METTLER methods for the DL15, DL22 F&B and DL28bikeitech.com/DATAS/es_free3/f_49780c1f5e3bf.pdf ·...

METTLER TOLEDO Titrators

METTLER methodsfor the DL15, DL22 F&B and DL28

Application brochure 33

Editorial

Dear Reader This application brochure represents another step in the tradition of METTLER TOLEDO’s comprehensive titration documentation on practical, every-day examples, and will surely support your analytical work with our new titrators DL15, D22 F&B and DL28. The DL15 titrator is mainly used to determine the acid and base content of a sample. The DL15 is the ideal solution for all requirements in the food and beverage industry, water/wastewater analysis, and the chemical industry when all that is needed is an endpoint titration or a pH measurement. The DL22 Food & Beverage Analyzer has been developed specially for the requirements of the food and beverage industry. It includes predefined methods for the applications most commonly used in these industries. When selecting the control parameters for the titration, you need only to select one of the three settings. No further modifications are necessary. “Fast”, “Normal” and “Cautious”: the choice is up to you! The DL28 Titrator is an easy-to-use, compact endpoint and equivalence point titrator for the food and beverage industry, water/wastewater analysis and the chemical industry. The most relevant methods from these areas have been included to make analyses as simple as possible to perform. Accuracy, precision, speed, GLP compliant documentation, and ease-of-use: these are some of the points we have improved in these new titrators to help you increase productivity. These titrators feature intuitive user guidance so that, for instance, simply pressing the Run button twice starts the method you last ran. Analytical methods have been developed, extensively tested and run on real samples by the applications chemists of the Market Support Group Analytical Chemistry. As a result, the optimized parameters of the titration methods were stored in the titrator as METTLER methods. These represent a great help for the user since they can be immediately run without additional method development work. They also represent a very good base to start with when a new method has to be created. Detailed methods, clear procedures, step-by-step guidance, and literature references: it is with great pleasure that we present you this collection of titration methods. We wish you much success titrating with the METTLER TOLEDO DL15, DL22 F&B and DL28.

Beat Flachsmann Cosimo A. De Caro Product Manager Titration Senior Applications Chemist

Contents Method Title Page

M388 Determination of acid content 1

M389 Determination of base content 4

M390 pH determination: General method 7

M330 Tartaric acid in wine 10

M331 Citric acid in orange juice 13

M332 Determination of malic acid in apple juice 16

M333 Acetic acid content in vinegar 19

M334 Acid number determination in milk 22

M335 Chloride content determination 25

M336 Free sulphur dioxide determination in wines 28

M337 Vitamin C: Voltametric determination 31

M338 Nitrogen determination according to Kjeldahl 34

M339 Determination of calcium and magnesium 37

M340 Reducing sugars determination in beverages according to Rebelein 40

M341 Back value determination for reducing sugars according to Rebelein 43

M342 Standardization value for reducing sugars det. according to Rebelein 46

M343 Iodine number in edible oils and fats according to Wijs 49

M344 Back value of Wijs solution 52

M345 Acid number of edible oils 55

M346 Peroxide number in edible oils and fats 58

M347 Total hardness of water 61

M348a p-value of water 64

M348b m-value of water 67

M349 Potassium content determination by direct measurement 70

M380 TAN Acid number determination according to ASTM D664 73

M381 TAN Blank determination according to ASTM D664 76

M382 TBN Base number determination according to ASTM D4739 79

M383 TBN Blank determination according to ASTM D4739 82

M384 TBN Base number determination according to ASTM D2896 85

M385 Copper content determination in aqueous solutions 88

M386 Nickel content determination in aqueous solutions 91

M387 Potassium content determination by direct measurement 94

M388

Hydrochloric acid, HClM(HCl)=36.46, z=1

50 mL deionized water

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

DL15, DL22 F&B, DL28OKI B4250 Printer(parallel cable ME-51108780)

HCl + NaOH = NaCl + H2O

Titration beakers ME-101974

METTLER TOLEDO

--Wastedisposal

Preparation and Procedures5 mL 0.1 M hydrochloric acidSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Determination of acid content

1) 5 mL 0.1 mol/L hydrochloric acid are added to 50 mLdeionized water.

2) DG115-SC pH glass electrode:The electrode is adjusted using pH buffers 4.01, 7.00, and9.21.

3) The sample is titrated with sodium hydroxide to pH 7.0.

General method for the determination of acid content(alkalimetry).

Remarks

R1: Content (g/L)Calculation

General method for the acid content determination by endpoint titration to pH 7.0 with sodium hydroxide(alkalimetry).

Standard Potassium hydrogen phthalate, 80 mg

Albert AichertAuthor

1

Table of measured values

-------------------------------------------------------------------Method ID 920 Title Acid content EP25-04-2005 17:15 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 HCl 1 Cont. 0.36306 [%]

2 HCl 1 Cont. 0.36291 [%]

3 HCl 1 Cont. 0.36289 [%]

4 HCl 1 Cont. 0.36290 [%]

5 HCl 1 Cont. 0.36298 [%]

6 HCl 1 Cont. 0.36288 [%]

Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 0.36294 0.00007 [%] 0.019

ResultsActive sample Deleted samples-------------------------------------------------------------------123456

Titration curve

Results

2

Method ID 920 Title Acid content EP25-04-2005 17:15 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . . HCl Entry type . . . . . . . . . . . . . . Volume Minimum [mL] . . . . . . . . . . . . . 0.1 Maximum [mL] . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 36.458 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 3.0 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 14 dVmin [mL] . . . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Termination param. Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 7.00Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . % Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 5 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes

MethodOther Control parameters

Set of parameters . . . . . . . Fast Addition . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 18 dVmin [mL] . . . . . . . . . . . 0.004 dVmax [mL] . . . . . . . . . . . 0.75 Measure mode . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . 20

Set of parameters . . . . . . . Cautious Addition . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . 0.25 Measure mode . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . 30

3

M389

Sodium hydroxide, NaOHM(NaOH)= 40.00, z=1


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




METTLER TOLEDO

--Wastedisposal

Preparation and Procedures5 mL 0.1 M sodium hydroxideSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Determination of base content

1) 5 mL 0.1 mol/L sodium hydroxide are added to 50 mLdeionized water.


3) The sample is titrated with hydrochloric acid to pH 7.0.

General method for the determination of base content(acidimetry).

Remarks

R1: Content (%)Calculation

General method for the base content determination by endpoint titration to pH 7.0 with hydrochloric acid(acidimetry).

Standard THAM, approx. 50 mg


4


-------------------------------------------------------------------Method ID 921 Title Base content EP26-04-2005 08:55 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 NaOH 1 Cont. 0.40286 [%]

2 NaOH 1 Cont. 0.40342 [%]

3 NaOH 1 Cont. 0.40362 [%]

4 NaOH 1 Cont. 0.40360 [%]

5 NaOH 1 Cont. 0.40321 [%]



Titration curve

Results

5

Method ID 921 Title Base content EP26-04-2005 08:55 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . . NaOH Entry type . . . . . . . . . . . . . . Volume Minimum [mL] . . . . . . . . . . . . . 0.1 Maximum [mL] . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 36.458 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 3.0 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 14 dVmin [mL] . . . . . . . . . . . . . 0.010 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Termination param. Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 7.00Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . % Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 5 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




6

M390

--

--

--


--


METTLER TOLEDO

--Wastedisposal

Preparation and ProceduresVarious aqueous solutions, 50 mLSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

pH determination: General method

1) 50 mL sample solution are added into the beaker.


3) The electrode is thoroughly cleaned after each sample withdeionized water.

General method for the determination of pH value in differentaqueous sample solutions.

Remarks

R1: pH

pH = -log(H+)

H+ : activity of hydrogen ions

Calculation

General method for the determination of pH values in different aqueous solutions.

Standard --

MSG AnaChemAuthor

7


-------------------------------------------------------------------Method ID 926 Title pH measure00-00-0000 00:00 Author-------------------------------------------------------------------Sensor DG115 Unit pH-------------------------------------------------------------------Sample 6Sample ID WineEntry type MassMass [g] 60Minimum [g] 0.01Maximum [g] 10Density [g/mL] 1.0Mol.m. [g/mol] 1.00Equival. number z 1Mixing time [s] 10Duration [min:s] 0:03Temp. [°C] 25.0

Result Calculat. Value Unit-------------------------------------------------------------------1 Meas. val. 3.602 [pH]

Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 3.603 0.001 [pH] 0.018

Other samples

Milk:Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 8 6.754 0.003 [pH] 0.043

pH 9.21 buffer solution:Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 10 9.226 0.001 [pH] 0.006

Titration curve

Results

8

Method ID 926 Title pH measure00-00-0000 00:00 Author

Sample para. Sample ID . . . . . . . . . . . . . . . Request Entry type . . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . . 0.01 Maximum [g] . . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 1.00 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10Measure Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH dE [mV] . . . . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . . 30Calculation 1 Calculation . . . . . . . . . . . . . . Meas. val. Unit . . . . . . . . . . . . . . . . . pH Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP

Method

9

M330

Tartaric acid, (CHOH)2(COOH)2 ;M=150.09 g/mol; z= 2

--

Sodium hydroxide, NaOHc(NaOH) = 1.0 mol/L;

DL22 F&B, DL28OKI B4250 Printer(parallel cable ME-51108780)

H2C4H4O6 + 2NaOH = Na2C4H4O6 +2H2O


METTLER TOLEDO

No special treatment is necessary.Wastedisposal

Preparation and Procedures50 mL wine from grapesSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Tartaric acid in wine

The samples should be degassed in an ultrasonic bath for fiveminutes to get rid of CO2.

Before the analysis a three point calibration of the electrode wasperformed using METTLER TOLEDO buffers of pH 4.01, 7.00and 9.21.

The principle acids found in grapes are tartaric and malic acids.Their proportions vary depending on the variety of grapes,however in the wine tartaric dominates.

Unripe grapes are sour due to the high concentration of tartaricacid. When the grapes ripen, much of this acid is converted tosugar. Then during the fermentation process the yeasts thenconvert these sugars into ethanol and carbon dioxide.

In the determination of total acidity in wine all the acid isassumed to be tartaric, so that the result is expressed as gramstartaric acid per liter of wine.

Total acidity of the wine affects taste, color, as well as resistanceto microbial spoilage.

Remarks

Tartaric acid is chosen to express theacid content in g/L in wine because it isthe predominantly present acid.

Calculation

General method for the determination of acidity of wines


M. BiberAuthor

10


-------------------------------------------------------------------Method ID 930 Title Tartaric acid08-04-2005 11:17 Author M. Biber-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 dry wine 1 Cont. 5.327 [g/L]

2 dry wine 1 Cont. 5.395 [g/L]



Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 4 5.385 0.011 [g/L] 0.209


Titration curve

Results

11

Method ID 930 Title Tartaric acid08-04-2005 11:17 Author M. Biber

Sample para. Sample ID . . . . . . . . . . . . . . . dry wine Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 50.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 150.09 Equival. number z . . . . . . . . . . . 2 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . NaOH 1.0 Conc.[mol/L] . . . . . . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 2.0 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.020 dVmax [mL] . . . . . . . . . . . . . 0.2 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Termination param. Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 7.00Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . g/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




12

M331

Citric acid, M=192.13 g/mol; z=3HOOC-CH2-COH(COOH)-CH2-COOH




H3C6H5O7 + 3NaOH =Na3C6H5O7 + 3H2O


METTLER TOLEDO

No special treatment is necessary.Wastedisposal

Preparation and Procedures5 mL orange juiceSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Citric acid in orange juice

1) 5 mL orange juice are added to 50 mL deionized water.

2) The samples should be degassed in an ultrasonic bath forfive minutes to get rid of CO2.


4) The sample is titrated with sodium hydroxide to pH 8.1 .

The principle acid found in orange juice is citric acid. In thedetermination of total acidity all the acid is assumed to be citric,so that the result is expressed as grams citric acid per liter ofjuice.

Literature

1) Titration Applications Brochure 19,"Determination in Beverages"Memory Card Application PackageME-51725013 (see applications M561-M562).

2) Endpoint titration to pH 8.1:Schweizerisches Lebensmittelbuch (Swiss Food Handbook),5th Edition, Volume 3, Chap. 28A (1994).

Remarks

R1 = Content (g/L)Calculation

Method for the determination of citric acid in orange juice by endpoint titration to pH 8.1



13


-------------------------------------------------------------------Method ID 931 Title Citric acid26-04-2005 15:25 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Orange jui 1 Cont. 7.281 [g/L]

2 Orange jui 1 Cont. 7.219 [g/L]






Titration curve

Results

14

Method ID 930 Title Citric acid26-04-2005 15:25 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . . Orange juice Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 5.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 192.13 Equival. number z . . . . . . . . . . . 3 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 3.0 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.020 dVmax [mL] . . . . . . . . . . . . . 0.2 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Termination param. Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 7.00Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . g/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




15

M332

Malic acid, HOOC-CH2-CH(OH)-COOHM = 134.09 g/mol, z=2




C4H6O5 + 2 NaOH =

C4H4O52- + 2 H2O + 2 Na+


METTLER TOLEDO

Neutralization before final disposal.Wastedisposal

Preparation and Procedures5 mL apple juiceSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Determination of malic acid in apple juice

1) 5 mL apple juice are added to 50 mL deionized water.

2) DG115-SC pH glass electrode:The electrode is adjusted using pH buffers 4.01, 7.00, an 9.21.

3) The sample is titrated with sodium hydroxide to pH 8.1 .

Literature:

1) Titration Applications Brochure 19,"Determination in Beverages"Memory Card Application PackageME-51725013 (see applications M561-M562).

2) Endpoint titration to pH 8.1:Schweizerisches Lebensmittelbuch (Swiss Food Handbook),5th Edition, Volume 3, Chap. 28A (1994).

Remarks

R1: Content (g/L)Calculation

The malic acid content in apple juice is determined by an endpoint titration to pH 8.2 with sodiumhydroxide.



16


-------------------------------------------------------------------Method ID 932 Title Malic acid24-04-2005 20:06 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 PrId Fix 1 Cont. 3.478 [g/L]

2 PrId Fix 1 Cont. 3.531 [g/L]







Titration curve

Results

17

Method ID 932 Title Malic acid24-04-2005 20:06 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . . PrID Fix Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 5 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 134.09 Equival. number z . . . . . . . . . . . 2 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 3 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 12 dVmin [mL] . . . . . . . . . . . . . 0.010 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Termination param. Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 8.10Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . g/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Set of parameters . . . . . . . Fast Addition . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 16 dVmin [mL] . . . . . . . . . . . 0.02 dVmax [mL] . . . . . . . . . . . 0.7 Measure mode . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . 20


18

M333

Acetic acid, CH3COOH,M = 60.05 g/mol, z = 1




CH3COOH + NaOH =CH3COONa + H2O

Titration beaker ME-101974

METTLER TOLEDO


Preparation and ProceduresVinegar, ca. 1 g.Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Acetic acid content in vinegar

1) Approximately 1 g vinegar is added to 50 mL deionizedwater.


3) The sample is titrated with sodium hydroxide using an EQPtitration method.

4) The content is expressed as % w/w.

Remarks


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


A. AichertAuthor

19


-------------------------------------------------------------------Method ID 933 Title Acetic acid24-04-2005 17:53 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Vinegar 1 Cont. 4.944 [%]

2 Vinegar 1 Cont. 4.929 [%]

3 Vinegar 1 Cont. 4.955 [%]



Titration curve

Results

20

Method ID 933 Title Acetic acid24-04-2005 17:53 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . Vinegar Entry type . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . 1.0 Maximum [g] . . . . . . . . . . . . . 10 Density [g/mL] . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . 60.05 Equival. number z . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . 10EQP titration Titrant . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . 1.000 Back value [mmol] . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . Normal Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 14.0 dVmin [mL] . . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . Positive Min Relevance . . . . . . . . . . 30.0 Threshold [pH/mL]. . . . . . . . . 5.0 St. jump only . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . 20.0 Evaluation Numb. Potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . % Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . Yes




21

M334

Lactic acid, CH3-CHOH-COOH;M(C3H6O3)=90.0 g/mol; z=1



HC3H5O3 + NaOH = NaC3H5O3 + H2O


METTLER TOLEDO

Neutralize the slightly alkaline wastebefore disposal.

Wastedisposal

Preparation and Procedures50 mL Whole milkSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Acid number determination in milk

Do not dilute the sample, otherwise less tri-calcium phosphatewill precipitate and the resulting acid number will be too low.

Before the analysis a three point calibration of the electrode wasperformed using METTLER TOLEDO buffers of pH 4.01, 7.00and 9.21.

The titratable acidity in milk is expressed as percent lactic acid.Bacteria growing in milk produce mainly lactic and acetic acids,however, bacterial count must increase millionfold before it isreflected in the acidity.

The acidity of fresh milk results from OH- uptake of phosphates,citrates, casein, whey proteins, and carbon dioxide, as well asfrom the fermentation by-products of lactic acid bacteria.

Titratable acidity is determined by titrating pH 8.30. Thisendpoint was chosen because it corresponds to the colorchange of the phenolphthalein indicator historically used. Thetitrant consumption in this determination, multiplied by 20,yields the acid number.

Rancid or sour milk will have an acid number which is too high.Udder health also influences acidity, with mastitis yielding lowacid numbers.

References:1) Schweizerisches Lebensmittelbuch, Band I, Chap. 1, Sect.2.32) Dairy Connection, Inc.: dairyconnection.com3) Dairy Research and Information Center, Department of FoodScience & Technology, University of California, Davis, seehttp://www.ucdavis.edu/academics/academic_depts.html

Remarks

The Swiss Food Handbook defines the acidnumber of milk as 20*a, where a = titrantconsumption (mL).

Calculation

Acid number is determined in milk by an endpoint titration to pH 8.3

Standard Potassium hydrogen phthalate

M. BiberAuthor

22


-------------------------------------------------------------------Method ID 934 Title Acid number in milk09-03-2005 09:09 Author M. Biber-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 whole milk 1 Cont. 151.859

2 whole milk 1 Cont. 150.093




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 150.596 0.714 0.474


Titration curve

Results

23

Method ID 934 Title Acid number milk09-03-2005 09:09 Author M. Biber

Sample para. Sample ID . . . . . . . . . . . . . . . milk Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 50.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 90.0 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 3EP titration Titrant . . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 0.00 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.020 dVmax [mL] . . . . . . . . . . . . . 0.2 Measure mode . . . . . . . . . . . . EQU ontrolled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Termination param. Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 8.30Calculation 1 Calculation . . . . . . . . . . . . . . Acid number Formula . . . . . . . . . . . . . . . . R=VEQ C . . . . . . . . . . . . . . . . . . . 1.0 Factor . . . . . . . . . . . . . . . . 20.0 Name . . . . . . . . . . . . . . . . . Acid number Unit . . . . . . . . . . . . . . . . . none Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




24

M335

Sodium chloride, NaCl,M = 58.44 g/mol, z = 1

50 mL H2SO4 (0.02 mol/L)

Silver nitrate c(AgNO3) = 0.1 mol/L;


NaCl + AgNO3 = AgCl + NaNO3

Titration beaker ME-101974,

METTLER TOLEDO

Filtration. The precipitate (AgCl) has tobe classified as special waste.The liquid has to be neutralized to pH 7before final disposal.

Wastedisposal

Preparation and ProceduresKetchup, 0.5 - 2 gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM141-SCIndication

Chloride content determination

50 mL diluted sulfuric acid (0.02 mol/L) are added to eachketchup sample prior to starting the titration.

After each sample, the electrode is conditioned in deionizedwater to completely remove any residue.Before starting the next sample, electrode and stirrer weredabbed dry with a soft tissue.

The total chloride content is calculated as sodium chloride(NaCl).

Sodium chloride is used as standard. Since small amounts ofsalt cannot be weighed in exactly it is better to prepare asolution of NaCl, and then add the standard with a pipette. Theexact concentration of the standard solution is entered in mol/Lin 'Setup', 'Standard'.

The choice of the Control Parameters (Fast, Normal, Cautious)does not have a significant influence on the accuracy of theresults. However, the different 'Addition' settings will greatlyinfluence the amount of titrant added after the EQP(overtitration), while the different 'Measure' settings influence theduration (the values given below are the mean of 6determinations):Fast : 0.44 mL excess, 89 s titration timeNormal : 0.22 mL excess, 100 s titration timeCautious: 0.08 mL excess, 180 s titration time

All results shown were obtained with the control parameter set<Normal>.

Remarks


The method represents a general purpose salt titration with parameters set to ensure a high degree ofaccuracy and precision.

Standard NaCl solution (approx. 0.0025 mM)

P. BurriAuthor

25


-------------------------------------------------------------------Method ID 935 Title Chloride content05-04-2005 10:39 Author P. Burri-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Ketchup 1 Cont. 3.155 [%]

2 Ketchup 1 Cont. 3.154 [%]





Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 3.152 0.003 [mg/L] 0.087


Titration curve

Results

26

Method ID 935 Title Chloride content05-04-2005 10:39 Author P. Burri

Sample para. Sample ID . . . . . . . . . . . . . . Ketchup Entry type . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . 0.5 Maximum [g] . . . . . . . . . . . . . 2 Density [g/mL] . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . 58.44 Equival. number z . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . 3EQP titration Titrant . . . . . . . . . . . . . . . AgNO3 0.1 Conc.[mol/L] . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM141 Unit . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . 1.000 Back value [mmol] . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . Normal Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 9 dVmin [mL] . . . . . . . . . . . . 0.008 dVmax [mL] . . . . . . . . . . . . 0.4 Measure mode . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . Positive Min Relevance . . . . . . . . . . 30 Threshold [mV/mL]. . . . . . . . . 250 St. jump only . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . 20.0 Evaluation Numb. Potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . % Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . Yes




27

M336

Sulphur dioxide (SO2)M = 64.06 g/mol; z = 2

5 mL KI (10%)5 mL H2SO4 (25%)

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


SO2 + I2 + 2 H2O = H2SO4 + 2 HI


METTLER TOLEDO


Preparation and ProceduresVarious wines, 50mLSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM143-SCIndication

Free sulphur dioxide in wines

1) In order to avoid loss of SO2, the samples must be takenfrom a freshly opened bottle. After opening the bottle, free SO2

can evaporate with CO2 or be oxidized while in contact with airresulting in too low results.

2) It is known that iodine is also reduced by other componentsin the wine. These competing reactions can partly be delayed bythe addition of 5 mL KI (10%)

3) The potassium iodide solution is prepared by dissolving 10gpotassium iodide in 100 mL deioized water and has to be keptin the dark.

4) The reaction only takes place in acidic medium. Therefore 5mL H2SO4 (25%) must be added immediately before titration.

Sulphur dioxide is added to wine as an antioxidant, anti-fermantation agent and to prevent microbiological degradation. Atoo high content causes an unpleasant odor in wine and has anadverse toxic effect on the person drinking it.

The upper limit is regulated by law, while the antioxidant andantiseptic activity resulting in a fresh taste is only achievedabove a certain value.

The free sulphur dioxide content in wine is determined by aniodometric titration. Iodine oxidizes SO2 according to the Bunsenequation.

Remarks

R1: Consumption (mL)R2: Content (mg/L)

Calculation

Iodometric method for determination of free sulphur dioxide in wines.

Standard Ascorbic acid (C6H8O6)

Lukas CandreiaAuthor

28


-------------------------------------------------------------------Method ID 936 Title Free SO210-08-2005 16:55 Author Lukas Candreia-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Red Wine 1 Consump. 2.358 [mL] 2 Cont. 30.50 [mg/L]

2 Red Wine 1 Consump. 2.339 [mL] 2 Cont. 30.26 [mg/L]




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 2.394 0.022 [mL] 0.9222 5 30.98 0.29 [mg/L] 0.922


Titration curve

Results

29

Method ID 936 Title Free SO210-08-2005 16:55 Author Lukas Candreia

Sample parameters Sample ID . . . . . . . . . . . . . . . Red Wine Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 50 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 64.062 Equival. number z . . . . . . . . . . . 2 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 30 Mixing time [s] . . . . . . . . . . . . 30EP titration Titrant . . . . . . . . . . . . . . . . 1/2 I2 0.02 Conc.[mol/L] . . . . . . . . . . . . 0.02 Sensor . . . . . . . . . . . . . . . . DM143 Unit . . . . . . . . . . . . . . . . mV

Pol. Curr. [ A]. . . . . . . . . . . 1.0 Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.0 Predis.[mL] . . . . . . . . . . . . . . 0.5 Back v. [mmol]. . . . . . . . . . . . . 0.0 Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 12 dVmin [mL] . . . . . . . . . . . . . 0.005 dVmax [mL] . . . . . . . . . . . . . 0.1 Measure. . . . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 2.0 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 1 t(max) [s] . . . . . . . . . . . . . 10 Recognition Tendency . . . . . . . . . . . . . . Negative Termination param. Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [mV] . . . . . . . . . . 100.0Calculation 1 Calculation . . . . . . . . . . . . . . Consump. Type . . . . . . . . . . . . . . . . . Consump. Unit . . . . . . . . . . . . . . . . . mL Which EP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mg/L Which EP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 2 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Set of parameters . . . . . . . . Fast Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 12 dVmin [mL] . . . . . . . . . . . . 0.005 dVmax [mL] . . . . . . . . . . . . 0.1 Measure . . . . . . . . . . . . . Fixed time Time incr. [s] . . . . . . . . . . 1

Set of parameters . . . . . . . . Cautious Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . 0.005 dVmax [mL] . . . . . . . . . . . . 0.05 Measure . . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . . 10

30

M337

L(+)-Ascorbic acid,M = 176.13g/mol, z = 2

50 mL deionized waterOxalic acid 2%NaOH 0.1 mol/L

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


C6H8O6 + DPI = C6H6O6 + H2-DPIAscorbic acid is oxidized by DPI:C6H8O6 = C6H6O6 + 2H+ + 2 e-

Red titration beakers ME-25777

METTLER TOLEDO

No special treatment is necessaryWastedisposal

Preparation and ProceduresFruit juice, ca. 0.5 - 10gSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM143Indication

Vitamin C: Voltametric determination

Ascorbic acid is sensitive to light, temperature and oxygen. Thesample should therefore not be exposed to these influences.Titration beakers with light protection as well as use of purgegas are recommended.

0.36 g (1.25 mmol) 2,6-Dichlorophenolindophenol (DPI)sodium salt monohydrate (M = 290.08 g/mol) is weighed in a250 mL volumetric flask, which is filled up with deionised waterto obtain a titrant concentration of 0.01 mol/L 1/2 DPI.If 2,6-Dichlorophenolindophenol sodium salt dihydrate is used,an excess has to be weighed in due to its bad solubility and thetitrant has to be filtrated prior to use.The DPI titrant has to be prepared fresh daily. It has to be storedin brown glass bottles to protect it from light.

The sample size depends on the amount of vitamin C present inthe sample. 1-15 mg vitamin C lead to a consumption of 0.5 -8.5 mL DPI. The juice samples were weighed directly into thetitration beaker, without special treatment such as filtration. Evena relatively high pulp content does not disturb the titration. Afteraddition of 50mL deionised water the sample can be purgedwith nitrogen to avoit oxidation of Vitamin C.

This method describes the oxidimetric titration of ascorbic acidwith 2,6-Dichlorophenolindophenol (DPI) as titrant. Theendpoint is indicated voltametrically: A constant polarisationcurrent of 1.0 μA is applied to a double pin platinum electrode(DM143). Potential readings allow the indication of theequivalence point thanks to a potential jump at the EQP.

Prior to analysis the pH of the sample solution has to beadjusted to 3.0 by either oxalic acid (2%) for samples with ahigher initial pH-value or with NaOH 0.1 mol/L for samples withan initial pH lower than 3.0 using an EP titration (Mettler method919).

A fresh 0.01 mol/L standard solution of ascorbic acid is used fortiter determination and kept in the dark.

1) Titration Applications Brochure 19,"Determinations in Beverages", ME-51725013.

Remarks

R1: Content (mg/100g)R2: Content (mmol/L)R3: Consumption (mL)

Calculation

The Vitamin C (ascorbic acid) content is determined by titration with 2,6-Dichlorophenolindophenol (DPI)and voltametric detection.

Standard L(+)-Ascorbic acid solution 0.01 mol/L


31


-------------------------------------------------------------------Method ID 937 Title Vitamin C07-04-2005 09:22 Author Lukas Candreia-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Orange juice 1 Vitamin C 49.860 [mg/100g] 2 Cont. 2.831 [mmol/L] 3 Consump. 3.616 [mL]

2 Orange juice 1 Vitamin C 49.869 [mg/100g] 2 Cont. 2.831 [mmol/L] 3 Consump. 3.626 [mL]

3 Orange juice 1 Vitamin C 49.989 [mg/100g] 2 Cont. 2.838 [mmol/L] 3 Consump. 3.619 [mL]

Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 3 49.906 0.072 [mg/100g] 0.1442 3 2.833 0.004 [mmol/L] 0.1443 3 3.620 0.005 [mL] 0.137


Titration curve

Results

32

Method ID 937 Title Vitamin C07-04-2005 09:22 Author Lukas Candreia

Sample parameters Sample ID . . . . . . . . . . . . . . . Fruit juice Entry type . . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . . 0.1 Maximum [g] . . . . . . . . . . . . . . 10 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 176.13 Equival. number z . . . . . . . . . . . 2 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 30 Mixing time [s] . . . . . . . . . . . . 3EQP titration Titrant . . . . . . . . . . . . . . . . 1/2 DPI 0.01 Conc.[mol/L] . . . . . . . . . . . . 0.01 Sensor . . . . . . . . . . . . . . . . DM143 Unit . . . . . . . . . . . . . . . . mV Pol. Curr. [µA]. . . . . . . . . . . 1.0 Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.0 Predis.[mL] . . . . . . . . . . . . . . 1.0 Back v. [mmol]. . . . . . . . . . . . . 0.0 Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Incremental Increment. . . . . . . . . . . . . . 0.05 Measure. . . . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 2 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min Relevance. . . . . . . . . . . . 30 Threshold [mV/mL]. . . . . . . . . . 600.0 St. jump only. . . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . . 1 Vmax [mL]. . . . . . . . . . . . . . 20.0 Evaluation Number Potentials. . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . User def. Name. . . . . . . . . . . . . . . . . . Vitamin C Formula . . . . . . . . . . . . . . . . R=Q*C/m C . . . . . . . . . . . . . . . . . . . 1.0 Factor. . . . . . . . . . . . . . . . . 8806.5 Unit . . . . . . . . . . . . . . . . . mg/100g Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mmol/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . Consumpt. Unit . . . . . . . . . . . . . . . . . mL Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Set of parameters . . . . . . . Fast Addition . . . . . . . . . . . . Incremental Increment. . . . . . . . . . . . 0.1 Measure. . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 2 dt[s] . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . 10

Set of parameters . . . . . . . Cautious Addition . . . . . . . . . . . . Incremental Increment. . . . . . . . . . . . 0.03 Measure. . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . 30

33

M338

Nitrogen, N, M = 14.01 g/mol, z=1

50 mL deionized water2% boric acid solution (collectingsolution for distilled ammonia).

Sulphuric acid, 1/2 H2SO4

c(1/2 H2SO4) = 0.1 mol/L


2 NH4[B(OH)4] + H2SO4 =(NH4)2SO4 + 2 H[B(OH)4]


METTLER TOLEDO


Preparation and Procedures5 mL ammonium borate solution, NH4

(B(OH)4)approx. 0.1 mol/L

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

Nitrogen determination according to Kjeldahl

1) The ammonium borate solution was prepared by addingpowdered boric acid into ammonium hydroxide solution toreach a concentration of approx. 0.1 mol/L in a 1 L volumetricflask.

2) 50 mL deionized water are added to the sample.


4) The sample is titrated with sulphuric acid to pH 4.6 .

5) If necessary, a blank titration has to be performed.

Literature:

1) Titration Applications Brochure 13,"Nitrogen determination by Kjeldahl Digestion"ME-51724769 (see applications M120-M122).

2) Endpoint titration to pH 4.6: seeSchweizerisches Lebensmittelbuch, 5th Edition, Volume 2.

3) See also:http://pb.merck.de/servlet/PB/menu/1045480/index.html

Remarks

R1: Content (mg/L)R2: Content (mmol/L)R3: Consumption (mL)

Calculation

The nitrogen content is determined according to Kjeldahl: The sample is first digested in sulphuric acidgiving ammonium sulfate which is distilled after addition of sodium hydroxide. Ammonia is released andcollected in a 2% boric acid solution. This solution is titrated to pH 4.6 with sulphuric acid.

Standard THAM, approx. 50 mg

C. De CaroAuthor

34


-------------------------------------------------------------------Method ID 938 Title Nitrogen Kjeldahl23-03-2005 15:48 Author C. De Caro-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Ammonium 1 Cont. 1342.146 [mg/L] 2 Cont. 95.799 [mmol/L] 3 Consump. 5.4537 [mL]

2 Ammonium 1 Cont. 1344.030 [mg/L] 2 Cont. 95.934 [mmol/L] 3 Consump. 5.4613 [mL]





Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 1342.396 1.844 [mg/L] 0.1372 6 95.817 0.128 [mmol/L] 0.1343 6 5.4547 0.0072 [mL] 0.132


Titration curve

Results

35

Method ID 938 Title Nitrogen Kjeldahl23-03-2005 15:48 Author C. De Caro

Sample para. Sample ID . . . . . . . . . . . . . . . Ammonium Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 5 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 14.01 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 15EP titration Titrant . . . . . . . . . . . . . . . . 1/2 H2SO4 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 1 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Termination param. Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 4.60Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mg/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mmol/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . Consumpt. Unit . . . . . . . . . . . . . . . . . mL Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




36

M339

Ca2+ M = 40.08 g/molMg2+ M = 24.31 g/mol

2 - 5 mL buffer solution pH 8.5:Acetylacetone (AcAc) 0.3 mol/L,tris(hydroxymethyl)-aminomethane(THAM) 0.2 mol/L

EDTA 0.1 mol/L


Ca2+ + EDTA = Ca-EDTAMg-AcAc + EDTA = Mg-EDTA + AcAc


METTLER TOLEDO

No special treatment is necessaryWastedisposal

Preparation and ProceduresWaterSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DX240 Ca-ISE, DX200 Ref. electrodeIndication

Determination of calcium and magnesium

Depending on the Ca and Mg concentration the sample has tobe diluted with deionised water. Before titration 2 - 5 mL buffersolution is added with a pipette.

24 g (0.20 mol) tris(hydroxymethyl)-aminomethane (TRIS) isdissolved in deionised water, 30 g (0.30 mol) Acetylacetone(AcAc) is added and the volume adjusted to 1000 mL in avolumetric flask. To improve the shape of the titration curve theAcAc mass can be adjusted.

1 - 8 mL Calcium carbonate standard solution 0.2 mol/L isused.

In alkaline buffered solutions Calcium and Magnesium ions canbe titrated sequentially with a solution of a complexing agent likeEDTA. To improve the difference between the two complexbuilding constants an auxiliary complexing agent likeAcetylacetone (AcAc) is added that only forms a relatively weakcomplex with Magnesium, but not with Calcium.

The concentration of the auxiliary complexing agent influencesthe shape of the curve strongly. A high concentration of AcAcamplifies the calcium jump while the magnesium jump isdiminished. A small AcAc concentration results in the oppositeeffect. The AcAc and buffer concentrations given in thisapplication might be the subject of changes to optmize the curveshape of other samples.

Remarks

R1: Ca Cont. (mg/L)R2: Mg Cont. (mg/L)

Calculation

Method for the determination of Calcium and Magnesium using a Calcium selective electrode

Standard Calcium carbonate


37


-------------------------------------------------------------------Method ID 939 Title Ca & Mg Ca ISE23-07-2005 15:41 Author Lukas Candreia-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Water 1 Cont. 69.869 [mg/L] 2 Mg Cont. 10.380 [mg/L]

2 Water 1 Cont. 70.118 [mg/L] 2 Mg Cont. 10.433 [mg/L]

3 Water 1 Cont. 70.204 [mg/L] 2 Mg Cont. 10.463 [mg/L]

Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 3 70.064 0.174 [mg/L] 0.2482 3 10.425 0.042 [mg/L] 0.400


Titration curve

Results

38

Method ID 939 Title Ca & Mg Ca ISE23-07-2005 15:41 Author Lukas Candreia

Sample parameters Sample ID . . . . . . . . . . . . . . . Water Entry type . . . . . . . . . . . . . . Volume Minimum [mL] . . . . . . . . . . . . . 0.001 Maximum [mL] . . . . . . . . . . . . . 50 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 40.08 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 3EQP titration Titrant . . . . . . . . . . . . . . . . EDTA 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DX240 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.0 Predis.[mL] . . . . . . . . . . . . . . 1.0 Back v. [mmol]. . . . . . . . . . . . . 0.0 Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 2 dVmin [mL] . . . . . . . . . . . . . 0.006 dVmax [mL] . . . . . . . . . . . . . 0.3 Measure. . . . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 20 Recognition Tendency . . . . . . . . . . . . . . Negative Min Relevance. . . . . . . . . . . . 1 Threshold [mV/mL]. . . . . . . . . . 30.0 St. jump only. . . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . . 2 Vmax [mL]. . . . . . . . . . . . . . 20 Evaluation Number Potentials. . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mg/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . User def. Name. . . . . . . . . . . . . . . . . . Mg Cont. Formula . . . . . . . . . . . . . . . . R=Q*C/m C . . . . . . . . . . . . . . . . . . . 24.31 Factor. . . . . . . . . . . . . . . . . 1000.0 Unit . . . . . . . . . . . . . . . . . mg/L Which EQP . . . . . . . . . . . . . . . 2 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Set of parameters . . . . . . . . Fast Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 6 dVmin [mL] . . . . . . . . . . . . 0.01 dVmax [mL] . . . . . . . . . . . . 0.3 Measure. . . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . 10

Set of parameters . . . . . . . . Cautious Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 1 dVmin [mL] . . . . . . . . . . . . 0.006 dVmax [mL] . . . . . . . . . . . . 0.3 Measure. . . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . 3 t(min) [s] . . . . . . . . . . . . 4 t(max) [s] . . . . . . . . . . . . 30

39

M340

Reducing sugars as glucose, C6H12O6

M = 180.16 g/mol, z=1

40 mL deionized waterFehling solution A, 5 mLFehling solution B, 5 mL10 mL 10% H2SO4, 10 mL 10% KI

Sodium thiosulphate, Na2S2O3

c(Na2S2O3) = 0.1 mol/L


I2 + 2 S2O32- = 2I- + S4O6

2-

Glass beakers ME-101446

METTLER TOLEDO

Precipitate copper by adding sodiumhydroxide. The filtrate has to beclassified as special waste.

Wastedisposal

Preparation and ProceduresWines and juices, variable samplesizes

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Reducing sugars determination in beverages according to Rebelein

1) 5 mL each of Fehling A and B solutions are added to thesample together with 40 mL deionised water.

2) The sample size depends on the sugar content of the sample.10 mL Fehling solutions A and B can reduce max. 43 mgglucose, thus the sample should contain 10-30 mg reducingsugars. Sample with a sugar content larger than 20 g/L have tobe diluted with water.

3) The mixture is boiled for and then cooledto room temperature.

4) 10 mL 10% H2SO4 and 10 mL 10% KI are added. Thesamples are then titrated with 0.1 mol/L Na2S2O3.

5) The calculation is expressed as g glucose/L. For thecalculation, the back value Ba (M341) and the standardizationvalue (M342) of sodium thiosulphate to 1 g glucose areneeded.

Method:1) Reducing sugars are oxidised with excess alkaline coppersulphate solution (Fehling solution), where copper(II) is reducedto copper(I):Red. sugars + 2 Cu2+ --> Cu(I), Cu(II)

2) Unreacted, excess copper(II) is then reduced to copper (I)after addition of potassium iodide, KI, and iodine is formed:Cu(II) + KI = I2 + CuI

3) Iodine is subsequently titrated with sodium thiosulphate:I2 + 2 S2O3

2- = 2I- + S4O62-

The thiosulphate consumption corresponds to the total excess ofcopper(II) added to the sample and, thus, it allows thecalculation of the sugar content by back titration.

Literature:1) Titration Applications Brochure 19,Memory Card Application Package for DL53/DL55/DL58"Determinations in Beverages"ME-51725013 (see applications M566-M568).

Remarks

The result is expressed as g glucose/L.R1=(Ba-Q)*C/mBa = Back value (tot. amount Cu(II) )C = 1000/STANDSTAND = Standardisation value inmmol Na2S2O3/g glucose (see M342)

Calculation

Reducing sugars are determined in beverages by titration of released iodine with sodium thiosulfate.See also applications M341 and M342.

Standard Glucose solution, 10.0 g/L

Craig GordonAuthor

40


-------------------------------------------------------------------Method ID 940 Title Reducing sugars00-00-0000 00:00 Author-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Rosé Wine 1 Content. 2.3755 [g/L]

2 Rosé Wine 1 Content. 2.3696 [g/L]

3 Rosé Wine 1 Content. 2.3316 [g/L]



Other results:

White wineStatistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 3 1.5895 0.0168 [g/L] 1.056

Red wineStatistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 3 2.5158 0.0559 [g/L] 2.221

Titration curve

Results

41

Method ID 940 Title Reducing sugars00-00-0000 00:00

Sample para. Sample ID . . . . . . . . . . . . . . . Request Entry type . . . . . . . . . . . . . . Volume Minimum [mL] . . . . . . . . . . . . . 2 Maximum [mL] . . . . . . . . . . . . . 20 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 180 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 40 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . Na2S2O3 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 1.000 Back value [mmol] . . . . . . . . . . . Request Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.02 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . . . 30 Threshold [mV/mL] . . . . . . . . . 100.0 St. jump only . . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Number potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . User def. Name . . . . . . . . . . . . . . . . . Content Formula . . . . . . . . . . . . . . . . R=(Ba-Q)*C/m C . . . . . . . . . . . . . . . . . . . 33.227 Factor . . . . . . . . . . . . . . . . 1.0 Unit . . . . . . . . . . . . . . . . . mg/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mmol/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . Consumpt. Unit . . . . . . . . . . . . . . . . . mL Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . No E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




42

M341

--





I2 + 2 S2O32- = 2I- + S4O6

2-


METTLER TOLEDO


Wastedisposal

Preparation and ProceduresFehling solutions a and BSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Back value for reducing sugars determination according to Rebelein

1) 5 mL each of Fehling A and B solutions are added to 40 mLdeionised water.



4) The calculation is expressed as mmol and gives the exactamount of copper(II) in Fehling solution. This value is then usedas back value Ba in the determination of reducing sugars(M340) as well as in the standaardization (M342).

Method (Back or Fehling value):

1) Copper(II) is reduced to copper (I) after addition of potassiumiodide, KI, and iodine is formed:Cu(II) + KI = I2 + CuI


2- = 2I- + S4O62-

The thiosulphate consumption corresponds to the total amountof copper(II) added to the sample.


Remarks

The result is expressed as mmolR1 = Q(Total amount Cu(II) in 10 mL Fehlingsolution)

Calculation



Craig GordonAuthor

43


-------------------------------------------------------------------Method ID 941 Title Fehling value00-00-0000 00:00 Author-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Back value 1 Consump. 1.3746 [mmol]

2 Back value 1 Consump. 1.3685 [mmol]

3 Back value 1 Consump. 1.3762 [mmol]

Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 3 1.3731 0.0041 [mmol] 0.296


Titration curve

Results

44

Method ID 941 Title Fehling value00-00-0000 00:00

Sample para. Sample ID . . . . . . . . . . . . . . . Back value Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 10 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 180 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 40 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . Na2S2O3 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 10.000 Back value [mmol] . . . . . . . . . . . Request Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.02 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . . . 30 Threshold [mV/mL] . . . . . . . . . 100.0 St. jump only . . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Number potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Consump. Unit . . . . . . . . . . . . . . . . . mmol Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . No E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




45

M342

Reducing sugars as glucose, C6H12O6

M = 180.16 g/mol, z=1





I2 + 2 S2O32- = 2I- + S4O6

2-


METTLER TOLEDO


Wastedisposal

Preparation and Procedures2 mL Glucose solution, 10 g/L(= 20 mg glucose/sample)

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Standardisation value for reducing sugars det. according to Rebelein

1) 5 mL each of Fehling A and B solutions are added to thesample together with 40 mL deionised water.

2) The sample size depends on the sugar content of the sample.10 mL Fehling solutions A and B can reduce max. 43 mgglucose, thus the sample should contain 10-30 mg reducingsugars. Sample with a sugar content larger than 20 g/L have tobe diluted with water.



4) The result is expressed as mmol Na2S2O3 / g glucose. Thisvalue is used in the calculation for the reducing sugardetermination (M340).

Method:1) Reducing sugars are oxidised with excess alkaline coppersulphate solution (Fehling solution), where copper(II) is reducedto copper(I):Red. sugars + 2 Cu2+ --> Cu(I), Cu(II)

2) Unreacted, excess copper(II) is then reduced to copper (I)after addition of potassium iodide, KI, and iodine is formed:Cu(II) + KI = I2 + CuI


2- = 2I- + S4O62-

The thiosulphate consumption corresponds to the total excess ofcopper(II) added to the sample and, thus, it allows thecalculation of the sugar content by back titration


Remarks

The result is expressed as mmol/gR1= Content

Calculation



Craig GordonAuthor

46


-------------------------------------------------------------------Method ID 942 Title Glucose standard00-00-0000 00:00 Author-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Glucose St 1 Cont. back 30.5688 [mmol/g] d

2 Glucose St 1 Cont. back 29.9899 [mmol/g] d

3 Glucose St 1 Cont. back 29.7293 [mmol/g] d

Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 3 30.0960 0.4297 [mmol/g] 1.428


Titration curve

Results

47

Method ID 942 Title Glucose standard00-00-0000 00:00

Sample para. Sample ID . . . . . . . . . . . . . . . Glucose Std Entry type . . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . . 0.015 Maximum [g] . . . . . . . . . . . . . . 0.025 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 180 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 40 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . Na2S2O3 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 1.0 Back value [mmol] . . . . . . . . . . . Request Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.02 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . . . 30 Threshold [mV/mL] . . . . . . . . . 70.0 St. jump only . . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . . 20.0 Evaluation Number potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. back titr. Unit . . . . . . . . . . . . . . . . . mmol/g Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . No E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




48

M343

Unsaturated compounds (doublebonds)

Wijs solution, 10mLPure acetic acid, 20 mLPotassium iodine 20%, 10 mL

Sodium thiosulfate, Na2S2O3



ICl3 + I2 = 3IClICl + KI = I2 + KCl2Na2S2O3 + I2 = 2NaI + Na2(S4O6)


METTLER TOLEDO

Halogenated organic solventsWastedisposal

Preparation and ProceduresOils, fatsSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Iodine number in edible oils and fats according to Wijs

1) Dissolve the sample in 20 mL pure acetic acid.

2) Add 10 mL Wijs solution and stir for 5 minutes.

3) Add 10 mL 20% potassium iodine.

4) Titrate inmediately with 0.1 mol/L sodium thiosulfate.

Note:To completely dissolve fat, margarine or butter, add 10 mL ofcyclohexane to the samples.

Back titration

the determination of the iodine value is done by back titration.Therefore the capacity of the Wijs solution, ICl3 solution in aceticacid, has to be determinated first. This is done with the method944 Back Iodine value. The mean value of 3 capacitydetermination is used in this method.

According to the Schweizerisches Lebensmittelbuch and mostinternational standards an incubation of one hour isrecommended after the Wijs solution is added to the sample.If the expected iodine value is higher than 150 g I2/100gsample, an incubation of two hours even is required.For this application the standard was modified. Instead ofincubating the samples, acetic acid is added. Afterwards thesample is stirred for five minutes, which guarantees that thedouble bonds react with the iodine monochloride.

Remarks

Back value determination (Meth. 944):R1 = Q

Iodine value det. (Method 943):R1 = (Ba-Q)*C/mC1 = 126.96Factor = 0.1

Calculation

General method for the determination of iodine value in oils and fats

Standard Potassium iodate

MJ SchmidAuthor

49


-------------------------------------------------------------------Method ID 943 Title Iodine value Wijs11-04-2005 13:17 Author Maria

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Peanut oil 1 Iodine no. 96.914 [g/L]

2 Peanut oil 1 Iodine no. 97.031 [g/L]




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 97.042 0.12 [g/100g] 0.123


Titration curve

Results

50

Method ID 943 Title Iodine value Wijs11-04-2005 13:17 Author Maria

Sample para. Sample ID . . . . . . . . . . . . . . Request Entry type . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . 0.05 Maximum [g] . . . . . . . . . . . . . 4.00 Density [g/mL] . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . 253.80 Equival. number z . . . . . . . . . . 2 Temp.sensor . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . RequestEQP titration Titrant . . . . . . . . . . . . . . . Na2S2O3 0.1 Conc.[mol/L] . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . Request Back value [mmol] . . . . . . . . . . Request Control parameters Set of parameters . . . . . . . . Normal Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 4 dVmin [mL] . . . . . . . . . . . . 0.04 dVmax [mL] . . . . . . . . . . . . 0.4 Measure mode . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100.0 Termination param. Vmax [mL] . . . . . . . . . . . . 15.0 Numb. EQPs . . . . . . . . . . . 1 Evaluation Numb. potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . User def. Name . . . . . . . . . . . . . . . . Iodine value Formula . . . . . . . . . . . . . . . R=(Ba-Q)*C/m C . . . . . . . . . . . . . . . . . . 126.96 Factor . . . . . . . . . . . . . . . 0.1 Unit . . . . . . . . . . . . . . . . gI2/100g Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . Yes




51

M344

0.1 mol/L ICl3 solution in acetic acid

Pure acetic acid, 20 mLPotassium iodine 20%, 10 mL


c(Na2S2O3) = 0.1 mol/L;


ICl3 + I2 = 3IClICl + KI = I2 + KCl2Na2S2O3 + I2 = 2NaI + Na2S4O6


METTLER TOLEDO


Preparation and ProceduresWijs solution, 10 mLSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Back value of Wijs Solution

1) Fill a beaker with 20 mL pure acetic acid

2) Add 10 mL Wijs solution and stir for 5 minutes.

3) Add 10 mL 20% potassium iodine.

4) Titrate inmediately with 0.1 mol/L sodium thiosulfate.

1) The determination of the iodine value is done by backtitration. Therefore the capacity of the Wijs solution, i.e. a ICl3solution in acetic acid, has to be determinated first. This isdescribed in this method.

2) The mean value of 3 capacity determination is then used inapplication M343 (iodine value determination).

Remarks

Back determination (Method 944):R1 = Q

Calculation

Method for the determination the capacity of the Wijs solution

Standard Potassium iodate

MJ SchmidAuthor

52


-------------------------------------------------------------------Method ID 944 Title Back Iodine value03-03-2005 15:27 Author Maria-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Wijs solution 1 Consumpt. 1.915 [mmol]

2 Wijs solution 1 Consumpt. 1.914 [mmol]

3 Wijs solution 1 Consumpt. 1.918 [mmol]



Titration curve

Results

53

Method ID 944 Title Back Iodine value03-03-2005 15:27 Author Maria

Sample para. Sample ID . . . . . . . . . . . . . . . Back Entry type . . . . . . . . . . . . . . Volumen Minimum [g] . . . . . . . . . . . . . . 10.0 Maximum [g] . . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 253.80 Equival. number z . . . . . . . . . . . 2 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 20EQP titration Titrant . . . . . . . . . . . . . . . . Na2S2O3 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 10.0 Back value [mmol] . . . . . . . . . . . 0.0 Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 4 dVmin [mL] . . . . . . . . . . . . . 0.04 dVmax [mL] . . . . . . . . . . . . . 0.4 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . . 100.0 Termination param. Vmax [mL] . . . . . . . . . . . . . 25.0 Numb. EQPs . . . . . . . . . . . . 1 Evaluation Numb. potentials . . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Consumpt. Name . . . . . . . . . . . . . . . . . Capacity Unit . . . . . . . . . . . . . . . . . mmol Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




54

M345

Acidic components, free fatty acids

Ethanol/diethyether 1:1, 60 mL

KOH in ethanol, c(KOH) = 0.02 mol/L


R-COOH + OH- = R-COO- + H2O

Titration beaker ME-101974Glass beaker ME-101446 (for titer)

METTLER TOLEDO

Organic solvent wasteWastedisposal

Preparation and ProceduresSunflower oil, 10 - 20 gOlive oil, 2 - 4 g

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG113-SCIndication

Acid number of edible oils

As with every titration, the standardization of the titrant has to beperformed first. The standardization of KOH with benzoic acidshows a steep jump in the E-V curve, which makes this analysisvery reliable.

The required amount of sample is weighed in. Then 60 mL ofthe solvent are added and the titration is started.

The standard benzoic acid was weighed in instead of adding asolution because it would have to be dissolved in ethanol oracetone (insoluble in water). Since the sample size has to berather small we recommend to use a balance with a resolutionof at least 0.1 mg. The standardization was performed in glassbeakers to reduce electrostatic effects during weighing.

Benzoic acid is an aggressive substance. Therefore, contact withskin, and eyes particularly, should be avoided.

1) The acid number is a measure of the decomposition by lipaseenzyme of the glycerides in oil ands fats. The decomposition isaccelerated by heat and light. Rancidity idue to decomposition isusually accompanied by free fatty acid formation.

2) Blank determination: Acidic impurities in the solvent are takeninto account by determining the solvent blank.

3) Electrode conditioning: To ensure hydration of the membraneglass, the DG113 electrode is stored over night in water. Beforetitraiton, clean the electrode with solvent.

4) Difficult samples: Samples can show a rather flat curve, andnoise can appear. Adding 1 mL 0.05 mol/L benzoic acid to oneliter solvent solves the problem.This also helps if the blank determination should not be possiblebecause the jump comes too early.


Remarks

R1: Acid Number [mg KOH/g]R2: FFA (oleic acid) [ g/100 g]

In the user formula the molecularweight is entered as constant C.The factor f is used for the unitconversion.

Calculation

Determination of the acid number and free fatty acids of edible oils.

Standard Benzoic acid

P. BurriAuthor

55


-------------------------------------------------------------------Method ID 945 Title AN non aqu.14-04-2005 13:28 Author P. Burri-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Olive oil 1 AN (KOH) 0.71625 [mg KOH/g] 2 FFA (oleic) 0.36057 [g/100 g]

2 Olive oil 1 AN (KOH) 0.71424 [mg KOH/g] 2 FFA (oleic) 0.35956 [g/100 g]




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 0.71622 0.00429 [mg KOH/g] 0.5982 5 0.36056 0.00216 [g/100 g] 0.598


Titration curve

Results

56

Method ID 945 Title AN non aqu.10-04-2005 13:28 Author P. Burri

Sample para. Sample ID . . . . . . . . . . . . . Olive oil Entry type . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . 0.5 Maximum [g] . . . . . . . . . . . . 20 Density [g/mL] . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . 56.11 Equival. number z . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . 20EQP titration Titrant . . . . . . . . . . . . . . KOH 0.02 EtOH Conc.[mol/L] . . . . . . . . . . 0.02 Sensor . . . . . . . . . . . . . . DG113 Unit . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . From list Solvent . . . . . . . . . . . . Acid non-aqueous Predis.[mL] . . . . . . . . . . . . 1.000 Back value [mmol] . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . Normal Addition . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 12 dVmin [mL] . . . . . . . . . . . 0.01 dVmax [mL] . . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . 20 Recognition Tendency . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . 40 Threshold [mV/mL]. . . . . . . . 450 St. jump only . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . 20.0 Evaluation Numb. Potentials . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . User def. Name . . . . . . . . . . . . . . . AN (KOH) Formula . . . . . . . . . . . . . . R=(Q-Bl)*C/m C . . . . . . . . . . . . . . . . . 56.11 Factor . . . . . . . . . . . . . . 1 Unit . . . . . . . . . . . . . . . mg KOH/g Which EQP . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . 3 Result limits . . . . . . . . . . . No Statistics . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . User def. Name . . . . . . . . . . . . . . . FFA (oleic) Formula . . . . . . . . . . . . . . R=(Q-Bl)*C/m C . . . . . . . . . . . . . . . . . 282.47 Factor . . . . . . . . . . . . . . 0.1 Unit . . . . . . . . . . . . . . . g/100 g Which EQP . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . 4 Result limits . . . . . . . . . . . No Statistics . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . Yes




57

M346

Peroxide, ROOR

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


c(Na2S2O3)= 0.01mol/L;


R-OOH + KI = R-OH + KOH + I2

I2 + 2Na2S2O3 = 2NaI + Na2S4O6

Red titration beaker ME-25777

METTLER TOLEDO

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

Wastedisposal

Preparation and ProceduresSunflower oil, 1 - 5 gOlive oil, 1 - 5 g

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Peroxide number in edible oils and fats

1) Beakers have to be cleaned very well. Invisible fat residues ormetal traces can affect the result strongly.Red beakers are used to protect the reaction from light.

2) To about 1 - 5 g of sample 20 mL of glacial acetic acid/chloroform (3:2) solvent was added.

3) Immediately afterwards 1 mL of saturated potassium iodidesolution was added manually. The solution is gently shaken andleft standing in the dark for exactly 60 seconds, for thegeneration of iodine.

4) 50 mL deionized water are added manually to the samplesolution, and the titration of the liberated iodine startedimmediately.

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.

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

Exactly 60 seconds were allowed for the generation of iodine, asis requested by the official method (AOAC No. 28.022). Earlierstudies, however, had indicated that the generation is notcomplete yet at this time. 200 to 300 seconds were found toyield the highest results. Longer generation times resulted in lowresults (secondary reactions between iodine and the oil).The duration of the generation time (time between 'adding the KIsolution' and 'adding the water + starting the titration') is thecritical point for repeatable results.


Remarks

R = (Q-Bl)*C/mC=1,Factor = 1000, meq/kg

Calculation

Method for the determination of the peroxide value in oil, fat and margarine.

Standard Potassium iodate, KIO3 0.1 mol/L

P. BurriAuthor

58


-------------------------------------------------------------------Method ID 946 Title Peroxide number19-04-2005 15:43 Author P. Burri-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Sunflower oil 1 PV 22.066 [meq/kg]

2 Sunflower oil 1 PV 21.684 [meq/kg]




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 21.799 0.311 [meq/kg] 1.425


Titration curve

Results

59

Method ID 946 Title Peroxide number19-04-2005 15:43 Author P. Burri

Sample para. Sample ID . . . . . . . . . . . . . Olive oil Entry type . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . 0.5 Maximum [g] . . . . . . . . . . . . 20 Density [g/mL] . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . 1.00 Equival. number z . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . 3EQP titration Titrant . . . . . . . . . . . . . . Na2S2O3 0.01 Conc.[mol/L] . . . . . . . . . . 0.01 Sensor . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . From list Solvent . . . . . . . . . . . . Peroxide number Predis.[mL] . . . . . . . . . . . . 1.000 Back value [mmol] . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . Normal Addition . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . 30 Threshold [mV/mL]. . . . . . . . 500 St. jump only . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . 20.0 Evaluation Numb. Potentials . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . User def. Name . . . . . . . . . . . . . . . PN Formula . . . . . . . . . . . . . . R=(Q-Bl)*C/m C . . . . . . . . . . . . . . . . . 1 Factor . . . . . . . . . . . . . . 1000 Unit . . . . . . . . . . . . . . . meq/kg Which EQP . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . 2 Result limits . . . . . . . . . . . No Statistics . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . Yes




60

M347

Magnesium (Mg2+) and calcium(Ca2+) as CaCO3, M=100.09; z = 1

--

EDTA,c(EDTA) = 0.1 mol/L


Ca2+ + EDTA-2H+ = Ca-EDTA + 2H+

Mg2+ + EDTA-2H+ = Mg-EDTA + 2H+


METTLER TOLEDO

Neutralization with hydrochloric acidbefore final disposal.

Wastedisposal

Preparation and Procedures50 mL drinking or surface waterSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DP5TM, wavelength 660 nm.Indication

Total hardness of water

1) Add 1 mL indicator (0.1% Eriochrome black T solution inethanol)

2) Add 10 mL 5% NH3 buffer solution. May use borate bufferinstead; Borate puffer pH10: Dissolve 40 g sodium hydroxide(NaOH) in 500 mL water (Caution: Solution gets hot!), add 65g boric acid (H3BO3) and fill up to 1000 mL with water.

3) Rinse with 0.01 mol/L hydrochloric acid if there is indicatorresidue on the DP5 mirror

4) Rinse with water.

Add the NH3 buffer only immediately beforetitration.

Always check the transmission of the phototrode in deion. waterbefore titrating: set it to 1000 mV.Avoid the formation of air bubbles during titration since theydisturb the photometric indication.The phototrode DP5 can be set to 550 nm instead of 660.

Literature:

1) Titration Applications Brochure 5,"Determination of the Total Hardness, the Ca2+ and Mg2+

Content" ME-51724634 (see applications M069, M513,M514).

Remarks

The total hardness (magnesium andcalcium) is expressed as calciumcarbonate (CaCO3).1 ppm CaCO3 = 1°US (USAhardness degree);10 mg/L CaCO3 = 1°f (Frenchhardness degree).

Calculation

The total hardness, Ca2+ and Mg2+ content of water is determined by titrating calcium and magnesium at pH10 with EDTA. The color change of the Erio T indicator (violet to blue) at the equivalence point is sensed bya phototrode.

Standard Zinc sulfate solution 0.1 mol/L

M. BiberAuthor

61


-------------------------------------------------------------------Method ID 947 Title Total hardness08-04-2005 11:17 Author M. Biber-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Water 1 Cont. 214.65 [ppm]

2 Water 1 Cont. 214.61 [ppm]




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 214.40 0.259 [ppm] 0.121


Titration curve

Results

62

Method ID 947 Title Total Hardness08-04-2005 11:17 Author M. Biber

Sample para. Sample ID . . . . . . . . . . . . . . . Water Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 50.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 100.09 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 3EQP titration Titrant . . . . . . . . . . . . . . . . EDTA 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DP5 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 0.500 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.02 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . none Min Relevance . . . . . . . . . . . 30 Threshold . . . . . . . . . . . . . 1000.0 Termination param. Numb. EQPs . . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation No. of potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . ppm Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 2 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Set of parameters . . . . . . . . . Fast Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.04 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 2.0 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 20

Set of parameters . . . . . . . . . Cautious Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.01 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . . 40

63

M348a

--

--





METTLER TOLEDO


Wastedisposal

Preparation and Procedures50 mL tap waterSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

p-Value of Water

Before the analysis a three-point calibration of the electrode wasperformed using METTLER TOLEDO buffers of pH 4.01, 7.00and 9.21.

Fill a (preferably) PE bottle to the brim with the water to beanalyzed. Keep it closed and at sampling temperature.Pour 50 mL into the titration beaker shortly before each titration.If there is no automatic temperature compensation, enter thecorrect temperature manually.For best results if the pH lies close to the end potential, use alower concentration of the corresponding titrant.

p values are determined in many different samples e.g. drinkingwater, waste water, caustic wash solutions.

p value, or total acidity, expresses the base neutralizing capacityof the water.

The name p value originates from the phenolphthalein indicatorformerly used in this titration. Phenolphthalein turns pink at pH8.2 and above.

The pH value and the acid and base capacity depend on theequilibrium of free CO2, bicarbonate, and carbonate in thecorresponding water and therefore on its temperature.

Remarks

Total acidity or phenolphthalein acidity (p value)is expressed in mg/L CaCO3 or mmol/L.

Calculation

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

Standard Potassium hydrogen phthalate

M. BiberAuthor

64


-------------------------------------------------------------------Method ID 948 Title p value in water07-03-2005 11:08 Author M. Biber-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 water 1 Cont. 0.285 mmol/L

2 water 1 Cont. 0.244 mmol/L




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 0.249 0.021 mmol/L 8.271


Titration curve

Results

65

Method ID 948 Title p value07-03-2005 11:08 Author M. Biber

Sample para. Sample ID . . . . . . . . . . . . . . . Tap water Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 50.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 18.0 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 3EP titration Titrant . . . . . . . . . . . . . . . . NaOH 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 0.00 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.020 dVmax [mL] . . . . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . . EQU ontrolled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Sensitivity . . . . . . . . . . . . . . 70 Threshold . . . . . . . . . . . . . . . 5.00 Termination param. Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Numb. Potentials . . . . . . . . . . 1 Potential 1 [pH] . . . . . . . . . . 8.20Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mmol/L Which EQP . . . . . . . . . . . . . . . Pot. 1 Name . . . . . . . . . . . . . . . . . p value Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




66

M348b

--

--

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



HCl + CO32- = HCO3

- + Cl-

HCl + HCO3- = CO2 + H2O + Cl-


METTLER TOLEDO


Wastedisposal

Preparation and Procedures50 mL tap waterSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG115-SCIndication

m-Value of Water

Before the analysis a three-point calibration of the electrode wasperformed using METTLER TOLEDO buffers of pH 4.01, 7.00and 9.21.

Fill a (preferably) PE bottle to the brim with the water to beanalyzed. Keep it closed and at sampling temperature.Pour 50 mL into the titration beaker shortly before each titration.If there is no automatic temperature compensation, enter thecorrect temperature manually.For best results if the pH lies close to the end potential, use alower concentration of the corresponding titrant.

The m value, or total alkalinity, represents the acid neutralizingcapacity of a water and is determined in many different samplese.g. drinking water, waste water, caustic wash solutions.

This acid capacity allows surface waters to resist suddenchanges in pH, e.g. due to organic acid waste, acid minedrainage, groundwater discharge or industrial waste, or due tonatural sources such as bacteria, Fe3+, hydrated Al3+, H2S, fattyacids, proteins, phosphoric acid, and CO2.

The acid capacity depends on the equilibrium of free CO2,bicarbonate, and carbonate in the corresponding water andtherefore 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)

The name m value originates from the methyl orange indicator(red to yellow-orange at pH 4.3) formerly used in this titration.

Increased acidity can affect corrosion, soil leaching, disinfectionprocesses, and aquatic life in general.

References:http://nas.cl.uh.edu/zhang/3431_04S/05_Acid-Base.ppt

Remarks

Total alkalinity or methyl orangealkalinity (m value) is expressed asmg/L CaCO3 or mmol/L

Calculation

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

Standard Tris(hydroxymethyl)-aminomethane

M. BiberAuthor

67


-------------------------------------------------------------------Method ID 948 Title m value in water19-03-2005 08:39 Author M. Biber-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 water 1 Cont. 3.821 mmol/L





Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 5 3.825 0.006 mmol/L 0.153


Titration curve

Results

68

Method ID 948 Title m value19-03-2005 08:39 Author M. Biber

Sample para. Sample ID . . . . . . . . . . . . . . . Tap water Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 50.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 18.0 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 3EP titration Titrant . . . . . . . . . . . . . . . . HCl 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG115 Unit . . . . . . . . . . . . . . . . pH Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 0.00 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.020 dVmax [mL] . . . . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . . EQU ontrolled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 2 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Positive Sensitivity . . . . . . . . . . . . . . 70 Threshold . . . . . . . . . . . . . . . 5.00 Termination param. Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Numb. Potentials . . . . . . . . . 1 Potential 1 [pH] . . . . . . . . . . 4.30Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mmol/L Which EQP . . . . . . . . . . . . . . . Pot. 1 Name . . . . . . . . . . . . . . . . . m value Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes




69

M349

Potassium ion, K+

M(K) = 39.10, z=1

ISA: 2.5 mL 0.5 M MgSO4 for 50 mLsample(1:10 ISA:sample, tot. 25 mM MgSO4 )

--


--


METTLER TOLEDO

--Wastedisposal

Preparation and ProceduresVarious aqueous solutionsSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DX239-K+ ISE, DX200 ref. electrode(Outer bridge electrolyte: 2 M MgSO4)

Indication

Potassium content determination by direct measurement

1) Preparation of the samples:

50 mL + 2.5 mL 0.5 M MgSO4

5 mL wine + 45 mL water (10 x dilution) + 2.5 mL 0.5 MMgSO4



2) The DX239-K+ electrode is adjusted with three standardsolutions (1, 10, and 100 mg/L K+)

3) The electrode is thoroughly cleaned after each sample withabundant water.

1) The DX239-K+ ISE electrode needs to be conditioned beforeuse. This is achieved by keeping the electrode in a dilutedpotassium standard solution for 10-15 min. or longer, ifnecessary.For more information, refer to the operating instructions.

2) The K+-Standard solutions can be prepared from potassiumchloride, KCl.

3) Adjustment of the DX239-K+ ISE:Always start the adjustement with the lowest concentratedstandard, i.e. 1mg/L, then 10 mg/L and finally 100 mg/L

LiteratureMETTLER-TOLEDO Titration Applications Brochure No. 6,"Direct Measurment with Ion Selective Electrodes",ME-51724646

METTLER-TOLEDO Titration Applications Brochure No. 12,"30 Selected Applications",ME-51724765

Remarks

R1: mg/LCalculation

Direct measurement of the potassium content by means of a DX239-K+ ISE in various aqueous samplessuch as mineral water, wines, fruit juices.

Standard 1, 10, 100 mg/L K+ standards

MSG AnaChemAuthor

70


-------------------------------------------------------------------Method ID 949 Title Potassium content00-00-0000 00:00 Author-------------------------------------------------------------------All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Rose wine 1 Messwert 239.568 [mg/L]

2 Rose wine 1 Messwert 240.297 [mg/L]




6 Rose wine 1 Messwert 242.496 [mg/L]Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 240.908 1.078 [mg/L] 0.447


Other samplesRed wine:Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 248.211 0.778 [mg/L] 0.314

Fruit juice:Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 7 505.775 0.000 [mg/L] 0.000

K+-solution (approx. 200 mg/L):Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 236 804 2 378 [mg/L] 1 004

Titration curve

Results

71

Method ID 949 Title Potassium content00-00-0000 00:00

Sample para. Sample ID . . . . . . . . . . . . . . . Request Entry type . . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . . 0.01 Maximum [g] . . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 1.00 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10Measure Sensor . . . . . . . . . . . . . . . . DX239 Unit . . . . . . . . . . . . . . . . mV dE [mV] . . . . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . . 100 t(max) [s] . . . . . . . . . . . . . . 120Calculation 1 Calculation . . . . . . . . . . . . . . User def. Name . . . . . . . . . . . . . . . . . Messwert Formula . . . . . . . . . . . . . . . . R=pw(-pX)*1000 C . . . . . . . . . . . . . . . . . . . 1.0 Factor . . . . . . . . . . . . . . . . 1.0 Unit . . . . . . . . . . . . . . . . . mg/L Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP

Method

72

M380

Acidic content in oil as mg KOH/g oilM = 56.11 g/mol, z = 1

60 mL solvent 664toluene/2-propanol/water= 500:495:5

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

DL28OKI B4250 Printer(parallel cable ME-51108780)

--


METTLER TOLEDO

Organic solventsWastedisposal

Preparation and ProceduresMotor oil, ca. 5 g.Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG113-SCIndication

TAN Acid number determination according to ASTM D664

Sample size depends on the expected AN:

AN expected Sample sizemg KOH/g0.05 - 0.9 20 g1.0 - 5.0 5 g5.0 - 19 1 g20 - 100 0.25 g100 - 200 0.1 g

Well homogenized sample is very important.

Before the analysis determine the buffer potential, using MERCKbuffer pH 11

Remarks

R1: AN (mg/g) EQPR2: SAN (mg/g) bufferpotential 1R3: AN (mg/g) bufferpotential 2

Calculation

Determination Acid number in mineraloil according ASTM D664


A. AichertAuthor

73


-------------------------------------------------------------------Method ID 980 Title TAN ASTM 66408-03-2005 15:02 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Oil 1 Cont.w.B 1.687 [mg/g] 2 Cont.w.B -0.059 [mg/g] 3 Cont.w.B 2.750 [mg/g]

2 Oil 1 Cont.w.B 1.433 [mg/g] 2 Cont.w.B -0.065 [mg/g] 3 Cont.w.B 2.806 [mg/g]


4 Oil 1 Cont.w.B 1.482 [mg/g] 2 Cont.w.B -0.042 [mg/g] 3 Cont.w.B 2.592 [mg/g]Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 4 1.500 0.130 [mg/g] 8.6722 4 -0.056 0.010 [mg/g] 17.8343 4 2.697 0.098 [mg/g] 3.640


Titration curve

Results

74

Method ID 980 Title TAN ASTM 66408-03-2005 15:02 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . Oil Entry type . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . 0.1 Maximum [g] . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . 56.11 Equival. number z . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . 30EQP titration Titrant . . . . . . . . . . . . . . . KOH 0.1 prop Conc.[mol/L] . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113 Unit . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . From list Solvent . . . . . . . . . . . . . TAN D664 Predis.[mL] . . . . . . . . . . . . . 1.000 Back value [mmol] . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . Normal Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 10.0 dVmin [mL] . . . . . . . . . . . . 0.01 dVmax [mL] . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 2 dt[s] . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . 60 Recognition Tendency . . . . . . . . . . . . . Negative Min Relevance . . . . . . . . . . 20.0 Threshold [mV/mL]. . . . . . . . . 50.0 St. jump only . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . 20.0 At potential [mV] . . . . . . . . -240.0 Evaluation Numb. Potentials . . . . . . . . . 2 Potential 1 [mV] . . . . . . . . . 170.0 Potential 2 [mV] . . . . . . . . . -212.1Calculation 1 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . Pot. 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . Pot. 2 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . Yes




75

M381

--

--

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


--


METTLER TOLEDO

Organic solventsWastedisposal

Preparation and Procedures60 mL solvent 664toluene/2-propanol/water= 500:495:5

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG113-SCIndication

TAN Blank determination according to ASTM D664

1) Before the analysis determine the buffer potential, usingMERCK buffer pH 11

2) Run it as blank determination, so the blank value isautomatically stored in the list of blank values.

Remarks

Consumption in mmol.Calculation

Method for the TAN blank determination according ASTM D664


A.AichertAuthor

76


-------------------------------------------------------------------Method ID 981 Title Blank TAN ASTM 66407-03-2005 14:54 Author A.Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Solvent 664 1 Blank 0.00495 [mmol]

2 Solvent 664 1 Blank 0.00478 [mmol]




Titration curve

Results

77

Method ID 981 Title Blank TAN ASTM 66407-03-2005 14:54 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . . Solvent 664 Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 60.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 56.11 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . KOH 0.1 prop Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG113 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 0.00 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 10.0 dVmin [mL] . . . . . . . . . . . . . 0.004 dVmax [mL] . . . . . . . . . . . . . 0.05 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 2 dt[s] . . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . . 60 Recognition Tendency . . . . . . . . . . . . . . Negative Termination param. Vmax [mL] . . . . . . . . . . . . . 2.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . -208.1Calculation 1 Calculation . . . . . . . . . . . . . . Consump. Unit . . . . . . . . . . . . . . . . . mmol Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 5 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Control parameters Set of parameters . . . . . . . . . Fast Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 15.0 dVmin [mL] . . . . . . . . . . . . . 0.004 dVmax [mL] . . . . . . . . . . . . . 0.05 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . . 60

Control parameters Set of parameters . . . . . . . . . Cautions Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.002 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 15 t(max) [s] . . . . . . . . . . . . . 60

78

M382

Acid capacity in oil as mg KOH/g oilM = 56.11 g/mol, z = 1

60 mL solvent 4739toluene/2-propanol/chloroform/water=10:10:10:0.3

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


--


METTLER TOLEDO


Preparation and ProceduresMotor oil, ca. 2.5 g.Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG113-SCIndication

TBN Base number determination according to ASTM D4739

1) The sample size depends on the expected BN:Sample size (g) = 7 / expected BN

2) Before starting the analysis, it is necessary to determine thebuffer potential using MERCK buffer pH 3

3) Use a well homogenized sample to get accurate results.

Remarks

R1: BN (mg/g) EQPR2: SBN (mg/g) buffer potential 1R3: BN (mg/g) buffer potential 2

Calculation

Determination base number in mineral oil according ASTM D4739

Standard Standardized KOH in 2-propanol

A. AichertAuthor

79


-------------------------------------------------------------------Method ID 982 Title TBN ASTM 473921-04-2005 17:28 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Oil 1 Cont.w.B 9.692 [mg/g] 2 Cont.w.B -0.015 [mg/g] 3 Cont.w.B 8.922 [mg/g]




Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 4 9.912 0.273 [mg/g] 2.7532 4 -0.015 0.000 [mg/g] 2.8763 4 8.895 0.143 [mg/g] 1.608


Titration curve

Results

80


Sample para. Sample ID . . . . . . . . . . . . . . Oil Entry type . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . 0.1 Maximum [g] . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . 56.11 Equival. number z . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . 30EQP titration Titrant . . . . . . . . . . . . . . . HCl 0.1 prop Conc.[mol/L] . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113 Unit . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . From list Solvent . . . . . . . . . . . . . TAN D4739 Predis.[mL] . . . . . . . . . . . . . 3.000 Back value [mmol] . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . Normal Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 10.0 dVmin [mL] . . . . . . . . . . . . 0.01 dVmax [mL] . . . . . . . . . . . . 0.4 Measure mode . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . . 3 t(min) [s] . . . . . . . . . . . . 15 t(max) [s] . . . . . . . . . . . . 60 Recognition Tendency . . . . . . . . . . . . . Positive Min Relevance . . . . . . . . . . 20.0 Threshold [mV/mL]. . . . . . . . . 90.0 St. jump only . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . 20.0 At potential [mV] . . . . . . . . 250.0 Evaluation Numb. Potentials . . . . . . . . . 2 Potential 1 [mV] . . . . . . . . . -208.00 Potential 2 [mV] . . . . . . . . . 233.0Calculation 1 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . Pot. 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . Pot. 2 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . Yes




81

M383

--

--

Hydrochloric acid,HCl in 2-propanolc(HCl) = 0.1 mol/L;


--


METTLER TOLEDO


Preparation and Procedures60 mL solvent 4739toluene/2-propanol/Chloroform/water=10:10:10:0.3

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG113-SCIndication

TBN Blank determination according to ASTM D4739

1) Before the analysis determine the buffer potential, usingMERCK buffer pH 3

2) Run it as blank determination, so the blank value isautomatically stored in the list of blank values.

Remarks

Consumption in mmol.Calculation

Method for the TBN blank determination according ASTM D4739


A.AichertAuthor

82


-------------------------------------------------------------------Method ID 983 Title Blank TAN ASTM 473919-04-2005 10:28 Author A.Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Solvent 4739 1 Blank 0.00081 [mmol]






Titration curve

Results

83

Method ID 983 Title Blank TAN ASTM 473919-04-2005 10:28 Author A. Aichert

Sample para. Sample ID . . . . . . . . . . . . . . . Solvent 4739 Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 60.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 56.11 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EP titration Titrant . . . . . . . . . . . . . . . . HCl 0.1 prop Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DG113 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . From list Solvent . . . . . . . . . . . . . . TBN D4739 Predis.[mL] . . . . . . . . . . . . . . 0.000 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . Normal Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 1.0 dVmin [mL] . . . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . . . 0.05 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . . . 4 t(min) [s] . . . . . . . . . . . . . 15 t(max) [s] . . . . . . . . . . . . . 180 Recognition Tendency . . . . . . . . . . . . . . Positive Termination param. Vmax [mL] . . . . . . . . . . . . . 2.0 Evaluation Numb. EPs . . . . . . . . . . . . . 1 End point 1 . . . . . . . . . . . . Absolute Potential 1 [pH] . . . . . . . . . . 230.0Calculation 1 Calculation . . . . . . . . . . . . . . Consump. Unit . . . . . . . . . . . . . . . . . mmol Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 5 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . No


Control parameters Set of parameters . . . . . . . . . Fast Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 1.0 dVmin [mL] . . . . . . . . . . . . . 0.004 dVmax [mL] . . . . . . . . . . . . . 0.05 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 2 dt[s] . . . . . . . . . . . . . . . 4 t(min) [s] . . . . . . . . . . . . . 5 t(max) [s] . . . . . . . . . . . . . 120

Control parameters Set of parameters . . . . . . . . . Cautions Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.002 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . . 5 t(min) [s] . . . . . . . . . . . . . 20 t(max) [s] . . . . . . . . . . . . . 180

84

M384

Acid capacity in oil as mg KOH/g oilM = 56.11 g/mol, z = 1

60 mL solvent 2896acetic acid / chlorobenzene = 1:2

Perchloric acid,HClO4 in acetic acidc(HClO4) = 0.1 mol/L


--


METTLER TOLEDO


Preparation and ProceduresMotor oil, ca. 2.8 g.Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DG113-SCIndication

TBN Base number determination according to ASTM D2896

1) The sample size depends on the expected BN:Sample size (g) = 28 / expected BN

2) The sample has to be well homogeneous to get accurateresults.

3) Use the same method for the blank determination .Start with "blank" instead of "sample"

Remarks

R1: BN (mg/g)R2: Consump. (mL)

Calculation

Determination base number in mineral oil according ASTM D2896

Standard KHP

A. AichertAuthor

85


Sample determination-------------------------------------------------------------------Method ID 984 Title TBN ASTM 289618-04-2005 07:33 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Oil 1 Cont.w.B 10.420 [mg/g] 2 Consump. 5.351 [mL]

2 Oil 1 Cont.w.B 10.401 [mg/g] 2 Consump. 5.383 [mL]



Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 4 10.429 0.023171 [mg/g] 0.222

Blank determination-------------------------------------------------------------------Method ID 984 Title TBN ASTM 289613-04-2005 13:56 Author A. Aichert-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Oil 1 Blank 0.00143 [mmol] 2 Consump. 0.014 [mL]

2 Oil 1 Cont.w.B 0.00150 [mmol] 2 Consump. 0.015 [mL]



Titration curve

Results

86


Sample para. Sample ID . . . . . . . . . . . . . . Oil Entry type . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . 0.1 Maximum [g] . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . 56.11 Equival. number z . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . 60EQP titration Titrant . . . . . . . . . . . . . . . HClO4 0.1 prop Conc.[mol/L] . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113 Unit . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . From list Solvent . . . . . . . . . . . . . TAN D2896 Predis.[mL] . . . . . . . . . . . . . 3.000 Back value [mmol] . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . Normal Addition . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . 8.0 dVmin [mL] . . . . . . . . . . . . 0.002 dVmax [mL] . . . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . 0.5 dt[s] . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . 10 t(max) [s] . . . . . . . . . . . . 60 Recognition Tendency . . . . . . . . . . . . . None Min Relevance . . . . . . . . . . 10.0 Threshold [mV/mL]. . . . . . . . . 100.0 St. jump only . . . . . . . . . . No Termination param. Numb. EQPs . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . 20.0 Evaluation Numb. Potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mg/g Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . Conump. Type . . . . . . . . . . . . . . . . Cont. w. blank Unit . . . . . . . . . . . . . . . . mL Which EQP . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . NoReport Output . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . Yes




87

M385

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

1-2 g potassium iodide, KI50 mL 0.1 mol/L hydrochloric acid,




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

I2 + 2S2O32- = 2I- + S4O6

2-


METTLER TOLEDO

Neutralization before final disposal asspecial waste.

Wastedisposal

Preparation and ProceduresAqueous copper solution, 5 mL(conc.: 0.1 mol/L)

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DM140-SCIndication

Copper content determination in aqueous solutions

1) Add 1-2 g potassium iodide to the sample beaker containingthe sample,

2) Add 50 mL 0.1 mol/L HCl,

3) Iodine is immediately generated after addition of hydrochloricacid,

4) To avoid loss of iodine, a low stirrer speed is applied (30%).

5) The electrode, the stirrer and the titration tube are cleanedwith deionized water. If needed, these parts are cleaned with apaper tissue.

Literature:

1) Titration Applications Brochure 12, "30 Selected Applications"ME-51724765 (see applications M509 and M510).

2) Titration Applications Brochure 18, "Standardizations ofTitrants", ME-51724917 (see application M526).

Remarks

R1: Content (g/L)R2: Consumption (mL)R3: Content (mol/L)

Calculation

The determination of copper in electroplating baths is perfomed by titration of generated iodine with sodiumthiosulphate after addition of iodide to the sample.

Standard Potassium iodate, 20-30 mg

C. De CaroAuthor

88


EQP titration------------------------------------------------------------------------------Method ID 985 Title Cu cont. normal10-02-2005 15:59 Author C. De Caro------------------------------------------------------------------------------Titrant Na2S2O3 0.1 Sensor DM140Conc.[mol/L] 0.1 Unit mV------------------------------------------------------------------------------Sample 6Sample ID 0.1 M Cu solutionVolume V [mL] 5Density [g/mL] 1.0Mol.m. [g/mol] 63.546Equival. number z 1Predisp.[mL] 1Mixing time [s] 90Init.pot. [mV] 340.6Consumption [mV] 5.610Duration [min:s] 3:20Temp.[°C] 25.0Termination param. All points reachedBlank [mmol] 0.00Black value [mmol] 0.00

Result EQP Calculat. Value Unit------------------------------------------------------------------------------1 1 Cont. 6.3141 [g/L]2 1 Consumpt. 4.968 [mL]3 1 Cont. 0.0994 [mol/L]

Statistics reportResult n x s Unit srel------------------------------------------------------------------------------1 6 6.2975 0.0116 [g/L] 0.184 [%]2 6 4.955 0.009 [mL] 0.183 [%]3 6 0.0991 0.0002 [mol/L] 0.187 [%]

Titration curve

Results

89

Method ID 985 Title Cu cont. normal10-02-2005 15:59 Author C. De Caro

Sample para. Sample ID . . . . . . . . . . . . . . . 0.1M Cu solution Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 5 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 63.546 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 30 Mixing time [s] . . . . . . . . . . . . 90EQP titration Titrant . . . . . . . . . . . . . . . . Na2S2O3 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DM140 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 1 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . . . 8 dVmin [mL] . . . . . . . . . . . . . 0.01 dVmax [mL] . . . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . . . 3 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min. relevance . . . . . . . . . . . 30 Threshold [mV/mL] . . . . . . . . . 500.0 St. Jump only . . . . . . . . . . . No Termination param. Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Numb. EQP's . . . . . . . . . . . . 1 Number Potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . g/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . Consumpt. Unit . . . . . . . . . . . . . . . . . g/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mol/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes



Set of parameters . . . . . . . Cautious Addition . . . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 6 dVmin [mL] . . . . . . . . . . . 0.01 dVmax [mL] . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . 1 dt[s] . . . . . . . . . . . . . 5 t(min) [s] . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . 30

90

M386

Ni2+, M = 58.69 g/mol, z=1

40 mL deionized water,5 drops murexide solution (ca. 0.2%)1-2 drops concentrated ammonia sol.

EDTAc(EDTA) = 0.1 mol/L


Ni2+ + Murexide2- = Ni-Murexide-

Ni-Murexide- + EDTA4- = Ni-EDTA2-


METTLER TOLEDO

Neutralization before final disposal asspecial waste.

Wastedisposal

Preparation and ProceduresAqueous nickel solution, 5 mL(conc.: 0.1 mol/L)

Sample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DP5 PhototrodeTM, 550 nmIndication

Nickel content determination in aqueous solutions

1) Add 40 mL deionized water to the sample,

2) Add 5 drops of a freshly prepared aqueous solution ofmurexide (approx. 0.1-0.2%). Note that murexide is not verystable in aqueous solution; a trituration of murexide with NaCl(1:100) is also recommended.

3) Nickel forms a yellow complex with murexide.

4) Ammonia solution (ca. 10-15%) is added to the solution.Since the sample solution is neutral, only 1 drop was used.

5) During titration, EDTA displaces murexide and forms a morestable complex with nickel ions. At the equivalence point, allnickel ions have reacted with EDTA, and a color change fromyellow from violet takes place. Murexide is dissolved into thealkaline solution.

6) The phototrode, the stirrer and the titration tube are cleanedwith deionized water. If needed, these parts are cleaned with apaper tissue.

1) The shape of the titration curve is affected by the amount ofcolor indicator added to the sample. Thus, do not add too muchindicator to avoid wwrong results.

2) Too much ammonia solution can lead to an increase inturbidity of the sample solution.

3) To improve repeatability, always the same amount ofindicator and ammonia solution was added to the sample.

Literature:

1) Titration Applications Brochure 1, "18 Customer Methods" ME-00724492 (see applications M215).

2) Titration Applications Brochure 18, "Standardizations ofTitrants", ME-51724917 (see application M528).

Remarks

R1: Content (mol/L)R2: Content (g/L)R3: Consumption (mL)

Calculation

The determination of nickel in electroplating baths is perfomed by photometric titration at pH 10 with EDTAusing murexide as a color indicator and a DP5 PhototrodeTM.

Standard 0.1 mol/L zinc sulfate sol., 5 mL

C. De CaroAuthor

91


-------------------------------------------------------------------Method ID 986 Title Nickel normal04-03-2005 17:15 Author C. De Caro-------------------------------------------------------------------

All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 0.1 M Ni 1 Cont. 0.0988 [mol/L] 2 Cont. 5.800 [g/L] 3 Consump. 4.9416 [mL]

2 0.1 M Ni 1 Cont. 0.0987 [mol/L] 2 Cont. 5.794 [g/L] 3 Consump. 4.9365 [mL]





Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 0.0985 0.0003 [mol/L] 0.3482 6 5.779 0.020 [g/L] 0.3513 6 4.9229 0.0171 [mL] 0.348


Titration curve

Results

92

Method ID 186 Title Nickel normal04-03-2005 17:15 Author C. De Caro

Sample para. Sample ID . . . . . . . . . . . . . . . 0.1 M Ni Entry type . . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . . . . 5 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 58.69 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 10EQP titration Titrant . . . . . . . . . . . . . . . . EDTA 0.1 Conc.[mol/L] . . . . . . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . . DP5 Unit . . . . . . . . . . . . . . . . mV Blank . . . . . . . . . . . . . . . . . Entry Value [mmol] . . . . . . . . . . . . 0.00 Predis.[mL] . . . . . . . . . . . . . . 4.5 Back value [mmol] . . . . . . . . . . . 0.00 Control parameters Set of parameters . . . . . . . . . User Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.02 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 30 Recognition Tendency . . . . . . . . . . . . . . Negative Min. Relevance . . . . . . . . . . . 30 Threshold [mV/mL] . . . . . . . . . 400.0 St. jump only . . . . . . . . . . . No Termination param. Numb. EQP's . . . . . . . . . . . . 1 Vmax [mL] . . . . . . . . . . . . . 10.0 Evaluation Number Potentials . . . . . . . . . 0Calculation 1 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . mol/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . Cont. Type . . . . . . . . . . . . . . . . . Cont. Unit . . . . . . . . . . . . . . . . . g/L Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 3 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 3 Calculation . . . . . . . . . . . . . . Consumpt. Unit . . . . . . . . . . . . . . . . . mL Which EQP . . . . . . . . . . . . . . . 1 Decimal places . . . . . . . . . . . . 4 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP Meas. val. table . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . . . Yes dE/dV curve . . . . . . . . . . . . . . Yes


Set of parameters . . . . . . . . . Fast Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.04 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 15

Set of parameters . . . . . . . . . Cautious Addition . . . . . . . . . . . . . . Incremental Increment . . . . . . . . . . . . . 0.01 Measure mode . . . . . . . . . . . . EQU controlled dE[mV] . . . . . . . . . . . . . . . 1.0 dt[s] . . . . . . . . . . . . . . . 2 t(min) [s] . . . . . . . . . . . . . 3 t(max) [s] . . . . . . . . . . . . . 40

93

M387

Fluoride, F-

M(F) = 19.00, z=1

5 mL TISAB III (ME-51340064) for 50mL sample

--


--


METTLER TOLEDO

--Wastedisposal

Preparation and ProceduresVarious aqueous solutions, 50 mLSample

Substance

Chemicals

Titrant

Instruments

Results

Chemistry

Accessories

DX219-F- ISE, DX200 ref. electrode(Outer bridge electrolyte: 3 M KCl)

Indication

Fluoride content determination by direct measurement

1) Preparation of the samples:

50 mL + 5 mL TISAB III

50 mL + 5 mL TISAB III

50 mL wine + 5 mL TISAB IIIToothpaste:ca. 10 g dissolved in 40 mL water, dilute to 50 mL withdeionised water, add 5 mL TISAB III.

2) The DX219-F- electrode is adjusted with three standardsolutions (1, 10, and 100 mg/L F-)

3) The electrode is thoroughly cleaned after each sample withabundant water.

1) The DX219-F- ISE electrode needs to be conditioned beforeuse. This is achieved by keeping the electrode in a dilutedfluoride standard solution for 10-15 min. or longer, if necessary.For more information, refer to the operating instructions.

2) The F--Standard solutions can be prepared from sodiumfluoride, KCl.

3) Adjustment of the DX219-F- ISE:Always start the adjustement with the lowest concentratedstandard, i.e. 1mg/L, then 10 mg/L and finally 100 mg/L

LiteratureMETTLER-TOLEDO Titration Applications Brochure No. 6,"Direct Measurment with Ion Selective Electrodes",ME-51724646

METTLER-TOLEDO Titration Applications Brochure No. 12,"30 Selected Applications",ME-51724765

Remarks

R1: ppmCalculation

Direct measurement of the fluoride content by means of a DX219-F- ISE in various aqueous samples.

Standard 1, 10, 100 mg/L F- standards

MSG AnaChemAuthor

94


-------------------------------------------------------------------Method ID 996 Title Fluoride content00-00-0000 00:00 Author-------------------------------------------------------------------All resultsSample Sample ID Result Calculat. Value Unit-------------------------------------------------------------------1 Toothpaste 1 Meas. value 23.55 [ppm]

2 Toothpaste 1 Meas. value 23.82 [ppm]





Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 23.55 0.21 [ppm] 0.878


Other samplesMineral water:Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 1.53 0.00 [ppm] 0.325

Rosé wine:Statistics reportResult n x s Unit srel [%]-------------------------------------------------------------------1 6 0.50 0.02 [ppm] 3.429

Titration curve

Results

95

Method ID 996 Title Fluoride content00-00-0000 00:00 Author

Sample para. Sample ID . . . . . . . . . . . . . . . Request Entry type . . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . . 0.01 Maximum [g] . . . . . . . . . . . . . . 10.0 Density [g/mL] . . . . . . . . . . . . 1.0 Mol.m. [g/mol] . . . . . . . . . . . . 1.00 Equival. number z . . . . . . . . . . . 1 Temp.sensor . . . . . . . . . . . . . . Manual Temp. [°C] . . . . . . . . . . . . . . 25.0Stir Speed [%] . . . . . . . . . . . . . . . 35 Mixing time [s] . . . . . . . . . . . . 3Measure Sensor . . . . . . . . . . . . . . . . DX219 Unit . . . . . . . . . . . . . . . . mV dE [mV] . . . . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . . . . 1 t(min) [s] . . . . . . . . . . . . . . 100 t(max) [s] . . . . . . . . . . . . . . 120Calculation 1 Calculation . . . . . . . . . . . . . . Meas. val. Unit . . . . . . . . . . . . . . . . . ppm Decimal places . . . . . . . . . . . . 2 Result limits . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . . YesCalculation 2 Calculation . . . . . . . . . . . . . . NoneCalculation 3 Calculation . . . . . . . . . . . . . . NoneReport Output . . . . . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . . . GLP

Method

96

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.

Subject to technical changes© 08/05 Mettler-Toledo GmbH, ME-51725065Printed in Switzerland.

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