaN
0.057
0.029
0.014
0.035
0.087
0.2
0.2
0.2
0.121
0.089
0.103
0.078
0.056
0.045
0.041
0.033
0.027
0.02
0.017
0.014
0.013
0.011
0.007
0.007
0.006
0.004
0.005
0.004
0.004
0.004
NaN
0.004
0.004
0.004
0.005
0.004
0.005
0.011
0.006
0.008
0.01

Signal
mV
161
160.9
160.4
160.2
160.3
158.7
154.4
149.4
143
137.9
133.8
128.3
122.9
118
113.3
108.2
103.1
97.9
93.2
88.1
83.7
78.3
72.9
68.3
63.3
58
53.5
47.8
42.6
36.7
30.7
27.7
25
17.9
12.7
6.6
1.3
-2
-10.7
-14.9
-19.3
-24.2

0.07
0.55

Titration curve
Change
mV
NaN
-0.1
-0.5
-0.2
0.1
-1.6
-4.3
-5
-6.4
-5.1
-4.1
-5.5
-5.4
-4.9
-4.7
-5.1
-5.1
-5.2
-4.7
-5.1
-4.4
-5.4
-5.4
-4.6
-5
-5.3
-4.5
-5.7
-5.2
-5.9
-6
NaN
-5.7
-7.1
-5.2
-6.1
-5.3
-3.3
-8.7
-4.2
-4.4
-4.9

1st deriv.
mV/mL
NaN
NaN
NaN
NaN
NaN
-15.74
-22.1
-28.41
-37.69
-45.94
-54.77
-68.8
-85.4
-102.81
-124.84
-154.59
-189.02
-231.57
-278.49
-335.6
-401.04
-491.7
-606.1
-704.71
-839.84
-977.31
-1090.51
-1234.77
-1364.69
-1472.06
-1517.89
-1552.6
-1545.86
-1427.73
-1302.62
-1135.67
-1019.34
NaN
NaN
NaN
NaN
NaN

Time
s
0
3
6
9
27
31
36
42
48
56
62
68
75
82
89
97
106
115
124
135
145
157
170
183
196
212
225
243
259
278
296
NaN
314
336
352
369
386
392
411
423
435
447

Temperature
C
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
NaN
25
25
25
25
25
25
25
25
25
25

56

16.279
9.749

Method
Method
Author

148 Chloride content in EtOH


schmid

18.12.2007 12:16:30

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
008 Record
Summary
Results
Raw results
Table of meas. values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d 2E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition
009 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition
010 Conditioning
Type
Interval
Position
Time
Speed
Condition
011 End of sample

001 Title
Type
General titration
Compatible with
T50 / T70 / T90
ID
148
Title
Chloride content in EtOH
Author
schmid
Date/Time
22.11.2007 12:09:49
Modified
18.12.2007 12:16:30
Modified by
schmid
Protect
No
SOP
None
002 Sample
Number of IDs
1
ID 1
Ethanol
Entry type
Weight
Lower limit
1 g
Upper limit
60 g
Density
1.0 g/mL
Correction factor
1.0
Temperature
25.0C
Entry
Arbitrary
003 Titration stand (Rondo/Tower A)
Type
Rondo/Tower A
Titration stand
Rondo60/1A
Lid handling
No
004 Dispense (normal) [1]
Titrant
HClO 4
Concentration
0.1 mol/L
Volume
1 mL
Dosing rate
60.0 mL/min
Condition
No
005 Stir
Speed
40 %
Duration
15 s
Condition
No
006 Titration (EQP) [1]
Titrant
Titrant
AgNO 3
Concentration
0.001 mol/L
Sensor
Type
mV
Sensor
DM148-SC
Unit
mV
Temperature acquisition
Temperature acquisition No
Stir
Speed
30%
Predispense
Mode
Volume
Volume
0.1 mL
Wait time
15 s
Control
Control
Cautious
Mode
Precipitation
Show parameters
Yes
Titrant addition
Dynamic
dE(set value)
5.0 mV
dV(min)
0.004 mL
dV(max)
0.2 mL
Meas. val. acquisition Equilibrium controlled
dE
0.5 mV
dt
2.0 s
t(min)
3.0 s
t(max)
30.0 s
Evaluation and Recognition
Procedure
Standard
Threshold
200.0 mV/mL
Tendency
Negative
Ranges
0
Add. EQP criteria
No
Termination
At Vmax
15 mL
At potential
No
At slope
No
After number
of recognized EQPs
Yes
Number of EQPs
1
Combined termination
criteria
No
Accompanying stating
Accompanying stating
No
Condition
Condition
No

Content
mg/kg
R1=(Q-B[Blank EtOH])*C/m
M*1000/z
M[Chloride]
z[Chloride]
3
No
Yes
No
No
No
No
Per sample
Per sample
Last titration function
Per series
No
Last titration function
Last titration function
No
No
No
No
No
No
No
No
No
No
No
No
Water
1
10 mL
Actual position
No
No
Fix
1
Conditioning beaker
10 s
30%
No

------------------------------------------------------Blank Titration
.......
Predispense
Mode
Volume
Volume
0 mL
Wait time
0 s
.......
007 Calculation R1
Result
Blank Ethanol
Result unit
mmol
Formula
R1=Q
Constant
1
M
M[None]
z
z[None]
Decimal places
5
Result limits
No
Record statistics
Yes
Extra statistical
functions
No
Send to buffer
No
Condition
No
.......
014 Blank
Name
Blank EtOH
Result unit
mmol
Formula
R2=Mean[R1]
.....

57

M372

METTLER TOLEDO

Titer Determination of 0.001 mol/L AgNO3


Titration Excellence Line: Method for the titer determination of 0.001 mol/L AgNO 3 by precipitation reaction
with sodium chloride as a primary standard.
Sample

5 mL sodium chloride iodate standard


solution, NaCl
c(NaCl) = 0.001 mol/L

Preparation and Procedures


1) Beakers have to be cleaned very well.
2) Add 5 mL 0.001 mol/L NaCl standard solution.

Substance

Sodium chloride, NaCl


M=58.44 g/mol ; z = 1

Chemicals

50 mL deionized water
Perchloric acid, HClO4 (0.1 mol/L)
1 mL

Titrant

Silver nitrate, AgNO 3


c(AgNO 3)= 0.01mol/L

Standard

---

Instruments

Titration Excellence T50/T70/T90


Rondo 20 Sample Changer with
PowerShowerTM

Accessories

1 additional dosing units


2 DV1010 Burettes
Glass titration beaker ME-101446
XS205 Balance, LabX 2.6

Indication

DMi148-SC

Chemistry

NaCl + AgNO 3 = AgCl + NaNO3

Calculation

R1=m/(VEQ*c*C)

3) 1 mL 0.1 mol/L HClO 4 is added to the solution using an


additional dosing unit. If this is not available, perchloric acid is
added using a manual pipette.
4) Place the beaker on the Rondo sample rack and start the
determination.

Remarks

C=1/(cst*z)
cst = concentration of standard solution
Results

Waste
Waste
disposal
disposal

Neutralization before final disposal as


heavy metal aqueous solutions.

Author

Maria-Jos Schmid

58

Results
Method:
148T
Titer of AgNO3
11.12.2007 14:27:36
Start time:
11.12.2007 14:27:51
___________________________________________________________________________________________

Results
No.
1/3
2/3
3/3
-/-

Comment / ID
NaCl
NaCl
NaCl

Start time
11.12.2007 14:27:51
11.12.2007 14:37:29
11.12.2007 14:47:01

Titer

0.991

Rx
R1=
R1=
R1=
R2=

Result
0.986
0.993
0.993
0.991

Unit
-----

Name
Titer
Titer
Titer
Mean Titer

SQC/Statistics
Rx
Name
n
Mean Value
Unit
s
srel[%]
____________________________________________________________________________________________
R1
R2

Titer
Mean Titer

3
1

0.991
0.991

---

Table of measured values

EQP1

Volume
mL
0
0.571
0.857
1
1.2
1.4
1.6
1.8
2
2.2
2.4
2.6
2.8
3
3.2
3.4
3.6
3.8
4
4.2
4.4
4.6
4.8
5
5.2
5.362
5.479
5.571
5.655
5.716
5.771
5.818
5.852
5.88
5.906
5.93
5.947
5.963
5.978
5.99
6
6.01
6.014073
6.021
6.03
6.042
6.054
6.066
6.084
6.104
6.128
6.154
6.19

Increment
mL
NaN
0.571
0.286
0.143
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.162
0.117
0.092
0.084
0.061
0.055
0.047
0.034
0.028
0.026
0.024
0.017
0.016
0.015
0.012
0.01
0.01
NaN
0.011
0.009
0.012
0.012
0.012
0.018
0.02
0.024
0.026
0.036

Signal
mV
116.3
113.9
112.4
111.6
110.4
109.1
107.8
106.5
105.1
103.6
102.2
100.6
98.9
97.2
95.4
93.4
91.4
89.2
86.7
84
81
77.7
73.8
69.3
63.7
58.1
53.1
48.4
43
38.3
33.4
27.9
23.2
18.3
13.7
8.1
3.4
-1.4
-6.8
-11.6
-16.4
-21
-23.1
-26.6
-30.8
-36
-41
-45.3
-50.6
-55.5
-60.7
-65.3
-70.5

0.004
NaN

Titration curve
Change
mV
NaN
-2.4
-1.5
-0.8
-1.2
-1.3
-1.3
-1.3
-1.4
-1.5
-1.4
-1.6
-1.7
-1.7
-1.8
-2
-2
-2.2
-2.5
-2.7
-3
-3.3
-3.9
-4.5
-5.6
-5.6
-5
-4.7
-5.4
-4.7
-4.9
-5.5
-4.7
-4.9
-4.6
-5.6
-4.7
-4.8
-5.4
-4.8
-4.8
-4.6
NaN
-5.6
-4.2
-5.2
-5
-4.3
-5.3
-4.9
-5.2
-4.6
-5.2

1st deriv.
mV/mL
NaN
NaN
NaN
NaN
NaN
-6.44
-6.64
-6.8
-7.05
-7.34
-7.66
-8.05
-8.44
-8.85
-9.36
-9.93
-10.72
-11.64
-12.73
-14
-15.66
-17.84
-20.92
-25.48
-32.7
-41.67
-51.27
-62.11
-76.65
-91.36
-110.67
-134.94
-159.1
-185.61
-218.32
-257.57
-292.97
-334.94
-383.1
-420.6
-456.08
-478.18
-479.1
-476.74
-454.01
-411.03
-369.07
-331.99
NaN
NaN
NaN
NaN
NaN

Time
s
0
6
10
13
18
22
26
30
35
39
43
48
52
57
62
66
71
76
82
87
93
98
104
111
118
125
132
140
147
155
163
172
181
191
200
212
223
234
247
259
272
285
NaN
300
312
326
340
352
365
377
389
401
412

Temperature
C
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
NaN
25
25
25
25
25
25
25
25
25
25

59

0.408
NaN

Method
Method
Author

148T
Titer of AgNO3
schmid

11.12.2007

007 Calculation R1
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
008 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain
Condition
009 Record
Summary
Results
Raw results
Table of meas. values
Sample data
E - V
dE/dV - V
log dE/dV - V
d 2E/dV2 - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & dE/dV - V
V - t & dV/dt - t
Method
Series data
Condition
Method
Series data
Condition
010 Conditioning
Type
Interval
Position
Time
Speed
Condition
011 End of sample
012 Titer
Titrant
Concentration
TITER=
Limits
Condition
013 Calculation R2
Result
Result unit
Formula
Constant
M
z
Decimal places
Result limits
Record statistics
Extra statistical
functions
Send to buffer
Condition
014 Record
Summary
Results
Raw results
Resource data
Calibration curve
Method
Series data
Condition

001 Title
Type
Titer determination
Compatible with
T50 / T70 / T90
ID
148T
Title
Titer of AgNO3
Author
schmid
Date/Time
26.11.2007 12:46:07
Modified
11.12.2007 14:27:36
Modified by
Administrator
Protect
No
SOP
None
LabX SOP
002 Sample (Titer)
Titrant
AgNO 3
Concentration [mol/L]
0.001
Standard
NaCl
Type of standard
liquid
Entry type
Fixed weight
Volume
5.0 mL
Correction factor
1.0
Temperature
25.0C
003 Titration stand (Rondo/Tower A)
Type
Rondo/Tower A
Titration stand
Rondo60/1A
Lid handling
No
004 Dispense (normal) [1]
Titrant
HClO 4
Concentration
0.1 mol/L
Volume
1.0 mL
Dosing rate
60.0 mL/min
Condition
No
005 Stir
Speed
30 %
Duration
10 s
Condition
No
006 Titration (EQP) [1]
Titrant
Titrant
AgNO 3
Concentration
0.001 mol/L
Sensor
Type
mV
Sensor
DM148-SC
Unit
mV
Temperature acquisition
Temperature acquisition No
Stir
Speed
30 %
Predispense
Mode
Volume
Volume
1.0 mL
Wait time
0 s
Control
Control
Normal
Mode
Precipitation
Show parameters
Yes
Titrant addition
Dynamic
dE(set value)
5.0 mV
dV(min)
0.004 mL
dV(max)
0.2 mL
Meas. val. acquisition Equilibrium controlled
dE
0.5 mV
dt
2.0 s
t(min)
3.0 s
t(max)
30.0 s
Evaluation and Recognition
Procedure
Standard
Threshold
200.0 mV/mL
Tendency
Negative
Ranges
0
Add. EQP criteria
No
Termination
At Vmax
10 mL
At potential
No
At slope
No
After number
of recognized EQPs
Yes
Number of EQPs
1
Combined termination
criteria
No
Accompanying stating
Accompanying stating
No
Condition
Condition
No

60

Titer
-R1=m/(VEQ*c*C)
1/(cst*z)
M[Sodium chloride]
z[Sodium chloride]
3
No
Yes
No
No
No
Water
1
10 mL
Actual position
No
No
No
Per sample
Per sample
Last titration function
No
Last titration function
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
Fix
1
Conditioning beaker
10 s
30%
No

AgNO3
0.001 mol/L
Mean[R1]
No
No
Mean Titer
-R2=Mean[R1]
1
M[None]
z[None]
3
No
Yes
No
No
No
Yes
Yes
No
No
No
No
No
No

M373

METTLER TOLEDO

Mercaptan Sulfur Content in Kerosine According to ASTM D3227-04a


Titration Excellence Line: The content of (thiol mercaptan) sulfur in kerosine is determined by precipitation
2titration in non aqueous solvent using silver nitrate in 2-propanol. The content is expressed as sulfur, S .
Sample

25 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

25 mL solvent ASTM D3227-04a


2 mL Ethyl mercaptan standard solve.
(see remarks)

2) Before sample analysis a blank value titration is determined


(result is stored as B[ASTM D 3227]).
3) Reagents addition:
- 25 mL solvent ASTM D3227-04a are added into the beaker.
4) A Rondo sample changer with a diaphragm pump was used.

Titrant

Silver nitrate, AgNO 3 , in 2-Propanol


c(AgNO 3) = 0.01 mol/L

Standard

NaCl, c(NaCl) = 0.01 mol/L , 5 mL

Instruments

Titration Excellence T50/T70/T90


2 additional dosing units
Rondo 20 Sample Changer

Accessories

2 DV1010 and 1 DV1020 Burettes


Glass titration beaker ME-101446
XS205 Balance
Olivetti Printer JobJet 210

Indication

DM405-SC

Chemistry

R-SH + AgNO3 = R-S-Ag + HNO 3

Calculation

R1: Mercaptan content (mg/kg)


R1 = (Q-B[ASTM D 3227])*C/(m*d),
C = M*1000/z
B[ASTM D3227]: Blank value of
mercaptan standard solution

Results

Waste
Waste
disposal
disposal

Filtration. The precipitate has to be


classified as special waste. The liquid
phase has to be disposed as organic
waste.

Author

Claudia Schreiner

5) For accurate sampling, kerosene 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
3
METTLER TOLEDO DR45 density meter (d = 0.7905 g/cm ,
25C)
6) The electrode was rinsed and conditioned using the ASTM
D3227 solvent (Functions RINSE, CONDITIONING in special
beaker 2, and CONDITIONING in conditioning beaker).

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.
4) 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:
ASTM D3227-04a, see www.astm.org
METTLER TOLEDO Appl. brochure 34, ME-51 725 066
METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

61

Results
Start time:

27.10.2007

Sample Data
No. 1/6
No. 2/6
No. 3/6
No. 4/6
No. 5/6
No. 6/6

Note / ID
Kerosene
Kerosene
Kerosene
Kerosene
Kerosene
Kerosene

Sample size
25 mL
25 mL
25 mL
25 mL
25 mL
25 mL

Results
No. 1/6
No. 2/6
No. 3/6
No. 4/6
No. 5/6
No. 6/6

Note / ID
Kerosene
Kerosene
Kerosene
Kerosene
Kerosene
Kerosene

Rx
R1=
R1=
R1=
R1=
R1=
R1=

Statistics
Rx
R1

Name
Mercaptans

Result
14.794
14.768
14.696
14.676
14.616
14.623

n
6

Unit
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L

Mean Value
14.70

Table of measured values

Unit
mg/L

Titration curve

62

s
0.07

srel[%]
0.50

Method
Method
Author

m373
Mercaptan sulfur ASTM D3227
METTLER TOLEDO

27.08.2007

Termination
At Vmax [mL]
At potential
At slope
After number
of recognized EQPs
Number of EQPs
Combined termination
criteria

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

General titration
T50 / T70 / T90
m373
Mercaptan sulfur ASTM D3227
METTLER TOLEDO
27.08.2007
--No
None

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

1
Kerosene
Fixed volume
25.0 mL
0.8 g/mL
1.0
25.0C

003 Titration stand


Type
Titration stand

Rondo/Tower A
Rondo60/1A

008 Calculation R1
Result
Result unit
Formula
(m*d)
Constant
M
z
Decimal place
Result limits
Record statistics
Extra statistical
functions
Condition

005 Dispense (normal) [1]


Titrant
Concentration
Volume
Dosing rate

ASTM D3227 solvent


25 mL

Kerosene
1
25 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
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

Yes
1
No

Content
mg/kg
R1=(Q-B[ASTM D3227])*C/
C=M*1000/z
M[Mercaptan sulfur]
z[Mercaptan sulfur]
3
No
No
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

004 Pump
Auxiliary reagent
Volume

3
No
No

30%
480 s

AgNO 3 in 2-Propanol
0.01 mol/L

010 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle [mL]
Position
Drain

mV
DM405-SC
mV

ASTM D3227 solvent


1
15
Actual position
No

No
30%
None
0 s
User
Dynamic
4.0
0.005 mL
0.05 mL
Equilibrium controlled
1.0 mV
2 s
10 s
30 s

011 Conditioning
Type
Interval
Position
Time [s]
Speed [%]

Fix
1
Special beaker 2
30
50

012 Conditioning
Type
Interval
Position
Time [s]
Speed [%]

Fix
1
Conditioning
30
50

013 End of sample

Standard
1000 mV/mL
Positive
0
No

63

M374-A

METTLER TOLEDO

Base Number Determination in Fresh Oils by Conductometric Titration


Titration Excellence Line: Determination of the base number of freshmotor and cutting oils by titration with
0.1 mol/L hydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe (IP400/94).
Sample

Substance
Chemicals

Fresh oils, 0.2-1 g

Alkaline components B,
expressed as mg KOH/g sample
55 mL solvent mixture
Toluene:isopropanol:distilled water
(50% (v/v):49.5%(v/v):0.5%(v/v) )

Titrant

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

Standard

TRIS (THAM), 50 mg

Instruments

Titration Excellence Line, T50/70/90


Conductivity board ME-51109840
Rondo 20 with PowerShower

Accessories

Glass titration beaker ME-101446


2 x SP250 Peristaltic pumps
ME-51108016
Printer, XP205 balance

Indication

InLab718 conductivity probe

Chemistry

Neutralization of all basic components


in oil.
General neutralization reactions:
1) HCl + NaOH = NaCl + H2O
2) HCl + B = HB+ + Cl-

Calculation

Base number (mg KOH/g)


R1= (Q-B[IP400])*C1/m
C1= 56.1
B[IP400]: solvent blank value

Preparation and Procedures


1) Titrant preparation:
If not commercially available, the titrant can be prepared by
adding 9 mL 37% v/v HCl and filling up to 1 L with 2-propanol
(isopropanol).
2) Depending on the BN number, 0.2-1 g oil are weighed into a
glass titration bealer. The higher the BN, the lower the sample
size.
3) 60 mL solvent are added automatically by a peristaltic
pump.
4) The titration is started after 60 s stirring time at 50% in order
to achieve a complete dissolution of the sample.

Remarks
1) To ensure a complete rinsing of the probe, the following
cleaning procedure was defined (see method):
1.1 Drain: The sample beaker is emptied
1.2 Pump: 35 mL of solvent are dosed
1.3 Stir:
To remove all residuals, the solvent is stirred 20 s at 70%.
1.4 Drain: The solvent is pumped out.
1.5 Rinse: Finally, the titration stand is rinsed two times after
each sample using the rinsing cycles defined in the method
function "Rinse".

Literature:
1) IP400/94 Standard, British Institute of Petroleum
(Now: Energy Institute, http://www.energyinst.org.uk/)
2) METTLER TOLEDO Applications M252/M253. and M099/
M100.

Results

Waste
Waste
disposal
disposal

Organic solvent waste


(aromatic solvents)

Author

Hans-Joachim Muhr

3) This application does not replace the standard.

64

Results
Method ID:
Date / Time:
Samples
Nr.
1
2
3
4
5
6

IP400B
09/20/2006 01:43:12 pm

Sample series ID
User name

ID
13

Sample size and results


0.2584 g
R1(BN)
38.798
R2(Titration time)
2.570
0.2535 g
R1(BN)
38.309
R2(Titration time)
2.470
0.2511 g
R1(BN)
38.490
R2(Titration time)
2.470
0.2541 g
R1(BN)
38.380
R2(Titration time)
2.570
0.2521 g
R1(BN)
38.560
R2(Titration time)
2.470
0.2 g
R1(BN)
38.263
R2(Titration time)
2.570

13
13
13
13
13

Statistics
R1(BN)
Number of samples
Mean value
s
srel

13
Administrator

mg KOH/g
min
mg KOH/g
min
mg KOH/g
min
mg KOH/g
min
mg KOH/g
min
mg KOH/g
min

6
38.467 mg KOH/g
0.196 mg KOH/g
0.511 %

TBN according to ASTM D4739:


40.4 mg KOH/g
--------------------------------------------------------------------------------------------Different samples of fresh oils
Sample

Size / g

Base number
mg KOH/g

s
mg KOH/g

srel
%

TBN ASTM D4739


mg KOH/g

CF15

0.5

18.947

0.106

0.559

20.0

58420

1.0

10.886

0.034

0.316

10.8

Table of measured values

Titration curve

65

Method
Method
Version

IP400B
Conductometric BN
09/20/2006 01:43:12 pm

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

General titration
T50/T70/T90
IP400B
Conductometric BN
Administrator
08/28/2006 03:09:17 pm
09/20/2006 01:43:12 pm
Administrator
No
None

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

1
13
Weight
0.0 g
5.0 g
1.0 g/mL
1.0
25.0 C
Before

003 Titration stand (Rondo/Tower A)


Type
Titration stand
Lid handling

Rondo/Tower A
Rondo60/1A
No

004 Pump
Auxiliary reagent
Volume
Condition

IP400 Solvent
55 mL
No

005 Stir
Speed
Duration
Condition

50 %
60 s
No

006 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
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
Steepest jumps
Termination
At Vmax
At potential
At slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition

007 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition

BN
mg KOH/g
R1=(Q-B[IP400])*C/m
56.1
M[None]
z[None]
3
No
Yes
No
No

008 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition

Titration time
min
R2=t
-M[None]
z[None]
3
No
No
No
No

009 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
2
2
d E/dV - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & DE/dV - V
V - t & dV/dt - V
Method
Series data
Condition

HCl in 2-Propanol
0.1 mol/L
Conductivity
InLab 718
S
No

Per sample
Per sample
Per sample
Last titration function

Per sample
No
Last titration function

No
No
Last titration function

No
No
No
No
No
No
No
No
No
No

010 Drain
Drain pump
Drain volume
Condition

SP250
60 mL
No

011 Pump
Auxiliary reagent
Volume
Condition

IP400 Solvent
35 mL
No

012 Stir
Speed
Duration
Condition

70 %
20 s
No

013 Drain
Drain pump
Drain volume
Condition

SP250
40 mL
No

014 Rinse
Auxiliary reagent
Rinse cycles
Vol. per cycle
Position
Drain
Drain pump
Condition

IP400 Solvent
2
10 mL
Actual position
Yes
SP250
No

30 %
None
0 s
User
Incremental
0.1 mL
Equilibrium controlled
0.5 S
1.0 s
10 s
20 s
Segmented
0.5 S mL2
0
Steepest jump
1
4 mL
No
No
Yes
1
No

015 End of sample

No
No

66

M374-B

METTLER TOLEDO

Base Number Determination in Used Oils by Conductometric Titration


Titration Excellence Line: Determination of the base number of various used oils by titration with 0.1 mol/L
hydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe according to IP400/94.
Sample

Substance
Chemicals

Used oils, 2-5 g

Alkaline components B,
expressed as mg KOH/g sample
60 mL solvent mixture
Toluene:isopropanol:distilled water
(50% (v/v):49.5%(v/v):0.5%(v/v) )

Preparation and Procedures


1) Titrant preparation:
If not commercially available, the titrant can be prepared
manually by adding 9 mL 37% v/v HCl and filling up to 1 L
with 2-propanol (isopropanol).
2) 2-4 g oil are weighed into a glass titration bealer.
3) 60 mL solvent are added automatically by a peristaltic
pump.
4) The titration is started after 300 s stirring time at 50% in
order to achieve a complete dissolution of the sample.

Titrant

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

Standard

TRIS (THAM), 50 mg

Instruments

Titration Excellence Line, T50/70/90


Conductivity board ME-51109840
Rondo 20 Sample Changer

Accessories

Glass titration beaker ME-101446


SP250 Peristaltic pump ME-51108016
Printer, XP205 balance

Indication

InLab718 conductivity probe

1) The conductivity probe is conditioned during 10 s in the fixed


conditioning beaker of the Rondo 20 sample changer.

Chemistry

Neutralization of all basic components


in oil.
General neutralization reactions:
1) HCl + NaOH = NaCl + H2O
2) HCl + B = HB+ + Cl-

2) Most oil samples may create sticky residues. In this case, it


is necessary to additionally clean the conductivity probe with a
paper tissue soaked in solvent mixture. Afterwards, the probe is
rinsed again with solvent mixture to remove the last impurities.

Calculation

Base number (mg KOH/g)


R1= (Q-B[IP400])*C1/m
C1= 56.1

1) IP400/94 Standard, British Institute of Petroleum


(Now: Energy Institute, http://www.energyinst.org.uk/)

B[IP400]: solvent blank value

2) METTLER TOLEDO Applications M252/M253, and M099/


M100.

Remarks

Literature:

3) This application does not replace the standard.

Results

Waste
Waste
disposal
disposal

Organic solvent waste


(aromatic solvents)

Author

Tobias Beckmann, MT-D

67

Results
Method ID:
Date / Time:

AIP400
14/08/2007 12:00:28

Sample series ID
User name

-Administrator

ID
WC 433591

Sample size and results


2.0134 g
R1(BN)
6.373
R2(Titration time)
5.070
2.0717 g
R1(BN)
6.396
R2(Titration time)
5.230
2.2171 g
R1(BN)
6.438
R2(Titration time)
5.500

Summary
Samples
Nr.
1

WC 433591

WC 433591

Statistics
R1(BN)
Number of samples
Mean value
s
srel

mg KOH/g
min
mg KOH/g
min
mg KOH/g
min

3
6.402 mg KOH/g
0.033 mg KOH/g
0.515 %

--------------------------------------------------------------------------------------------Different samples of used oils


Sample
Size / g
n
Base number
mg KOH/g

srel
%

WC 529913

2.2

5.780

0.062

1.068

WC 526402

2.2

4.599

0.299

4.974

WC 471807

2.3

4.571

0.290

6.349

WC 457700

2.2

3.250

0.101

3.095

WC 541628

2.1

1.820

0.007

0.405

Table of measured values

Titration curve

68

Method
Method
Version

AIP400
Conductometric BN
14/08/2007 12:00:28

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

General titration
T50/T70/T90
AIP400
Conductometric BN
Administrator
14/08/2007 09:19:49
14/08/2007 12:00:28
Administrator
No
None

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

1
WC 433591
Weight
0.0 g
5.0 g
1.0 g/mL
1.0
25.0 C
Before

003 Titration stand (Rondo/Tower A)


Type
Titration stand
Lid handling

Rondo/Tower A
Rondo60/1A
No

004 Pump
Auxiliary reagent
Volume
Condition

IP400
60 mL
No

005 Stir
Speed
Duration
Condition

50 %
300 s
No

006 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
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
Steepest jumps
Termination
At Vmax
At potential
At slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition

007 Conditioning
Type
Interval
Positioning
Time
Speed
Condition

Fix
1
Conditioning beaker
10 s
30 %
No

008 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

BN
mg KOH/g
R1=(Q-B[IP400])*C/m
56.1
M[None]
z[None]
3
No
Yes
No
No
No

009 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

Titration time
min
R2=t
-M[None]
z[None]
3
No
No
No
No
No

010 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
2
2
d E/dV - V
BETA - V
E - t
V - t
dV/dt - t
T - t
E - V & DE/dV - V
V - t & dV/dt - V
Method
Series data
Condition

HCl in 2-Propanol
0.1 mol/L
Conductivity
InLab 718
S
No
30 %
None
0 s
User
Incremental
0.05 mL
Equilibrium controlled
1.0 S
2 s
3 s
15 s

Per series
Per sample
Per sample
Last titration function

Per sample
No
Last titration function

No
No
Last titration function

No
No
No
No
No
No
No
No
No
No

011 End of sample


---------------------------------------------------Blank value determination and storage as B[IP400]
......
Control
Control
User
Titrant addition
Incremental
dV
0.01 mL
Meas. val. acquisition
Equilibrium controlled
dE
0.5 S
dt
1.0 s
t(min)
10 s
t(max)
20 s
Evaluation and Recognition
Procedure
Segmented
Threshold
0.5 S mL2
Ranges
0
Add. EQP criteria
Steepest jump
Steepest jumps
1
Termination
At Vmax
1.5 mL
At potential
No
At slope
No
After number of recognized EQPs
Yes
Number of EQPs
1

Segmented
2
10 S mL
0
Steepest jump
1
10 mL
No
No
Yes
1
No
No
No

69

M375

METTLER TOLEDO

Titer of 0.1 mol/L HCl in 2-Propanol by Conductometric Titration (IP400)


Titration Excellence Line: Titer determination of 0.1 mol/L hydrochloric acid in 2-propanol (isopropanol, IPA)
by conductometric titration using TRIS (Tris-hydroxymethyl-aminomethane, THAM) as a primary standard.
Sample

Substance
Chemicals

Primary standard:
TRIS (THAM), 50-80 mg

TRIS, Tris-hydroxymethyl-aminomethane
M=121.14, z=1
60 mL solvent mixture
Toluene:isopropanol:distilled water
(50% (v/v):49.5%(v/v):0.5%(v/v) )

Preparation and Procedures


1) Titrant preparation:
If not commercially available, the titrant can be prepared
manually by adding 9 mL 37% v/v HCl and filling up to 1 L
with 2-propanol (isopropanol).
2) 50-80 mg TRIS are weighed into a glass titration bealer.
3) 60 mL solvent are added automatically by a peristaltic
pump.
4) The titration is started after 120 s stirring in order to achieve
a complete dissolution of TRIS.

Titrant

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

Standard

--

Instruments

Titration Excellence Line, T50/70/90


Conductivity board ME-51109840
Rondo 20 Sample Changer

Accessories

Glass titration beaker ME-101446


SP250 Peristaltic pump ME-51108016
Printer, XP205 balance

Indication

InLab718 conductivity probe

Chemistry

Neutralization of all basic components


in oil.
General neutralization reactions:
1) HCl + NaOH = NaCl + H2O
2) HCl + B = HB+ + Cl-

Remarks

Calculation

Titer determination
R = m/(VEQ*c*C)
C = M/(10*p*z)

1) The conductivity probe is conditioned during 10 s in the fixed


conditioning beaker of the Rondo 20 sample changer.

Literature:
1) IP400/94 Standard, British Institute of Petroleum
(Now: Energy Institute, http://www.energyinst.org.uk/)
2) METTLER TOLEDO Applications M099/M100, M253
3) This application does not replace the standard.

p: purity of solid primary standard [%]


Results

Waste
Waste
disposal
disposal

Organic solvent waste


(aromatic solvents)

Author

Tobias Beckmann, MT-D

70

Results
Method ID:
Date / Time:

AIP8014
14/08/2007 10:01:04

All results
Method ID
Sample 1/3
R1
Sample 2/3
R1
Sample 3/3
R1
Statistics
Method ID
R1 (Titer)
Number of samples
Mean value
s
srel
All results
R2(mean Titer)

Sample series ID
User name

-Administrator

AIP8014
TRIS
0.986
TRIS
0.993
TRIS
0.995

AIP8014
3
0.991
0.005
0.477

0.991

Table of measured values

Titration curve

71

Method
Method
Version

AIPB8014
Titer HCl in 2-Propanol
14/08/2007 10:01:04

001 Title
Type
Compatible with
ID
Titel
Author
Date / Time
Modified at
Modified by
Protect
SOP
002 Sample (Titer)
Titrant
Concentration
Standard
Type of standard
Entry Type
Low limit
Upper limit
Correction factor
Temperature
Entry
003 Titration stand (Rondo/Tower A)
Type
Titration stand
Lid handling

General titration
T50/T70/T90
AIP8014

Fix
1
Conditioning beaker
10 s
30 %
No

008 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

Titer
-R1=m/(VEQ*c*C)
M/(10*p*z)
M[TRIS]
z[TRIS]
3
No
Yes
No
No
No

Titer HCl in 2-Propanol

Administrator
14/08/2007 09:19:49
14/08/2007 10:01:04
Administrator
No
None

HCl in 2-Propanol
0.1 mol/L
TRIS
Solid
Weight
0.05 g
0.08 g
1.0
25.0 C
Arbitrary

009 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V

Rondo/Tower A
Rondo60/1A
No

004 Pump
Auxiliary reagent
Volume
Condition

IP400
60 mL
No

005 Stir
Speed
Duration
Condition

40 %
120 s
No

006 Titration (EQP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
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
Accompanying stating
Accompanying stating
Condition
Condition

007 Conditioning
Type
Interval
Positioning
Time
Speed
Condition

d E/dV - V
...........
Method
Series data
Condition

No
Per sample
Per sample
Last titration function

No
No
Last titration function

No
No
Last titration function

No
No
No

010 End of sample

HCl in 2-Propanol
0.1 mol/L
Conductivity
InLab 718
S
No
30 %
None
0 s
User
Incremental
0.1 mL
Equilibrium controlled
1.0 S
2 s
3 s
30 s
Segmented
10 S mL2
0
No
10.0 mL
No
No
Yes
1
No
No
No

72

011 Titer
Titrant
Concentration
TITER=
Limits
Condition

HCl in 2-Propanol
0.1 mol/L
Mean[R1]
No
No

012 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition

Mean Titer
-R2=Mean[R1]
1
M[None]
z[None]
3
No
Yes
No
No
No

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

No
Yes
No
No
No
No
No
No

M376

METTLER TOLEDO

Anionic Content in Shower Gels by Potentiometric Two-Phase Titration


Titration Excellence Line: Determination of anionic surfactant content in shower gels by titration with 0.004
mol/L Hyamine 1622 in a two-phase mixed system using a DS800 TwoPhase electrode according to DIN
EN 14480-2004.
Sample

Substance

5 mL aliquots of aqueous solutions


prepared with shower gels and
shampoo.
Anionics as Na-dodecylsulfate, C12 H25 NaO4S

M(SDS)=288.38 g/mol, z=1

Chemicals

40 mL deion water
20 mL MIBK:EtOH 1:1 solvent

Titrant

Hyamine 1622, c(Hyamine)=0.004 M


Hydrochloric acid, HCl, c(HCl)=0.1 M

Standard

SDS (for Hyamine), THAM (for HCl)

Instruments

Titration Excellence Line T70/T90


2 additional dosing units
Rondolino Sample Changer

Accessories

Titration beaker ME-101974

Indication

DS800 TwoPhase surfactant electrode,


InLab RReference , DG111-SC

Chemistry

SDS- + Hyamine + = SDS-Hyamine

Preparation and Procedures


Note: MIBK is an organic solvent which is strongly and
intensively smelling. It is recommended to work in a fume hood.
1) 40 mL of deionised water are added to the 5 mL sample.
2) The titration beaker is placed on the Rondolino sample
changer.
3) The pH value is first adjusted to pH 3 with HCl by means of
the second titration burette (EN DIN 14480).
4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensed
by means of an additional dosing unit.
MIBK: Methylisobutylketone (4-Methylpentan-2-one)
EtOH: Ethanol
5) To obtain a homogeneous emulsion the solution is stirred at
a high speed (80%).
6) The anionic surfactant content is expressed as SDS content, i.
e. the molecular mass of SDS is used for the calculation.
DS800 TwoPhase surfactant sensitive electrode:
1) Fill the DS800 TwoPhase and the electrode tip with the
electrolyte.
2) Screw the electrode tip onto the shaft.
3) Shake the electrode 2-3 times to avoid the presence of air
bubbles into the electrode tip. Rinse it with deion. water.
4) Condition the electrode first in deionised water for e.g. 15
minutes, and then perform 1-2 test titrations with the sample.

Remarks

Calculation

R1=Q[2]*C/m
C= M/(10*z)

1) The determination of anionic surfactants is performed at pH 3


according to DIN EN 14480. This is perfomed to avoid
interference due to the presence of free fatty acids (FFA) in the
products, otherwise the result will be higher. In fact, at pH 3 the
FFA are fully protonated, therefore they can not be titrated with
hyamine.
2) Standard solutions of the different products are prepared by
dissolving in 1 L volumetric flask approx. 5-10 g of the
products. The resulting concentration in g/L = mg/mL is stored
as auxiliary value e.g. H[Anionic] in the titrator.
3) The electrode is cleaned and conditioned after each sample in
deionised water in the conditioning beaker of Rondolino
(Position 5: 120 s).
4) When working with the LabX Software, select "Rondolino
Mode" in the LabX window at the PC and activate it.

Results

Waste
Waste
disposal
disposal

Neutralize the sample solution before


final disposal as organic solvent.

Author

C. De Caro

Literature:
1) DIN EN 14480-2004
2) METTLER TOLEDO Application brochure 34,
"Selected METTLER TOLEDO methods for Titration Excellence
Line", ME-51 725 066.
3) METTLER TOLEDO Application brochure 22,
"Surfactant titration", ME-51 725 015.

73

Results
Method ID:
Date / Time:

0214
09/07/2007 07:50:32

Sample series ID
User name

All results
Method ID
Sample 1/5
R1
Sample 2/5
R1
Sample 3/5
R1
Sample 4/5
R1
Sample 5/5
R1

-Administrator

0214LAS
0214
24.726 %
0214
24.677 %
0214
24.669 %
0214
24.622 %
0214
24.641 %

Statistics
Method ID
R1 (Content)
Number of samples
Mean value
s
srel

0214LAS
5
24.667 %
0.040 %
0.161 %

---------------------------------------------------------------------------------------------Different samples
Sample type
exp./%SDS
n
Result
s
srel
content
/%SDS
/%SDS
/%
0214

viscous

24

5
8

24.667
24.494

0.040
0.033

0.161
0.136

pH 3
pH 5.5

H[0214]=0.005056 g/L

0273

viscous

25

8
7

25.290
25.291

0.034
0.031

0.136
0.123

pH 3
pH 3

H[0273]=0.005019 g/L

0411

powder

20

3
5

20.274
20.303

0.055
0.073

0.273
0.359

pH 3
pH 3

H[0411]=0.010012 g/L

0193

formulation 8-9

5
6

9.303
9.253

0.031
0.048

0.332
0.521

pH 3
pH 3

H[0193]=0.010033 g/L

0Liq

liquid det. 5-15

6
9

7.317
7.365

0.060
0.080

0.817
1.092

pH 3
pH 3

H[0Liq]=0.00805 g/L

Table of measured values

Titration curve

74

Method
Method
Version

0214
SDS content potentiometric
09/07/2007 07:50:32

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

General titration
T70/ T90
0214
SDS content potentiometric

Administrator
06/07/2007 17:56:59
09/07/2007 07:50:32
No
None

002 Sample
Number of IDs
ID 1
Entry Type
Volume
Density
Correction factor
Temperature [C]

1
0214
Fixed volume
5 mL
1.0
1.0
25.0

003 Titration stand (Rondolino TTL)


Type
Titration stand

Rondolino TTL
Rondolino TTL 1

004 Stir
Speed
Duration
Condition

35 %
45 s
No

005 Titration (EP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
Wait time [s]
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
Accompanying stating
Accompanying stating
Condition
Condition

008 Titration (EQP) [2]


Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
Volume
Wait time [s]
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Mode
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
At slope
After number of recognized EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition

HCl
0.1 mol/L
pH
DG111-SC
pH
No

Hyamine 1622
0.004 mol/L
mV
DS800
mV
No
80 %
Volume
1.5 mL
15 s
User
Dynamic
8.0 mV
0.01 mL
0.4 mL
Equilibrium controlled
1.0 mV
1 s
5 s
30 s
Standard
100 mV/mL
Positive
0
No
8
No
No
No
No
No
No

30 %
009 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition

None
0
Absolute
Negative
3 pH
2.0 pH
10.0 mL/min
500 L/min
Yes
0 s
10.0 mL
Infinite

010 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d 2E/dV2 - V
....
Method
Series data
Condition

No
No

006 Dispense (normal) [1]


Titrant
Concentration
Volume
Dosing rate
Condition

MIBK-EtOH 1:1
1
20 mL
60.0 mL/min
No

007 Stir
Speed
Duration
Condition

80 %
60 s
No

Content
%
R1=Q[2]*C/(m*H[0214])
M/(10*z)
M[Sodium dodecylsulfate]
z[Sodium dodecylsulfate]
3
No
Yes
No
No

No
Per sample
Per sample
Last titration function

Yes
No
Last titration function
Last titration function

No
No
No
No
No

011 End of sample


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

75

Yes
Yes
No
No
No
No
No
No

M377

METTLER TOLEDO

Anionic Content in Cutting Oils by Potentiometric Two-Phase Titration


Titration Excellence Line: Determination of anionic surfactant content in cutting oils by titration with 0.004
mol/L Hyamine 1622 in a two-phase mixed system using a DS800 TwoPhase electrode according to DIN
EN 14480-2004 (pH 3).
Sample

Substance

0.1-0.3 g cutting oil, depending on


anionic surfactant content.

Anionics as Na-dodecylsulfate, C12 H25 NaO4S

M(SDS)=288.38 g/mol, z=1

Chemicals

40 mL deion water
20 mL MIBK:EtOH 1:1 solvent

Titrant

Hyamine 1622, c(Hyamine)=0.004 M


Hydrochloric acid, HCl, c(HCl)=1 M
Sodium hydroxide, c(NaOH)=1 M

Standard

SDS (for Hyamine)

Instruments

Titration Excellence Line T70/T90


2 additional dosing units
Rondolino Sample Changer

Accessories

Titration beaker ME-101974

Indication

DS800 TwoPhase surfactant electrode,


InLab RReference , DG111-SC

Chemistry

SDS- + Hyamine + = SDS-Hyamine

Preparation and Procedures


Note: MIBK is an organic solvent which is strongly and
intensively smelling. It is recommended to work in a fume hood.
1) 40 mL of deionised water are added to the 5 mL sample.
2) The titration beaker is placed on the Rondolino sample
changer.
3) The pH value is adjusted to pH 3 (DIN EN 14480) with HCl
or to pH 11 with NaOH by means of the second titration burette.
4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensed
by means of an additional dosing unit.
MIBK: Methylisobutylketone (4-Methylpentan-2-one)
EtOH: Ethanol
5) To obtain a homogeneous emulsion the solution is stirred at
a high speed (80%).
6) The anionic surfactant content is expressed as SDS content, i.
e. the molecular mass of SDS is used for the calculation.
DS800 TwoPhase surfactant sensitive electrode:
1) Fill the DS800 TwoPhase and the electrode tip with the
electrolyte.
2) Screw the electrode tip onto the shaft.
3) Shake the electrode 2-3 times to avoid the presence of air
bubbles into the electrode tip. Rinse it with deion. water.
4) Condition the electrode first in deionised water for e.g. 15
minutes, and then perform 1-2 test titrations with the sample.

Remarks

Calculation

R1=Q[2]*C/m
C= M/(10*z)

1) The determination of anionic surfactants is performed at pH 3


according to DIN EN 14480. This is done in order to avoid
interference due to the presence of free fatty acids (FFA) in the
products, otherwise the result will be higher. In fact, at pH 3 the
FFA are fully protonated, therefore they can not be titrated with
hyamine.
2) In the case where samples contain anionic surfactants with
R-COOH end groups, it is necessary to titrate the sample at an
alkaline pH value of e.g. pH 11 (see also DIN EN 14669) to be
able to precipitate them with Hyamine.
3) The electrode is cleaned and conditioned after each sample in
deionised water in the conditioning beaker of Rondolino
(Position 5: 120 s).
4) When working with the LabX Software, select "Rondolino
Mode" in the LabX window at the PC and activate it.

Results

Waste
Waste
disposal
disposal

Neutralize the sample solution before


final disposal as organic solvent.

Author

C. De Caro

Literature:
1) DIN EN 14480-2004 and 14669-2005
2) METTLER TOLEDO Application brochure 34,
"Selected METTLER TOLEDO methods for Titration Excellence
Line", ME-51 725 066.
3) METTLER TOLEDO Application brochure 22,
"Surfactant titration", ME-51 725 015.

76

Results
Method ID:
m377
Date / Time:
11/12/2007 09:02:23 am
Summary
Samples
No.
ID
1
00883-03
2

00883-03

00883-03

00883-03

00883-03

00883-03

Sample series ID
User name

Sample size
0.1773 g
R1(Anionics
0.1873 g
R1(Anionics
0.1537 g
R1(Anionics
0.2101 g
R1(Anionics
0.1782 g
R1(Anionics
0.1624 g
R1(Anionics

-Administrator

and results
Content)

4.91 %

Content)

4.88 %

Content)

4.82 %

Content)

4.86 %

Content)

4.86 %

Content)
4.88 %
Statistics
R1 (Anionics Content)
Number of samples
6
Mean value
4.87 %
s
0.03 %
srel
0.636 %
===========================================================================================
Various samples
n
Result/%SDS
s/%SDS
srel/%
------------------------------------------------------------------00883-03
6
4.87
0.03
0.576
pH 3
01325-01

3
5

2.73
2.66

0.02
0.02

0.559
0.734

pH 3
pH 3

02800-01
C93 18656

2.01

0.01

0.733

pH 3

6
6
6

61.07
61.14
61.48

0.47
0.31
0.48

0.764
0.506
0.783

pH 3
pH 3
pH 3

V43 18571

6
6
6

30.93
30.96
30.92

0.05
0.08
0.04

0.155
0.256
0.141

pH 3
pH 3
pH 3

11675-01

4
6
4
6

13.57
13.61
4.49
4.55

0.17
0.20
0.05
0.01

1.228
1.486
1.155
0.231

pH
pH
pH
pH

01125-02

Table of measured values

11
11
11
11

Titration curve

77

0.004
0.01
0.004
0.01

M
M
M
M

Hyamine
CPC
Hyamine
CPC

Method
Method
Version

m377
SDS content potentiometric
11/12/2007 09:02:23 am

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

General titration
T70/ T90
m377
SDS content potentiometric

Administrator
11/12/2007 07:22:42 am
11/12/2007 09:02:23 am
No
None

002 Sample
Number of IDs
ID 1
Entry Type
Lower limit
Upper limit
Density
Correction factor
Temperature [C]
Entry

1
00883-03
Weight
0 g
5 g
1.0 g/mL
1.0
25.0C
Before

003 Titration stand (Rondolino TTL)


Type
Titration stand

Rondolino TTL
Rondolino TTL 1

004 Stir
Speed
Duration
Condition

35 %
60 s
No

005 Titration (EP) [1]


Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
Wait time [s]
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
Accompanying stating
Accompanying stating
Condition
Condition
006 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate
Condition

008 Titration (EQP) [2]


Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
Wait time [s]
Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Mode
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
At slope
After number of recognized EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition

HCl
1 mol/L
pH
DG111-SC
pH
No

009 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition

35 %
None
0
Absolute
Negative
3 pH
2.0 pH
10.0 mL/min
500 L/min

010 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
log dE/dV - V
d 2E/dV2 - V
....
Method
Series data
Condition

Yes
0 s
10.0 mL
Infinite
No
No

MIBK-EtOH 1:1
1
20 mL
60.0 mL/min
No

Hyamine 1622
0.004 mol/L
mV
DS800
mV
No
80 %
None
0 s
User
Dynamic
8.0 mV
0.1 mL
0.5 mL
Equilibrium controlled
0.5 mV
2 s
8 s
45 s
Standard
30 mV/mL
Positive
0
No
20 mL
No
No
No
No
No
No

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

No
Per sample
Per sample
Last titration function

Yes
No
Last titration function
Last titration function

No
No
No
No
No

011 End of sample


007 Stir
Speed
Duration
Condition

80 %
60 s
No

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

78

Yes
Yes
No
No
No
No
No
No

M378

METTLER TOLEDO

Titer Determination of Hyamine by Potentiometric Two-Phase Titration


Titration Excellence Line: Titer determination of 0.004 mol/L Hyamine 1622 with sodium dodecylsulfate
(SDS) as a standard in a two-phase mixed system using a DS800 TwoPhase surfactant sensitive electrode
according to DIN EN 14480-2004.
5 mL 0.004 SDS
SDS: Sodium dodecylsulfate

Preparation and Procedures

Substance

Sodium dodecylsulfate, C12 H25 NaO4S


M(SDS)=288.38 g/mol, z=1

Chemicals

40 mL deion water
20 mL MIBK:EtOH 1:1 solvent

Titrant

Hyamine 1622, c(Hyamine)=0.004 M


Hydrochloric acid, HCl, c(HCl)=0.1 M

1) 40 mL of deionised water are added to the 5 mL sample.


2) The titration beaker is placed on the Rondolino sample
changer.
3) The pH value is first adjusted to pH 3 with HCl by means of
the second titration burette (EN DIN 14480).
4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensed
by means of an additional dosing unit.
MIBK: Methylisobutylketone (4-Methylpentan-2-one)
EtOH: Ethanol
5) To obtain a homogeneous emulsion the solution is stirred at
a high speed (80%).

Standard

For HCl: THAM (TRIS)

Instruments

Titration Excellence Line T70/T90


2 additional dosing units
Rondolino Sample Changer

Accessories

Rondolino Sample Changer


Titration beaker ME-101974

Indication

DS800 TwoPhase surfactant electrode,


InLab RReference , DG111-SC

Rondolino:

Chemistry

SDS- + Hyamine + = SDS-Hyamine

1) The electrode is cleaned and conditioned after each sample in


deionised water in the conditioning beaker of Rondolino
(Position 5: 120 s).

Sample

Note: MIBK is an organic solvent which is strongly and


intensively smelling. It is recommended to work in a fume hood.

DS800 TwoPhase surfactant sensitive electrode:


1) Fill the DS800 TwoPhase and the electrode tip with the
electrolyte.
2) Screw the electrode tip onto the shaft.
3) Shake the electrode 2-3 times to avoid the presence of air
bubbles into the electrode tip. Rinse it with deion. water.
4) Condition the electrode first in deionised water for e.g. 15
minutes, and then perform 1-2 test titrations with the sample.

Remarks

2) When working with the LabX Software, select "Rondolino


Mode" in the LabX window at the PC and activate it.

Calculation

Titer:
R=m/(VEQ[2]*c[2]*C)
C=1/(cst*z)
Note: "cst" is the concentration of the
SDS standard solution.

Results

Waste
Waste
disposal
disposal

Organic solvent

Author

C. De Caro

Literature:
1) DIN EN 14480-2004
2) METTLER TOLEDO Application brochure 34,
"Selected METTLER TOLEDO methods for Titration Excellence
line", ME-51 725 066.
3) METTLER TOLEDO Application brochure 22,
"Surfactant titration", ME-51 725 015.

79

Results
Method ID:
Date / Time:

414Titer
06/07/2007 17:15:16

Sample series ID
User name

-Administrator

ID

Sample size and results

SDSTiter414

SDSTiter414

SDSTiter414

SDSTiter414

5 mL
R1 (Titer)
5 mL
R1 (Titer)
5 mL
R1 (Titer)
5 mL
R1 (Titer)
5 mL
R1 (Titer)
5 mL
R1 (Titer)

Summary
Samples
No.

SDSTiter414

SDSTiter414

1.002013

1.001679

1.000487

0.997958

0.998080

0.998976

Statistics
R1 (Titer)
Number of samples
Mean value
s
srel

6
0.999866
0.001784
0.178%

Titer
Titrant
New titer

Hyamine 1622
0.99987

Results
R2 (Hyamine)

0.999866

Table of measured values

Titration curve

80

Method
Method
Version

414Titer
Titer Hyamine 1622
06/07/2007 17:15:16

001 Title
Type
Compatible with
ID
Titel
Author
Date / Time
Modified at
Protect
SOP
002 Sample (Titer)
Titrant
Concentration
Standard
Type of standard
Entry Type
Volume
Correction factor
Temperature [C]
003 Titration stand (Rondolino TTL)
Type
Titration stand
004 Stir
Speed
Duration
Condition
005 Titration (EP) [1]
Titrant
Titrant
Concentration
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
Wait time [s]
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
Accompanying stating
Accompanying stating
Condition
Condition
006 Dispense (normal) [1]
Titrant
Concentration
Volume
Dosing rate
Condition
007 Stir
Speed
Duration
Condition
008 Titration (EQP) [2]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed
Predispense
Mode
Volume
Wait time [s]

Control
Control
Titrant addition
dE(set value)
dV(min)
dV(max)
Mode
dE
dt
t(min)
t(max)
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
At slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
009 Calculation R1
Result
Result unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition
010 Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
...
Calibration curve
Method
Series data
Condition
011 End of sample
012 Titer
Titrant
Concentration
TITER=
Limits
Condition
013 Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Condition
014 Record
Summary
Results
Raw results
Resource data
Calibration curve
Method
Series data
Condition

General titration
T70/ T90
414Titer
Titer Hyamine 1622
Administrator
28/08/2006 14:53:19
06/07/2007 17:15:16
No
None
Hyamine 1622
0.004 mol/L
SDSTiter414
liquid
Fixed volume
5 mL
1.0
25.0
Rondolino TTL
Rondolino TTL 1
30 %
45 s
No

HCl
0.1 mol/L
pH
DG111-SC
pH
No
35 %
None
0
Absolute
Negative
3 pH
2.0 pH
0.2 mL/min
50 L/min
Yes
0 s
10.0 mL
Infinite
No
No
MIBK-EtOH 1:1
1
20 mL
60.0 mL/min
No
80 %
60 s
No

Hyamine 1622
0.004 mol/L
mV
DS800
mV
No
80 %
Volume
1.5 mL
15 s

81

User
Dynamic
8.0 mV
0.01 mL
0.5 mL
Equilibrium controlled
1.0 mV
1 s
5 s
30 s
Standard
100 mV/mL
Positive
0
No
10
No
No
Yes
1
No
No
No
Titer
R=m/(VEQ[2]*c[2]*C
M/(cst*z)
M[Sodium dodecylsulfate]
z[Sodium dodecylsulfate]
6
No
Yes
No
No
No
Per sample
Per sample
Last titration function

No
No
Last titration function

No
No
No
No
No

Hyamine 1622
0.004 mol/L
Mean[R]
No
No
Titer Hyamine
R2=Mean[R1]
M[None]
z[None]
6
No
Yes
No
No
Yes
No
No
No
No
No
No
No

M379

METTLER TOLEDO

Acid and Chloride Content in Wine


Titration Excellence Line: Method for the determination of tartaric acid and chloride in wine

Sample

Preparation and Procedures

Wine, 40 mL

Before the acid content analysis is performed the pH electrode


needs to be adjusted by use of the METTLER TOLEDO buffers
4.01, 7.00 and 9.21 and method M436.

Substance

Tartaric acid ((CHOH) 2(COOH)2)


Chloride (Cl -)

Chemicals

H2SO4 (10%)

Titrant

NaOH, 1.0 mol/L (sodium hydroxide)


AgNO3, 0.02 mol/L (silver nitrate)

Standard

NaCl for AgNO 3, KHP for NaOH

Instruments

Titration Excellence T70/T90


2 additional dosing units

Accessories

LabX Pro Titration ME-51106500


Rondo30 sample changer (51108004)
with sample beakers (51108030)

Indication

DGi102-Mini (pH sensor)


DMi102-SC (silver electrode)

Chemistry

EP titration:
C 4H6O6 + 2NaOH = Na2C 4H4O6 +2H2O
EQP titration:
Cl- + Ag + + NO3- = AgCl + NO3-

Remarks

Calculation

R1: Consumption NaOH (mL)


R2: Measurement pH value (pH)
R3: Chloride content (mg/L)

When working with Rondo30 and two mini electrodes lower


sample volumes can be used for two consecutive titrations in the
same sample.
In this method conditioning in the conditioning beaker is used for
electrode cleaning, alternatively, rinsing with the Rondo30 power
shower can be used.
When automation with Rondo30 is not required, microtitration
beakers can also be used when wanting to use smaller sample
volumes.

Results

Waste
Waste
disposal
disposal

AgCl has to be disposed of as special


waste.

Author

Melanie Nijman

82

Results
Mettler Toledo T90 Titrator

Method
Measured

Mettler Toledo AG
Market Support Laboratory
15.10.2007

m379
Acid and Chloride Content in Wine
11.10.2007

RESULTS
No.
1

ID
Wine

Wine

Wine

Wine

Wine

Wine

Sample size and results


40.0
ml
R1 =
3.0744
ml
R2 =
1.660
pH
R3 =
33.6713 mg/L
40.0
ml
R1 =
3.0925
ml
R2 =
1.662
pH
R3 =
33.7785 mg/L
40.0
ml
R1 =
3.1120
ml
R2 =
1.670
pH
R3 =
33.8016 mg/L
40.0
ml
R1 =
3.0839
ml
R2 =
1.669
pH
R3 =
33.7493 mg/L
40.0
ml
R1 =
3.0739
ml
R2 =
1.669
pH
R3 =
33.7564 mg/L
40.0
ml
R1 =
3.0859
ml
R2 =
1.671
pH
R3 =
33.8069 mg/L

Content
pH value
Chloride content
Content
pH value
Chloride content
Content
pH value
Chloride content
Content
pH value
Chloride content
Content
pH value
Chloride content
Content
pH value
Chloride content

STATISTICS
Number results
R1
Mean value
Standard deviation
Relative standard deviation

n =
x =
s =
srel =

6
3.0871
0.0141
0.4570

Number results
R2
Mean value
Standard deviation
Relative standard deviation

n =
x =
s =
srel =

6
1.667
0.005
0.277

Number results
R3
Mean value
Standard deviation
Relative standard deviation

n =
x =
s =
srel =

6
33.7607 mg/L
0.0495
0.1470
%

ml

Consumption
Consumption

pH

pH value
pH value

Table of measured values

Chloride content
Chloride content

Titration curve

83

Method
Method:
User:

m379 Acid and Chloride Content in Wine 10.10.2007


Nijman

001 Title
Type
Compatible with
ID
Titel
Author
Date / Time
Modified at
Protect
SOP
LabX SOP
002 Sample
Number of IDs
ID 1
Entry Type
Volume [mL]
Density [g/mL]
Correction factor
Temperature [C]
003 Titration stand
Type
Titration stand
Lid handling
004 Stir
Speed [%]
Duration [s]
Condition
005 Titration (EP) [1]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]
Predispense
Mode
Wait time [s]
Control
Mode
Tendency
End point value
Control band
Dosing rate (max) [mL/min]
Dosing rate (min) [mL/min]
Termination
At EP
Termination delay [s]
At Vmax [mL]
Max. time[s]
Accompanying stating
Accompanying stating
Condition
Condition
006 Dispense (normal) [1]
Titrant
Concentration [mol/L]
Volume [mL]
Dosing rate [mL/min]
Condition
007 Measure (normal) [1]
Sensor
Type
Sensor
Unit
Temperature acquisition
Temperature measurement
Stir
Speed [%]
Aquisition of measured values
Aquisition
dE
dt [s]
t(min) [s]
t(max) [s]
Mean value
Condition
Condition
008 Titration (EQP) [2]
Titrant
Titrant
Concentration [mol/L]
Sensor
Type
Sensor
Unit
Temperature aquisition
Temperature measurement
Stir
Speed [%]

General titration
T70/ T90
MxxxMN2
Acid and Chloride Content in Wine
Mettler Toledo
10.10.2007
10.10.2007
No
None

1
Wine
Fixed volume
40.0
1.0
1.0
25.0
Rondo60/Tower A
Rondo60/1A
No
30
10
No

009

NaOH
1.0
pH
DG102-Mini
pH
No
30
None
0

010
Absolute
None
7.0
0.2
20
300
Yes
0
5
20000
011

No
No
H2 SO4 10%
1
2.0
60.0
No

pH
DG102-Mini
pH

012

No
30
Equilibrium controlled
0.5
1
10
30
No

013

No

AgNO3
0.02
014
mV
DM102-SC
mV
No
30

84

Predispense
Mode
Volume [mL]
Wait time [s]
Control
Control
Titrant addition
dE (set value)
dV (min)
dV (max)
Mode
dE
dt [s]
t(min) [s]
t(max) [s]
Evaluation and Recognition
Procedure
Threshold
Tendency
Ranges
Add. EQP criteria
Termination
At Vmax [mL]
At potential
At Slope
After number of recognized EQPs
Number of EQPs
Combined termination criteria
Accompanying stating
Accompanying stating
Condition
Condition
Calculation R1
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition
Calculation R2
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition
Calculation R3
Result
Result Unit
Formula
Constant C=
M
z
Decimal places
Result limits
Record statistics
Extra statistical functions
Send to buffer
Condition
Conditioning
Type
Interval
Position
Time [s]
Speed [%]
Condition
Record
Summary
Results
Raw results
Table of measured values
Sample data
Resource data
E - V
dE/dV - V
......
Condition
End of sample

Volume
0.2
5
User
Dynamic
6
0.02
0.2
Equilibrium controlled
1.0
2
10
30
Standard
150
None
0
No
6.0
No
No
Yes
1
No
No
No
Consumption
mL
R1=VEQ[1]
1
M[None]
z[None]
5
No
Yes
No
No
No
pH value
pH
R2=E
1
M[None]
z[None]
3
No
Yes
No
No
No
Chloride content
mg/L
R3=Q[2]*C/m
M*1000/z
M[Chloride]
z[Chloride]
5
No
Yes
No
No
No
Fix
1
Conditioning beaker
20
35
No
No
Per
Per
No
No
No
All
All
No

sample
sample

titration functions
titration functions

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 35
A Choice of Methods for Various Probes
The models of the Titration Excellence line of METTLER TOLEDO
are an ideal base to build fully automated titration systems.
Thanks to the method concept and the color touch screen,
operation is made easy. A single sample or an entire series of
samples can be started with a touch to the shortcut:
True One Click Titration.
This Application Brochure contains a selection of methods
illustrating the applicative power or METTLER TOLEDO.

Titration Excellence Line


T70 Terminal, Rondo 20 with PowerShower and
LabX titration

Plug & Play Electrodes


Reliable and secure
handling

www.mt.com
Mettler-Toledo AG, Analytical
Sonnenbergstrasse 74
CH-8603 Schwerzenbach, Switzerland
Tel +41-44 806 77 11
Fax +41-44 806 73 50
Subjet to technical changes.
03/2008 Mettler-Toledo AG
Market Support AnaChem

For more information

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