METTLER TOLEDO Titrators. 30 Selected Applications Application brochure 12

Transcription

1 METTLER TOLEDO Titrators 30 Selected Applications Application brochure 12

2 Editorial Dear Reader You have in your hands the paper version of the METTLER methods for titrators of the DL50 series. We d like to show you how you can use these titrators and what kind of results you can expect. Included in the applications are lots of hints for sample preparation, for the methods, for control parameters and for disposal. We d especially like to direct your attention to titration applications M505 to M514. Here you ll find one example each of a completely formulated method for a rapid and exact determination in acidimetry, alkalimetry, argentometry, complexometry and redox titration. The exact methods have a high reproducibility which you can match or beat using careful, good laboratory techniques. The rapid methods shorten analysis times considerably. The increased operational capacity for samples is paid for with a decrease in reproducibility. You can easily use these 10 titration applications as examples for your own method optimization. The instructions manual will tell you which METTLER method is electronically stored and need only be recalled for each of the DL50Graphix, DL53, DL55 and DL58 titrators. We wish you lots of success titrating with the METTLER TOLEDO DL50Graphix, DL53, DL55 and DL58. Christian Walter Manager Market Support AnaChem Rolf M. Rohner Marketing Manager Page 2 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

3 Content M501 Acid Content... 4 M502 Calibration of a ph Electrode... 6 M503 Calibration of an Ion Selective Fluoride Electrode... 8 M504 Fluoride Content M505 Content of H 2 SO 4 -exact M506 Content of H 2 SO 4 -fast M507 Content of NaOH -exact M508 Content of NaOH -fast M509 Determination of CuSO 4 with Na 2 S 2 O 3 -exact M510 Determination of CuSO 4 with Na 2 S 2 O 3 -fast M511 Chloride in Ketchup -exact M512 Chloride in Ketchup -fast M513 Total hardness in tap water -exact M514 Total hardness in tap water -fast Water determination according to Karl Fischer M515 Karl Fischer Titration M516 Karl Fischer Drift Determination (and standby) Determination of acid number (AN) and base number (BN) in oils M517 Blank determination according to ASTM D M518 Blank determination according to ASTM D M519 AN (acid number) according to ASTM D M520 BN (base number) ASTM D M521 of NaOH 0.1 mol/l M522 of HCl 0.1 mol/l M523 of Tetrabutyl ammonium hydroxide (TBAH) 0.1 mol/l M524 of HClO mol/l M525 of AgNO mol/l M526 of Na 2 S 2 O mol/l M527 of 1/5 KMnO mol/l M528 of EDTA 0.1 mol/l M529 of Karl Fischer Reagent 5 g H 2 O/L M530 of SDS 0.01 mol/l Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 3

4 METTLER TOLEDO Titration Application No. M501 Acid Content Sample: Substance: Preparation: Titrant: Standard: 5 ml Hydrochloric acid ca. 0.1 mol/l HCl M = deion. water Sodium hydroxide c(naoh) = 0.1 mol/l Potassium hydrogen phthalate Instruments: METTLER TOLEDO DL50 Printer (HP DeskJet 500) Method: METTLER Method Accessories: Titration beaker ME Results: METTLER TOLEDO DL50 Titrator V1.0 Mettler-Toledo AG 002 Market Support Laboratory Method Acid content 01-Jul :00 Measured 12-Jul :04 User ALL RESULTS No. ID Sample size and results 1 HCl 5.0 ml R1 = ml Consumption R2 = mol/l Acid content R3 = g/l Acid content 2 HCl 5.0 ml R1 = ml Consumption R2 = mol/l Acid content R3 = g/l Acid content 3 HCl 5.0 ml R1 = ml Consumption R2 = mol/l Acid content R3 = g/l Acid content 4 HCl 5.0 ml R1 = ml Consumption R2 = mol/l Acid content R3 = g/l Acid content 5 HCl 5.0 ml R1 = ml Consumption R2 = mol/l Acid content R3 = g/l Acid content Number results R1 n = 5 Mean value x = ml Consumption Standard deviation s = ml Consumption Rel. standard deviation srel = % Number results R3 n = 5 Mean value x = g/l Acid content Standard deviation s = g/l Acid content Rel. standard deviation srel = % Page 4 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

5 Method Method Acid content Version 01-Jul :00 Title Method ID Title Acid content Date/time Jul :00 Sample Sample ID Entry type Volume Lower limit [ml] Upper limit [ml] Molar mass M Equivalent number z Titration stand Stand 1 Temperature sensor Manual Stir Speed [%] Time [s] EQP titration Titrant/Sensor Titrant NaOH Concentration [mol/l] Sensor DG111 Unit of meas ph Predispensing to volume Volume [ml] Titrant addition Dynamic de(set) [mv] dv(min) [ml] dv(max) [ml] Measure mode Equilibrium controlled de [mv] dt [s] t(min) [s] t(max) [s] Recognition Threshold Steepest jump only No Range No Tendency None Termination at maximum volume [ml] at potential No at slope No after number EQPs No comb. termination conditions.. No Evaluation Procedure Standard Potential No Potential No Stop for reevaluation No Formula R=VEQ Constant Decimal places Result unit ml Result name Consumption Formula R2=Q*C2/m Constant C2=1 Decimal places Result unit mol/l Result name Acid content Statistics No Formula R3=Q*C3/m Constant C3=M/z Decimal places Result unit g/l Result name Acid content Report Output unit Printer Results No All results Yes Raw results Yes Table of measured values Yes Sample data No E - V curve Yes de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks The determination of the acid content of a diluted hydrochloric acid represents a demo method. It is stored in the titrator as method and is described step by step in the tutorial (ME ). Here also the various types of records are shown. The unit of measurement of the sensor DG111 is ph. The threshold for recognition of the equivalence point has to be modified if the unit is changed to [mv] in the Setup data of the sensor. Entering a value of 100 mv/ml is recommended. (See function EQP TITRATION). Waste disposal Neutralization with hydrochloric acid Other titrators Method also runs with the following titrators: DL53, DL55, DL58 DL67, DL70ES, DL77 Author: A. Aichert Table of measured values Volume Increment Signal Change 1st deriv. Time ml ml ph ph ph/ml min:s ET : : :15 ET : : : : : : : : : : : : :40 EQP : : : : : : : : : : : : : : : :47 E V Curve 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 5

6 METTLER TOLEDO Titration Application No. M502 Calibration of a ph Electrode Sample: Substance: Preparation: Titrant: Standard: Buffer solutions ph 4 / ph 7 / ph 10 Instruments: METTLER TOLEDO DL50 Printer (HP DeskJet 500) Method: METTLER Method Accessories: Indication: Titration beaker ME DG111 Results: METTLER TOLEDO DL50 Titrator V1.0 Mettler-Toledo AG 002 Market Support Laboratory Method Calibration ph elektrode 01-Jul :00 Measured 17-Jul :26 User ALL RESULTS No. ID Sample size and results ml ph R1 = mv ml ph R1 = mv ml ph R1 = mv CALIBRATION Sensor DG111 Buffer type ph (METTLER TOLEDO) Zero point ph0 Slope mv/ph Calibration temperature 25.0 C Page 6 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

7 Method Method Calibration ph elektrode Version 01-Jul :00 Title Method ID Title Calibration ph elektrode Date/time Jul :00 Sample Sample ID Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand Stand 1 Temperature sensor Manual Stir Speed [%] Time [s] Measure Sensor DG111 Unit of meas mv de [mv] dt [s] t(min) mode Fix t(min) [s] t(max) [s] Formula R=E Constant Decimal places Result unit mv Result name Statistics No Calibration Sensor DG111 Buffer type ph (METTLER TOLEDO) First buffer ph 4.01 Second buffer ph 7.00 Third buffer ph Fourth buffer ph 2.0 Fifth buffer ph 2.0 Sixth buffer ph 2.0 Seventh buffer ph 2.0 Eighth buffer ph 2.0 Result R Minimal slope Maximal slope Report Output unit Printer Results No All results Yes Raw results No Table of measured values No Sample data No E - V curve No de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks The calibration of a ph electrode represents a demo method. It is stored in the titrator as method and is described step by step in the tutorial (ME ). The calibration data are automatically stored in the setup data of the titrator. They are assigned to the sensor used in the method and are only valid for this sensor. Up to 8 buffer values can be taken for the calibration. If only one buffer is used, the titrator only corrects the zero point (ph0). The reference data of buffers available from METTLER TOLEDO, MERCK and the NIST (NBS) are stored in the titrator. These buffers can be selected from the menu (see Operating Instructions, chapter ). Other buffer values can be entered manually. If the sensor is used at a different temperature at a later time the titrator corrects the slope of the sensor by manual entry or temperature measurement. More details are given in the book «Fundamentals of Titration» (ME ). In the appendix the buffer values at various temperatures are given. Waste disposal Neutralization Other titrators Method also runs with the following titrators: DL53, DL55, DL58 DL67, DL70ES, DL77 Authors: A. Aichert, K. Sägesser 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 7

8 METTLER TOLEDO Titration Application No. M503 Calibration of an Ion Selective Fluoride Electrode Sample: 50 ml Fluoride solutions 10 and 0.1 mg/l Substance: Fluoride M = Preparation: Titrant: Standard: 5 ml TISAB III (MERCK) Instruments: METTLER TOLEDO DL50 Printer (HP DeskJet 500) Method: METTLER Method Accessories: Indication: Titration beaker ME Ion selective fluoride electrode DX219 Reference electrode DX200 Results: METTLER TOLEDO DL50 Titrator V1.0 Mettler-Toledo AG 014 Market Support Laboratory Method Calibration F - electrode 01-Jul :00 Measured 18-Jul :16 User ALL RESULTS No. ID Sample size and results ml ph,pm,px R1 = mv ml ph,pm,px R1 = mv CALIBRATION Sensor DX219 Buffer type ph, pm, px Zero point px0 Slope mv/px Calibration temperature 23.5 C Page 8 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

9 Method Method Calibration F - electrode Version 01-Jul :00 Title Method ID Title Calibration F - electrode Date/time Jul :00 Sample Sample ID Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand Stand 1 Temperature sensor Manual Stir Speed [%] Time [s] Measure Sensor DX219 Unit of meas mv de [mv] dt [s] t(min) mode Fix t(min) [s] t(max) [s] Formula R=E Constant Decimal places Result unit mv Result name Statistics No Calibration Sensor DX219 Buffer type ph, pm, px First buffer Second buffer Third buffer Fourth buffer Fifth buffer Sixth buffer Seventh buffer Eighth buffer Result R Minimal slope Maximal slope Report Output unit Printer Results No All results Yes Raw results No Table of measured values.... No Sample data No E - V curve No de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks Calibration and measurement solutions should always be at the same temperature. All measurements should be performed using the same stirring conditions. This means the same speed, stirrer type, distance to electrode, etc. It is necessary to stir for approx. 3 minutes per measurement to attain a stable measured value. Rinse electrode with deion. water after each measurement and remove adhering water drops with a soft paper tissue. The calibration data are automatically stored in the setup data of the titrator. They are assigned to the sensor used in the method and are only valid for this sensor. Up to 8 buffer values can be taken for the calibration. If only one buffer is used, the titrator only corrects the zero point. Waste disposal Other titrators Method also runs with the following titrators: DL53, DL55, DL58 DL67, DL70ES, DL77 Authors: A. Aichert, K. Sägesser 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 9

10 METTLER TOLEDO Titration Application No. M504 Fluoride Content Sample: 50 ml Tap water Substance: Fluoride M = Preparation: 5 ml TISAB III (MERCK) Titrant: Standard: Instruments: METTLER TOLEDO DL50 Printer (HP DeskJet 500) Method: METTLER Method Accessories: Indication: Titration beaker ME Ion selective fluoride electrode DX219 Reference electrode DX200 Results: METTLER TOLEDO DL50 Titrator V1.0 Mettler-Toledo AG 014 Market Support Laboratory Method Fluoride content 01-Jul :00 Measured 18-Jul :37 User ALL RESULTS No. ID Sample size and results 1 water 50.0 ml R1 = px R2 = mg/l F content 2 water 50.0 ml R1 = px R2 = mg/l F content 3 water 50.0 ml R1 = px R2 = mg/l F content 4 water 50.0 ml R1 = px R2 = mg/l F content 5 water 50.0 ml R1 = px R2 = mg/l F content Number results R2 n = 5 Mean value x = mg/l F content Standard deviation s = mg/l F content Rel. standard deviation srel = % Page 10 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

11 Method Method Fluoride content Version 01-Jul :00 Title Method ID Title Fluoride content Date/time Jul :00 Sample Sample ID Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand Stand 1 Temperature sensor..... Manual Stir Speed [%] Time [s] Measure Sensor DX219 Unit of meas px de [mv] dt [s] t(min) mode Fix t(min) [s] t(max) [s] Formula R=E Constant Decimal places Result unit px Result name Statistics No Formula R2=pw(-E)*1000 Constant Decimal places Result unit mg/l Result name F content Statistics Yes Report Output unit Printer Results No All results Yes Raw results Yes Table of measured values.. No Sample data No E - V curve No de/dv - V curve No d2e/dv2 - V curve..... No log de/dv - V curve.... No E - t curve No V - t curve No dv/dt - t curve No Remarks Calibration and measurement solutions should always be at the same temperature. All measurements should be performed using the same stirring conditions. This means the same speed, stirrer type, distance to electrode, etc. Is necessary to stir for approx. 3 minutes per measurement to attain a stable measured value. Rinse electrode with deion. water after each measurement and remove adhering water drops with a soft paper tissue. For more information about ion selective electrodes see Application Brochure 6 «Direct Measurement with Ion Selective Electrodes» ME or «Guideline to Ion Selective Measurement» ME Waste disposal Other titrators Method also runs with the following titrators: DL53, DL55, DL58 DL67, DL70ES, DL77 Authors: A. Aichert, K. Sägesser 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 11

12 METTLER TOLEDO Titration Application No. M505 Content of H 2 SO 4 -exact- Sample: 5 ml Sulfuric acid 0.05 mol/l Substance: H 2 SO 4 M = ; z = 2 Preparation: deion. water 50 ml Titrant: Standard: Sodium hydroxide c(naoh) = 0.1 mol/l Potassium hydrogen phthalate Instruments: METTLER TOLEDO DL53 METTLER ST20A Sample changer Printer (HP DeskJet 510) Method: METTLER Method Accessories: Indication: Titration beaker ME Peristaltic pump ME DG111 Results METTLER TOLEDO DL53 Titrator V1.0 Mettler-Toledo AG 007 Market Support Laboratory Method ph aqu acid exact 01-Jul :00 Measured 07-Jul :42 User ALL RESULTS No. ID Sample size and results 1 H2SO4 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 2 H2SO4 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 3 H2SO4 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 4 H2SO4 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 5 H2SO4 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 6 H2SO4 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption Number results R1 n = 6 Mean value x = % [g/ml]content Standard deviation s = % [g/ml]content Rel. standard deviation srel = % Number results R2 n = 6 Mean value x = mol/l Concentration Standard deviation s = mol/l Concentration Rel. standard deviation srel = % Page 12 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

13 Method Method ph aqu acid exact Version 01-Jul :00 Title Method ID Title ph aqu acid exact Date/time Jul :00 Sample Sample ID H 2 SO 4 Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand ST20A Pump Yes Solvent H 2 O Volume [ml] Rinse Yes Solvent H 2 O Volume [ml] Conditioning No Temperature sensor Manual Stir Speed [%] Time [s] EQP titration Titrant/Sensor Titrant NaOH Concentration [mol/l] Sensor DG111 Unit of meas ph Predispensing No Titrant addition Dynamic de(set) [mv] dv(min) [ml] dv(max) [ml] Measure mode Equilibrium controlled de [mv] dt [s] t(min) [s] t(max) [s] Recognition Threshold Steepest jump only No Range No Tendency Positive Termination at maximum volume [ml] at potential No at slope No after number EQPs Yes n = comb. termination conditions.. No Evaluation Procedure Standard Potential No Potential No Stop for reevaluation No Formula R=Q*C/m Constant C=M/(10*z) Decimal places Result unit % [g/ml] Result name Content Formula R2=Q*C2/m Constant C2=1/z Decimal places Result unit mol/l Result name Concentration Formula R3=VEQ Constant Decimal places Result unit ml Result name Consumption Statistics No Report Output unit Printer Results No All results Yes Raw results No Table of measured values Yes Sample data No E - V curve Yes de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks The unit of measurement of the DG111 electrode is ph. If you switch the unit to mv in the setup data of the sensors, then the threshold for the equivalence point recognition has to be changed in the EQP-TITRATION function to a value of 100 mv/ml. The measuring time can be reduced to approximately 50 % by predispensing to volume 4.5 ml in the function EQP-TITRATION. Sample changer ST20A is used in this method for a fully automatic procedure. The method can easily be modified for manual operation: enter «Stand 1» as titration stand in the function SAMPLE. After each sample, the electrode is rinsed with water by means of a pump connected to the ST20A output «Rinse». Waste disposal Neutralization with hydrochloric acid. Other titrators Method also runs with the following titrators: DL50, DL55, DL58 DL67, DL70ES, DL77 Authors: C. De Caro, A. Sartra Table of measured values Volume Increment Signal Change 1st deriv. Time ml ml ph ph ph/ml min:s ET : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : : :20 EQP : : :19 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 13

14 METTLER TOLEDO Titration Application No. M506 Content of H 2 SO 4 -fast- Sample: 5 ml Sulfuric acid 0.05 mol/l Substance: H 2 SO 4 M = ; z = 2 Preparation: deion. water 50 ml Titrant: Standard: Sodium hydroxide c(naoh) = 0.1 mol/l Potassium hydrogen phthalate Instruments: METTLER TOLEDO DL58 METTLER ST20A Sample changer Printer (HP DeskJet 510) Method: METTLER Method Accessories: Indication: Titration beaker ME Peristaltic pump ME DG111 Results: METTLER TOLEDO DL58 Titrator V2.0 Mettler-Toledo AG 003 Market Support Laboratory Method Content of H 2 SO 4 fast 01-Jan :00 Measured 07-Jan :52 User ALL RESULTS No. ID Sample size and results 1 H 2 SO ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 2 H 2 SO ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 3 H 2 SO ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 4 H 2 SO ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 5 H 2 SO ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 6 H 2 SO ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption Number results R1 n = 6 Mean value x = % [g/ml]content Standard deviation s = % [g/ml]content Rel. standard deviation srel = % Number results R2 n = 6 Mean value x = mol/l Concentration Standard deviation s = mol/l Concentration Rel. standard deviation srel = % Page 14 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

15 Method Content of H 2 SO 4 fast Version 01-Jan :00 Title Method ID Title Content of H 2 SO 4 fast Date/time Jan :00 Sample Sample ID H 2 SO 4 Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand ST20A Pump Yes Solvent H 2 O Volume [ml] Stir No Pump No Rinse Yes Solvent H 2 O Volume [ml] Conditioning No Temperature sensor Manual Stir Speed [%] Time [s] EP titration Titrant/Sensor Titrant NaOH Concentration [mol/l] Sensor DG111 Unit of meas ph Predispensing No Titrant addition Dynamic de(set) [mv] dv(min) [ml] dv(max) [ml] de [mv] dt [s] t(min) [s] t(max) [s] End point EP absolute Potential [mv,ph,..] Tendency Tendency Positive Termination Maximum volume [ml] Delay [s] Formula R=Q*C/m Constant C=M/(10*z) Decimal places Result unit % [g/ml] Result name Content Formula R2=Q*C2/m Constant C2=1/z Decimal places Result unit mol/l Result name Concentration Formula R3=VEQ Constant Decimal places Result unit ml Result name Consumption Statistics No Report Output unit Printer Results No All results Yes Raw results No Table of measured values Yes Sample data No E - V curve Yes de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks The unit of measurement of the DG111 electrode is ph. If you switch the unit to mv in the setup of the sensors, then the end point value has to be changed in the EP-TITRATION function. By performing an end point titration the equivalence point will usually be found below or above the defined end point value. In this method the end point was defined at ph 7.4 since the equivalence point was found to be slightly below this value. Sample changer ST20A is used in this method for a fully automatic analysis procedure. The method can easily be modified for manual operation: enter «Stand 1» as titration stand in the function SAMPLE. After each sample, the electrode is rinsed with water by means of a pump connected to the ST20A output «Rinse». Waste disposal Neutralization with hydrochloric acid. Other titrators Method also runs with the following titrators: DL50, DL53, DL55 DL67, DL70ES, DL77 Author: C. De Caro Table of measured values Volume Increment Signal Change 1st deriv. Time ml ml ph ph ph/ml min:s ET : : : : : : : : : : : : : : : : : : :47 EQP :47 E V curve 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 15

16 METTLER TOLEDO Titration Application No. M507 Content of NaOH -exact- Sample: Substance: Preparation: Titrant: Standard: 5 ml Sodium hydroxide ca. 0.1 mol/l NaOH M = 40 ; z = 1 deion. water 50 ml Hydrochloric acid c(hcl) = 0.1 mol/l Tris(hydroxymethyl) aminomethane (THAM) Instruments: METTLER TOLEDO DL53 METTLER ST20A Sample changer Printer (HP DeskJet 510) Method: METTLER Method Accessories: Titration beaker ME Peristaltic pump ME Results: METTLER TOLEDO DL53 Titrator V1.0 Mettler-Toledo AG 007 Market Support Laboratory Method ph aqu base exact 01-Jul :00 Measured 13-Jul :32 User ALL RESULTS No. ID Sample size and results 1 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 2 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 3 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 4 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 5 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 6 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption Number results R1 n = 6 Mean value x = % [g/ml]content Standard deviation s = % [g/ml]content Rel. standard deviation srel = % Number results R2 n = 6 Mean value x = mol/l Concentration Standard deviation s = mol/l Concentration Rel. standard deviation srel = % Page 16 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

17 Method Method ph aqu base exact Version 01-Jul :00 Title Method ID Title ph aqu base exact Date/time Jul :00 Sample Sample ID NaOH Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand ST20A Pump Yes Solvent H 2 O Volume [ml] Rinse Yes Solvent H 2 O Volume [ml] Conditioning No Temperature sensor Manual Stir Speed [%] Time [s] EQP titration Titrant/Sensor Titrant HCl Concentration [mol/l] Sensor DG111 Unit of meas ph Predispensing No Titrant addition Dynamic de(set) [mv] dv(min) [ml] dv(max) [ml] Measure mode Equilibrium controlled de [mv] dt [s] t(min) [s] t(max) [s] Recognition Threshold Steepest jump only No Range No Tendency Negative Termination at maximum volume [ml] at potential No at slope No after number EQPs Yes n = comb. termination conditions.. No Evaluation Procedure Standard Potential No Potential No Stop for reevaluation No Formula R=Q*C/m Constant C=M/(10*z) Decimal places Result unit % [g/ml] Result name Content Formula R2=Q*C2/m Constant C2=1/z Decimal places Result unit mol/l Result name Concentration Formula R3=VEQ Constant Decimal places Result unit ml Result name Consumption Statistics No Report Output unit Printer Results No All results Yes Raw results No Table of measured values Yes Sample data No E - V curve Yes de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks The unit of measurement of the DG111 electrode is ph. If you switch the unit to mv in the setup data of the sensors, then the threshold value in the EQP-TITRATION function also has to be changed (Threshold: 100 mv/ml). The analysis procedure can be shortened by predispensing in the function EQP titration. Sample changer ST20A is used in this method for a fully automatic procedure. The method can easily be modified for manual operation: enter «Stand 1» as titration stand in the function SAMPLE. After each sample, the electrode is rinsed with water by means of a pump connected to the ST20A output «Rinse». Waste disposal Neutralization with sodium hydroxide. Other titrators Method also runs with the following titrators: DL50, DL55, DL58 DL67, DL70ES, DL77 Authors: C. De Caro, A. Sartra Table of measured values Volume Increment Signal Change 1st deriv. Time ml ml ph ph ph/ml min:s ET : : : : : : : : : : : : : : : : : : : : : : :09 EQP : : :10 E V curve 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 17

18 METTLER TOLEDO Titration Application No. M508 Content of NaOH -fast- Sample: Substance: Preparation: Titrant: Standard: Results: 5 ml Sodium hydroxide ca. 0.1 mol/l NaOH M = 40 ; z = 1 deion. water 50 ml Hydrochloric acid c(hcl) = 0.1 mol/l Tris(hydroxymethyl) aminomethane (THAM) Instruments: METTLER TOLEDO DL58 METTLER ST20A Sample changer Printer (HP DeskJet 510) Method: METTLER Method Accessories: Indication: Titration beaker ME Peristaltic pump ME DG111 METTLER TOLEDO DL58 Titrator V2.0 Mettler-Toledo AG 003 Market Support Laboratory Method Content of NaOH fast 01-Jan :00 Measured 07-Jan :14 User ALL RESULTS No. ID Sample size and results 1 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 2 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 3 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 4 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 5 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption 6 NaOH 5.0 ml R1 = % [g/ml] Content R2 = mol/l Concentration R3 = ml Consumption Number results R1 n = 6 Mean value x = % [g/ml]content Standard deviation s = % [g/ml]content Rel. standard deviation srel = % Number results R2 n = 6 Mean value x = mol/l Concentration Standard deviation s = mol/l Concentration Rel. standard deviation srel = % Page 18 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

19 Method Method Content of NaOH fast Version 01-Jan :00 Title Method ID Title Content of NaOH fast Date/time Jan :00 Sample Sample ID NaOH Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand ST20A Pump Yes Solvent H 2 O Volume [ml] Stir No Pump No Rinse Yes Solvent H 2 O Volume [ml] Conditioning No Temperature sensor Manual Stir Speed [%] Time [s] EP titration Titrant/Sensor Titrant HCl Concentration [mol/l] Sensor DG111 Unit of meas ph Titrant addition Dynamic de(set) [mv] dv(min) [ml] dv(max) [ml] de [mv] dt [s] t(min) [s] t(max) [s] End point EP absolute Potential [mv,ph,..] Tendency Tendency Negative Termination Maximum volume [ml] Delay [s] Formula R=Q*C/m Constant C=M/(10*z) Decimal places Result unit % [g/ml] Result name Content Formula R2=Q*C2/m Constant C2=1/z Decimal places Result unit mol/l Result name Concentration Formula R3=VEQ Constant Decimal places Result unit ml Result name Consumption Statistics No Report Output unit Printer Results No All results Yes Raw results No Table of measured values Yes Sample data No E - V curve Yes de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks The unit of measurement of the DG111 electrode is ph. If you switch the unit to mv in the setup data of the sensors, then the end point value in the EP-TITRATION function also has to be changed. The end point value was fixed at ph 8.2 because in a preliminary titration the equivalence point was found to be close to this value. Sample changer ST20A is used in this method for a fully automatic procedure. The method can easily be modified for manual operation: enter «Stand 1» as titration stand in the function SAMPLE. The electrode is rinsed with water after every titration by means of a pump connected to the output «Rinse» of the ST20A sample changer. The fast completion of this method leads to a slightly higher relative standard deviation compared to the exact method (see statistics). Nevertheless, the accuracy is not affected: the results of both methods and show a very good agreement. Waste disposal Neutralization with sodium hydroxide. Other titrators Method also runs with the following titrators: DL50, DL53, DL55 DL67, DL70ES, DL77 Author: C. De Caro Table of measured values Volume Increment Signal Change 1st deriv. Time ml ml ph ph ph/ml min:s ET : : : : : : : : : : : : : : : :38 EQP :38 E V curve 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 19

20 METTLER TOLEDO Titration Application No. M509 Determination of CuSO 4 with Na 2 S 2 O 3 -exact- Sample: Substance: Results: 2 ml Copper sulfate solution mol/l CuSO 4 5 H 2 O M = ; z = 1 Preparation: 5 ml Potassium iodide (KI) 10% 50 ml Hydrochloric acid (HCl) 0.1 mol/l Titrant: Standard: Sodium thiosulfate c(na 2 S 2 O 3 ) = 0.1 mol/l Potassium iodate METTLER TOLEDO DL55 Titrator V1.0 Mettler Toledo AG 007 Market Support Laboratory Method Redox exact 01-Jul :00 Measured 12-Jul :09 User ALL RESULTS Instruments: METTLER TOLEDO DL55 METTLER ST20A Sample changer Printer (HP DeskJet 510) Method: METTLER Method Accessories: Indication: Titration beaker ME Peristaltic pumps ME DM140 No. ID Sample size and results 1 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 2 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 3 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 4 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 5 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 6 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration Number results R1 n = 6 Mean value x = g/l Content Standard deviation s = g/l Content Rel. standard deviation srel = % Number results R2 n = 6 Mean value x = mg Content Standard deviation s = mg Content Rel. standard deviation srel = % Number results R3 n = 6 Mean value x = mol/l Concentration Standard deviation s = mol/l Concentration Rel. standard deviation srel = % Page 20 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications

21 Method Redox exact Version 01-Jul :00 Title Method ID Title Redox exact Date/time Jul :00 Sample Sample ID CuSO 4.5H 2 O Entry type Fixed volume Volume [ml] Molar mass M Equivalent number z Titration stand ST20A Pump Yes Solvent HCl 0.1 mol/l Volume [ml] Rinse Yes Solvent H 2 O Volume [ml] Conditioning No Temperature sensor Manual Dispense Titrant KI Concentration [mol/l] Volume [ml] Stir Speed [%] Time [s] EQP titration Titrant/Sensor Titrant Na 2 S 2 O 3 Concentration [mol/l] Sensor DM140 Unit of meas mv Predispensing to (factor x sample size) Factor Titrant addition Dynamic de(set) [mv] dv(min) [ml] dv(max) [ml] Measure mode Equilibrium controlled de [mv] dt [s] t(min) [s] t(max) [s] Recognition Threshold Steepest jump only No Range No Tendency Negative Termination at maximum volume [ml] at potential No at slope No after number EQPs Yes n = comb. termination conditions.. No Evaluation Procedure Standard Potential No Potential No Stop for reevaluation No Formula R=Q*C/m Constant C=M/z Decimal places Result unit g/l Result name Content Formula R2=R1*m Constant Decimal places Result unit mg Result name Content Formula R3=Q*C3/m Constant C3=1/z Decimal places Result unit mol/l Result name Concentration Report Output unit Printer Results No All results Yes Raw results No Table of measured values Yes Sample data No E - V curve Yes de/dv - V curve No d2e/dv2 - V curve No log de/dv - V curve No E - t curve No V - t curve No dv/dt - t curve No Remarks CuSO 4 5 H 2 O is used as the sample because of its good solubility in water. 5 ml KI 10% (ca. 0.6 mol/l) are dispensed with the second burette of the DL55 titrator. By means of two pumps, 50 ml hydrochloric acid are added and the electrode is rinsed with water after each titration. The pumps are connected at the ST20A outputs «Rinse» (water) and «Dose» (hydrochloric acid). This method allows a fully automatic analysis procedure. Because of the iodine loss during titration, a slow stirrer speed is applied (30%). The method can easily be modified for manual operation with the DL50 and DL53 titrators: 1) Select «Stand 1» as titration stand; 2) Add 1-2 g potassium iodide; 3) Dissolve with 50 ml hydrochloric acid 0.1 mol/l. Waste disposal Copper solutions have to be classified as special waste. Other titrators Method also runs with the following titrators: DL50, DL53, DL58 DL67, DL70ES, DL77 Authors: C. De Caro, A. Sartra Table of measured values Volume Increment Signal Change 1st deriv. Time ml ml mv mv mv/ml min:s ET : : :22 ET : : : : : : : : : : :39 EQP : : :11 E V curve 30 Selected Applications METTLER TOLEDO DL50 DL53 DL55 DL58 / Page 21

22 METTLER TOLEDO Titration Application No. M510 Determination of CuSO 4 with Na 2 S 2 O 3 -fast- Sample: Substance: Results: 2 ml Copper sulfate solution mol/l CuSO 4 5 H 2 O M = ; z = 1 Preparation: 5 ml Potassium iodide (KI) 10% 50 ml Hydrochloric acid (HCl) 0.1 mol/l Titrant: Standard: Sodium thiosulfate c(na 2 S 2 O 3 ) = 0.1 mol/l Potassium iodate METTLER TOLEDO DL55 Titrator V1.0 Mettler-Toledo AG 007 Market Support Laboratory Method Redox fast 01-Jul :00 Measured 13-Jul :38 User ALL RESULTS Instruments: METTLER TOLEDO DL55 METTLER ST20A Sample changer Printer (HP DeskJet 510) Method: METTLER Method Accessories: Indication: Titration beaker ME Peristaltic pumps ME DM140 No. ID Sample size and results 1 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 2 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 3 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 4 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 5 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration 6 CuSO 4.5H 2 O 2.0 ml R1 = g/l Content R2 = mg Content R3 = mol/l Concentration Number results R1 n = 6 Mean value x = g/l Content Standard deviation s = g/l Content Rel. standard deviation srel = % Number results R2 n = 6 Mean value x = mg Content Standard deviation s = mg Content Rel. standard deviation srel = % Number results R3 n = 6 Mean value x = mol/l Concentration Standard deviation s = mol/l Concentration Rel. standard deviation srel = % Page 22 / METTLER TOLEDO DL50 DL53 DL55 DL58 30 Selected Applications