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35Application Brochure

Excellence Line Titrators

Selected Applicationsfor METTLER TOLEDO Titration Excellence Line

METTLER TOLEDO

I

Contents Method Electrode Title Page

M361 DGi112-Pro Buffer Capacity of the Acidic Mixture

HCl, CH3COOH and NH4Cl 1

M362 DGi112-Pro Buffer Capacity of Coca Cola 4

M363-A DGi116-Solvent Acid Number in Used Motor Oil According to ASTM D664-07 7

M363-B DGi116-Solvent Blank Value of Acid Number Solvent

According to ASTM D664-07 10

M363-C DGi116-Solvent Blank Value for Strong Acid Number


M363-D DGi116-Solvent Buffer Value pH 11 for Acid Number


M363-E DGi116-Solvent Buffer Value pH 4 for Acid Number


M363-F DGi116-Solvent Titer Determination of 0.1 mol/L KOH in 2-Propanol 22

M364-A DGi116-Solvent Base Number in Used Motor Oil

According to ASTM D4739-06a 25

M364-B DGi116-Solvent Blank Value of Base Number Solvent


M364-C DGi116-Solvent Titer Determination of 0.1 mol/L HCl in 2-Propanol 31

M364-D DGi116-Solvent Titer Determination of 0.1 mol/L KOH in 2-Propanol 34

M365 DG117-Water m-Value of Tap Water

with Automatic Temperature Compensation 37

M366 DX202-SC

Sb850-S7 Na2O and SiO2 in Waterglass 40

M367 DMi145-SC Chloride Content in Used Motor Oil 43

METTLER TOLEDO

II

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


M374-A InLab®718 Base Number Determination in Fresh Oils

by Conductometric Titration According to IP400-1994 64

M374-B InLab®718 Base Number Determination in Used Oils

by Conductometric Titration According to IP400-1994 67

M375 InLab®718 Titer Determination of 0.1 mol/L HCl in 2-Propanol

by Conductometric Titration 70

M376 DS800 -

TwoPhase

Anionic Content in Shower Gels by Potentiometric Two-Phase

Titration According to DIN EN 14480 73

M377 DS800-

TwoPhase

Anionic Content in Cutting Oils by Potentiometric Two-Phase

Titration According to DIN EN 14480 76

M378 DS800-

TwoPhase

Titer Determination of 0.004 mol/L Hyamine by Potentiometric

Two-Phase Titration According to DIN EN 14480 79

M379 DGi102-Mini

DMi102-Mini Acid and Chloride Content in Wine 81

III

Titration Probes: An Overview

DGi101-SC DGi102-Mini DGi111-SC DGi112-Pro DGi114-SC DGi115-SC DGi117-Water

DGi113-SC DGi116-Solvent DG300-SC Half-Cell pH sensor

DX200 Glass reference sensor

DX202-SC Plastic reference sensor

IV

DMi102-SC DMi141-SC DMi145-SC DMi148-SC DM405-SC

DMi101-SC DMi140-SC DMi144-SC

Sensor for Rondo 20 COD set 149.5 mm

DMi147-SC DM143-SC Sb850-S7/120

InLab®717 Conductometric

titration

Conductivity range: 10 μS/cm – 500 mS/cm

InLab®718 Conductometric

titration

Conductivity range: 0.1 – 200 μS/cm

DS500 Surfactant Titration

Medium:: Aqueous solutions

DS800-TwoPhase Surfactant Titration

Medium: Mixed two-phase system (water, MIBK)

V

pH electrodes for aqueous media Product name Electrolyte

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: 0-100°C

- 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

-

DGi101-SC

3 mol/L KCl

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


- 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

DGi102-Mini

3 mol/L KCl

Combined pH electrode for general direct pH measurements and acid/base titrations:

- Standard aqueous solutions

- pH range: 0-14


- 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

3 mol/L KCl saturated with AgCl

VI

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


- Movable PTFE-sleeve junction

- ARGENTHALTM reference system

- Double junction with refillable reference and bridge electrolyte

- Tubular HA glass membrane with low alkali error

DGi112-Pro

Reference electrolyte:

3 mol/L KCl

Bridge electrolyte: selectable

(standard delivery :

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




- 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


- Fixed ground glass sleeve junction (higher electrolyte flow)


- Silver ion trap

- Large tubular HA glass membrane → excellent response, stable signal

DGi115-SC

3 mol/L KCl

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: 0-100°C

- 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

DGi117-Water

Bridge electrolyte:

1 mol/L KCl

VII

pH electrodes for non-aqueous media Product name Electrolyte

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




- Tubular A41 glass membrane with low resistance (Membrane glass with excellent chemical resistance)

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 Na-Methylate 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


- Gold shielding for efficient electrical and static shielding


- Movable glass sleeve junction

- Spherical A41 glass membrane of low resistance for fast and sensitive pH response and chemical resistance

DGi116-Solvent

1 mol/L LiCl in ethanol

Silver ring electrodes

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


- 6 mm shaft

- Ceramic junction, Ag/AgCl reference system

DMi102-SC

1 mol/L KNO3

VIII

Combined silver ring electrode for argentometric precipitation titration in aqueous media


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


- 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)


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

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


- Movable sleeve junction


DMi145-SC

1 mol/L KNO3

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


- Junction-free bulb pH glass reference, no electrolyte

DMi148-SC

--

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)


- Annular ceramic junction → Faster response than bulb pH glass reference of DMi148

DM405-SC

1 mol/L KNO3

IX

Platinum ring electrode

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)


- 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)


- Ceramic junction


DMi140-SC


AgCl

Combined platinum ring electrode for redox titration in aqueous media

- Dedicated electrode for automatic COD determinations on the Rondo 20 COD rack


- Ceramic junction


DMi144-SC


AgCl

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


- Junction-free bulb pH glass reference, no electrolyte

DMi147-SC

--

X

XI

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

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


- pH range: 0-14

- Fixed 4 mm banana plug cable


- Movable glass sleeve junction

DX200

Reference electrolyte: 3 mol/L KCl

saturated with AgCl


Standard delivery:

3 mol/L KCl 1 mol/L KNO3

0.9 mol/L Al2(SO4)3

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


- pH range: 0-14

- S7-screw cap connection

- Internal Ag/AgCl reference system

- Porous plastic junction

DX202-SC

Internal Ag/AgCl

reference system

(not refillable)


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


- pH range: 0-13

- S7-Screw cap connection

DG300-SC

--

M361

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

Ammonium chloride (NH4Cl), all approx. 0.1 mol/L

40 mL deionized waterpH 4, 7 and 9 buffer solutions

Sodium hydroxide (NaOH)c(NaOH) = 0.1 mol/L

Titration Excellence Line T70/T90Rondolino Sample Changer withPowerShowe and pump

pH 2.8-5.0:HCl+NaOH = Na++Cl-+H2OpH 5.0-9.0:HOAc+NaOH = -OAc+Na++H2OpH 9.0-11.5:NH4Cl+NaOH = Na++Cl-+NH3+H2O

Titration beaker ME-101974LabX Titration Software

METTLER TOLEDO

Neutralize the sample before finaldisposal as aqueous solution

Wastedisposal

Preparation and Procedures3 mL acidic mixture (1 mL of eachacid)

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi112-ProIndication

Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl

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

2) The acidic mixture is prepared by adding 1 mL of each acidsolution into the titration beaker.

3) The mixture is diluted with 40 mL deionized water beforetitration. Since 3 mL acidic mixture is used , the total samplevolume is 43 mL.

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

A mixture of three different acids (HCl, HOAc, NH4Cl) with clearlydifferent pKa values (HCl: -7, HOAc: 4.75, NH4Cl: 9.25) istitrated with 0.1 mol/L NaOH. The buffer capacity is used todescribe this complex mixture. Since three EQPs are found threedifferent half neutralization values can be calculated (HNV1-HNV3, see titration curve).

Three different series (6 samples) have been performed. Thestatistics of one series is shown below:

R1 HCl 0.1088 mol/L 0.00143 1.318R2 HOAc 0.08263 mol/L 0.00151 1.827R3 NH4Cl 0.09374 mol/L 0.00084 0.896

R4 BETAHNV1 3.47 mmol/(L*pH) 0.15824 4.56R5 BETAHNV2 1.18667 mmol/(L*pH) 0.00516 0.435R6 BETAHNV3 1.21333 mmol/(L*pH) 0.01033 0.851R7 BETAHNV1+2 4.65667 mmol/(L*pH) 0.15908 3.416R8 BETAHNV1+2+3 5.87 mmol/(L*pH) 0.15849 2.7

In the following the mean value range and the srel-rangeobtained for these three different series are shown:

R1: 0.1081 - 0.10939 0.7 - 2.4R2: 0.08263 - 0.08344 1.8 - 3.3R3: 0.09374 - 0.09455 0.9 - 1.5R4: 3.47 - 3.53833 3.0 - 8.8R5: 1.175 - 1.195 0.4 - 3.2R6: 1.21333 - 1.225 0.8 - 3.0R7: 4.65667 - 4.73333 1.7 - 6.2R8: 5.87 - 5.95833 1.5 - 4.8

Remarks

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 (NH4Cl 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)

Calculation

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

Standard Potassium hydrogen phthalate, 80 mg

Thomas HitzAuthor

Wastedisposal

1

HNV1

HNV2 HNV3

HNV1

HNV2 HNV3

Table of measured values

No. Comment / ID Rx Result Unit Name 1/6 -- R1 = 0.109 mol/L HCl

R2 = 0.07941 mol/L HOAc R3 = 0.09244 mol/L NH4Cl R4 = 3.71 mmol/(L*pH) BETAHNV1 R5 = 1.15 mmol/(L*pH) BETAHNV2 R6 = 1.19 mmol/(L*pH) BETAHNV3 R7 = 4.86 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 6.05 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3

2/6 -- R1 = 0.10712 mol/L HCl R2 = 0.08107 mol/L HOAc R3 = 0.09558 mol/L NH4Cl R4 = 3.52 mmol/(L*pH) BETAHNV1 R5 = 1.17 mmol/(L*pH) BETAHNV2 R6 = 1.24 mmol/(L*pH) BETAHNV3 R7 = 4.69 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 5.93 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3





Titration curve

Results

2

Method: m361 Buffer Capacity 08.01.2008User: Thomas Hitz

001 Title Typ General titration Compatible with T70/T90 ID m361 Titel Buffer Capacity Author Thomas Hitz Date / Time 08.01.2008 Modified at 08.01.2008 Protect No SOP None002 Sample

Number of IDs 1 ID 1 -- Entry Type Fixed volume Volume [mL] 43 Density [g/ml] 1 Correction factor 1.0 Temperature [°C] 25.0°C003 Titration stand (Rondolino TTL) Typ Rondolino TTL Titration stand Rondolino TTL 1004 Stir Speed 50 % Duration 20 s Condition No005 Titration (EQP) [1]

Titrant Titrant NaOH Concentration [mol/L] 0.1

Sensor Type pH Sensor DG112-SC Unit pH

Temperature acquisition Temperature acquisition No

Stir Speed [%] 30

PredispenseMode None

Wait time [s] 0Control

Control Normal Mode Acid/base Show parameters Yes Titrant addition Dynamic dE(set value) 10 dV(min) [mL] 0.005 dV(max) [mL] 0.2 Mode Equilibrium controlled dE 0.5 dt [s] 2.0 t(min)[s] 3.0 t(max)[s] 30.0

Evaluation and recognitionProcedure Standard

Threshold [pH/mL] 1.5 Tendency None Ranges 0 Add. EQP criteria No Buffer capacity Yes

TerminationAt Vmax [mL] 5

At potential No At Slope No After numbered of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating No

Condition Condition No006 Calculation R1 Result HCl Result unit mol/L Formula R1=Q1*C/1 Constant C= 1/z M M[Hydrochloric acid] z z[Hydrochloric acid] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No007 Calculation R2 Result HOAc Result unit mol/L Formula R2=Q2*C/1 Constant C= 1/z M M[Acetic acid] z z[Acetic acid] Decimal places 5 Result limits No Record statistics Yes

Extra statistical functions No Send to buffer No Condition No

Method008 Calculation R3 Result NH4Cl Result unit mol/L Formula R3=Q3*C/1 Constant C= 1/z M M[Ammonium chloride] z z[Ammonium chloride] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No009 Calculation R4 Result Buffer capacity HCl Result unit mmol/(L*pH) Formula R4=BETAHNV1 Constant C= 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 No010 Calculation R5 Result Buffer capacity HOAc Result unit mmol/(L*pH) Formula R5=BETAHNV2 Constant C= 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 No011 Calculation R6 Result Buffer capacity NH4Cl Result unit mmol/(L*pH) Formula R6=BETAHNV3 Constant C= 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 No012 Calculation R7 Result Buffer capacity sum1 Result unit mmol/(L*pH) Formula R7=BETAHNV1+BETAHNV2 Constant C= 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 No013 Calculation R8 Result Buffer capacity sum2 Result unit mmol/(L*pH) Formula R8=BETAHNV1+BETAHNV2+BETAHNV3 Constant C= 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 No014 Record Summary No Results Per sample Raw results Per sample Table of measured values No Sample data No Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - V Last titration function E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No

3

M362

Acidic components

pH 4, 7 and 9 buffer solutions

Sodium hydroxide, NaOHc(NaOH) = 0.1 mol/L

Titration Excellence Line T70/T90Rondolino Sample Changer withPowerShower and pump

HX + NaOH = NaX + H2O

Olivetti JobJet 210 PrinterLabX Titration Software

METTLER TOLEDO

Neutralization before final disposal asaqueous solution.

Wastedisposal

Preparation and ProceduresCoca Cola, 50 mLSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi112-ProIndication

Buffer Capacity of Coca Cola

- 1 L of Coca Cola is added to an Erlenmeyer flask anddegassed by stirring and while heating for 1 hour.

- The degassed Coca Cola is stored in a sealed bottle, which isonly opened for sample aliquotation.

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

3) The titration is started.

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

The determination of the buffer capacity represents an alternativeway to analyze the general behaviour of e.g. an acid solution.

In particular, it can be used to describe complex acid/basemixtures that can be found in electroplating baths, in beveragesas well as in saliva.

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)).

Remarks

R1 = BETAHNV1R2 = BETAHNV2R3 = BETAHNV1+BETAHNV2

Units: mmol/(L*pH)

Calculation

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

Standard Potassium hydrogen phthalate (KHP)

Thomas HitzAuthor

Wastedisposal

4

HNV1

HNV2

HNV1

HNV2


No. Comment / ID Start time Rx Result Unit

1/5 CocaCola 10.09.2007 15:54:43 R1 = 5.24 mmol/(L*pH) R2 = 3.62 mmol/(L*pH) R3 = 8.86 mmol/(L*pH)





Statistics

Rx n Mean value Unit s srel[%]

R1 5 5.19000 mmol/(L*pH) 0.03742 0.721R2 5 3.57200 mmol/(L*pH) 0.08167 2.286R3 5 8.76200 mmol/(L*pH) 0.10986 1.254

Titration curve

Results

5

Method: m362 Buffer Capacity Coca Cola 10.09.2007User: Thomas Hitz

001 Title Typ General titration Compatible with T50/T70/T90 ID m362 Titel Buffer Capacity Coca Cola Author Thomas Hitz Date / Time 01.09.2007 Modified at 10.09.2007 Protect No SOP None

002 Sample Number of IDs 1 ID 1 Coca Cola Entry Type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature [°C] 25.0

003 Titration stand (Rondolino TTL) Typ Rondolino TTL Titration stand Rondolino TTL 1

004 Stir Speed 30 % Duration 10 s Condition No

005 Titration (EQP) Titrant Titrant NaOH Concentration [mol/L] 0.1 mol/L Sensor Type pH Sensor DG112-SC Unit pH Temperature acquisition Temperature acquisition No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 12 dV (min) 0.005 dV (max) 0.5 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and recognition Procedure Standard Threshold 0.7 pH/mL Tendency Positive Ranges 0 Add. EQP criteria No Buffer capacity Yes Termination At Vmax 15 mL At potential No At Slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating

Accompanying stating No Condition

Condition No006 Calculation

Result BufferCapacity Result Unit mmol/(L*pH) Formula R1 = BETAHNV1 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No

Method007 Calculation

Result BufferCapacity Result Unit mmol/(L*pH) Formula R2 = BETAHNV2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No

008 CalculationResult BufferCapacity

Result Unit mmol/(L*pH) Formula R3 = BETAHNV1+BETAHNV2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No

009 RecordSummary No

Results Per sample Raw results Per sample 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 Beta-V Last titration function E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No Condition No

010 End of sample

6

M363-A

Acid components as mg KOH/gsample, M=56.1 g/mol, z=1

60 mL ASTM D664-07 solvent:Toluene:2-propanol:deion. water500 mL : 495 mL : 5 mL

Potassium hydroxide in 2-propanolKOH, c(KOH) = 0.1 mol/L

Titration Excellence T70/T90Rondo20 with two membrane pumpsLabX Titration Software

KOH + HA = KA + H2O

HA: Acid components

DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer

METTLER TOLEDO

Dispose as aromatic organic solvent(toluene)

Wastedisposal

Preparation and ProceduresUsed motor oil,approx. 3 g for AN 5 -10

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi116-SolventIndication

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

1) The titer is determined using potassium hydrogen phthalate(KHP): add approx. 80 mg KHP into a glass titration beakerand 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] andH[Buffer pH11]. See M363-D (pH 11) and M363-E (pH 4).

3) A blank value is determined for every new batch of solventmixture 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 sampleamounts are requested:AN / mg KOH/g Sample size/g0.05 - <1.0 20.0 +/- 2.01.0 - <5.0 5.0 +/- 0.55 - <20 1.0 +/- 0.120 - <100 0.25 +/- 0.02100 - <260 0.1 +/- 0.01

5) After each sample titration the DG116-Solvent electrode isrinsed and conditioned in a chloroform/toluene 1:1 mixtureduring 5 minutes. Subsequently, it is conditioned in deionizedwater during additional 5 minutes.

1) This application does not replace the ASTM standard.

2) The method parameters have been optimised for the sampleused in this application. Thus, it may be necessary to slightlyadapt the method to your specific sample.

3) The acid number indicates the amount of base as mg KOH/gsample needed to titrate the acidic constituents in a sampleunder specific conditions, i.e. specified solvent and endpoint.

4) The sample is titrated using an EQP method function. If noinflection point is detected, endpoints are taken at meter readingscorresponding to those found for aqueous acidic and basicbuffer solutions for SAN at pH 4 and AN at pH 11

5) CalculationsR1 = AN to EQP in mg KOH/gR2 = mmol consumption to buffer potential pH 11R3 = AN to buffer potential pH 11 in mg KOH/gR4 = mmol consumption to buffer potential pH 4R5 = 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

Remarks

R1= (Q-B[ASTM 664 AN])*C/mC = M/zR2= QE(H[Buffer pH11])R3= (R2-B[ASTM 664 AN])*C/mC = M/zR4 = QE(H[Buffer pH4])R5= (R4+B[ASTM 664 SAN])*C/mC = M/z

Calculation

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 toASTM D664-07.


Albert AichertAuthor

Wastedisposal

7

Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C

0 NaN 187 NaN NaN 0 250.05 0.05 181.1 -5.9 NaN 5 250.1 0.05 174.4 -6.7 NaN 10 25

0.153 0.053 167.3 -7.1 NaN 15 250.214 0.061 159.5 -7.8 NaN 20 250.278 0.064 151 -8.5 -131.19 25 250.337 0.059 143.4 -7.6 -130.39 30 25

0.4 0.063 135 -8.4 -131.91 36 250.46 0.06 127.3 -7.7 -133.33 41 25

0.521 0.061 118.9 -8.4 -135.08 46 250.578 0.057 111.3 -7.6 -137.04 51 250.639 0.061 102.6 -8.7 -138.96 56 250.692 0.053 95.5 -7.1 -140.91 61 250.754 0.062 86.5 -9 -142.71 66 250.806 0.052 79.2 -7.3 -145.46 71 250.865 0.059 70.5 -8.7 -146.73 76 250.916 0.051 63 -7.5 -147.09 81 250.972 0.056 54.7 -8.3 -145.08 86 251.023 0.051 47.2 -7.5 -141.58 91 251.08 0.057 39.5 -7.7 -137.1 97 25

1.144 0.064 30.8 -8.7 -131.48 102 251.204 0.06 23 -7.8 -127.32 108 251.266 0.062 15.4 -7.6 -124.03 114 251.336 0.07 6.7 -8.7 -120.47 119 251.399 0.063 -0.6 -7.3 -117.37 124 251.476 0.077 -9.8 -9.2 -113.94 130 251.538 0.062 -16.7 -6.9 -111.36 136 251.616 0.078 -25.2 -8.5 -109.72 142 251.693 0.077 -33.6 -8.4 -108.28 147 251.764 0.071 -41.1 -7.5 -106.87 152 251.844 0.08 -49.8 -8.7 -106.95 157 251.914 0.07 -57.5 -7.7 -104.32 163 251.987 0.073 -64.6 -7.1 -102.22 169 252.08 0.093 -74.3 -9.7 -100.26 174 25

2.149 0.069 -81.4 -7.1 -99.8 179 252.232 0.083 -88.7 -7.3 -98.69 184 252.334 0.102 -99.4 -10.7 -97.91 189 25

2.4 0.066 -105.9 -6.5 -96.27 194 252.484 0.084 -114 -8.1 -94.33 200 252.57 0.086 -121.5 -7.5 -91.47 205 252.67 0.1 -131 -9.5 -86.83 210 252.75 0.08 -137.5 -6.5 -85.12 215 252.86 0.11 -146.8 -9.3 -82.14 220 25

2.952 0.092 -154.2 -7.4 -80.26 225 253.059 0.107 -162.5 -8.3 -77.69 230 253.164 0.105 -171.1 -8.6 -76.36 235 253.257 0.093 -177.6 -6.5 -74.67 240 253.39 0.133 -187.7 -10.1 -73.03 245 25

3.488 0.098 -194.5 -6.8 -71.37 250 253.614 0.126 -203.7 -9.2 -70.21 255 253.717 0.103 -210.7 -7 -69.31 260 253.845 0.128 -219.5 -8.8 -66.44 266 253.957 0.112 -226.6 -7.1 -64.23 271 254.098 0.141 -236.1 -9.5 -60.27 276 254.21 0.112 -242.2 -6.1 -57.67 282 254.39 0.18 -252 -9.8 -53.15 288 25

4.536 0.146 -259.9 -7.9 -49.99 294 254.686 0.15 -266.7 -6.8 -46.27 300 254.886 0.2 -276 -9.3 -41.8 305 255.051 0.165 -282.3 -6.3 -37.81 310 255.251 0.2 -289.7 -7.4 -33.28 315 255.451 0.2 -295.5 -5.8 -29.4 320 255.651 0.2 -301.3 -5.8 -25.75 325 255.851 0.2 -306.1 -4.8 -23 330 256.051 0.2 -310.4 -4.3 -20.38 336 256.251 0.2 -314.3 -3.9 NaN 341 256.451 0.2 -317.7 -3.4 NaN 346 256.651 0.2 -320.9 -3.2 NaN 351 256.851 0.2 -323.6 -2.7 NaN 356 257.051 0.2 -326.2 -2.6 NaN 361 25


Summary Method-ID m363ASample No. ID Sample size and results 1 Used oil 3.04742 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.376 mmol R3 (TAN BP) 6.849 mg KOH/g R4 (Consumption SAN) 0.011 mmol R5 (SAN BP) 0.312 mg KOH/g 2 Used oil 3.31062 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.405 mmol R3 (TAN BP) 6.796 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.355 mg KOH/g 3 Used oil 3.27543 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.402 mmol R3 (TAN BP) 6.817 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.359 mg KOH/g 4 Used oil 3.09854 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.381 mmol R3 (TAN BP) 6.826 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.379 mg KOH/g 5 Used oil 3.16791 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.388 mmol R3 (TAN BP) 6.801 mg KOH/g R4 (Consumption SAN) 0.016 mmol R5 (SAN BP) 0.389 mg KOH/g 6 Used oil 3.27816 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.401 mmol R3 (TAN BP) 6.794 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.358 mg KOH/gStatistics R3 TAN BP Samples 6 Mean 6.814 mg KOH/g s 0.021311 mg KOH/g srel 0.313 % R5 SAN BP Samples 6 Mean 0.359 mg KOH/g s 0.026553 mg KOH/g srel 7.403 %

Titration curve

Results

8

Method m363 SAN & AN ASTM D664 29.01.2008Author Albert Aichert

001 Title Type General titration Compatible with T70 / T90 ID m363 Title SAN & AN ASTM D664 Author Albert Aichert Date/Time 29.01.2008 10:12:42 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Used oil Entry type Weight Lower limit 1.0 g Upper limit 10.0 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary

003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A

004 Pump Auxiliary reagent ASTM 664 solvent Volume 60 mL Condition No005 Stir Speed 35 % Duration 60 s Condition No

006 Titration (EQP) [1] Titrant Titrant KOH in 2-Propanol Concentration 0.1 mol/L

Sensor Type pH Sensor DG116-SC Unit mV


Stir Speed 30 %

Predispense Mode None Wait time 0 s

Control Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.05 mL dV(max) 0.2 mL Meas. value acquisition Equilibrium controlled dE 0.5 mV dt 1 s t(min) 5 s t(max) 60 s

Evaluation and recognition Procedure Standard Threshold 150 mV/mL Tendency None Ranges 1 Lower limit -400.0 mV Upper limit 0.0 mV Add. EQP criteria No

Termination At Vmax 15.0 mL At potential Yes Potential H[Buffer pH11]-100 mV Termination tendency None At slope No After number of recognized EQPs No Number of EQPs No Combined termination criteria No

Accompanying stating Accompanying stating No

Condition Condition No

007 Conditioning Type Fix Interval 1 Position Special beaker 1 Time 180 s Speed 100 % Condition no

Method008 Conditioning Type Fix Interval 1 Position Conditioning beaker Time 300 s Speed 30 % Condition no009 Calculation R1 Result TAN (EQP) Result unit mg KOH/g Formula R1=(Q-B[ASTM 664 AN])*C/m Constant C z/M M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No010 Calculation R2 Result Consumption EP Result unit mmol Formula R2=QE(H[Buffer pH11]) Constant C 1 M M[none] z z[none] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No011 Calculation R3 Result TAN (BP) Result unit mg KOH/g Formula R3=(R2-B[ASTM 664 AN])*C/m Constant C z/M M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Calculation R4 Result Consumption SAN Result unit mmol Formula R4=QE(H[Buffer pH4]) Constant C 1 M M[none] z z[none] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No013 Calculation R5 Result SAN (BP) Result unit mg KOH/g Formula R5=(R4+B[ASTM 664 SAN])*C/m Constant C z/M M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No014 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No015 End of sample

016 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No 017 Record Summary Yes Results No Raw results No Table of meas. value No E - V No dE/dV - V No Condition No

9

M363-B

--

--


Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software

KOH + HA = KA + H2O

HA: Acid components


METTLER TOLEDO


Wastedisposal

Preparation and Procedures60 mL solvent ASTM 664-07mixture of 2-propanol/toluene/water inthe ratio 495 mL : 500 mL : 5 mL

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


Blank Value for Acid Number According to ASTM D664-07

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

2) For the blank determination, an EQP titration is used and theresult is calculated at the potential value obtained for pH 11buffer, i.e. QE(H[Buffer pH11]).This value was previously determined with application M363-Dand stored as auxiliary value H[Buffer pH11].

3) Finally, the result QE(H[Buffer pH11]) in mmol is stored asblank value B[ASTM 664 AN]



3) The titrant has to be protected against the uptake of CO2 fromthe air. NaOH on carrier (e.g. "Sodium hydroxide on support",MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKANr. 03350) is an effective medium to avoid such formation ofcarbonate.

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.

Remarks

R1= QE(H[Buffer pH11])Calculation

Titration Excellence Line: Method for the blank value determination to pH 11 of the acid number in thesolvent ASTM D664-07 with potassium hydroxide in 2-propanol.



Wastedisposal

10


0 NaN -189.2 NaN NaN 0 250.002 0.002 -177.9 11.3 NaN 10 250.004 0.002 -171.9 6 NaN 20 250.009 0.005 -169 2.9 NaN 31 250.019 0.01 -168.7 0.3 NaN 41 250.029 0.01 -172.8 -4.1 NaN 52 250.039 0.01 -189.4 -16.6 NaN 62 250.044 0.005 -256.5 -67.1 NaN 87 25


Summary Method-ID T202Sample 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) 0.004210Statistics R1 Blank pH11 Samples 3 Mean 0.004040 mmol s 0.000148 mg KOH/g srel 3.654 %

Titration curve

Results

11

Method T202 Blank AN pH11 ASTM D664 07.12.2007Author Albert Aichert

001 Title Type General titration Compatible with T50 / T70 / T90 ID T202 Title Blank AN pH11 ASTM D664 Author Albert Aichert Date/Time 07.12.2007 10:12:42 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Solvent 664 Entry type Fixed volume Volume 60 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary


004 Pump Auxiliary reagent ASTM 664 solvent Volume 60 mL Condition No





Stir Speed 30 %



Evaluation and recognition Procedure Standard Threshold 200 mV/mL Tendency Negative Ranges 0 Add. EQP criteria No

Termination At Vmax 15.0 mL At potential Yes Potential H[Buffer pH11]-30 mV Termination tendency None At slope No After number of recognized EQPs No Number of EQPs No Combined termination criteria No


Condition Condition No007 Rinse Auxiliary reagent ASTM 664 solvent Rinse cycles 1 Vol. per cycle 15 mL Position Actual sample Drain No Condition No

Method008 Calculation R1 Result Blank pH11 Result unit mmol Formula R1=QE(H[Buffer pH11]) Constant C 1 M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No009 Blank Name ASTM 664 AN Value B= Mean[R1] Unit mmol Limits No Condition No010 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No011 End of sample


12

M363-C

--

--

Hydrochloric acid in 2-PropanolHCl, c(HCl) = 0.1 mol/L


KOH + HA = KA + H2O

HA: Acid components


METTLER TOLEDO


Wastedisposal

Preparation and Procedures60 mL solvent ASTM 664-07mixture of 2-propanol/toluene/water inthe ratio 495 mL : 500 mL : 5 mL

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


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

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

2) For the blank determination, an EQP titration is used and theresult is calculated at the potential value obtained for pH 4buffer, i.e. QE(H[Buffer pH4]).This value was previously determined with application M363-Eand stored as auxiliary value H[Buffer pH4]

3) Finally, the result QE(H[Buffer pH4]) in mmol is stored asblank value B[ASTM 664 SAN].




Remarks

R1= QE(H[Buffer pH4])Calculation

Titration Excellence Line: Method for the blank value determination to pH 4 in the solvent ASTM D664-07with hydrochloric acid in 2-propanol.

Standard Tris-(hydroxymethyl)-aminomethane, 80 mg


Wastedisposal

13


0 NaN 44.5 NaN NaN 0 250.002 0.002 67.8 23.3 NaN 10 250.004 0.002 80 12.2 NaN 20 250.008 0.004 92.6 12.6 NaN 30 250.016 0.008 107.1 14.5 NaN 41 250.026 0.01 120.8 13.7 997.3 51 250.036 0.01 133.2 12.4 1010.34 62 250.046 0.01 146.5 13.3 1673.72 72 250.054 0.008 161.2 14.7 2863.48 82 250.06 0.006 175.6 14.4 NaN 92 25

0.062 0.002 187.1 11.5 NaN 103 250.064 0.002 197.4 10.3 NaN 113 250.066 0.002 210.7 13.3 NaN 124 250.068 0.002 227.6 16.9 NaN 134 25


Summary Method-ID T212Sample 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) 0.005733Statistics R1 Blank pH4 Samples 4 Mean 0.005938 mmol s 0.000173 mg KOH/g srel 2.918 %

Titration curve

Results

14

Method T212 Blank SAN pH4 ASTM D664 17.01.2008Author Albert Aichert

001 Title Type General titration Compatible with T50 / T70 / T90 ID T212 Title Blank SAN pH4 ASTM D664 Author Albert Aichert Date/Time 17.01.2008 10:12:42 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Solvent 664 Entry type Fixed volume Volume 60 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary


004 Pump Auxiliary reagent ASTM 664 solvent Volume 60 mL Condition No005 Stir Speed 35 % Duration 60 s Condition No

006 Titration (EQP) [1] Titrant Titrant HCl in 2-propanol Concentration 0.1 mol/L



Stir Speed 30 %



Evaluation and recognition Procedure Standard Threshold 200 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No

Termination At Vmax 15.0 mL At potential Yes Potential H[Buffer pH4]+50 mV Termination tendency None At slope No After number of recognized EQPs No Number of EQPs No Combined termination criteria No



007 Rinse Auxiliary reagent ASTM 664 solvent Rinse cycles 1 Vol. per cycle 15 mL Position Actual sample Drain No Condition No

Method008 Calculation R1 Result Blank pH4 Result unit mmol Formula R1=QE(H[Buffer pH4]) Constant C 1 M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No009 Blank Name ASTM 664 SAN Value B= Mean[R1] Unit mmol Limits No Condition No010 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No011 End of sample


15

M363-D

--

--

--


--


METTLER TOLEDO

Neutralize before final disposal asqueous solution.

Wastedisposal

Preparation and Procedures50 mL pH 11 buffer solutionSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


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

1) Always use fresh pH 11 buffer solution. The buffer pH 11 isnot stable when exposed to air.

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

3) Before measure the buffer potential, the electrode shouldconditioned in aquous media (water pH 5-6) for 3 - 5 minutes.

4) The measured potential value for buffer pH 11 is stored asauxilliary value H[Buffer pH11].

5) Finally, the electrode is parked in the condioning beakercontaining slightly acidic water (pH 5-6).


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 theair is strongly improved.For instance, the potential value (mV) in an open beaker withbuffer pH 11.can change of 0.1 mV/minThe potential value of an opened bottle of pH 11 buffer solutioncan rapidly change.Thus, it is very important to use fresh pH 11 buffer solution everytime a new value has to be determined


Remarks

R1= ECalculation

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

Standard --


Wastedisposal

16


Method-ID T102

Data / Time 07.01.2008 03:12:05 pm

All results Sample 1/1 Buffer pH11 R1(Buffer pH11) -222.400 mV

Titration curve

Results

17

Method T102 Buffer value AN pH11 ASTM D664 17.12.2007Author Albert Aichert

001 Title Type General titration Compatible with T50 / T70 / T90 ID T102 Title Buffer value AN pH11 ASTMD664 Author Albert Aichert Date/Time 17.12.2007 10:12:42 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Buffer pH11 Entry type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary



005 Measure (normal) [1] Sensor

Type pH Sensor DG116-SC Unit mV


Stir Speed 30 %

Acquisition of the measured value Acquisition Fix Time 30 s Mean value No t(min) 10 s t(max) 60 s


006 Calculation R1 Result Buffer pH11 Result unit mV Formula R1=E Constant C 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No

007 Auxiliary value Name Buffer pH11 Value B= R1 Unit mV Limits No Condition No

008 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V No dE/dV - V No Condition No

009 End of sample

010 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No

Method

18

M363-E

--

--

--


--


METTLER TOLEDO

Neutralize before final disposal asqueous solution.

Wastedisposal

Preparation and Procedures50 mL pH 4 buffer solutionSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


Buffer Value pH4 for Strong Acid Number According to ASTM D664-07

1) Always use fresh pH 4 buffer solution.

2) 50 mL pH 4 buffer solution are added into a titration beaker.

3) Before measure the buffer potential, the electrode shouldconditioned in aquous media (water pH 5-6) for 3 - 5 minutes.

4) The measured potential value for buffer pH 4 is stored asauxilliary value H[Buffer pH4].

5) Finally, the electrode is parked in the condioning beakercontaining slightly acidic water (pH 5-6).


2) Before measure the buffer potential, the electrode shouldconditioned in aqueous media (water pH 5-6) for 3 - 5minutes.


Remarks

R1= ECalculation

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

Standard --


Wastedisposal

19


Method-ID T112

Data / Time 17.01.2008 11:12:05 pm

All results Sample 1/1 Buffer pH4 R1(Buffer pH4) 169.200 mV

Titration curve

Results

20

Method T112 Buffer value SAN pH4 ASTM D664 16.01.2008Author Albert Aichert

001 Title Type General titration Compatible with T70 / T90 ID T112 Title Buffer value SAN pH4 ASTMD664 Author Albert Aichert Date/Time 16.01.2008 10:12:42 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Buffer pH4 Entry type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary



005 Measure (normal) [1] Sensor

Type pH Sensor DG116-SC Unit mV


Stir Speed 30 %

Acquisition of the measured value Acquisition Fix Time 30 s Mean value No t(min) 10 s t(max) 60 s


006 Calculation R1 Result Buffer pH4 Result unit mV Formula R1=E Constant C 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No

007 Auxiliary value Name Buffer pH4 Value B= R1 Unit mV Limits No Condition No

008 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V No dE/dV - V No Condition No

009 End of sample


Method

21

M363-F

Potassium hydrogen phthalateM=204.23 g/mol z=1

50 mL CO2-free, deionized water



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


METTLER TOLEDO

Neutralize before final disposal asaqueous solution.

Wastedisposal

Preparation and ProceduresPrimary standardPotassium hydrogen phthalate,70 - 100 mg

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


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

1) Weigh the primary standard into the glass titration beaker toavoid electrostatic influence.

2) Add 50 mL CO2-free deionized water to dissolve the sample.

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

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


2) The titrant has to be protected against the uptake of CO2 fromthe air. NaOH on carrier (e.g. "Sodium hydroxide on support",MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKANr. 03350) is an effective medium to avoid such formation ofcarbonate.


Remarks

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

p: purity of standard

Calculation

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



Wastedisposal

22


Summary Method-ID T001

Sample No. ID Sample size and results 1 KHP 0.11936 g R1 (Titer) 0.961720 2 KHP 0.12372 g R1 (Titer) 0.961095 3 KHP 0.11054 g R1 (Titer) 0.960251 4 KHP 0.11502 g R1 (Titer) 0.960945

Statistics R1 Titer Samples 4 Mean 0.961003 s 0.000603 srel 0.063 %

Titer Titrant KOH in 2-Propanol New titer 0.96100

Titration curve

Results

23

Method m363F Titer of KOH in 2-propanol 02.10.2007Author Albert Aichert

001 Title Type General titration Compatible with T50 / T70 / T90 ID m363F Title Titer of KOH in 2-propanol Author Albert Aichert Date/Time 02.10.2007 10:51:42 Modified -- Modified by -- Protect No SOP None

002 Sample (Titer) Titrant KOH in 2-Propanol Concentration 0.1 mol/L Standard KHP Type of standard solid Entry type Weight Lower limit 0.07 g Upper limit 0.12 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary


004 Pump Auxiliary reagent Water Volume 60 mL Condition No005 Stir Speed 60 % Duration 60 s Condition No




Stir Speed 30 %

Predispense Mode Volume Volume 1.0 mL Wait time 5 s


Evaluation and recognition Procedure Standard Threshold 3.0 pH/mL Tendency Positive Ranges 0 Add. EQP criteria No

Termination At Vmax 10.0 mL At potential No Tendency None At slope No After number of recognized EQPs Yes Number of EQP's 1 Number of EQPs No Combined termination criteria No



007 Rinse Auxiliary reagent Water Rinse cycles 1 Vol. per cycle 15 mL Position Actual sample Drain No Condition No

Method008 Calculation R1 Result Titer Result unit -- Formula R1=(m/(VEQ*c*C) Constant C M/(10*p*z) M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

009 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No010 End of sample

011 Titer Titrant KOH in 2-Propanol Concentration 0.1 mol/L TITER= Mean[R1] Limits No Condition No


013 Record Summary Yes Results No Raw results No Table of meas. value No E - V No dE/dV - V No Condition No

24

M364-A

Alkaline components in oil expressedas KOH, M=56.1 g/mol , z=1

60 mL ASTM D4739-06a solvent(see Preparation and Procedures)pH 3 and pH 10 buffer solutions

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

Titration Excellence T70/T90Rondo 20 Sample changer1 additional dosing unit (20 mL)

HCl + KOH = Cl- + K+ + H2O

KOH represents the alkalinecomponents.

DV1010 and DV1020 BurettesTitration beakers ME-101974XS205 Balance, SP250 pumpPC with LabX Software

METTLER TOLEDO

Dispose of as halogenated organicwaste

Wastedisposal

Preparation and ProceduresUsed Motor oil, ~2.5 gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


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

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

2) The titer is determined by titration of previously standardizedKOH in 2-propanol solution. The latter has been standardizedusing potassium hydrogen phthalate (KHP), see M364-D.

3) The acidic (pH 3) and the alkaline (pH 10) aqueous bufferpotentials are measured and stored as auxiliary values pH 3 (H[Buffer pH3] ) and ( H[Buffer pH10] ).

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

5) Add the oil sample into the titration beaker. The appropriatesample size is calculated according to the following formula:sample size (g) = 7/expected BN

6) 60 mL ASTM D4739-06a solvent are added using anadditional dosing unit. This step can be performed manuallyusing a dispenser or a graduated cylinder.

This method allows a fully automated procedure using asample changer and an additional dosing unit. It can bemodified for manual operation. Select "Manual stand" in themethod function "Titration stand".

1) This application does not replace the ASTM standard.The method parameters have been optimised for the sampleused in this application. Thus, it may be necessary to slightlyadapt the method to your specific sample.

2) The base number BN is defined as the consumption ofhydrochloric acid to a specific endpoint to neutralize the alkalinecomponents of the oil. It is expressed as mg KOH/g sample:- If an EQP is found between the acidic buffer potential value anda 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 atthe potential value of the acidic buffer.

3) Between each sample it is necessary to condition theelectrode under stirring during 300 s in deion. water. Theelectrode is parked in buffer pH 4 (Rinse beaker).

Literature:1) ASTM D4739-06a and draft next version, see www.astm.org2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Remarks

Base number mg KOH/g:R1=(Q-B[ASTM D4739])*C/mC=M/z

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

Calculation

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

Standard KOH in 2-propanol 0.1 mol/L / KHP

Melanie NijmanAuthor

Wastedisposal

25


Mettler Toledo T90 Titrator Mettler Toledo AGMarket Support Laboratory17.01.2008

Method M364_A Base Number According to ASTM D4739-06a

RESULTS with DG116-Solvent electrodeNo. ID Sample size and results1 Used Motor Oil 2.54656 g

R1 = 3.50 mg KOH/g Content (EQP)R2 = 1.87 mg KOH/g Content (Buffer Potential)

2 Used Motor Oil 2.67162 gR1 = 3.48 mg KOH/g Content (EQP)R2 = 1.80 mg KOH/g Content (Buffer Potential)





STATISTICSNumber results R1 n = 6Mean value x = 3.47 mg KOH/g Content (EQP)Standard deviation s = 0.02 mg KOH/g Content (EQP)Relative standard deviation srel = 0.682 %

Number results R2 n = 6Mean value x = 1.82 mg KOH/g Content (Buffer Potential)Standard deviation s = 0.03 mg KOH/g Content (Buffer Potential)Relative standard deviation srel = 1.501 %

RESULTS with DG113-SC electrode

STATISTICSNumber results R1 n = 6Mean value x = 3.46 mg KOH/g Content (EQP)Standard deviation s = 0.06 mg KOH/g Content (EQP)Relative standard deviation srel = 1.659 %

Number results R2 n = 6Mean value x = 1.71 mg KOH/g Content (Buffer Potential)Standard deviation s = 0.05 mg KOH/g Content (Buffer Potential)Relative standard deviation srel = 3.072 %

Titration curve

Results

26

Method: m364A Base number ASTM D4739 17.01.2008User: Melanie Nijman

001 Title Type General titration Compatible with T70/ T90 ID m364A Title Base number ASTM D4739 Author Melanie Nijman Date / Time 17.01.2008 Modified at 11.01.2008 Modified by Administrator Protect No SOP None LabX SOP None

002 Conditioning Titration stand Rondo60/1A Position Conditioning beaker Time [s] 20 Speed [%] 30 Condition No

003 Sample Number of IDs 1 ID 1 Motor Oil Entry Type Weight Lower limit [g] 0.0 Upper limit [g] 10.0 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0 Entry Arbitrary

004 Titration stand Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No

005 Dispense (normal) [1]Titrant ASTM D4739 solvent

Concentration [mol/L] 1 Volume [mL] 60 Dosing rate [mL/min] 60.0 Condition No

006 Stir Speed [%] 35 Duration [s] 60 Condition No

007 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG116-Solvent Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 35 Predispense Mode Volume Volume 0.5 Wait time [s] 60 Predispense Mode Volume Volume [mL] 0.2 Wait time [s] 5 Control Control User Titrant addition Incremental dV (mL) 0.1 Mode Fixed time dt [s] 90 Evaluation and Recognition Procedure Standard Threshold [mV/mL] 80.0 Tendency None Ranges 1 Lower limit 1 [mV] H[Buffer pH3] Upper limit 1 [mV] H[Buffer pH3]+100 Add. EQP criteria No Termination At Vmax [mL] 5.0 At potential Yes Potential H[Buffer pH3]+140 Termination tendency Positive At Slope No After number of recognized EQPs No Combined termination criteria No

Accompanying stating Accompanying stating No Condition Condition No

Method008 Calculation R1 Result Content EQP Result Unit mg KOH/g Formula R1=(Q-B[ASTM D4739])*C/m Constant C= M/z M M[Potassium hydroxide] z z[Potassium hydroxide] Decimal places 2 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

009 Calculation R2 Result Content (Buffer Potential) Result Unit mg KOH/g Formula R1=(QE(H[Buffer pH3]) -B[ASTM D4739])*C/m Constant C= M/z M M[Potassium hydroxide] z z[Potassium hydroxide] Decimal places 2 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

010 RinseAuxiliary reagent ASTM D4739

Rinse cycles 3 Vol. per cycle [mL] 20.0 Position Actual position Drain Yes Drain pump SP250 Condition No

011 Conditioning Type Fix Interval 1 Position Conditioning beaker Time [s] 300 Speed [%] 30 Condition No

012 Record Summary No Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - 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 Method No Series data No Condition No

013 End of sample

014 Park Titration stand Rondo60/1A Position Rinse beaker

Condition No

27

M364-B

--

pH 3 and pH 10 buffer solutions

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

Titration Excellence T70/T90Rondo 20 Sample changer1 additional dosing unit (20 mL)

--

DV1010 and DV1020 BurettesTitration beakers ME-101974XS205 Balance, SP250PC with LabX Software

METTLER TOLEDO

Dispose of as halogenated organicwaste

Wastedisposal

Preparation and Procedures60 mL solvent ASTM D4739-06aSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


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

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

3) The acidic and the alkaline aqueous buffers are measuredand stored as auxiliary values H[Buffer pH3] (BN) and H[BuffferpH10] (SBN, Strong Base Number). The values are then usedfor the EQP termination and the calculation R1.

4) 60 mL ASTM D4739-06a solvent are added using anadditional dosing unit. This step can be performed manuallyusing a dispenser or a graduated cylinder.

5) Blank value determinations are performed for every newbatch of solvent by titration with HCl in 2-propanol to pH 3potential value. The result is stored as blank B[ASTM D4739].

6) For SBN, the solvent is titrated with KOH in 2-propanol to pH10 buffer potential value and stored as B[ASTM D4739 pH10].

This method allows a fully automated procedure using a samplechanger and an additional dosing unit. It can be modified formanual operation. Select "Manual stand" in the method function"Titration stand".


2) The base number BN is defined as the consumption ofhydrochloric acid to a specific endpoint to neutralize the alkalinecomponents of the oil. It is expressed as mg KOH/g sample:- If an EQP is found between the acidic buffer potential value anda 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 atthe potential value of the acidic buffer pH3.

3) Between each sample it is necessary to condition theelectrode under stirring during 300 s in deion. water. Theelectrode is parked in buffer pH 4 (Rinse beaker).


Remarks

Consumption of HCl in 2-Propanol up toEQP or acidic potential value:R1=Q (mmol) orR1=QE(H[Buffer pH3])SBN blank: Consumption of KOH in 2-Propanol up to EQP/potential value:R1=Q (mmol) orR1=QE(H[Buffer pH10])

Calculation

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

Standard KOH in 2-propanol 0.1 mol/L / KHP


Wastedisposal

28



Method m364B Blank Base Number According to ASTM D4739-06a

Measured 17.01.2007

RESULTSNo. ID Sample size and results1 ASTM D4739 Solvent 60.0 mL

R1 = 0.00478 mmol Consumption (Buffer potential)R3 = 0.00469 mmol Consumption (EQP)

2 ASTM D4739 Solvent 60.0 mLR1 = 0.00487 mmol Consumption (Buffer potential)R3 = 0.00478 mmol Consumption (EQP)




STATISTICSNumber results R1 n = 5Mean value x = 0.00482 mmol Consumption (Buffer potential)Standard deviation s = 0.00003 mmol Consumption (Buffer potential)Relative standard deviation srel = 0.697 %

Number results R3 n = 5Mean value x = 0.00473 mmol Consumption (EQP)Standard deviation s = 0.00003 mmol Consumption (EQP)Relative standard deviation srel = 0.694 %

Titration curve

Results

29

Method: m364B Blank BN According to ASTM 17.01.2008User: Nijman

001 Title Type General titration Compatible with T70/ T90 ID M364_B Title Blank ASTM D4739 Author Mettler Toledo Date / Time 17.01.2008 Modified at 17.01.2008 Modified by Administrator Protect No SOP None LabX SOP002 Conditioning Titration stand Rondo60/1A

Position Conditioning beaker Time [s] 20 Speed [%] 30 Condition No003 Sample Number of IDs 1

ID 1 ASTM D4739 Solvent Entry Type Fixed volume Volume [mL] 60.0 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0004 Titration stand

Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No005 Dispense (normal) [1] Titrant ASTM D4739 solvent Concentration [mol/L] 1 Volume [mL] 60 Dosing rate [mL/min] 60.0 Condition No006 Stir Speed [%] 30

Duration [s] 10 Condition No007 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG116-Solvent Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode Volume Volume 0.02 Wait time [s] 10 Predispense Mode Volume Volume [mL] 0.2 Wait time [s] 5 Control Control User Titrant addition Incremental dV (mL) 0.002 Mode Fixed time dt [s] 30 Evaluation and Recognition Procedure Standard Threshold [mV/mL] 7500.0 Tendency Positive Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 1.0 At potential Yes Potential H[Buffer pH3]+100 Termination tendency Positive At Slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No008 Calculation R1

Result Consumption (Buffer potential) Result Unit mmol Formula R1=QE(H[Buffer pH3]) Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No

Method009 Calculation R3

Result Consumption (EQP) Result Unit mmol Formula R3=Q Constant C= 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 No010 Record Summary No Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - 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 Method No Series data No Condition No011 Conditioning

Type Fix Interval 1 Position Conditioning beaker Time [s] 300 Speed [%] 30 Condition No012 End of sample013 Park

Titration stand Rondo60/1A Position Rinse beaker

Condition No014 Blank

Name ASTM D4739 Value B= Mean[R1] Unit mmol Limits No Condition Yes

Formula Mean[R1]>0015 Blank

Name ASTM D4739 Value B= Mean[R3] Unit mmol Limits No Condition Yes Formula Mean[R3]>0016 Calculation R2

Result Mean Consumption (Buffer potential) Result Unit mmol Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Send to buffer No Condition No017 Calculation R4

Result Mean Consumption (EQP) Result Unit mmol Formula R4=Mean[R3] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Send to buffer No Condition No018 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No

30

M364-C

Potassium hydroxide, KOHM(KOH)=56.1 g/mol, z=1

50 mL deionized water

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

Titration Excellence T50/T70/T90Rondo 20 Sample changer1 additional dosing unit

HCl + KOH = Cl- + K+ + H2O

DV1010 BurettesTitration beakers ME-101974PC with LabX Software

METTLER TOLEDO

Disposal as halogenated organic wasteWastedisposal

Preparation and ProceduresStandardized KOH in 2-Propanolc(KOH) = 0.1 mol/L, 8.00 mL

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi111-SCIndication

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

1) Add 50 ml deionized into the titration beaker

2) 8 mL KOH in 2-propanol are added automaticlayy by menasot an additional dosing unit. If this is not available, the samplecan be added manaully using a pipette.

3) The mean value of the titer determinations is savedautomatically as the titer for the titrant by means of the functionTITER in the method.


Remarks

Titer HCl:

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

The real value for the KOH concentrationdetermined in M364_D is used for the titerdetermination of HCl in 2-Propanol.

Calculation

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

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


Wastedisposal

31



Method m364C Titer HCl in 2-PropanolMeasured 07.03.2008

RESULTSNo. ID Sample size and results1 KOH in 2-Propanol 8.0 mL

R1 = 0.99689 -- Titer HCl2 KOH in 2-Propanol 8.0 mL






R1 = 0.99694 -- Titer HCl

STATISTICSNumber results R1 n = 7Mean value x = 0.99652 -- Titer HClStandard deviation s = 0.00033 -- Titer HClRelative standard deviation srel = 0.034 %

Titration curve

Results

32

Method: m364C Titer of HCl in 2-Propanol 07.03.2008User: Melanie Nijman

001 Title Type Titer determination Compatible with T50 / T70 / T90 ID M364_C Title Titer of HCl in 2-Propanol Author melanie Nijman Date / Time 26.02.2008 Modified at 07.03.2008 Modified by Administrator Protect No SOP None LabX SOP

002 Sample (Titer) Titrant HCl in 2-Propanol Concentration 0.1 Standard KOH in 2-Propanol Type of standard liquid Entry type Fixed volume Volume [mL] 8.0 Correction factor 1.0 Temperature [°C] 25.0


004 Dispense (normal) [1] Titrant KOH in 2-Propanol

Concentration [mol/L] 0.1 Volume [mL] 8.0 Dosing rate [mL/min] 60.0 Condition No

005 Stir Speed [%] 30

Duration [s] 10 Condition No

006 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG111-SC Unit pH Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 8.0 dV(min) [mL] 0.01 dV(max) [mL] 0.5 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold [pH/mL] 3.0 Tendency None Ranges 0 Add. EQP criteria No Buffer capacity No Termination At Vmax [mL] 10.0 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

007 Calculation R1 Result Titer Result Unit -- Formula R1=VENDDi/(VEQ*c*C) Constant C= 1/(cst*H[KOH Titer]*z) M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No

Method008 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - 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 Method No Series data No Condition No

009 End of sample

010 Titer Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 TITER= Mean[R1] Limits No

Condition No

011 ParkTitration stand Rondo60/1A

Position Conditioning beaker Condition No

012 Calculation R2 Result Mean Titer Result Unit -- Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Send to buffer No Condition No

013 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No

Condition No

33

M364-D

Potassium hydrogen phthalateM = 204.23 g/mol; z=1

50 mL deionized water

KOH in 2-propanolc(KOH) = 0.1 mol/L

Titration Excellence T50/T70/T90Rondo 20 Sample changer

KHC8H4O4 + KOH = H20 + K2C8H4O4

DV1010 BurettesTitration beakers ME-101974PC with LabX Software

METTLER TOLEDO

Disposal as halogenated organic wasteWastedisposal

Preparation and ProceduresPrimary standard KHPm = ~ 0.11 g

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi111-SCIndication

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

1) weigh the standard into the glass titration beaker in order toavoid electrostatic interferences.

2) Add 50 ml deionized into the titration beaker.

3) The mean value of the titer determinations is savedautomatically as the titer for the titrant by means of the functionTITER in the method.

1) The titrant has to be protected against the uptake of CO2 fromthe air.NaOH on carrier (e.g. "Sodium hydroxide on support", MERCKno. 101564, or "Sodium hydroxide on carrier", FLUKA Nr.03350) is an effective medium to avoid such formation ofcarbonate.


Remarks

Titer KOH:

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

Calculation

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

Standard --


Wastedisposal

34



Method m364D Titer of KOH in 2-propanolMeasured 28.02.2008

RESULTSNo. ID Sample size and results1 KHP 0.1057 g

R1 = 0.9870 -- Titer KOH2 KHP 0.1030 g

R1 = 0.9920 -- Titer KOH3 KHP 0.1018 g

R1 = 0.9960 -- Titer KOH4 KHP 0.1209 g

R1 = 0.9900 -- Titer KOH5 KHP 0.1183 g

R1 = 0.9920 -- Titer KOH6 KHP 0.1205 g

R1 = 0.9930 -- Titer KOH

STATISTICSNumber results R1 n = 6Mean value x = 0.992 -- Titer KOHStandard deviation s = 0.003 -- Titer KOHRelative standard deviation srel = 0.304 %

Titration curve

Results

35

Method: m364D Titer of KOH in 2-Propanol 28.02.2008User: Melanie Nijman

001 Title Type Titer determination Compatible with T50 / T70 / T90 ID M364_D Title Titer of KOH in 2-Propanol Author Melanie Nijman Date / Time 26.02.2008 Modified at 28.02.2008 Modified by Administrator Protect No SOP None LabX SOP

002 Sample (Titer) Titrant KOH in 2-Propanol Concentration 0.1 Standard Potassium hydrogen phthalate Type of standard solid Entry type Weight Lower limit 0.0 Upper limit 0.5 Correction factor 1.0 Temperature [°C] 25.0 Input Arbitrary


004 Stir Speed [%] 30

Duration [s] 30 Condition No

005 Titration (EQP) [1] Titrant Titrant KOH in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG111-SC Unit pH Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 8.0 dV(min) [mL] 0.01 dV(max) [mL] 0.5 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold [pH/mL] 3.0 Tendency None Ranges 0 Add. EQP criteria No Buffer capacity No Termination At Vmax [mL] 10.0 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

006 Calculation R1 Result Titer Result Unit -- Formula R1=m/(VEQ*c*C) Constant C= M/(10*p*z) M M[Potassium hydrogen phthalate] z z[Potassium hydrogen phthalate] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

Method007 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - 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 Method No Series data No Condition No

008 End of sample

009 Titer Titrant KOH in 2-Propanol Concentration [mol/L] 0.1 TITER= Mean[R1] Limits No

Condition No

010 ParkTitration stand Rondo60/1A

Position Conditioning beaker Condition No

011 Calculation R2 Result Mean Titer Result Unit -- Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Send to buffer No Condition No

012 Auxiliary value Name KOH Titer Formula H= R2 Limits No Condition No

013 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No

Condition No

36

M365

--

--

Hydrochloric acid, HClc(HCl) = 0.1 mol/L

Titration Excellence T50/T70/T90Rondolino Sample changer

HCl + NaOH = NaCl + H2O

HCl + CO32- = HCO3

- + Cl-

HCl + HCO3- = CO2 + H2O + Cl-

LabX Titration Software1 DV1010 buretteTitration beakers ME-101974Cable MultiPinTM-Lemo/Pt1000

METTLER TOLEDO

Neutralization of the acidic waste beforefinal disposal.

Wastedisposal

Preparation and Procedures50 mL tap waterSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi117-SC with internal temperaturesensor Pt1000

Indication

m-Value of Tap Water with Automatic Temperature Compensation

Note: This method allows a fully automated analysis procedureby using a Rondolinos sample changer. The method can beeasily modified for manual operation. Select "Manual stand" inthe method function "Titration stand".

1) Before the analysis an electrode calibration was performedusing 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 beanalyzed. Keep it closed and at sampling temperature.

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

4) The samples were analysed using a Rondolino samplechanger. The electrode was rinsed during 2 s and conditionedduring 10 s (Rondolino settings: 6). In this way, the electrode iscleaned with deionised water before starting the subsequentsample.

5) The automatic temperature compensation was achievedusing the new DG117-SC titration electrode with theMultiPinTM-Lemo/Pt1000 cable, connected to the analogueboard of the T50.

See also: Application M415, Brochure 34, ME-51 725 066

1) The method parameters have been optimised for the sampleused in this application. It may be necessary to slightly adaptthe method to your specific sample.

2) Automatic temperature compensation during titrationincreases 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 missingtemperature correction. However the obtained m-valuesdetermined with both sensors are, as expected, rather similar.

4) The m-value (total alkalinity) represents the acid neutralizingcapacity and is determined in e.g. drinking water. Acidity canaffect corrosion, soil leaching and aquatic life in general. Thename originates from the methyl orange color indicator (red toyellow-orange at pH 4.3) formerly used. The acid capacitydepends on the equilibrium of free CO2, bicarbonate HCO3

-, andcarbonate CO3

2- in the on its temperature.Mineral weathering buffers groundwaters, e.g. limestone rockCaCO3 (s) + CO2 (g) = Ca2+ (aq) + 2 HCO3

- (aq)The bicarbonate ion then acts as a base to neutralize acids:HCO3

- (aq) + H+ (aq) = CO2 (g) + H2O (l)

Remarks

Total alkalinity or methyl orangealkalinity (m-value) is expressed asmmol/L or mg/L CaCO3

Calculation

Titration Excellence Line: The m-value of tap water is determined by endpoint titration to pH 4.3 with theDG117-SC sensor, which allows automatic temperature compensation during titration.

Standard Tris(hydroxymethyl)-aminomethane, 50-100 mg

Thomas HitzAuthor

Wastedisposal

37

EP-titraion (m-value of tap water)

3

4

5

6

7

8

9

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6

Volume (mL)

pH-v

alue


All results Method-ID m365 Sample Tap water (1/8) R1 (Content) 2.62200 mmol/L Sample Tap water (2/8) R1 (Content) 2.61534 mmol/L Sample Tap water (3/8) R1 (Content) 2.61600 mmol/L Sample Tap water (4/8) R1 (Content) 2.61250 mmol/L Sample Tap water (5/8) R1 (Content) 2.62000 mmol/L Sample Tap water (6/8) R1 (Content) 2.61800 mmol/L Sample Tap water (7/8) R1 (Content) 2.61600 mmol/L Sample Tap water (8/8) R1 (Content) 2.63200 mmol/L

Statistics Method-ID m365 Content R1 Samples 8 Mean 2.61898 mmol/L s 0.00602 mmol/L srel 0.230 %

Titration curve

Results

38

Method m365 m-Value of tap water 10.08.2007Author Thomas Hitz

001 Title Type General titration Compatible with T50 / T70 / T90 ID m365 Title m-Value of tap water Author Thomas Hitz Date/Time 10.08.2007 10:00:00 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Tap water Entry type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C

003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1

004 Stir Speed 50 % Duration 10 s

005 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L

Sensor Type pH Sensor DG117 Unit pH

Temperature acquisition Temperature acquisition Yes Temerature sensor interner Sensor 1 Unit °C

Stir Speed 50 %


Control Control User End point type Absolute Tendency Negative Endpoint value 4.30 pH Control band 3.0 pH Dosing rate (max) 10 mL/min Dosing rate (min) 10 mL/min

Termination At EP Yes Tuermination delay 10 s At Vmax 10.0 mL Max. time 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

Method007 Record Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No d2E/dV2 - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No

008 End of sample

39

M366

Na2O, SiO2

KF solution, 25%

HCl, 2.0 mol/L (hydrochloric acid)NaOH, 1.0 mol/L (sodium hydroxide)

Titration Excellence T70/T902 additional dosing units

Na2SiO3 + 2HCl -> 2NaCl + SiO2 + H2OSiO2+6KF+2H2O -> Na2SiF6 + 4NaOHHCl + NaOH -> NaCl + H2O

Titration beakers ME-101974LabX Titration SoftwareRondo 20 Sample Changer

METTLER TOLEDO

Dilute and non-acidic fluoride solutionsdo not have to be treated as specialwaste.

Wastedisposal

Preparation and ProceduresWaterglass ~1.0 gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

Sb850-S7/120 (pH sensor input)DX202-SC (ref. electrode)

Indication

Na2O and SiO2 in Waterglass

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

Add excess KF to form NaOH from SiO2:SiO2 + 6 KF + 2 H2O -> Na2SiF6 + 4 NaOH

Neutralise NaOH formed with excess HCl, back-titrate remainingHCl with NaOH in Titration (EQP) [2]:HCl + NaOH -> NaCl + H2O

1) Because of the high fluoride content in acidic environmentglass electrodes and titration beakers cannot be used for thedetermination of Na2O and SiO2 in waterglass.

2) For this reason only the polypropylene titration beakers canbe used. Care needs to be taken when weighing in thewaterglass samples in the polypropylene beakers that staticelectricity is avoided as much as possible.

3) Also, no glass sensors may be used for this determination asthese will be the corroded as well.All fluoride solutions should be kept in plastic bottles.

The titration curve for the first EQP titration shows clearly thatmore than one site is present for the alkali metal oxide (mainlyNa2O) 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

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

Remarks

R1: Na2O content (%)R2: SiO2 content (%)R3: Relative amounts Na2O/SiO2 (-)

Calculation

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

Standard TRIS/THAM for HCl, KHP for NaOH


Wastedisposal

40


Method m366 Na2O and SiO2 in waterglass

RESULTSNo. ID Sample size and results

1 Waterglass 0.9365 gR1 = 49.91661 % ContentR2 = 44.05010 % ContentR3 = 1.13318 -







STATISTICSNumber results R1 n = 7Mean value x = 49.9043 % ContentStandard deviation s = 0.03298 ContentRelative standard deviation srel = 0.066 %

Number results R2 n = 7Mean value x = 44.21186 % ContentStandard deviation s = 0.12739 ContentRelative standard deviation srel = 0.288 %

Number results R3 n = 7Mean value x = 1.12876 -Standard deviation s = 0.00333 -Relative standard deviation srel = 0.295 %

Titration curve

Results

41

Method: m366 Na2O and SiO2 in waterglass 08.08.2007User: Melanie Nijman

001 Title Type General titration Compatible with T70/ T90 ID m366 Titel Na2O/SiO2 in Waterglass Author Melanie Nijman Date / Time 03.08.2007 Modified at 08.08.2007 Protect No SOP None LabX SOP002 Sample Number of IDs 1

ID 1 Waterglass Entry Type Weight Lower limit [g] 0.8 Upper limit [g] 1.2 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0 Entry Arbitrary003 Titration stand Type Rondo60/Tower A Titration stand Rondo60/1A Lid handling No004 Stir Speed [%] 50 Duration [s] 60 Condition No005 Titration (EQP)

Titrant Titrant HCl Concentration [mol/L] 2.0 Sensor Type mV Sensor Sb-850 Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 9.0 dV (min) 0.008 dV (max) 0.4 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold 1500 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 10 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 No006 Calculation R1 Result Na2O Content Result Unit % Formula R1=Q*C/m Constant C= M/(10*z) M M[Sodium oxide] z z[Sodium oxide] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No007 Dispense (normal) Titrant 25% KF Concentration [mol/L] 25 Volume [mL] 10.0 Dosing rate [mL/min] 60.0 Condition No008 Dispense (normal) Titrant HCl Concentration [mol/L] 2.0 Volume [mL] 16.0 Dosing rate [mL/min] 60.0 Condition No

Method009 Stir Speed [%] 30 Duration [s] 30 Condition No010 Titration (EQP)

Titrant Titrant NaOH Concentration [mol/L] 1.0 Sensor Type mV Sensor Sb-850 Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 5 dV (min) 0.002 dV (max) 0.4 Mode Equilibrium controlled dE 1 dt [s] 1.0 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold 150 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 15 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 No011 Calculation R2 Result SiO2 Content Result Unit % Formula R2=(QEX[1]+QENDDi[2]-Q[2])*C/m Constant C= M/(10*z) M M[Silicon dioxide] z z[Silicon dioxide] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No012 Calculation R3 Result Na2O/SiO2 Result Unit - Formula R2=R1/R2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No013 Conditioning Type Fix Interval 1 Position Conditioning beaker Time [s] 20 Speed [%] 50 Condition No014 Record Summary No Results Per sample Raw results Per sample Table of measured values No Sample data No Resource data No E - V All titration functions dE/dV - V All titration functions ... E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No Condition No015 End of sample

42

M367

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

50 mL Solvent (ASTM 3227)2-Propanol p.a.Toluene p.a.Sodium acetate (anhydrous)

Silver nitrate (AgNO3) in 2-Propanolc(AgNO3) = 0.01 mol/L

Titration Excellence T70/T90Rondo 20 Sample Changer withPowerShowerTM

NaCl + AgNO3 = AgCl + NaNO3

1 DV1005 BuretteGlass titration beaker ME-101446XS205 BalanceLabX Titration Software

METTLER TOLEDO

Filtration. The precipitate (AgCl) has tobe classified as special waste. Theliquid phase has to be disposed asorganic waste.

Wastedisposal

Preparation and ProceduresUsed motor oil, approx. 10 gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DMi145-SC (with 1 mol/L KNO3)Indication

Chloride Content in Used Motor Oil

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

2) 2.5 mL 0.01mol/L NaCl standard solution are added tospike the sample since the chloride content is too low(Standard-Addition).

3) 50 mL Solvent ASTM 3227 will be added automatically withthe Rondo membrane pump.

4) The sample serie is analysed using a Rondo 20 samplechanger. Special beaker 1 and 2 are filled with toluene andthe 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 themark 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 fillup to the mark with 2-Propanol (c=0.1 mol/L)

- take 100.0 mL of this solution and dilute it with 2- Propanolto 1L in a volumetric flask (c=0.01 mol/L)

- The method parameters have been developed and optimisedfor the above mentioned sample. It may be necessary toslightly adapt the method to your specific sample. The weightof the sample can vary from 0.5 to 30 g (depending on thekind of oil).

- Sulfides interfere with the analysis. If necessary, they have tobe oxidised to sulfates by adding 10 mL 30% H2O2 previousto the analysis. In this application, this was not the case.

Literature:1) METTLER TOLEDO Application brochure 20, ME-51 725 0202) METTLER TOLEDO Application brochure 34, ME-51 725 066

Remarks

R1: Content (mg/L Chloride)

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

1 mL AgNO3 (0.01 mol/l) is equal to0.354 mg Chloride

Calculation

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

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

Claudia SchreinerAuthor

Wastedisposal

43


Start time: 04.12.2007

Sample Data Note / ID Sample size No. 1/6 Motor Oil 10.0318 g No. 2/6 Motor Oil 10.1953 g No. 3/6 Motor Oil 10.0720 g No. 4/6 Motor Oil 10.1120 g No. 5/6 Motor Oil 10.1386 g No. 6/6 Motor Oil 10.1322 g

Results Note / ID Rx Result Unit No. 1/6 Motor Oil R1= 28.25 mg/L No. 2/6 Motor Oil R1= 27.80 mg/L No. 3/6 Motor Oil R1= 26.33 mg/L No. 4/6 Motor Oil R1= 27.35 mg/L No. 5/6 Motor Oil R1= 27.28 mg/L No. 6/6 Motor Oil R1= 26.38 mg/L

Statistics Rx Name n Mean Value Unit s srel[%] R1 Chloride 6 27.23 mg/L 0.76 2.8

Titration curve

Results

44

Method 367 Chloride content in motor oil 04.12.2007Author Claudia Schreiner

001 Title Type General titration Compatible with T70 / T90 ID 367 Title Chloride in motor oil Author Claudia Schreiner Date/Time 04.12.2007 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Motor oil Entry type Weight Lower limit 0 g Upper limit 15 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary


004 PumpAuxiliary reagent ASTM D3227 solvent

Volume 50.0 mL

005 Stir Speed 60% Duration 120 s

006 Titration (EQP) [1]Titrant

Titrant AgNO3 Concentration 0.01 mol/L

Sensor Type mV Sensor DMi145-SC Unit mV


Stir Speed 40%


Control Control User Titrant addition Incremental dV 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t(min) 5 s t(max) 30 s

Evaluation and Recognition Procedure Standard Threshold 100 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No

Termination At Vmax 5 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No

Method007 Calculation R1 Result Chloride Result unit mg/L Formula R=(Q-H[Std NaCl])*C/m Constant C= M*1000/z M M[Chloride] z z[Chloride] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

008 RinseAuxiliary reagent ASTM D3227 solventRinse cycles 1Vol. per cycle [mL] 15Position Actual positionDrain NoCondition No

009 ConditioningType FixInterval 1Position Special beaker 1Time 120sSpeed 60%

010 ConditioningType FixInterval 1Position Special beaker 2Time 300sSpeed 60%

011 ConditioningType FixInterval 1Position Conditioning beakerTime 120sSpeed 60%

012 End of sample

45

M368

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

50 mL Solvent (ASTM 3227)2-Propanol p.a.Toluene p.a.Sodium acetate (anhydrous)

Silver nitrate (AgNO3) in 2-Propanolc(AgNO3) = 0.01 mol/L

Titration Excellence T50/T70/T90Rondo 20 Sample Changer withPowerShowerTM


1 DV1005 BuretteGlass titration beaker ME-101446XS205 BalanceLabX Titration Software

METTLER TOLEDO

Filtration. The precipitate (AgCl) has tobe classified as special waste. Theliquid phase has to be disposed asorganic waste.

Wastedisposal

Preparation and ProceduresPrimary standardSodium chloride solution (0.01 mol/L),2.5 mL

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DMi145-SC (with 1 mol/L KNO3)Indication

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

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

2) 50 mL Solvent ASTM 3227 will be added automatically withthe Rondo membrane pump.

3) The sample serie is analysed using a Rondo 20 samplechanger. The condition beaker is filled with solvent ASTM3227.

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 themark 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 fillup to the mark with 2-Propanol (c=0.1 mol/L)

- take 100.0 mL of this solution and dilute it with 2- Propanolto 1L in a volumetric flask (c=0.01 mol/L)

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

Remarks

R1: Titer

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

1 mL AgNO3 (0.01 mol/l) is equal to0.584 mg sodium chloride

Calculation

Titration Excellence Line: Method for the titer determination of 0.01 mol/L AgNO3 by precipitation titration withsodium chloride as a primary standard.

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


Wastedisposal

46



Sample Data Note / ID Sample size No. 1/6 NaCl solution 2.5 mL No. 2/6 NaCl solution 2.5 mL No. 3/6 NaCl solution 2.5 mL No. 4/6 NaCl solution 2.5 mL No. 5/6 NaCl solution 2.5 mL No. 6/6 NaCl solution 2.5 mL

Results Note / ID Rx Result Unit No. 1/6 NaCl solution R1= 0.9694 mg/L No. 2/6 NaCl solution R1= 0.9684 mg/L No. 3/6 NaCl solution R1= 0.9704 mg/L No. 4/6 NaCl solution R1= 0.9690 mg/L No. 5/6 NaCl solution R1= 0.9708 mg/L No. 6/6 NaCl solution R1= 0.9711 mg/L

Statistics Rx Name n Mean Value Unit s srel[%] R1 Titer 6 0.9698 mg/L 0.0011 0.11

Titration curve

Results

47

Method 368 Titer 0.01 mol/L AgNO3 04.12.2007Author Claudia Schreiner

001 Title Type General titration Compatible with T50 / T70 / T90 ID 368 Title Titer 0.01 mol/L AgNO3 Author Claudia Schreiner Date/Time 04.12.2007 Modified -- Modified by -- Protect No SOP None

002 Sample (Titer) Titrant AgNO3 Concentration 0.01 mol/L Standard NaCl Type of standard liquid Entry type Fixed volume Volume 2.5 mL Correction factor 1.0 Temperature 25.0°C



Volume 50.0 mL



Titrant AgNO3 Concentration 0.01 mol/L

Sensor Type mV Sensor DMi145-SC Unit mV


Stir Speed 40%

Predispense Mode Volume Volume 1.5 mL Wait time 15 s

Control Control User Titrant addition Incremental dV 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t(min) 5 s t(max) 30 s


Termination At Vmax 5 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No

Method007 Calculation R1 Result Titer Result unit --- Formula R= m/(VEQ*c*C) Constant C= 1/(cst*z) M M[Sodium chloride] z z[Sodium chloride] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

008 RinseAuxiliary reagent ASTM D3227 solventRinse cycles 1Vol. per cycle [mL] 15Position Actual positionDrain NoCondition No

009 ConditioningType FixInterval 1Position Conditioning beakerTime 120sSpeed 60%

010 End of sample

011 Titer Titrant AgNO3 Concentration 0.01 mol/L Titer = Mean[R1] Limits No

48

M369

Peroxide functional group, R-OOH

20 mL acetic acid/chloroform (3:2)1 mL saturated KI solution50 mL deion. water

Sodium thiosulfate, Na2S2O3

c(Na2S2O3)= 0.01mol/L


R-OOH + 2 I- + 2 H3O+ =

R-OH + I2 + 3 H2O

I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6

2 additional dosing units1 DV1020 and 2 DV1010 BurettesGlass titration beaker ME-101446XS205 Balance, LabX 2.6

METTLER TOLEDO

The waste contains halogenatedorganic solvents and has to bedisposed of accordingly.

Wastedisposal

Preparation and ProceduresSunflower oil, 4-5 gOlive oil, 1 gMargarine, 2 g

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DMi147-SCIndication

Peroxide Value of Edible Oils and Fats

1) Beakers have to be cleaned very well. Invisible fat residues ormetal traces can strongly affect the result.

2) About 3 g of sample were dissolved in 20 mL of acetic acid/chloroform (3:2) The acetic acid/chloroform mixture was addedby the function DISPENSE.

3) 1 mL saturated KI solution is added by an additional burette.The reaction takes place and iodine is formed.

4) 50 mL deionized water are added by the membrane pump ofRondo 20.

5) Iodine is titrated with sodium thiosulphate.

127 g KI were dissolved in 100 mL water to obtain thesaturated KI solution. The solution has to be kept in the dark.

Impurities of the solvent are taken into account by a blank valuedetermination. The blank value determination is done under thesame conditions as the peroxide value determination itself. Thevalue is stored under B[1].

1) Fats and oils undergo changes during storage due tooxidation with air (oxidative rancidity). The compounds formedreact as peroxides. Their content is commonly expressed as the"peroxide value" in milliequivalents peroxidic oxygen per kg ofsample.

2) Peroxide values higher than 10 to 20 meq O2/kg arecommonly interpreted as rancidity. Unrefined oils have higherperoxide values. They are usually in the range between 5 to 20meq 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 isnot complete yet at this time. 200 to 300 seconds were foundto yield the highest results. Longer generation times resulted inlow results (secondary reactions between iodine and the oil).

3) The duration of the generation time (time between 'adding theKI solution' and 'adding the water + starting the titration') is thecritical point for repeatable results.

Remarks

R = (Q-B[1])*C/mC = 1000, meq/kg

B[1]: Solvent blank value, mmol

Calculation

Titration Excellence Line: Method for the determination of the peroxide value in oil, fat and margarine byiodometric titration with sodium thiosulphate of released iodine.

Standard Potassium iodate, KIO3

Maria-José SchmidAuthor

Wastedisposal

49

Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN -16.7 NaN NaN 0 250.057 0.057 -8 8.7 NaN 3 250.086 0.029 -11.3 -3.3 NaN 8 250.1 0.014 -11.2 0.1 NaN 13 250.135 0.035 -10.9 0.3 NaN 18 250.222 0.087 -10.4 0.5 5.85 23 250.322 0.1 -10.1 0.3 4.51 28 250.422 0.1 -9.6 0.5 4.57 33 250.522 0.1 -9.1 0.5 4.98 38 250.622 0.1 -8.6 0.5 5.57 43 250.722 0.1 -8.1 0.5 6.12 48 250.822 0.1 -7.3 0.8 6.4 53 250.922 0.1 -6.7 0.6 6.84 58 251.022 0.1 -6 0.7 7.31 64 251.122 0.1 -5.3 0.7 7.76 69 251.222 0.1 -4.5 0.8 8.08 74 251.322 0.1 -3.6 0.9 8.42 79 251.422 0.1 -2.7 0.9 8.92 84 251.522 0.1 -1.8 0.9 9.72 89 251.622 0.1 -0.9 0.9 10.58 94 251.722 0.1 0.2 1.1 12.06 99 251.822 0.1 1.7 1.5 13.44 104 251.922 0.1 3.1 1.4 15.57 109 252.022 0.1 4.7 1.6 17.35 114 252.122 0.1 6.8 2.1 16.96 120 252.222 0.1 8.9 2.1 22.42 125 252.322 0.1 12.2 3.3 36.29 130 252.422 0.1 15.7 3.5 64.9 135 252.522 0.1 21.7 6 129.96 142 252.622 0.1 35.3 13.6 311.23 158 252.642 0.02 42.2 6.9 520.27 169 252.648 0.006 46.4 4.2 822.53 180 252.654 0.006 50 3.6 1165.65 190 252.661 0.007 57.2 7.2 1330.43 202 252.666 0.005 66.2 9 1635.55 217 252.671 0.005 78.3 12.1 1915.47 232 25

EQP1 2.671216 NaN 78.8 NaN 1916.21 NaN NaN2.676 0.005 89.8 11.5 1536.17 247 252.681 0.005 97.7 7.9 1263.43 262 252.686 0.005 104 6.3 1191.38 277 252.694 0.008 109.9 5.9 774.71 292 252.704 0.01 114.2 4.3 NaN 303 252.728 0.024 120.3 6.1 NaN 318 252.772 0.044 125.3 5 NaN 330 252.872 0.1 130 4.7 NaN 342 252.972 0.1 132.5 2.5 NaN 351 25


Method: DM1471 Peroxide number 10/25/2007 11:27:34 AMStart time: 25.10.2007 1:53:24 PM___________________________________________________________________________________________

Sample Data Comment / ID Sample size No. 1/5 Olive oil 0.8164 g No. 2/5 Olive oil 0.8523 g No. 3/5 Olive oil 0.815 g No. 4/5 Olive oil 0.8149 g No. 5/5 Olive oil 0.8235 g

Results No. Comment / ID Start time Rx Result Unit Name 1/5 Olive oil 10/25/2007 1:53:25 PM R1= 0.024 mmol Consumption R2= 25.601 meq/kg Content 2/5 Olive oil 10/25/2007 2:05:29 PM R1= 0.025 mmol Consumption R2= 25.795 meq/kg Content 3/5 Olive oil 10/25/2007 2:17:32 PM R1= 0.024 mmol Consumption R2= 26.013 meq/kg Content 4/5 Olive oil 10/25/2007 2:29:19 PM R1= 0.024 mmol Consumption R2= 25.888 meq/kg Content 5/5 Olive oil 10/25/2007 2:41:10 PM R1= 0.024 mmol Consumption R2= 26.074 meq/kg ContentSQC/Statistics

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

R1 Consumption 5 0.024 mmol 0.000 1.848 R2 Content 5 25.874 meq/kg 0.187 0.724

Additional results

Sample Size n Mean value Unit s srel[%] ____________________________________________________________________________________________

Sunflower oil 4-5 g 5 0.028 mmol 0.000 1.609 5.583 meq/kg 0.044 0.791

Margarine 2 g 6 0.022 mmol 0.001 4.624 11.759 meq/kg 0.578 4.918

Mais oil 4-5 g 5 0.021 mmol 0.000 2.150 3.980 meq/kg 0.043 1.087

Titration curve

Results

50

Method DM1471 Peroxide number 25.10.2007Author schmid

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 None002 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 25.0°C Entry Arbitrary003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant AA/Chloroform Concentration 32 Volume 20 mL Dosing rate 60.0 mL/min Condition No005 Stir Speed 40 % Duration 30 s Condition No006 Dispense (normal) [2] Titrant KI Concentration 63.5 Volume 1 mL Dosing rate 60.0 mL/min Condition No007 Stir Speed 30 % Duration 30 s Condition No008 Stir Speed 0 % Duration 60 s Condition No009 Pump

Auxiliary reagent Water Volume 50.0 mL Condition No010 Titration (EQP) [1]Titrant

Titrant Na2S2O3

Concentration 0.01 mol/LSensor

Type mV Sensor DM147 Unit mVTemperature acquisition

Temperature acquisition NoStir

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

MethodEvaluation and Recognition

Procedure Standard Threshold 200.0 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination

At Vmax 20 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria NoAccompanying stating

Accompanying stating NoCondition

Condition No011 Calculation R1 Result Consumption Result unit mmol Formula R1=Q Constant 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Calculation R2 Result Content Result unit meq/kg Formula R2=(Q-B[1])*C/m Constant 1000 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No013 Record ......014 Rinse

Auxiliary reagent WaterRinse cycles 1Vol. per cycle [mL] 10 mLPosition Actual positionDrain NoCondition No

015 ConditioningType FixInterval 1Position According to intervalTime 60 sSpeed 30%

Condition No016 Rinse


017 ConditioningType FixInterval 1Position Conditioning beakerTime 10 sSpeed 30 %

Condition No 018 End of sample019 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No

51

M370

Potassium iodate, KIO3

M=213.99 g/mol ; z = 6

40 mL HCl 0.1 mol/L1 mL saturated KI solution

Sodium thiosulfate, Na2S2O3

c(Na2S2O3)= 0.01mol/L


IO3- + 5 I- + 6 H+ = 3 I2 + 3 H2O

I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6

2 additional dosing units1 DV1020 and 2 DV1010 BurettesGlass titration beaker ME-101446XS205 Balance, LabX 2.6

METTLER TOLEDO

Inorganic salt solutionWastedisposal

Preparation and Procedures1 mL potassium iodate standardsolution, KIO3

c(KIO3) = 0.01 mol/L

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DMi147-SCIndication

Titer Determination of 0.01 mol/L Na2S2O3

1) Beakers have to be cleaned very well. Fat residues or metaltraces can strongly affect the result.

2) About 3 g of sample were dissolved in 20 mL of acetic acid/chloroform (3:2) The acetic acid/chloroform mixture was addedby the function DISPENSE.

3) 1 mL saturated KI solution is added by an additional burette.The reaction takes place and iodine is formed.

4) 50 mL deionized water are added by the membrane pump ofRondo 20.

5) Iodine is titrated with sodium thiosulphate.

127 g KI were dissolved in 100 mL water to obtain thesaturated KI solution. The solution has to be kept in the dark.

Impurities of the solvent are taken into account by a blank valuedetermination. The blank value determination is done under thesame conditions as the peroxide value determination itself. Thevalue is stored under B[1].

1) Fats and oils undergo changes during storage due tooxidation with air (oxidative rancidity). The compounds formedreact as peroxides. Their content is commonly expressed as the"peroxide value" in milliequivalents peroxidic oxygen per kg ofsample.

2) Peroxide values higher than 10 to 20 meq O2/kg arecommonly interpreted as rancidity. Unrefined oils have higherperoxide values. They are usually in the range between 5 to 20meq 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 isnot complete yet at this time. 200 to 300 seconds were foundto yield the highest results. Longer generation times resulted inlow results (secondary reactions between iodine and the oil).

3) The duration of the generation time (time between 'adding theKI solution' and 'adding the water + starting the titration') is thecritical point for repeatable results.

Remarks

R1=m/(VEQ*c*C)

C=1/(cst*z)

cst = concentration of standard solution

Calculation

Titration Excellence Line: Method for the titer determination of 0.01 mol/L Na2S2O3 by redox titration withpotassium iodate as a primary standard.

Standard ---


Wastedisposal

52

Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN 18.4 NaN NaN 0 251.143 1.143 19.6 1.2 NaN 6 251.714 0.571 20.6 1 NaN 11 252 0.286 21.1 0.5 NaN 16 252.1 0.1 21.3 0.2 NaN 21 252.2 0.1 21.4 0.1 1.86 26 252.3 0.1 21.6 0.2 1.83 31 252.4 0.1 21.8 0.2 1.89 36 252.5 0.1 22 0.2 2.1 41 252.6 0.1 22.2 0.2 2.2 46 252.7 0.1 22.4 0.2 2.2 51 252.8 0.1 22.7 0.3 2.36 56 252.9 0.1 22.9 0.2 2.44 62 253 0.1 23.1 0.2 2.5 67 253.1 0.1 23.4 0.3 2.56 72 253.2 0.1 23.7 0.3 2.64 77 253.3 0.1 23.9 0.2 2.8 82 253.4 0.1 24.2 0.3 2.8 87 253.5 0.1 24.5 0.3 2.9 92 253.6 0.1 24.8 0.3 3.05 97 253.7 0.1 25.1 0.3 3.2 102 253.8 0.1 25.4 0.3 3.3 107 253.9 0.1 25.8 0.4 3.5 112 254 0.1 26.1 0.3 3.64 117 254.1 0.1 26.5 0.4 3.86 122 254.2 0.1 26.9 0.4 4 128 254.3 0.1 27.3 0.4 4.08 133 254.4 0.1 27.7 0.4 4.36 138 254.5 0.1 28.2 0.5 4.54 143 254.6 0.1 28.6 0.4 4.84 148 254.7 0.1 29.1 0.5 5.1 153 254.8 0.1 29.7 0.6 5.4 158 254.9 0.1 30.2 0.5 5.69 163 255 0.1 30.8 0.6 6.1 168 255.1 0.1 31.4 0.6 6.44 173 255.2 0.1 32.1 0.7 6.88 178 255.3 0.1 32.8 0.7 7.5 183 255.4 0.1 33.6 0.8 7.99 188 255.5 0.1 34.4 0.8 8.58 194 255.6 0.1 35.3 0.9 9.23 199 255.7 0.1 36.3 1 10.07 204 255.8 0.1 37.3 1 11.05 209 255.9 0.1 38.5 1.2 12.35 214 256 0.1 39.8 1.3 13.82 219 256.1 0.1 41.3 1.5 15.51 224 256.2 0.1 43 1.7 17.1 229 256.3 0.1 45 2 18.16 234 256.4 0.1 47.3 2.3 23.2 239 256.5 0.1 50.2 2.9 36.4 244 256.6 0.1 54.1 3.9 64.74 250 256.7 0.1 60.4 6.3 131.13 258 256.79 0.09 71.4 11 293.52 272 256.815 0.025 79.3 7.9 480.39 285 256.822 0.007 83.3 4 710.68 294 256.829 0.007 87.6 4.3 987.73 304 256.836 0.007 95.1 7.5 1151.71 319 256.841 0.005 103.2 8.1 1337.28 334 256.846 0.005 111.9 8.7 1610.88 349 25

EQP1 6.846215 NaN 112.3 NaN 1611.06 NaN NaN6.851 0.005 120.2 8.3 1474.04 364 256.856 0.005 127.6 7.4 1174.26 379 256.861 0.005 134.1 6.5 1070.14 394 256.866 0.005 139.3 5.2 881.97 408 256.875 0.009 144.3 5 NaN 420 256.892 0.017 150.4 6.1 NaN 434 256.919 0.027 155.5 5.1 NaN 445 256.981 0.062 161 5.5 NaN 456 257.081 0.1 165.3 4.3 NaN 466 25


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

Results

No. Comment / ID Start time Rx Result Unit Name 1/5 Potassium iodate 09.10.2007 13:42:03 R1= 0.901 -- Titer 2/5 Potassium iodate 09.10.2007 13:55:31 R1= 0.909 -- Titer 3/5 Potassium iodate 09.10.2007 14:08:40 R1= 0.910 -- Titer 4/5 Potassium iodate 09.10.2007 14:21:55 R1= 0.908 -- Titer 5/5 Potassium iodate 09.10.2007 14:35:14 R1= 0.908 -- Titer

SQC/Statistics


R1 Titer 5 0.906 -- 0.004 0.437

Titration curve

Results

53

Method T147 Titer Na2S2O3 09.10.2007Author schmid

001 Title Type Titer determination Compatible with T70 / T90 ID T147 Title Titer Na2S2O3

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 SOP002 Sample (Titer) Titrant Na2S2O3

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 25.0°C003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant HCl Concentration 0.1 mol/L Volume 40.0 mL Dosing rate 60.0 mL/min Condition No005 Dispense (normal) [2] Titrant KI Concentration 63.5 mol/L Volume 1.0 mL Dosing rate 60.0 mL/min Condition No006 Stir Speed 30 % Duration 30 s Condition No007 Stir Speed [%] 0 % Duration [s] 60 s Condition No008 Titration (EQP) [1]Titrant

Titrant Na2S2O3

Concentration 0.01 mol/LSensor

Type mV Sensor DM147 Unit mVTemperature acquisition


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

MethodEvaluation and Recognition

Procedure Standard Threshold 200.0 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination



Condition No009 Rinse


010 Calculation R1 Result Titer Result unit -- Formula R1=m/(VEQ*c*C) Constant 1/(cst*z) M M[Potassium iodate] z z[Potassium iodate] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No011 Record Summary No Results Per sample Raw results Per sample Table of meas. values Last titration function Sample data No ............... Method No Series data No Condition No012 End of sample013 Titer Titrant Na2S2O3

Concentration 0.01 mol/L TITER= Mean[R1] Limits No Condition No014 Park

Titration stand Rondo60/1A Position Conditioning beaker Condition No015 Calculation R2 Result Mean Titer Result unit -- Formula R2=Mean[R1] Constant 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No016 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No

54

M371

Chloride ions, Cl-

M(Cl) = 35.45 g/mol, z = 1

Perchloric acid, HClO4 (0.1 mol/L)Sodium chloride, NaCl (0.001 mol/L)

Silver nitrate, AgNO3

c(AgNO3)= 0.001mol/L



1 additional dosing unit2 DV1010 BurettesTitration beaker ME-101974XS205 Balance, LabX 2.6

METTLER TOLEDO

Neutralization before final disposal asheavy metal aqueous solutions.

Wastedisposal

Preparation and ProceduresEthanol, 40 g(approx. 60 mL)

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DMi148-SCIndication

Chloride Determination in Ethanol

The samples have been prepared by spiking high purity ethanolwith NaCl solution in order to achieve different chorideconcentrations. In this way, several NaCl ethanolic solutionshave 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 thesample.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 thedetermination.

1) Weigh accurately 40 g ethanol into the titration beaker.2) Add 1 mL 0.001 mol/L NaCl standard solution to spike theblank sample.3) 1 mL 0.1 mol/L HClO4 is added to the blank solution usingan additional dosing unit. if this is not available, perchloric acidis added using a manual pipette.4) Place the beaker on the Rondo sample rack and start theblank value determination.

Literature:

1. "Standard Tests Methods for Chloride Ion in Water"ASTM D512-04

2. METTLER TOLEDO Titration Application M359,"Chloride content determination in ethanol based on ASTM D512-04".

3. "Selected METTLER TOLEDO Methods for Biofuel Analysis"Application Brochure 36, May 2007, ME-51725070

Remarks

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

B[Blank EtOH]:Solvent blank value, mmol

Calculation

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

Standard NaCl solution, 1 mL 0.001 mol/L


Wastedisposal

55

Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN 161 NaN NaN 0 250.057 0.057 160.9 -0.1 NaN 3 250.086 0.029 160.4 -0.5 NaN 6 250.1 0.014 160.2 -0.2 NaN 9 250.135 0.035 160.3 0.1 NaN 27 250.222 0.087 158.7 -1.6 -15.74 31 250.422 0.2 154.4 -4.3 -22.1 36 250.622 0.2 149.4 -5 -28.41 42 250.822 0.2 143 -6.4 -37.69 48 250.943 0.121 137.9 -5.1 -45.94 56 251.032 0.089 133.8 -4.1 -54.77 62 251.135 0.103 128.3 -5.5 -68.8 68 251.213 0.078 122.9 -5.4 -85.4 75 251.269 0.056 118 -4.9 -102.81 82 251.314 0.045 113.3 -4.7 -124.84 89 251.355 0.041 108.2 -5.1 -154.59 97 251.388 0.033 103.1 -5.1 -189.02 106 251.415 0.027 97.9 -5.2 -231.57 115 251.435 0.02 93.2 -4.7 -278.49 124 251.452 0.017 88.1 -5.1 -335.6 135 251.466 0.014 83.7 -4.4 -401.04 145 251.479 0.013 78.3 -5.4 -491.7 157 251.49 0.011 72.9 -5.4 -606.1 170 251.497 0.007 68.3 -4.6 -704.71 183 251.504 0.007 63.3 -5 -839.84 196 251.51 0.006 58 -5.3 -977.31 212 251.514 0.004 53.5 -4.5 -1090.51 225 251.519 0.005 47.8 -5.7 -1234.77 243 251.523 0.004 42.6 -5.2 -1364.69 259 251.527 0.004 36.7 -5.9 -1472.06 278 251.531 0.004 30.7 -6 -1517.89 296 25

EQP1 1.533123 NaN 27.7 NaN -1552.6 NaN NaN1.535 0.004 25 -5.7 -1545.86 314 251.539 0.004 17.9 -7.1 -1427.73 336 251.543 0.004 12.7 -5.2 -1302.62 352 251.548 0.005 6.6 -6.1 -1135.67 369 251.552 0.004 1.3 -5.3 -1019.34 386 251.557 0.005 -2 -3.3 NaN 392 251.568 0.011 -10.7 -8.7 NaN 411 251.574 0.006 -14.9 -4.2 NaN 423 251.582 0.008 -19.3 -4.4 NaN 435 251.592 0.01 -24.2 -4.9 NaN 447 25


Method: 148 Chloride content in EtOH 12/18/2007 12:17:35 PMStart time: 12/18/2007 12:17:35 AM___________________________________________________________________________________________

Sample Data Comment / ID Sample size No. 1/5 Ethanol 38.672 g No. 2/5 Ethanol 38.4992 g No. 3/5 Ethanol 38.791 g No. 4/5 Ethanol 38.983 g No. 5/5 Ethanol 38.9095 g

Results No. Comment / ID Start time Rx Result Unit Name 1/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.45 mg/kg Content

2/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.48 mg/kg Content




SQC/Statistics


R1 Content 5 0.46 mg/kg 0.01 2.942

Additional results


R1 Content 3 4.61 mg/kg 0.06 1.253 R1 Content 5 12.15 mg/kg 0.04 0.291 R1 Content 5 23.60 mg/kg 0.08 0.318

DM140 electrode results


R1 Content 3 0.43 mg/kg 0.07 16.279 R1 Content 3 5.60 mg/kg 0.55 9.749

Titration curve

Results

56

Method 148 Chloride content in EtOH 18.12.2007 12:16:30Author schmid

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 None002 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 25.0°C Entry Arbitrary003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant HClO4 Concentration 0.1 mol/L Volume 1 mL Dosing rate 60.0 mL/min Condition No005 Stir Speed 40 % Duration 15 s Condition No006 Titration (EQP) [1]Titrant

Titrant AgNO3 Concentration 0.001 mol/LSensor

Type mV Sensor DM148-SC Unit mVTemperature acquisition


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 sEvaluation and Recognition

Procedure Standard Threshold 200.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria NoTermination



Condition No

Method007 Calculation R1 Result Content Result unit mg/kg Formula R1=(Q-B[Blank EtOH])*C/m Constant M*1000/z M M[Chloride] z z[Chloride] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No008 Record Summary No Results Per sample Raw results Per sample Table of meas. values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No

d2E/dV2 - V No BETA - 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 Method No Series data No Condition No009 Rinse


010 ConditioningType FixInterval 1Position Conditioning beakerTime 10 sSpeed 30%

Condition No 011 End of sample

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

Sodium chloride, NaClM=58.44 g/mol ; z = 1

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

Silver nitrate, AgNO3

c(AgNO3)= 0.01mol/L



1 additional dosing units2 DV1010 BurettesGlass titration beaker ME-101446XS205 Balance, LabX 2.6

METTLER TOLEDO

Neutralization before final disposal asheavy metal aqueous solutions.

Wastedisposal

Preparation and Procedures5 mL sodium chloride iodate standardsolution, NaClc(NaCl) = 0.001 mol/L

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DMi148-SCIndication

Titer Determination of 0.001 mol/L AgNO3

1) Beakers have to be cleaned very well.

2) Add 5 mL 0.001 mol/L NaCl standard solution.

3) 1 mL 0.1 mol/L HClO4 is added to the solution using anadditional dosing unit. If this is not available, perchloric acid isadded using a manual pipette.

4) Place the beaker on the Rondo sample rack and start thedetermination.

Remarks

R1=m/(VEQ*c*C)

C=1/(cst*z)

cst = concentration of standard solution

Calculation

Titration Excellence Line: Method for the titer determination of 0.001 mol/L AgNO3 by precipitation reactionwith sodium chloride as a primary standard.

Standard ---


Wastedisposal

58

Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN 116.3 NaN NaN 0 250.571 0.571 113.9 -2.4 NaN 6 250.857 0.286 112.4 -1.5 NaN 10 251 0.143 111.6 -0.8 NaN 13 251.2 0.2 110.4 -1.2 NaN 18 251.4 0.2 109.1 -1.3 -6.44 22 251.6 0.2 107.8 -1.3 -6.64 26 251.8 0.2 106.5 -1.3 -6.8 30 252 0.2 105.1 -1.4 -7.05 35 252.2 0.2 103.6 -1.5 -7.34 39 252.4 0.2 102.2 -1.4 -7.66 43 252.6 0.2 100.6 -1.6 -8.05 48 252.8 0.2 98.9 -1.7 -8.44 52 253 0.2 97.2 -1.7 -8.85 57 253.2 0.2 95.4 -1.8 -9.36 62 253.4 0.2 93.4 -2 -9.93 66 253.6 0.2 91.4 -2 -10.72 71 253.8 0.2 89.2 -2.2 -11.64 76 254 0.2 86.7 -2.5 -12.73 82 254.2 0.2 84 -2.7 -14 87 254.4 0.2 81 -3 -15.66 93 254.6 0.2 77.7 -3.3 -17.84 98 254.8 0.2 73.8 -3.9 -20.92 104 255 0.2 69.3 -4.5 -25.48 111 255.2 0.2 63.7 -5.6 -32.7 118 255.362 0.162 58.1 -5.6 -41.67 125 255.479 0.117 53.1 -5 -51.27 132 255.571 0.092 48.4 -4.7 -62.11 140 255.655 0.084 43 -5.4 -76.65 147 255.716 0.061 38.3 -4.7 -91.36 155 255.771 0.055 33.4 -4.9 -110.67 163 255.818 0.047 27.9 -5.5 -134.94 172 255.852 0.034 23.2 -4.7 -159.1 181 255.88 0.028 18.3 -4.9 -185.61 191 255.906 0.026 13.7 -4.6 -218.32 200 255.93 0.024 8.1 -5.6 -257.57 212 255.947 0.017 3.4 -4.7 -292.97 223 255.963 0.016 -1.4 -4.8 -334.94 234 255.978 0.015 -6.8 -5.4 -383.1 247 255.99 0.012 -11.6 -4.8 -420.6 259 256 0.01 -16.4 -4.8 -456.08 272 256.01 0.01 -21 -4.6 -478.18 285 25

EQP1 6.014073 NaN -23.1 NaN -479.1 NaN NaN6.021 0.011 -26.6 -5.6 -476.74 300 256.03 0.009 -30.8 -4.2 -454.01 312 256.042 0.012 -36 -5.2 -411.03 326 256.054 0.012 -41 -5 -369.07 340 256.066 0.012 -45.3 -4.3 -331.99 352 256.084 0.018 -50.6 -5.3 NaN 365 256.104 0.02 -55.5 -4.9 NaN 377 256.128 0.024 -60.7 -5.2 NaN 389 256.154 0.026 -65.3 -4.6 NaN 401 256.19 0.036 -70.5 -5.2 NaN 412 25


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

Results

No. Comment / ID Start time Rx Result Unit Name 1/3 NaCl 11.12.2007 14:27:51 R1= 0.986 -- Titer 2/3 NaCl 11.12.2007 14:37:29 R1= 0.993 -- Titer 3/3 NaCl 11.12.2007 14:47:01 R1= 0.993 -- Titer -/- R2= 0.991 -- Mean Titer Titer 0.991

SQC/Statistics


R1 Titer 3 0.991 -- 0.004 0.408 R2 Mean Titer 1 0.991 -- NaN NaN

Titration curve

Results

59

Method 148T Titer of AgNO3 11.12.2007Author schmid

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 SOP002 Sample (Titer) Titrant AgNO3

Concentration [mol/L] 0.001 Standard NaCl

Type of standard liquid Entry type Fixed weight Volume 5.0 mL Correction factor 1.0 Temperature 25.0°C003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant HClO4 Concentration 0.1 mol/L Volume 1.0 mL Dosing rate 60.0 mL/min Condition No005 Stir Speed 30 % Duration 10 s Condition No006 Titration (EQP) [1]Titrant

Titrant AgNO3 Concentration 0.001 mol/LSensor

Type mV Sensor DM148-SC Unit mVTemperature acquisition



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 sEvaluation and Recognition

Procedure Standard Threshold 200.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria NoTermination



Condition No

Method007 Calculation R1 Result Titer Result unit -- Formula R1=m/(VEQ*c*C) Constant 1/(cst*z) M M[Sodium chloride] z z[Sodium chloride] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No008 Rinse


009 Record Summary No Results Per sample Raw results Per sample Table of meas. values Last titration function Sample data No E - V Last titration function dE/dV - V No log dE/dV - V No

d2E/dV2 - V No BETA - 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 Method No Series data No Condition No Method No Series data No Condition No010 Conditioning

Type FixInterval 1Position Conditioning beakerTime 10 sSpeed 30%

Condition No011 End of sample012 Titer Titrant AgNO3 Concentration 0.001 mol/L TITER= Mean[R1] Limits No Condition No013 Calculation R2 Result Mean Titer Result unit -- Formula R2=Mean[R1] Constant 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No014 Record Summary Yes Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No

60

M373

Mercaptan sulfur, R-S-,M = 32.06 g/mol, z = 1

25 mL solvent ASTM D3227-04a2 mL Ethyl mercaptan standard solve.(see remarks)

Silver nitrate, AgNO3 , in 2-Propanolc(AgNO3) = 0.01 mol/L

Titration Excellence T70/T902 additional dosing unitsRondo 20 Sample Changer

R-SH + AgNO3 = R-S-Ag + HNO3

2 DV1010 and 1 DV1020 BurettesGlass titration beaker ME-101446XS205 BalanceOlivetti Printer JobJet 210

METTLER TOLEDO

Filtration. The precipitate has to beclassified as special waste. The liquidphase has to be disposed as organicwaste.

Wastedisposal

Preparation and Procedures25 mL, kerosineSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM405-SCIndication

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

1) Dissolved oxygen is removed by purging the solvent and thetitrant solutions with nitrogen gas for at least 10 min prior touse. The solutions must be kept protected from atmosphere.

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.

5) For accurate sampling, kerosene was added with a pipetteinstead of weighing (volatility). Thus, its density must be takeninto account. The density of flight petrol was measured using aMETTLER TOLEDO DR45 density meter (d = 0.7905 g/cm3 ,25°C)

6) The electrode was rinsed and conditioned using the ASTMD3227 solvent (Functions RINSE, CONDITIONING in specialbeaker 2, and CONDITIONING in conditioning beaker).

1) The method parameters have been optimised for the abovementioned sample. It may be necessary to slightly adapt themethod to your specific sample.

2) A fully automated procedure is performed by using twoadditional burette drives and a sample changer. It can be easilymodified for manual operation. Select "Manual stand" in themethod function "Titration stand".

3) ASTM D3227-04a alkaline solvent:Dissolve 1.6 g anhydrous sodium acetate (NaC2H3O2) in 25 mLof deion. water and pour into 1 L flask. Fill up to the mark with2-propanol. This solvent allows a good dissolution of the oil.

4) The 0.02 mol/L mercaptan standard is prepared bydissolving approx. 1.24 g ethyl mercaptan in a 1 L volumetricflask and filling up with the ASTM D3227 solvent.Literature:ASTM D3227-04a, see www.astm.orgMETTLER TOLEDO Appl. brochure 34, ME-51 725 066METTLER TOLEDO Appl. brochure 20, ME-51 725 020.

Remarks

R1: Mercaptan content (mg/kg)

R1 = (Q-B[ASTM D 3227])*C/(m*d),C = M*1000/z

B[ASTM D3227]: Blank value ofmercaptan standard solution

Calculation

Titration Excellence Line: The content of (thiol mercaptan) sulfur in kerosine is determined by precipitationtitration in non aqueous solvent using silver nitrate in 2-propanol. The content is expressed as sulfur, S2-.

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


Wastedisposal

61



Sample Data Note / ID Sample size No. 1/6 Kerosene 25 mL No. 2/6 Kerosene 25 mL No. 3/6 Kerosene 25 mL No. 4/6 Kerosene 25 mL No. 5/6 Kerosene 25 mL No. 6/6 Kerosene 25 mL

Results Note / ID Rx Result Unit No. 1/6 Kerosene R1= 14.794 mg/L No. 2/6 Kerosene R1= 14.768 mg/L No. 3/6 Kerosene R1= 14.696 mg/L No. 4/6 Kerosene R1= 14.676 mg/L No. 5/6 Kerosene R1= 14.616 mg/L No. 6/6 Kerosene R1= 14.623 mg/L

Statistics Rx Name n Mean Value Unit s srel[%] R1 Mercaptans 6 14.70 mg/L 0.07 0.50

Titration curve

Results

62

Method m373 Mercaptan sulfur ASTM D3227 27.08.2007Author METTLER TOLEDO

001 Title Type General titration Compatible with T70 / T90 ID m373 Title Mercaptan sulfur ASTM D3227 Author METTLER TOLEDO Date/Time 27.08.2007 Modified -- Modified by -- Protect No SOP None

002 Sample Number of IDs 1 ID 1 Kerosene Entry type Fixed volume Volume 25.0 mL Density 0.8 g/mL Correction factor 1.0 Temperature 25.0°C

003 Titration stand Type Rondo/Tower A Titration stand Rondo60/1A


Volume 25 mL

005 Dispense (normal) [1]Titrant Kerosene

Concentration 1 Volume 25 mL Dosing rate 60.0 mL/min



Titrant AgNO3 in 2-Propanol Concentration 0.01 mol/L

Sensor Type mV Sensor DM405-SC Unit mV


Stirrer Speed 30%


Control Control User Titrant addition Dynamic dE(set value) 4.0 dV(min) 0.005 mL dV(max) 0.05 mL Meas. val. acquisition Equilibrium controlled dE 1.0 mV dt 2 s t(min) 10 s t(max) 30 s


Method Termination At Vmax [mL] 3 At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No

008 Calculation R1 Result Content Result unit mg/kg Formula R1=(Q-B[ASTM D3227])*C/(m*d) Constant C=M*1000/z M M[Mercaptan sulfur] z z[Mercaptan sulfur] Decimal place 3 Result limits No Record statistics No Extra statistical functions No Condition No

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

010 Rinse Auxiliary reagent ASTM D3227 solvent Rinse cycles 1 Vol. per cycle [mL] 15 Position Actual position Drain No

011 Conditioning Type Fix Interval 1 Position Special beaker 2 Time [s] 30 Speed [%] 50

012 Conditioning Type Fix Interval 1 Position Conditioning Time [s] 30 Speed [%] 50

013 End of sample

63

M374-A

Alkaline components B,expressed as mg KOH/g sample

55 mL solvent mixtureToluene:isopropanol:distilled water(50% (v/v):49.5%(v/v):0.5%(v/v) )

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

Titration Excellence Line, T50/70/90Conductivity board ME-51109840Rondo 20 with PowerShower

Neutralization of all basic componentsin oil.General neutralization reactions:1) HCl + NaOH = NaCl + H2O

2) HCl + B = HB+ + Cl-

Glass titration beaker ME-1014462 x SP250 Peristaltic pumpsME-51108016Printer, XP205 balance

METTLER TOLEDO

Organic solvent waste(aromatic solvents)

Wastedisposal

Preparation and ProceduresFresh oils, 0.2-1 gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

InLab718 conductivity probeIndication

Base Number Determination in Fresh Oils by Conductometric Titration

1) Titrant preparation:If not commercially available, the titrant can be prepared byadding 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 aglass titration bealer. The higher the BN, the lower the samplesize.

3) 60 mL solvent are added automatically by a peristalticpump.

4) The titration is started after 60 s stirring time at 50% in orderto achieve a complete dissolution of the sample.

1) To ensure a complete rinsing of the probe, the followingcleaning procedure was defined (see method):1.1 Drain: The sample beaker is emptied1.2 Pump: 35 mL of solvent are dosed1.3 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 aftereach sample using the rinsing cycles defined in the methodfunction "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.

3) This application does not replace the standard.

Remarks

Base number (mg KOH/g)R1= (Q-B[IP400])*C1/mC1= 56.1

B[IP400]: solvent blank value

Calculation

Titration Excellence Line: Determination of the base number of freshmotor and cutting oils by titration with0.1 mol/L hydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe (IP400/94).

Standard TRIS (THAM), 50 mg

Hans-Joachim MuhrAuthor

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64


Method ID: IP400B Sample series ID 13 Date / Time: 09/20/2006 01:43:12 pm User name Administrator

Samples Nr. ID Sample size and results

1 13 0.2584 g R1(BN) 38.798 mg KOH/g R2(Titration time) 2.570 min 2 13 0.2535 g R1(BN) 38.309 mg KOH/g R2(Titration time) 2.470 min



Statistics R1(BN) Number of samples 6 Mean value 38.467 mg KOH/g s 0.196 mg KOH/g srel 0.511 %

TBN according to ASTM D4739: 40.4 mg KOH/g---------------------------------------------------------------------------------------------

Different samples of fresh oils

Sample Size / g n Base number s srel TBN ASTM D4739 mg KOH/g mg KOH/g % mg KOH/g

CF15 0.5 6 18.947 0.106 0.559 20.0

58420 1.0 6 10.886 0.034 0.316 10.8

Titration curve

Results

65

Method IP400B Conductometric BNVersion 09/20/2006 01:43:12 pm

001 Title Type General titration Compatible with T50/T70/T90 ID IP400B Titel Conductometric BN Author Administrator Date / Time 08/28/2006 03:09:17 pm Modified at 09/20/2006 01:43:12 pm Modified by Administrator Protect No SOP None

002 Sample Number of IDs 1 ID 1 13 Entry Type Weight Lower limit 0.0 g Upper limit 5.0 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0 °C Entry Before

003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No

004 PumpAuxiliary reagent IP400 Solvent

Volume 55 mL Condition No


006 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration 0.1 mol/L Sensor Type Conductivity Sensor InLab 718

Unit STemperature aquisition

Temperature measurement NoStir


Mode None Wait time 0 s Control Control User Titrant addition Incremental dV 0.1 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 4 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

Method007 Calculation R1 Result BN Result unit mg KOH/g Formula R1=(Q-B[IP400])*C/m Constant C= 56.1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Condition No

008 Calculation R2 Result Titration time Result Unit min Formula R2=t Constant C= -- M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Condition No

009 Record Summary Per sample Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Per sample Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No

d2E/dV2 - V Last titration function BETA - 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 - V No Method No Series data No Condition No

010 Drain Drain pump SP250 Drain volume 60 mL Condition No

011 Pump Auxiliary reagent IP400 Solvent Volume 35 mL Condition No


013 Drain Drain pump SP250 Drain volume 40 mL Condition No

014 Rinse Auxiliary reagent IP400 Solvent Rinse cycles 2 Vol. per cycle 10 mL Position Actual position Drain Yes Drain pump SP250 Condition No

015 End of sample

66

M374-B

Alkaline components B,expressed as mg KOH/g sample



Titration Excellence Line, T50/70/90Conductivity board ME-51109840Rondo 20 Sample Changer


2) HCl + B = HB+ + Cl-

Glass titration beaker ME-101446SP250 Peristaltic pump ME-51108016Printer, XP205 balance

METTLER TOLEDO


Wastedisposal

Preparation and ProceduresUsed oils, 2-5 gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


Base Number Determination in Used Oils by Conductometric Titration

1) Titrant preparation:If not commercially available, the titrant can be preparedmanually by adding 9 mL 37% v/v HCl and filling up to 1 Lwith 2-propanol (isopropanol).

2) 2-4 g oil are weighed into a glass titration bealer.


4) The titration is started after 300 s stirring time at 50% inorder to achieve a complete dissolution of the sample.

1) The conductivity probe is conditioned during 10 s in the fixedconditioning beaker of the Rondo 20 sample changer.

2) Most oil samples may create sticky residues. In this case, itis necessary to additionally clean the conductivity probe with apaper tissue soaked in solvent mixture. Afterwards, the probe isrinsed again with solvent mixture to remove the last impurities.

Literature:


2) METTLER TOLEDO Applications M252/M253, and M099/M100.


Remarks

Base number (mg KOH/g)R1= (Q-B[IP400])*C1/mC1= 56.1

B[IP400]: solvent blank value

Calculation

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

Standard TRIS (THAM), 50 mg

Tobias Beckmann, MT-DAuthor

Wastedisposal

67


Method ID: AIP400 Sample series ID -- Date / Time: 14/08/2007 12:00:28 User name Administrator

Summary

Samples Nr. ID Sample size and results

1 WC 433591 2.0134 g R1(BN) 6.373 mg KOH/g R2(Titration time) 5.070 min



Statistics R1(BN) Number of samples 3 Mean value 6.402 mg KOH/g s 0.033 mg KOH/g srel 0.515 %

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

Different samples of used oilsSample Size / g n Base number s srel mg KOH/g %

WC 529913 2.2 3 5.780 0.062 1.068

WC 526402 2.2 3 4.599 0.299 4.974

WC 471807 2.3 3 4.571 0.290 6.349

WC 457700 2.2 3 3.250 0.101 3.095

WC 541628 2.1 3 1.820 0.007 0.405

Titration curve

Results

68

Method AIP400 Conductometric BNVersion 14/08/2007 12:00:28

001 Title Type General titration Compatible with T50/T70/T90 ID AIP400 Titel Conductometric BN Author Administrator Date / Time 14/08/2007 09:19:49 Modified at 14/08/2007 12:00:28 Modified by Administrator Protect No SOP None

002 Sample Number of IDs 1 ID 1 WC 433591 Entry Type Weight Lower limit 0.0 g Upper limit 5.0 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0 °C Entry Before


004 PumpAuxiliary reagent IP400








dE 1.0 S dt 2 s t(min) 3 s t(max) 15 s Evaluation and Recognition Procedure Segmented

Threshold 10 S mL2

Ranges 0 Add. EQP criteria Steepest jump Steepest jumps 1 Termination At Vmax 10 mL


Method007 Conditioning Type Fix Interval 1 Positioning Conditioning beaker Time 10 s Speed 30 % Condition No

008 Calculation R1 Result BN Result unit mg KOH/g Formula R1=(Q-B[IP400])*C/m Constant C= 56.1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

009 Calculation R2 Result Titration time Result Unit min Formula R2=t Constant C= -- M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No

010 Record Summary Per series Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Per sample Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No

d2E/dV2 - V Last titration function BETA - 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 - V No Method No Series data No Condition 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

69

M375

TRIS, Tris-hydroxymethyl-aminomethaneM=121.14, z=1



Titration Excellence Line, T50/70/90Conductivity board ME-51109840Rondo 20 Sample Changer


2) HCl + B = HB+ + Cl-

Glass titration beaker ME-101446SP250 Peristaltic pump ME-51108016Printer, XP205 balance

METTLER TOLEDO


Wastedisposal

Preparation and ProceduresPrimary standard:TRIS (THAM), 50-80 mg

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


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

1) Titrant preparation:If not commercially available, the titrant can be preparedmanually by adding 9 mL 37% v/v HCl and filling up to 1 Lwith 2-propanol (isopropanol).

2) 50-80 mg TRIS are weighed into a glass titration bealer.


4) The titration is started after 120 s stirring in order to achievea complete dissolution of TRIS.

1) The conductivity probe is conditioned during 10 s in the fixedconditioning beaker of the Rondo 20 sample changer.

Literature:


2) METTLER TOLEDO Applications M099/M100, M253


Remarks

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

p: purity of solid primary standard [%]

Calculation

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.

Standard --

Tobias Beckmann, MT-DAuthor

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70


Method ID: AIP8014 Sample series ID -- Date / Time: 14/08/2007 10:01:04 User name Administrator

All resultsMethod ID AIP8014

Sample 1/3 TRIS R1 0.986 Sample 2/3 TRIS R1 0.993 Sample 3/3 TRIS R1 0.995

Statistics Method ID AIP8014 R1 (Titer) Number of samples 3 Mean value 0.991 s 0.005 srel 0.477

All results R2(mean Titer) 0.991

Titration curve

Results

71

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

001 Title Type General titration Compatible with T50/T70/T90 ID AIP8014 Titel Titer HCl in 2-Propanol Author Administrator Date / Time 14/08/2007 09:19:49 Modified at 14/08/2007 10:01:04 Modified by Administrator Protect No SOP None

002 Sample (Titer) Titrant HCl in 2-Propanol

Concentration 0.1 mol/L Standard TRIS Type of standard Solid Entry Type Weight Low limit 0.05 g Upper limit 0.08 g Correction factor 1.0 Temperature 25.0 °C Entry Arbitrary


004 PumpAuxiliary reagent IP400








dE 1.0 S dt 2 s t(min) 3 s t(max) 30 s Evaluation and Recognition Procedure Segmented

Threshold 10 S mL2

Ranges 0 Add. EQP criteria No Termination At Vmax 10.0 mL


Method007 Conditioning Type Fix Interval 1 Positioning Conditioning beaker Time 10 s Speed 30 % Condition No

008 Calculation R1 Result Titer Result unit -- Formula R1=m/(VEQ*c*C) Constant C= M/(10*p*z) M M[TRIS] z z[TRIS] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

009 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No

d2E/dV2 - V Last titration function ........... Method No Series data No Condition No

010 End of sample

011 Titer Titrant HCl in 2-Propanol Concentration 0.1 mol/L TITER= Mean[R1] Limits No Condition No

012 Calculation R2 Result Mean Titer Result Unit -- Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No

013 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No

72

M376

Anionics as Na-dodecylsulfate, C12H25NaO4SM(SDS)=288.38 g/mol, z=1

40 mL deion water20 mL MIBK:EtOH 1:1 solvent

Hyamine 1622, c(Hyamine)=0.004 MHydrochloric acid, HCl, c(HCl)=0.1 M

Titration Excellence Line T70/T902 additional dosing unitsRondolino Sample Changer

SDS- + Hyamine+ = SDS-Hyamine

Titration beaker ME-101974

METTLER TOLEDO

Neutralize the sample solution beforefinal disposal as organic solvent.

Wastedisposal

Preparation and Procedures5 mL aliquots of aqueous solutionsprepared with shower gels andshampoo.

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DS800 TwoPhase surfactant electrode,InLabRReference , DG111-SC

Indication

Anionic Content in Shower Gels by Potentiometric Two-Phase Titration

Note: MIBK is an organic solvent which is strongly andintensively 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 samplechanger.3) The pH value is first adjusted to pH 3 with HCl by means ofthe second titration burette (EN DIN 14480).4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensedby means of an additional dosing unit.MIBK: Methylisobutylketone (4-Methylpentan-2-one)EtOH: Ethanol5) To obtain a homogeneous emulsion the solution is stirred ata 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 theelectrolyte.2) Screw the electrode tip onto the shaft.3) Shake the electrode 2-3 times to avoid the presence of airbubbles into the electrode tip. Rinse it with deion. water.4) Condition the electrode first in deionised water for e.g. 15minutes, and then perform 1-2 test titrations with the sample.

1) The determination of anionic surfactants is performed at pH 3according to DIN EN 14480. This is perfomed to avoidinterference due to the presence of free fatty acids (FFA) in theproducts, otherwise the result will be higher. In fact, at pH 3 theFFA are fully protonated, therefore they can not be titrated withhyamine.

2) Standard solutions of the different products are prepared bydissolving in 1 L volumetric flask approx. 5-10 g of theproducts. The resulting concentration in g/L = mg/mL is storedas auxiliary value e.g. H[Anionic] in the titrator.

3) The electrode is cleaned and conditioned after each sample indeionised water in the conditioning beaker of Rondolino(Position 5: 120 s).

4) When working with the LabX Software, select "RondolinoMode" in the LabX window at the PC and activate it.

Literature:1) DIN EN 14480-20042) METTLER TOLEDO Application brochure 34,"Selected METTLER TOLEDO methods for Titration ExcellenceLine", ME-51 725 066.3) METTLER TOLEDO Application brochure 22,"Surfactant titration", ME-51 725 015.

Remarks

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

Calculation

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

Standard SDS (for Hyamine), THAM (for HCl)

C. De CaroAuthor

Wastedisposal

73


Method ID: 0214 Sample series ID -- Date / Time: 09/07/2007 07:50:32 User name Administrator

All resultsMethod ID 0214LAS

Sample 1/5 0214 R1 24.726 % Sample 2/5 0214 R1 24.677 % Sample 3/5 0214 R1 24.669 % Sample 4/5 0214 R1 24.622 % Sample 5/5 0214 R1 24.641 %

Statistics Method ID 0214LAS R1 (Content) Number of samples 5 Mean value 24.667 % s 0.040 % srel 0.161 %

----------------------------------------------------------------------------------------------Different samplesSample type exp./%SDS n Result s srel content /%SDS /%SDS /%

0214 viscous 24 5 24.667 0.040 0.161 pH 3 H[0214]=0.005056 g/L 8 24.494 0.033 0.136 pH 5.5

0273 viscous 25 8 25.290 0.034 0.136 pH 3 H[0273]=0.005019 g/L 7 25.291 0.031 0.123 pH 3

0411 powder 20 3 20.274 0.055 0.273 pH 3 H[0411]=0.010012 g/L 5 20.303 0.073 0.359 pH 3

0193 formulation 8-9 5 9.303 0.031 0.332 pH 3 H[0193]=0.010033 g/L 6 9.253 0.048 0.521 pH 3

0Liq liquid det. 5-15 6 7.317 0.060 0.817 pH 3 H[0Liq]=0.00805 g/L 9 7.365 0.080 1.092 pH 3

Titration curve

Results

74

Method 0214 SDS content potentiometricVersion 09/07/2007 07:50:32

001 Title Type General titration Compatible with T70/ T90 ID 0214 Titel SDS content potentiometric Author Administrator Date / Time 06/07/2007 17:56:59 Modified at 09/07/2007 07:50:32 Protect No SOP None

002 Sample Number of IDs 1

ID 1 0214 Entry Type Fixed volume Volume 5 mL Density 1.0 Correction factor 1.0 Temperature [°C] 25.0



005 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L Sensor Type pH Sensor DG111-SC Unit pHTemperature aquisition



Mode None Wait time [s] 0Control

End point type Absolute Tendency Negative End point value 3 pH Control band 2.0 pH Dosing rate (max) 10.0 mL/min

Dosing rate (min) 500 L/minTermination

At EP Yes Termination delay 0 s At Vmax 10.0 mL Max. time InfiniteAccompanying stating


Condition No

006 Dispense (normal) [1] Titrant MIBK-EtOH 1:1 Concentration 1 Volume 20 mL Dosing rate 60.0 mL/min Condition No


Method008 Titration (EQP) [2] Titrant

Titrant Hyamine 1622 Concentration [mol/L] 0.004 mol/L Sensor Type mV

Sensor DS800 Unit mV Temperature aquisition Temperature measurement No

Stir Speed 80 % Predispense

Mode Volume Volume 1.5 mL Wait time [s] 15 sControl

Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.01 mL dV(max) 0.4 mL Mode Equilibrium controlled dE 1.0 mV dt 1 s t(min) 5 s t(max) 30 sEvaluation and Recognition

Procedure Standard Threshold 100 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination

At Vmax [mL] 8 At potential No At slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating NoCondition

Condition No

009 Calculation R1 Result Content Result unit % Formula R1=Q[2]*C/(m*H[0214]) Constant C= M/(10*z) M M[Sodium dodecylsulfate] z z[Sodium dodecylsulfate] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Condition No

010 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Yes Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No

d2E/dV2 - V No .... Method No Series data No Condition No

011 End of sample

012 Record Summary Yes Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No

75

M377

Anionics as Na-dodecylsulfate, C12H25NaO4SM(SDS)=288.38 g/mol, z=1


Hyamine 1622, c(Hyamine)=0.004 MHydrochloric acid, HCl, c(HCl)=1 MSodium hydroxide, c(NaOH)=1 M



Titration beaker ME-101974

METTLER TOLEDO

Neutralize the sample solution beforefinal disposal as organic solvent.

Wastedisposal

Preparation and Procedures0.1-0.3 g cutting oil, depending onanionic surfactant content.

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


Indication

Anionic Content in Cutting Oils by Potentiometric Two-Phase Titration


1) 40 mL of deionised water are added to the 5 mL sample.2) The titration beaker is placed on the Rondolino samplechanger.3) The pH value is adjusted to pH 3 (DIN EN 14480) with HClor to pH 11 with NaOH by means of the second titration burette.4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensedby means of an additional dosing unit.MIBK: Methylisobutylketone (4-Methylpentan-2-one)EtOH: Ethanol5) To obtain a homogeneous emulsion the solution is stirred ata 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.


1) The determination of anionic surfactants is performed at pH 3according to DIN EN 14480. This is done in order to avoidinterference due to the presence of free fatty acids (FFA) in theproducts, otherwise the result will be higher. In fact, at pH 3 theFFA are fully protonated, therefore they can not be titrated withhyamine.

2) In the case where samples contain anionic surfactants withR-COOH end groups, it is necessary to titrate the sample at analkaline pH value of e.g. pH 11 (see also DIN EN 14669) to beable to precipitate them with Hyamine.



Literature:1) DIN EN 14480-2004 and 14669-20052) METTLER TOLEDO Application brochure 34,"Selected METTLER TOLEDO methods for Titration ExcellenceLine", ME-51 725 066.3) METTLER TOLEDO Application brochure 22,"Surfactant titration", ME-51 725 015.

Remarks

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

Calculation

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

Standard SDS (for Hyamine)

C. De CaroAuthor

Wastedisposal

76


Method ID: m377 Sample series ID -- Date / Time: 11/12/2007 09:02:23 am User name AdministratorSummary Samples No. ID Sample size and results

1 00883-03 0.1773 g R1(Anionics Content) 4.91 %





6 00883-03 0.1624 g R1(Anionics 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 2.73 0.02 0.559 pH 3 5 2.66 0.02 0.734 pH 3

02800-01 6 2.01 0.01 0.733 pH 3

C93 18656 6 61.07 0.47 0.764 pH 3 6 61.14 0.31 0.506 pH 3 6 61.48 0.48 0.783 pH 3

V43 18571 6 30.93 0.05 0.155 pH 3 6 30.96 0.08 0.256 pH 3 6 30.92 0.04 0.141 pH 3

11675-01 4 13.57 0.17 1.228 pH 11 0.004 M Hyamine 6 13.61 0.20 1.486 pH 11 0.01 M CPC01125-02 4 4.49 0.05 1.155 pH 11 0.004 M Hyamine 6 4.55 0.01 0.231 pH 11 0.01 M CPC

Titration curve

Results

77

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

001 Title Type General titration Compatible with T70/ T90 ID m377 Titel SDS content potentiometric Author Administrator Date / Time 11/12/2007 07:22:42 am Modified at 11/12/2007 09:02:23 am Protect No SOP None

002 Sample Number of IDs 1

ID 1 00883-03 Entry Type Weight Lower limit 0 g Upper limit 5 g Density 1.0 g/mL Correction factor 1.0 Temperature [°C] 25.0°C Entry Before



005 Titration (EP) [1] Titrant Titrant HCl Concentration 1 mol/L Sensor Type pH Sensor DG111-SC Unit pHTemperature aquisition








Condition No

006 Dispense (normal) [1] Titrant MIBK-EtOH 1:1 Concentration 1 Volume 20 mL Dosing rate 60.0 mL/min Condition No


Method008 Titration (EQP) [2] Titrant




Mode None Wait time [s] 0 sControl



At Vmax [mL] 20 mL At potential No At slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating NoCondition

Condition No

009 Calculation R1 Result Anionics Content Result unit % Formula R1=Q[2]*C/m Constant C= M/(10*z) M M[Sodium dodecylsulfate] z z[Sodium dodecylsulfate] Decimal places 2 Result limits No Record statistics Yes Extra statistical functions No Condition No

010 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Yes Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No

d2E/dV2 - V No .... Method No Series data No Condition No

011 End of sample

012 Record Summary Yes Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No

78

M378

Sodium dodecylsulfate, C12H25NaO4SM(SDS)=288.38 g/mol, z=1


Hyamine 1622, c(Hyamine)=0.004 MHydrochloric acid, HCl, c(HCl)=0.1 M



Rondolino Sample ChangerTitration beaker ME-101974

METTLER TOLEDO

Organic solventWastedisposal

Preparation and Procedures5 mL 0.004 SDSSDS: Sodium dodecylsulfate

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories


Indication

Titer Determination of Hyamine by Potentiometric Two-Phase Titration


1) 40 mL of deionised water are added to the 5 mL sample.2) The titration beaker is placed on the Rondolino samplechanger.3) The pH value is first adjusted to pH 3 with HCl by means ofthe second titration burette (EN DIN 14480).4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensedby means of an additional dosing unit.MIBK: Methylisobutylketone (4-Methylpentan-2-one)EtOH: Ethanol5) To obtain a homogeneous emulsion the solution is stirred ata high speed (80%).


Rondolino:



Literature:

1) DIN EN 14480-2004

2) METTLER TOLEDO Application brochure 34,"Selected METTLER TOLEDO methods for Titration Excellenceline", ME-51 725 066.

3) METTLER TOLEDO Application brochure 22,"Surfactant titration", ME-51 725 015.

Remarks

Titer:R=m/(VEQ[2]*c[2]*C)C=1/(cst*z)

Note: "cst" is the concentration of theSDS standard solution.

Calculation

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 electrodeaccording to DIN EN 14480-2004.

Standard For HCl: THAM (TRIS)

C. De CaroAuthor

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79


Method ID: 414Titer Sample series ID -- Date / Time: 06/07/2007 17:15:16 User name Administrator

Summary

Samples No. ID Sample size and results

1 SDSTiter414 5 mL R1 (Titer) = 1.002013 2 SDSTiter414 5 mL R1 (Titer) = 1.001679 3 SDSTiter414 5 mL R1 (Titer) = 1.000487 4 SDSTiter414 5 mL R1 (Titer) = 0.997958 5 SDSTiter414 5 mL R1 (Titer) = 0.998080 6 SDSTiter414 5 mL R1 (Titer) = 0.998976

Statistics R1 (Titer) Number of samples 6 Mean value 0.999866 s 0.001784 srel 0.178%

Titer Titrant Hyamine 1622 New titer 0.99987

Results R2 (Hyamine) 0.999866

Titration curve

Results

80

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

001 Title Type General titration Compatible with T70/ T90 ID 414Titer Titel Titer Hyamine 1622 Author Administrator Date / Time 28/08/2006 14:53:19 Modified at 06/07/2007 17:15:16 Protect No SOP None002 Sample (Titer) Titrant Hyamine 1622

Concentration 0.004 mol/L Standard SDSTiter414 Type of standard liquid Entry Type Fixed volume Volume 5 mL Correction factor 1.0 Temperature [°C] 25.0003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1004 Stir Speed 30 % Duration 45 s Condition No005 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L Sensor Type pH Sensor DG111-SC Unit pHTemperature aquisition








Condition No006 Dispense (normal) [1] Titrant MIBK-EtOH 1:1 Concentration 1 Volume 20 mL Dosing rate 60.0 mL/min Condition No007 Stir Speed 80 % Duration 60 s Condition No008 Titration (EQP) [2] Titrant




Mode Volume Volume 1.5 mL Wait time [s] 15 s

MethodControl



At Vmax [mL] 10 At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating NoCondition

Condition No009 Calculation R1 Result Titer Result unit Formula R=m/(VEQ[2]*c[2]*C) Constant C= 1/(cst*z) M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Condition No010 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V No ... Calibration curve No Method No Series data No Condition No011 End of sample012 Titer Titrant Hyamine 1622 Concentration 0.004 mol/L TITER= Mean[R] Limits No Condition No013 Calculation R2 Result Titer Hyamine Result Unit Formula R2=Mean[R1] Constant C= M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Condition No014 Record Summary Yes Results No Raw results No Resource data No Calibration curve No Method No Series data No Condition No

81

M379

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

Chloride (Cl-)

H2SO4 (10%)

NaOH, 1.0 mol/L (sodium hydroxide)AgNO3, 0.02 mol/L (silver nitrate)

Titration Excellence T70/T902 additional dosing units

EP titration:C4H6O6 + 2NaOH = Na2C4H4O6 +2H2OEQP titration:Cl- + Ag+ + NO3

- = AgCl + NO3-

LabX Pro Titration ME-51106500Rondo30 sample changer (51108004)with sample beakers (51108030)

METTLER TOLEDO

AgCl has to be disposed of as specialwaste.

Wastedisposal

Preparation and ProceduresWine, 40 mLSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DGi102-Mini (pH sensor)DMi102-SC (silver electrode)

Indication

Acid and Chloride Content in Wine

Before the acid content analysis is performed the pH electrodeneeds to be adjusted by use of the METTLER TOLEDO buffers4.01, 7.00 and 9.21 and method M436.

When working with Rondo30 and two mini electrodes lowersample volumes can be used for two consecutive titrations in thesame sample.

In this method conditioning in the conditioning beaker is used forelectrode cleaning, alternatively, rinsing with the Rondo30 powershower can be used.

When automation with Rondo30 is not required, microtitrationbeakers can also be used when wanting to use smaller samplevolumes.

Remarks

R1: Consumption NaOH (mL)R2: Measurement pH value (pH)R3: Chloride content (mg/L)

Calculation

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

Standard NaCl for AgNO3, KHP for NaOH


Wastedisposal

82



Method m379 Acid and Chloride Content in WineMeasured 11.10.2007

RESULTSNo. ID Sample size and results1 Wine 40.0 ml

R1 = 3.0744 ml ContentR2 = 1.660 pH pH valueR3 = 33.6713 mg/L Chloride content

2 Wine 40.0 mlR1 = 3.0925 ml ContentR2 = 1.662 pH pH valueR3 = 33.7785 mg/L Chloride content





STATISTICSNumber results R1 n = 6Mean value x = 3.0871 ml ConsumptionStandard deviation s = 0.0141 ConsumptionRelative standard deviation srel = 0.4570 %

Number results R2 n = 6Mean value x = 1.667 pH pH valueStandard deviation s = 0.005 pH valueRelative standard deviation srel = 0.277 %

Number results R3 n = 6Mean value x = 33.7607 mg/L Chloride contentStandard deviation s = 0.0495 Chloride contentRelative standard deviation srel = 0.1470 %

Titration curve

Results

83

Method: m379 Acid and Chloride Content in Wine 10.10.2007User: Nijman

001 Title Type General titration Compatible with T70/ T90 ID MxxxMN2 Titel Acid and Chloride Content in Wine Author Mettler Toledo Date / Time 10.10.2007 Modified at 10.10.2007 Protect No SOP None LabX SOP002 Sample Number of IDs 1

ID 1 Wine Entry Type Fixed volume Volume [mL] 40.0 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0003 Titration stand Type Rondo60/Tower A Titration stand Rondo60/1A Lid handling No004 Stir Speed [%] 30 Duration [s] 10 Condition No005 Titration (EP) [1]

Titrant Titrant NaOH Concentration [mol/L] 1.0 Sensor Type pH Sensor DG102-Mini Unit pH Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Mode Absolute Tendency None End point value 7.0 Control band 0.2 Dosing rate (max) [mL/min] 20 Dosing rate (min) [mL/min] 300 Termination At EP Yes Termination delay [s] 0 At Vmax [mL] 5 Max. time[s] 20000

Accompanying stating Accompanying stating No Condition Condition No006 Dispense (normal) [1] Titrant H2SO4 10% Concentration [mol/L] 1 Volume [mL] 2.0 Dosing rate [mL/min] 60.0 Condition No007 Measure (normal) [1] Sensor Type pH Sensor DG102-Mini Unit pH Temperature acquisition Temperature measurement No Stir Speed [%] 30 Aquisition of measured values Aquisition Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 10 t(max) [s] 30 Mean value No Condition Condition No008 Titration (EQP) [2]

Titrant Titrant AgNO3 Concentration [mol/L] 0.02 Sensor Type mV Sensor DM102-SC Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30

Method Predispense Mode Volume Volume [mL] 0.2 Wait time [s] 5 Control Control User Titrant addition Dynamic dE (set value) 6 dV (min) 0.02 dV (max) 0.2 Mode Equilibrium controlled dE 1.0 dt [s] 2 t(min) [s] 10 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold 150 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 6.0 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 No009 Calculation R1 Result Consumption Result Unit mL Formula R1=VEQ[1] Constant C= 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 No010 Calculation R2 Result pH value Result Unit pH Formula R2=E Constant C= 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No011 Calculation R3 Result Chloride content Result Unit mg/L Formula R3=Q[2]*C/m Constant C= M*1000/z M M[Chloride] z z[Chloride] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Conditioning Type Fix Interval 1 Position Conditioning beaker Time [s] 20 Speed [%] 35 Condition No013 Record Summary No Results Per sample Raw results Per sample Table of measured values No Sample data No Resource data No E - V All titration functions dE/dV - V All titration functions ...... Condition No014 End of sample

84

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.

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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

LineT70 Terminal, Rondo 20 with

PowerShower™ and LabX titration

Plug

& Play ElectrodesReliable

and secure

handling

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