Senseor For T50

Selected Applications
35
Application Brochure
Excellence Line Titrators
Selected Applications for METTLER TOLEDO Titration Excellence Line
METTLER TOLEDO
Contents
Method M361 Electrode
DGi112-Pro
Title
Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl
Page 1
M362
DGi112-Pro
Buffer Capacity of Coca Cola
M363-A
DGi116-Solvent
Acid Number in Used Motor Oil According to ASTM D664-07
M363-B
DGi116-Solvent
Blank Value of Acid Number Solvent According to ASTM D664-07
10
M363-C
DGi116-Solvent
Blank Value for Strong Acid Number According to ASTM D664-07
13
M363-D
DGi116-Solvent
Buffer Value pH 11 for Acid Number According to ASTM D664-07
16
M363-E
DGi116-Solvent
19
M363-F
DGi116-Solvent
Titer Determination of 0.1 mol/L KOH in 2-Propanol
22
M364-A
DGi116-Solvent
Base Number in Used Motor Oil According to ASTM D4739-06a
25
M364-B
DGi116-Solvent
Blank Value of Base Number Solvent According to ASTM D4739-06a
28
M364-C
DGi116-Solvent
Titer Determination of 0.1 mol/L HCl in 2-Propanol
31
M364-D
DGi116-Solvent
Titer Determination of 0.1 mol/L KOH in 2-Propanol
34
M365
DG117-Water
m-Value of Tap Water with Automatic Temperature Compensation
37
M366
DX202-SC Sb850-S7
Na2O and SiO2 in Waterglass
40
M367
DMi145-SC
Chloride Content in Used Motor Oil
43
METTLER TOLEDO
M368
DMi145-SC Titer Determination of 0.01 mol/L AgNO3 in 2-Propanol
46
M369
DMi147-SC
Peroxide Value of edible Oils and Fats
49
M370
DMi147-SC
Titer Determination of 0.01 mol/L Na2S2O3
52
M371
DMi148-SC
Chloride Determination in Ethanol
55
M372
DMi148-SC
Titer Determination of 0,001 mol/L AgNO3
58
M373
DM405-SC
Mercaptan Sulfur Content in Kerosine According to ASTM D3227-04a
61
M374-A
InLab718
Base Number Determination in Fresh Oils by Conductometric Titration According to IP400-1994
64
M374-B
InLab718
Base Number Determination in Used Oils by Conductometric Titration According to IP400-1994
67
M375
InLab718
Titer Determination of 0.1 mol/L HCl in 2-Propanol by Conductometric Titration
70
M376
DS800 TwoPhase
Anionic Content in Shower Gels by Potentiometric Two-Phase Titration According to DIN EN 14480 Anionic Content in Cutting Oils by Potentiometric Two-Phase Titration According to DIN EN 14480 Titer Determination of 0.004 mol/L Hyamine by Potentiometric Two-Phase Titration According to DIN EN 14480 Acid and Chloride Content in Wine
73
M377
DS800TwoPhase
76
M378
DS800TwoPhase
79
M379
DGi102-Mini DMi102-Mini
81
II
Titration Probes: An Overview
DGi101-SC
DGi102-Mini
DGi111-SC
DGi112-Pro
DGi114-SC
DGi115-SC
DGi117-Water
DGi113-SC
DGi116-Solvent
DG300-SC
Half-Cell pH sensor
DX200
Glass reference sensor
DX202-SC
Plastic reference sensor
III
DMi102-SC
DMi141-SC
DMi145-SC
DMi148-SC
DM405-SC
DMi101-SC
DMi140-SC DMi144-SC
Sensor for Rondo 20 COD set 149.5 mm
DMi147-SC
DM143-SC
Sb850S7/120
IV
InLab717 Conductometric titration Conductivity range:

10 S/cm 500 mS/cm
InLab718 Conductometric titration Conductivity range:

0.1 200 S/cm
DS500 Surfactant Titration Medium:: Aqueous solutions
DS800-TwoPhase Surfactant Titration Medium: Mixed two-phase system (water, MIBK)
pH electrodes for aqueous media

Combined micro pH electrode for direct pH measurements and acid/base titrations in aqueous solutions: Combined semi micro pH electrode for direct pH measurements and acid/base titrations in aqueous solutions For small sample volumes 1) 10-25 mL, suitable for micro-titration beaker ME-23516 2) Automation with Rondo 30 and Rondo 60 plus pH range: 0-14 Temperature range: 0-100C 6 mm shaft Ceramic junction ARGENTHALTM reference system (increased life span and heat resistance) Silver ion trap (avoid precipitation of e.g. silver sulfide at the ceramic frit) U glass bulb For very small sample volumes (min. volume 1 mL) pH range: 0-14 Temperature range: 0-100C 3 mm shaft ceramic junction ARGENTHALTM reference system (increased life span and heat resistance) Silver ion trap (avoid precipitation of e.g. silver sulfide at the ceramic junction) U glass bulb
Product name
Electrolyte 3 mol/L KCl
DGi101-SC
3 mol/L KCl
DGi102-Mini
Combined pH electrode for general direct pH measurements and acid/base titrations: Standard aqueous solutions pH range: 0-14 Temperature range: 0-80C Ceramic junction Ag/AgCl reference element Large U cone glass membrane: Large surface area and low membrane resistance allow for a fast and stable electrode response DGi111-SC
3 mol/L KCl saturated with AgCl
VI
Professional, combined pH electrode with movable sleeve junction for direct pH measurements and acid/base titrations Difficult, aqueous matrices (e.g. suitable to avoid contamination with chloride in water samples with very low chloride content) pH range: 0-14 Temperature range: 0-60C Movable PTFE-sleeve junction ARGENTHALTM reference system Double junction with refillable reference and bridge electrolyte Tubular HA glass membrane with low alkali error DGi112-Pro
Reference electrolyte: 3 mol/L KCl
Bridge electrolyte: selectable (standard delivery : 3 mol/L KCl)
Combined pH electrode for direct pH measurements and acid/base titrations: Dirty aqueous matrices Protein containing samples such as milk and yoghurt Sulfide containing samples (e.g. white and green liquors in pulp and paper industry, tall oil) pH range: 0-14 Temperature range: 0-60C Movable PTFE-sleeve junction ARGENTHALTM reference system Tubular HA glass membrane
3 mol/L KCl
DGi114-SC
Combined pH electrode for direct pH measurements and acid/base titrations: Low ionic strength media (e.g. pure water, organic solvents such as alcohols) pH range: 0-14 Temperature range: 0-100C Fixed ground glass sleeve junction (higher electrolyte flow) ARGENTHALTM reference system Silver ion trap Large tubular HA glass membrane excellent response, stable signal DGi115-SC
3 mol/L KCl
Combined pH electrode and integrated temperature sensor for direct pH measurements and acid/base titrations Simultaneous temperature measurement in aqueous solutions (Integrated Pt1000 T-sensor) Low ionic strength aqueous media (e.g. pure and rain water) pH range: 1-11, temperature range: 0-100C ARGENTHALTM reference system, gold shielding Double junction with 3 M KCl-based reference gel electrolyte Fixed ground glass sleeve junction (higher electrolyte flow) Spherical LoT glass membrane with low resistance DGi117-Water
Bridge electrolyte: 1 mol/L KCl
VII
pH electrodes for non-aqueous media

Combined glass pH electrode for non-aqueous media with moderate electrostatic effects Acid/base titrations in standard organic solvents such as alcohols and acetic acid pH range: 0-12 Temperature range: 0-60C ARGENTHALTM reference system Movable PTFE-sleeve junction Tubular A41 glass membrane with low resistance (Membrane glass with excellent chemical resistance)
Product name
Electrolyte 1 mol/L LiCl in ethanol
DGi113-SC
Combined glass pH electrode for non-aqueous matrices with strong electrostatic effects High performance titrations that require fast response times and quick equilibration of measured values Applications: 1. TAN/TBN determinations in oil products according to oil standards 2. Perchloric acid titrations 3. Cyclohexylamine and alcoholic HCl as titrants 4. Titrations using alcoholic KOH, NaOH, TBAOH and NaMethylate as titrants, 5. Epoxy number in epoxy resins 6. Acid value and numbers (AN) in polymers 7. Free fatty acids (FFA) in oil or fat 8. Saponification number in resins pH range: 0-12 Temperature range: 0-60C Gold shielding for efficient electrical and static shielding ARGENTHALTM reference system Movable glass sleeve junction Spherical A41 glass membrane of low resistance for fast and sensitive pH response and chemical resistance
1 mol/L LiCl in ethanol
DGi116Solvent
Silver ring electrodes

Combined semi micro silver ring electrode for argentometric precipitation titration in aqueous media For small sample volumes: 1) 10-25 mL, suitable for micro-titration beaker ME-23516 2) Automation with Rondo 30 and Rondo 60 plus Determination of e.g. chlorides, bromides, iodides, cyanides and thiocyanides Sulfidation is possible: titration of sulfides, hydrogen sulfides and mercaptans, in particular in petroleum and oil products Temperature range: 0-80C 6 mm shaft Ceramic junction, Ag/AgCl reference system DMi102-SC 1 mol/L KNO3
VIII
Combined silver ring electrode for argentometric precipitation titration in aqueous media Determination of e.g. chlorides, bromides, iodides, cyanides and thiocyanides Sulfidation is possible: argentometric titration of sulfides, hydrogen sulfides and mercaptans Temperature range: 0-80C Ceramic junction Ag/AgCl reference system DMi141-SC
1 mol/L KNO3
Combined silver ring electrode for argentometric precipitation titration in aqueous and non-aqueous media Dirty or viscous samples (e.g. chloride in used oils) Determination of e.g. chlorides, bromides, iodides, cyanides and thiocyanides Low level chloride determinations (e.g. 0.1 ppm Cl- in ethanol) Sulfidation is possible: argentometric titration of sulfides, hydrogen sulfides and mercaptans Temperature range: 0-80C Movable sleeve junction Ag/AgCl reference system DMi145-SC
1 mol/L KNO3
Combined silver ring electrode for argentometric precipitation titration in aqueous and non-aqueous media Without change of the pH value Application examples: 1. Chloride, bromide, iodide and cyanide 2. Chloride, sulfide, hydrogen sulfide, mercaptans in mineral oil 3. Chloride in physiological solutions for dialysis or infusions 4. Chloride in bioethanol Temperature range: 0-80C Junction-free bulb pH glass reference, no electrolyte DMi148-SC
--
Combined Ag2S-sulfidized silver billet electrode for argentometric precipitation titrations Chloride in physiological solutions with low concentration Chloride, bromide, iodide, cyanide and thiocyanides in e.g. electroplating baths Sulfur containing compounds (hydrogen sulfide, mercaptans, sulfides) Temperature range: 0-80C Annular ceramic junction Faster response than bulb pH glass reference of DMi148 DM405-SC
1 mol/L KNO3
IX
Platinum ring electrode

Combined semi micro platinum ring electrode for redox titration in aqueous media For small sample volumes: 1) 10-25 mL, suitable for micro-titration beaker ME-23516 2) Automation with Rondo 30 and Rondo 60 plus Oxidation with potassium permanganate Cerium sulfate (e.g. gold determination) Iodine (e.g. copper determination) Reduction with sodium thiosulfate (back titration reagent for iodometric determinations) Ammonium ferrous sulfate (back titration reagent for a variety of oxidation reactions) Temperature range: 0-80C 6 mm shaft Ceramic junction, Ag/AgCl reference system 3 mol/L KCl saturated with AgCl DMi101-Mini 3 mol/L KCl saturated with AgCl
Combined platinum ring electrode for redox titration in aqueous media Oxidation with potassium permanganate Cerium sulfate (e.g. gold determination) Iodine (e.g. copper determination) Reduction with sodium thiosulfate (back titration reagent for iodometric determinations) Ammonium ferrous sulfate (back titration reagent) Temperature range: 0-80C Ceramic junction Ag/AgCl reference system DMi140-SC
Combined platinum ring electrode for redox titration in aqueous media Dedicated electrode for automatic COD determinations on the Rondo 20 COD rack Temperature range: 0-80C Ceramic junction Ag/AgCl reference system DMi144-SC
3 mol/L KCl saturated with AgCl
Combined platinum ring electrode for redox titrations For very dirty samples and in oils Without change of the pH value Application examples: 1. Chloride, bromide, iodide and cyanide 2. Chloride, sulfide, hydrogen sulfide and mercaptans in mineral oils and petroleum products 3. Chloride in physiological solutions for dialysis or infusions 4. Chloride in bioethanol Temperature range: 0-80C Junction-free bulb pH glass reference, no electrolyte
--
DMi147-SC
Double pin platinum electrode Voltametric titration 1. Karl Fischer titration 2. Vitamin C determination (Voltam. det. with DPI as a titrant) 3. Sulphur dioxide in wine 4. Bromine number and Bromine index (Petroleum products) Amperometric titration 1. Vitamin C determination (Amperom. det. with DPI as a titrant) No junction, no reference electrolyte
--
DM143-SC
Half-cell electrodes
Double junction glass half-cell reference electrode Ion selective measurements with ISE half-cell In combination with pH half cell electrodes in aqueous or non aqueous media In combination with metal half cell electrodes in aqueous or non aqueous media Temperature range: 0-80C pH range: 0-14 Fixed 4 mm banana plug cable Ag/AgCl reference system Movable glass sleeve junction Reference electrolyte: 3 mol/L KCl saturated with AgCl Bridge electrolyte: selectable Standard delivery: 3 mol/L KCl 1 mol/L KNO3 0.9 mol/L Al2(SO4)3 Internal Ag/AgCl reference system (not refillable) Bridge electrolyte: selectable Standard delivery: 3 mol/L KCl 1 mol/L KNO3
DX200
Plastic reference half-cell electrode Especially suitable for applications in hydrofluoric acid containing samples (in combination with Sb850-S7/120 antimony half-cell measuring electrode) Ion selective measurements (in particular, fluoride) In combination with pH or metal half cell electrodes in aqueous media Temperature range: 0-80C pH range: 0-14 S7-screw cap connection Internal Ag/AgCl reference system Porous plastic junction DX202-SC
Half cell pH electrode for direct pH measurements and acid/base titrations for difficult aqueous and non-aqueous matrices in conjunction with reference electrode DX200 Temperature range: 0-100C pH range: 0-13 S7-Screw cap connection DG300-SC
--
XI
METTLER TOLEDO
M361
Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl

Titration Excellence Line: The buffer capacity of the acidic mixture HCl, CH3COOH and NH4Cl and the concentration of each acid was determined by potentiometric titration with the DG112-Pro electrode. Sample
3 mL acidic mixture (1 mL of each acid)
Preparation and Procedures

1) The electrode is calibrated using METTLER TOLEDO pH 4, 7 and 9 buffer solutions. 2) The acidic mixture is prepared by adding 1 mL of each acid solution into the titration beaker. 3) The mixture is diluted with 40 mL deionized water before titration. Since 3 mL acidic mixture is used , the total sample volume is 43 mL. 4) After each sample, the electrode is rinsed with water during 2 s and conditioned during 10 s (Rondolino mode: 6).
Substance Chemicals
Hydrochloric acid (HCl), Acetic acid (HOAc), Ammonium chloride (NH 4Cl), all approx. 0.1 mol/L
40 mL deionized water pH 4, 7 and 9 buffer solutions
Titrant
Sodium hydroxide (NaOH) c(NaOH) = 0.1 mol/L
Standard Instruments
Potassium hydrogen phthalate, 80 mg Titration Excellence Line T70/T90 Rondolino Sample Changer with PowerShowe and pump Titration beaker ME-101974 LabX Titration Software
Accessories
Remarks Indication Chemistry

DGi112-Pro
A mixture of three different acids (HCl, HOAc, NH4Cl) with clearly different pKa values (HCl: -7, HOAc: 4.75, NH4Cl: 9.25) is titrated with 0.1 mol/L NaOH. The buffer capacity is used to describe this complex mixture. Since three EQPs are found three different half neutralization values can be calculated (HNV1HNV3, see titration curve). Three different series (6 samples) have been performed. The statistics of one series is shown below:
R1 R2 R3 R4 R5 R6 R7 R8 HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+2 BETAHNV1+2+3 0.1088 0.08263 0.09374 3.47 1.18667 1.21333 4.65667 5.87 mol/L 0.00143 mol/L 0.00151 mol/L 0.00084 mmol/(L*pH) 0.15824 mmol/(L*pH) 0.00516 mmol/(L*pH) 0.01033 mmol/(L*pH) 0.15908 mmol/(L*pH) 0.15849 1.318 1.827 0.896 4.56 0.435 0.851 3.416 2.7
pH 2.8-5.0: + HCl+NaOH = Na +Cl +H 2O pH 5.0-9.0: + HOAc+NaOH = OAc+Na +H 2O pH 9.0-11.5: NH4Cl+NaOH = Na ++Cl- +NH 3+H 2O R1=Q1*C/1, C=1/z (HCl in mol/L) R2=Q2*C/1, C=1/z (HOAc in mol/L) R3=Q3*C/1, C=1/z (NH 4Cl in mol/L) R4=BETAHNV1, unit: mmol/(L*pH) R5=BETAHNV2, unit: mmol/(L*pH) R6=BETAHNV3, unit: mmol/(L*pH) R7=BETAHNV1+BETAHNV2, unit: mmol/(L*pH) R8=BETAHNV1+BETAHNV2+BETAHNV3, unit: mmol/(L*pH)
Calculation
Results
In the following the mean value range and the srel-range obtained for these three different series are shown:
R1: R2: R3: R4: R5: R6: R7: R8: 0.1081 - 0.10939 0.08263 - 0.08344 0.09374 - 0.09455 3.47 - 3.53833 1.175 - 1.195 1.21333 - 1.225 4.65667 - 4.73333 5.87 - 5.95833 0.7 - 2.4 1.8 - 3.3 0.9 - 1.5 3.0 - 8.8 0.4 - 3.2 0.8 - 3.0 1.7 - 6.2 1.5 - 4.8
Waste Waste disposal disposal
Neutralize the sample before final disposal as aqueous solution
Author
Thomas Hitz
Results
No. 1/6 Comment / ID -Rx R1 R2 R3 R4 R5 R6 R7 R8 R1 R2 R3 R4 R5 R6 R7 R8 R1 R2 R3 R4 R5 R6 R7 R8 R1 R2 R3 R4 R5 R6 R7 R8 R1 R2 R3 R4 R5 R6 R7 R8 R1 R2 R3 R4 R5 R6 R7 R8 = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = Result 0.109 0.07941 0.09244 3.71 1.15 1.19 4.86 6.05 0.10712 0.08107 0.09558 3.52 1.17 1.24 4.69 5.93 0.10798 0.08468 0.09327 3.4 1.26 1.22 4.66 5.88 0.10756 0.08358 0.0955 3.47 1.19 1.21 4.66 5.87 0.10756 0.0863 0.09445 3.53 1.19 1.2 4.72 5.92 0.10886 0.08557 0.09606 3.6 1.21 1.29 4.81 6.1 Unit mol/L mol/L mol/L mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mol/L mol/L mol/L mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mol/L mol/L mol/L mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mol/L mol/L mol/L mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mol/L mol/L mol/L mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mol/L mol/L mol/L mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) Name HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+BETAHNV2 BETAHNV1+BETAHNV2+BETAHNV3 HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+BETAHNV2 BETAHNV1+BETAHNV2+BETAHNV3 HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+BETAHNV2 BETAHNV1+BETAHNV2+BETAHNV3 HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+BETAHNV2 BETAHNV1+BETAHNV2+BETAHNV3 HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+BETAHNV2 BETAHNV1+BETAHNV2+BETAHNV3 HCl HOAc NH4Cl BETAHNV1 BETAHNV2 BETAHNV3 BETAHNV1+BETAHNV2 BETAHNV1+BETAHNV2+BETAHNV3
2/6
--
3/6
--
4/6
--
5/6
--
6/6
--
Table of measured values
Titration curve
HNV1
HNV2
HNV3
Method
Method: User: m361 Buffer Capacity Thomas Hitz 08.01.2008 001 Title Typ Compatible with ID Titel Author Date / Time Modified at Protect SOP 002 Sample Number of IDs ID 1 Entry Type Volume [mL] Density [g/ml] Correction factor Temperature [C] 003 Titration stand (Rondolino TTL) Typ Titration stand 004 Stir Speed Duration Condition 005 Titration (EQP) [1] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed [%] Predispense Mode Wait time [s] Control Control Mode Show parameters Titrant addition dE(set value) dV(min) [mL] dV(max) [mL] Mode dE dt [s] t(min)[s] t(max)[s] Evaluation and recognition Procedure Threshold [pH/mL] Tendency Ranges Add. EQP criteria Buffer capacity Termination At Vmax [mL] At potential At Slope After numbered of recognized EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 006 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 007 Calculation R2 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 008 Calculation R3 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical Send to buffer Condition 009 Calculation R4 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical Send to buffer Condition 010 Calculation R5 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical Send to buffer Condition 011 Calculation R6 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical Send to buffer Condition 012 Calculation R7 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical Send to buffer Condition 013 Calculation R8 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical Send to buffer Condition 014 Record Summary Results Raw results Table of measured Sample data Resource data E - V dE/dV - V log dE/dV - V d2 E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition NH4 Cl mol/L R3=Q3*C/1 1/z M[Ammonium chloride] z[Ammonium chloride] 5 No Yes No No No Buffer capacity HCl mmol/(L*pH) R4=BETAHNV1 1 M[None] z[None] 5 No Yes No No No Buffer capacity HOAc mmol/(L*pH) R5=BETAHNV2 1 M[None] z[None] 5 No Yes No No No Buffer capacity NH4 Cl mmol/(L*pH) R6=BETAHNV3 1 M[None] z[None] 5 No Yes No No No Buffer capacity sum1 mmol/(L*pH) R7=BETAHNV1+BETAHNV2 1 M[None] z[None] 5 No Yes No No No Buffer capacity sum2 mmol/(L*pH) R8=BETAHNV1+BETAHNV2+BETAHNV3 1 M[None] z[None] 5 No Yes No No No No Per sample Per sample No No No Last titration function Last titration function No No Last titration function No No No No No No No No No
General titration T70/T90 m361 Buffer Capacity Thomas Hitz 08.01.2008 08.01.2008 No None 1 -Fixed volume 43 1 1.0 25.0C Rondolino TTL Rondolino TTL 1 50 % 20 s No
functions
functions
NaOH 0.1 pH DG112-SC pH No 30 None 0 Normal Acid/base Yes Dynamic 10 0.005 0.2 Equilibrium controlled 0.5 2.0 3.0 30.0 Standard 1.5 None 0 No Yes 5 No No No No No No HCl mol/L R1=Q1*C/1 1/z M[Hydrochloric acid] z[Hydrochloric acid] 5 No Yes No No No HOAc mol/L R2=Q2*C/1 1/z M[Acetic acid] z[Acetic acid] 5 No Yes No No No
functions
functions
functions
functions
values
METTLER TOLEDO
M362
Buffer Capacity of Coca Cola

Titration Excellence Line: The buffer capacity of Coca Cola is determined by titration with sodium hydroxide
Sample
Coca Cola, 50 mL
Substance Chemicals
Acidic components
- 1 L of Coca Cola is added to an Erlenmeyer flask and degassed by stirring and while heating for 1 hour. - The degassed Coca Cola is stored in a sealed bottle, which is only opened for sample aliquotation.
pH 4, 7 and 9 buffer solutions
Titrant
Sodium hydroxide, NaOH c(NaOH) = 0.1 mol/L
2) 50 mL of degassed Coca Cola are dispensed into a titration beaker. 3) The titration is started. 4) After each sample, the electrode is rinsed with water during 2 s and conditioned during 10 s (Rondolino mode: 6).
Potassium hydrogen phthalate (KHP) Titration Excellence Line T70/T90 Rondolino Sample Changer with PowerShower and pump Olivetti JobJet 210 Printer LabX Titration Software
Accessories

DGi112-Pro
The determination of the buffer capacity represents an alternative way to analyze the general behaviour of e.g. an acid solution. In particular, it can be used to describe complex acid/base mixtures that can be found in electroplating baths, in beverages as well as in saliva. Remarks to the graph: - HNV stands for half neutralization value. - HNV1 indicates the half neutralization value of the 1 EQP (EQP1). - HNV2 indicates the half neutralization value of the second EQP (EQP2). - The dashed line represents the buffer capacity curve (unit: mmol/(L*pH)).
HX + NaOH = NaX + H2O
Calculation
R1 = BETAHNV1 R2 = BETAHNV2 R3 = BETAHNV1+BETAHNV2 Units: mmol/(L*pH)
Results
Neutralization before final disposal as aqueous solution.
Author
Thomas Hitz
Results
No. 1/5 Comment / ID CocaCola Start time 10.09.2007 15:54:43 Rx R1 = R2 = R3 = R1 = R2 = R3 = R1 = R2 = R3 = R1 = R2 = R3 = R1 = R2 = R3 = Result 5.24 3.62 8.86 5.17 3.64 8.81 5.22 3.63 8.85 5.16 3.51 8.67 5.16 3.46 8.62 Unit mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) mmol/(L*pH)
2/5
CocaCola
10.09.2007 16:00:04
3/5
CocaCola
10.09.2007 16:05:15
4/5
CocaCola
10.09.2007 16:10:22
5/5
CocaCola
10.09.2007 16:15:35
Statistics Rx R1 R2 R3 n 5 5 5 Mean value 5.19000 3.57200 8.76200 Unit mmol/(L*pH) mmol/(L*pH) mmol/(L*pH) s 0.03742 0.08167 0.10986 srel[%] 0.721 2.286 1.254
Titration curve
HNV1
HNV2
Method
Method: User: m362 Buffer Capacity Coca Cola Thomas Hitz 10.09.2007 007 Calculation Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 008 Calculation Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 009 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d2E/dV2 - V Beta-V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Calibration curve Method Series data Condition 010 End of sample BufferCapacity mmol/(L*pH) R2 = BETAHNV2 1 M[None] z[None] 5 No Yes No No
001 Title Typ Compatible with ID Titel Author Date / Time Modified at Protect SOP 002 Sample Number of IDs ID 1 Entry Type Volume Density Correction factor Temperature [C]
General titration T50/T70/T90 m362 Buffer Capacity Coca Cola Thomas Hitz 01.09.2007 10.09.2007 No None
1 Coca Cola Fixed volume 50 mL 1.0 g/mL 1.0 25.0
003 Titration stand (Rondolino TTL) Typ Rondolino TTL Titration stand Rondolino TTL 1 004 Stir Speed Duration Condition 005 Titration (EQP) Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed [%] Predispense Mode Wait time [s] Control Control Titrant addition dE (set value) dV (min) dV (max) Mode dE dt [s] t(min) [s] t(max) [s] Evaluation and recognition Procedure Threshold Tendency Ranges Add. EQP criteria Buffer capacity Termination At Vmax At potential At Slope After number of recognized EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 006 Calculation Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions
BufferCapacity mmol/(L*pH) R3 = BETAHNV1+BETAHNV2 1 M[None] z[None] 5 No Yes No No
30 % 10 s No
NaOH 0.1 mol/L pH DG112-SC pH No 30 None 0 User Dynamic 12 0.005 0.5 Equilibrium controlled 0.5 1 3 30 Standard 0.7 pH/mL Positive 0 No Yes 15 mL No No No No No No BufferCapacity mmol/(L*pH) R1 = BETAHNV1 1 M[None] z[None] 5 No Yes No
No Per sample Per sample Last titration Per series No Last titration Last titration No No Last titration No No No No No No No No No No
function
functions functions
function
METTLER TOLEDO
M363-A
Acid Number in Used Motor Oil According to ASTM D664-07

Titration Excellence Line: Method for the determination of the Acid Number (AN) and Strong Acid Number (SAN) in used motor oil by potentiometric titration with potassium hydroxide in 2-propanol according to ASTM D664-07. Sample
Used motor oil, approx. 3 g for AN 5 -10

1) The titer is determined using potassium hydrogen phthalate (KHP): add approx. 80 mg KHP into a glass titration beaker and dissolve it with 60 mL deion. water (See M363-F). 2) The buffer potential 1 (pH 4) and the buffer potential 2 (pH 11) are determined using aqueous pH buffers. These values are stored as auxiliary values H[Buffer pH4] and H[Buffer pH11]. See M363-D (pH 11) and M363-E (pH 4). 3) A blank value is determined for every new batch of solvent mixture and stored as B[ASTM 664 AN] and B[ASTM 664 SAN] See applications M363-B for AN and M363-C for SAN. 4) Depending on the AN of the sample, different sample amounts are requested: AN / mg KOH/g Sample size/g 0.05 - <1.0 20.0 +/- 2.0 1.0 - <5.0 5.0 +/- 0.5 5 - <20 1.0 +/- 0.1 20 - <100 0.25 +/- 0.02 100 - <260 0.1 +/- 0.01 5) After each sample titration the DG116-Solvent electrode is rinsed and conditioned in a chloroform/toluene 1:1 mixture during 5 minutes. Subsequently, it is conditioned in deionized water during additional 5 minutes.
Substance Chemicals
Acid components as mg KOH/g sample, M=56.1 g/mol, z=1 60 mL ASTM D664-07 solvent: Toluene:2-propanol:deion. water 500 mL : 495 mL : 5 mL Potassium hydroxide in 2-propanol KOH, c(KOH) = 0.1 mol/L
Titrant
Potassium hydrogen phthalate, 80 mg Titration Excellence T70/T90 Rondo20 with two membrane pumps LabX Titration Software DV1010 Burette Glass titration beaker ME-101446 XS205 Balance Olivetti JobJet 210 Printer DGi116-Solvent
Accessories
Remarks
1) This application does not replace the ASTM standard. 2) The method parameters have been optimised for the sample used in this application. Thus, it may be necessary to slightly adapt the method to your specific sample. 3) The acid number indicates the amount of base as mg KOH/g sample needed to titrate the acidic constituents in a sample under specific conditions, i.e. specified solvent and endpoint. 4) The sample is titrated using an EQP method function. If no inflection point is detected, endpoints are taken at meter readings corresponding to those found for aqueous acidic and basic buffer solutions for SAN at pH 4 and AN at pH 11 5) Calculations R1 = AN to EQP in mg KOH/g R2 = mmol consumption to buffer potential pH 11 R3 = AN to buffer potential pH 11 in mg KOH/g R4 = mmol consumption to buffer potential pH 4 R5 = SAN to buffer potential pH 4 in mg KOH/g Literature: - ASTM D664-07, see www.astm.org - METTLER TOLEDO Appl. brochure 34, ME-51 725 066 - METTLER TOLEDO Appl. brochure 20, ME-51 725 020
Indication Chemistry
KOH + HA = KA + H2O HA: Acid components
Calculation
Results
R1= (Q-B[ASTM 664 AN])*C/m C = M/z R2= QE(H[Buffer pH11]) R3= (R2-B[ASTM 664 AN])*C/m C = M/z R4 = QE(H[Buffer pH4]) R5= (R4+B[ASTM 664 SAN])*C/m C = M/z Dispose as aromatic organic solvent (toluene)
Author
Albert Aichert
Results
Summary Sample No. ID 1 Used oil Method-ID Sample size and 3.04742 g R1 (TAN EQP) R2 (Consumption R3 (TAN BP) R4 (Consumption R5 (SAN BP) 3.31062 g R1 (TAN EQP) R2 (Consumption R3 (TAN BP) R4 (Consumption R5 (SAN BP) 3.27543 g R1 (TAN EQP) R2 (Consumption R3 (TAN BP) R4 (Consumption R5 (SAN BP) 3.09854 g R1 (TAN EQP) R2 (Consumption R3 (TAN BP) R4 (Consumption R5 (SAN BP) 3.16791 g R1 (TAN EQP) R2 (Consumption R3 (TAN BP) R4 (Consumption R5 (SAN BP) 3.27816 g R1 (TAN EQP) R2 (Consumption R3 (TAN BP) R4 (Consumption R5 (SAN BP) m363A results ----0.376 6.849 0.011 0.312 ----0.405 6.796 0.015 0.355 ----0.402 6.817 0.015 0.359 ----0.381 6.826 0.015 0.379 ----0.388 6.801 0.016 0.389 ----0.401 6.794 0.015 0.358 mg KOH/g mmol mg KOH/g mmol mg KOH/g mg KOH/g mmol mg KOH/g mmol mg KOH/g mg KOH/g mmol mg KOH/g mmol mg KOH/g mg KOH/g mmol mg KOH/g mmol mg KOH/g mg KOH/g mmol mg KOH/g mmol mg KOH/g mg KOH/g mmol mg KOH/g mmol mg KOH/g
BP) SAN)
Used oil
BP) SAN)
Used oil
BP) SAN)
Used oil
BP) SAN)
Used oil
BP) SAN)
Used oil
BP) SAN)
Statistics R3 Samples Mean s srel R5 Samples Mean s srel TAN BP 6 6.814 0.021311 0.313 SAN BP 6 0.359 0.026553 7.403
mg KOH/g mg KOH/g %
mg KOH/g mg KOH/g %

Volume mL 0 0.05 0.1 0.153 0.214 0.278 0.337 0.4 0.46 0.521 0.578 0.639 0.692 0.754 0.806 0.865 0.916 0.972 1.023 1.08 1.144 1.204 1.266 1.336 1.399 1.476 1.538 1.616 1.693 1.764 1.844 1.914 1.987 2.08 2.149 2.232 2.334 2.4 2.484 2.57 2.67 2.75 2.86 2.952 3.059 3.164 3.257 3.39 3.488 3.614 3.717 3.845 3.957 4.098 4.21 4.39 4.536 4.686 4.886 5.051 5.251 5.451 5.651 5.851 6.051 6.251 6.451 6.651 6.851 7.051 Increment Signal Change mL mV mV NaN 187 NaN 0.05 181.1 -5.9 0.05 174.4 -6.7 0.053 167.3 -7.1 0.061 159.5 -7.8 0.064 151 -8.5 0.059 143.4 -7.6 0.063 135 -8.4 0.06 127.3 -7.7 0.061 118.9 -8.4 0.057 111.3 -7.6 0.061 102.6 -8.7 0.053 95.5 -7.1 0.062 86.5 -9 0.052 79.2 -7.3 0.059 70.5 -8.7 0.051 63 -7.5 0.056 54.7 -8.3 0.051 47.2 -7.5 0.057 39.5 -7.7 0.064 30.8 -8.7 0.06 23 -7.8 0.062 15.4 -7.6 0.07 6.7 -8.7 0.063 -0.6 -7.3 0.077 -9.8 -9.2 0.062 -16.7 -6.9 0.078 -25.2 -8.5 0.077 -33.6 -8.4 0.071 -41.1 -7.5 0.08 -49.8 -8.7 0.07 -57.5 -7.7 0.073 -64.6 -7.1 0.093 -74.3 -9.7 0.069 -81.4 -7.1 0.083 -88.7 -7.3 0.102 -99.4 -10.7 0.066 -105.9 -6.5 0.084 -114 -8.1 0.086 -121.5 -7.5 0.1 -131 -9.5 0.08 -137.5 -6.5 0.11 -146.8 -9.3 0.092 -154.2 -7.4 0.107 -162.5 -8.3 0.105 -171.1 -8.6 0.093 -177.6 -6.5 0.133 -187.7 -10.1 0.098 -194.5 -6.8 0.126 -203.7 -9.2 0.103 -210.7 -7 0.128 -219.5 -8.8 0.112 -226.6 -7.1 0.141 -236.1 -9.5 0.112 -242.2 -6.1 0.18 -252 -9.8 0.146 -259.9 -7.9 0.15 -266.7 -6.8 0.2 -276 -9.3 0.165 -282.3 -6.3 0.2 -289.7 -7.4 0.2 -295.5 -5.8 0.2 -301.3 -5.8 0.2 -306.1 -4.8 0.2 -310.4 -4.3 0.2 -314.3 -3.9 0.2 -317.7 -3.4 0.2 -320.9 -3.2 0.2 -323.6 -2.7 0.2 -326.2 -2.6 1st deriv. Time Temperature mV/mL s C NaN 0 25 NaN 5 25 NaN 10 25 NaN 15 25 NaN 20 25 -131.19 25 25 -130.39 30 25 -131.91 36 25 -133.33 41 25 -135.08 46 25 -137.04 51 25 -138.96 56 25 -140.91 61 25 -142.71 66 25 -145.46 71 25 -146.73 76 25 -147.09 81 25 -145.08 86 25 -141.58 91 25 -137.1 97 25 -131.48 102 25 -127.32 108 25 -124.03 114 25 -120.47 119 25 -117.37 124 25 -113.94 130 25 -111.36 136 25 -109.72 142 25 -108.28 147 25 -106.87 152 25 -106.95 157 25 -104.32 163 25 -102.22 169 25 -100.26 174 25 -99.8 179 25 -98.69 184 25 -97.91 189 25 -96.27 194 25 -94.33 200 25 -91.47 205 25 -86.83 210 25 -85.12 215 25 -82.14 220 25 -80.26 225 25 -77.69 230 25 -76.36 235 25 -74.67 240 25 -73.03 245 25 -71.37 250 25 -70.21 255 25 -69.31 260 25 -66.44 266 25 -64.23 271 25 -60.27 276 25 -57.67 282 25 -53.15 288 25 -49.99 294 25 -46.27 300 25 -41.8 305 25 -37.81 310 25 -33.28 315 25 -29.4 320 25 -25.75 325 25 -23 330 25 -20.38 336 25 NaN 341 25 NaN 346 25 NaN 351 25 NaN 356 25 NaN 361 25
Titration curve
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Lower limit Upper limit Density Correction factor Temperature Entry 1 Used oil Weight 1.0 g 10.0 g 1.0 g/mL 1.0 25.0C Arbitrary General titration T70 / T90 m363 SAN & AN ASTM D664 Albert Aichert 29.01.2008 10:12:42 --No None m363 SAN & AN ASTM D664 Albert Aichert 29.01.2008 008 Conditioning Type Interval Position Time Speed Condition 009 Calculation R1 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 010 Calculation R2 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 011 Calculation R3 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 012 Calculation R4 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 013 Calculation R5 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 014 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition 015 End of sample 016 Park Titration stand Position Condition 017 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition Rondo60/1A Conditioning beaker No Yes No No No No No No Fix 1 Conditioning beaker 300 s 30 % no TAN (EQP) mg KOH/g R1=(Q-B[ASTM 664 AN])*C/m z/M M[Potassium hydroxid] z[Potassium hydroxid] 3 No Yes No No No Consumption EP mmol R2=QE(H[Buffer pH11]) 1 M[none] z[none] 3 No No No No No TAN (BP) mg KOH/g R3=(R2-B[ASTM 664 AN])*C/m z/M M[Potassium hydroxid] z[Potassium hydroxid] 3 No Yes No No No Consumption SAN mmol R4=QE(H[Buffer pH4]) 1 M[none] z[none] 3 No No No No No SAN (BP) mg KOH/g R5=(R4+B[ASTM 664 SAN])*C/m z/M M[Potassium hydroxid] z[Potassium hydroxid] 3 No Yes No No No No Per sample Per sample No Last titration function Last titration function No
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Pump Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Predispense Mode Wait time Control Control Titrant addition dE(set value) dV(min) dV(max) Meas. value acquisition dE dt t(min) t(max) Evaluation and recognition Procedure Threshold Tendency Ranges Lower limit Upper limit Add. EQP criteria Termination At Vmax At potential Potential Termination tendency At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 007 Conditioning Type Interval Position Time Speed Condition 35 % 60 s No ASTM 664 solvent 60 mL No
KOH in 2-Propanol 0.1 mol/L pH DG116-SC mV No 30 % None 0 s User Dynamic 8.0 mV 0.05 mL 0.2 mL Equilibrium controlled 0.5 mV 1 s 5 s 60 s Standard 150 mV/mL None 1 -400.0 mV 0.0 mV No 15.0 mL Yes H[Buffer pH11]-100 mV None No No No No No No
Fix 1 Special beaker 1 180 s 100 % no
METTLER TOLEDO
M363-B
Blank Value for Acid Number According to ASTM D664-07

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

1) Use the empty beaker for the blank determination. Add the solvent by means of the first membrane pump of Rondo 20. 2) For the blank determination, an EQP titration is used and the result is calculated at the potential value obtained for pH 11 buffer, i.e. QE(H[Buffer pH11]). This value was previously determined with application M363-D and stored as auxiliary value H[Buffer pH11]. 3) Finally, the result QE(H[Buffer pH11]) in mmol is stored as blank value B[ASTM 664 AN]
Substance Chemicals
--
Titrant
Potassium hydroxide in 2-propanol KOH, c(KOH) = 0.1 mol/L
Potassium hydrogen phthalate, 80 mg Titration Excellence T50/T70/T90 Rondo20 with two membrane pumps LabX Titration Software DV1010 Burette Glass titration beaker ME-101446 XS205 Balance Olivetti JobJet 210 Printer DGi116-Solvent
Accessories
Remarks
1) This application does not replace the ASTM standard. 2) The method parameters have been optimised for the sample used in this application. Thus, it may be necessary to slightly adapt the method to your specific sample. 3) The titrant has to be protected against the uptake of CO2 from the air. NaOH on carrier (e.g. "Sodium hydroxide on support", MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKA Nr. 03350) is an effective medium to avoid such formation of carbonate. Literature: - ASTM D664-07, see www.astm.org - METTLER TOLEDO Appl. brochure 34, ME-51 725 066 - METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Calculation
R1= QE(H[Buffer pH11])
Results
Dispose as aromatic organic solvent (toluene)
Author
Albert Aichert
10
Results
Method-ID T202 Summary Sample No. ID Sample size and results 1 Solvent 664 60 mL R1 (Blank pH11) 0.003970 2 Solvent 664 60 mL R1 (Blank pH11) 0.003941 3 Solvent 664 60 mL R1 (Blank pH11) 0.004210 Statistics R1 Blank pH11 Samples 3 Mean 0.004040 mmol s 0.000148 mg KOH/g srel 3.654 %

Volume mL 0 0.002 0.004 0.009 0.019 0.029 0.039 0.044 Increment Signal Change 1st deriv. mL mV mV mV/mL NaN -189.2 NaN NaN 0.002 -177.9 11.3 NaN 0.002 -171.9 6 NaN 0.005 -169 2.9 NaN 0.01 -168.7 0.3 NaN 0.01 -172.8 -4.1 NaN 0.01 -189.4 -16.6 NaN 0.005 -256.5 -67.1 NaN Time s 0 10 20 31 41 52 62 87 Temperature C 25 25 25 25 25 25 25 25
Titration curve
11
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Volume Density Correction factor Temperature Entry General titration T50 / T70 / T90 T202 Blank AN pH11 ASTM D664 Albert Aichert 07.12.2007 10:12:42 --No None T202 Blank AN pH11 ASTM D664 Albert Aichert 07.12.2007 008 Calculation R1 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 009 Blank Name Value B= Unit Limits Condition 010 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition 011 End of sample 012 Park Titration stand Position Condition 013 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition Rondo60/1A Conditioning beaker No Yes No No No No No No Blank pH11 mmol R1=QE(H[Buffer pH11]) 1 M[None] z[None] 6 No Yes No No No ASTM 664 AN Mean[R1] mmol No No No Per sample Per sample No Last titration function Last titration function No
1 Solvent 664 Fixed volume 60 mL 1.0 g/mL 1.0 25.0C Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Pump Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Predispense Mode Wait time Control Control Titrant addition dE(set value) dV(min) dV(max) Meas. value acquisition dE dt t(min) t(max) Evaluation and recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential Potential Termination tendency At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 007 Rinse Auxiliary reagent Rinse cycles Vol. per cycle Position Drain Condition 35 % 60 s No ASTM 664 solvent 60 mL No
KOH in 2-Propanol 0.1 mol/L pH DG116-SC mV No 30 % None 0 s User Dynamic 12.0 mV 0.002 mL 0.01 mL Equilibrium controlled 0.5 mV 1 s 10 s 60 s Standard 200 mV/mL Negative 0 No 15.0 mL Yes H[Buffer pH11]-30 mV None No No No No No No ASTM 664 solvent 1 15 mL Actual sample No No
12
METTLER TOLEDO
M363-C
Blank Value for Strong Acid Number According to ASTM D664-07

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

1) Use the empty beaker for the blank determinaton. Add the solvent by means of the first membrane pump of Rondo 20. 2) For the blank determination, an EQP titration is used and the result is calculated at the potential value obtained for pH 4 buffer, i.e. QE(H[Buffer pH4]). This value was previously determined with application M363-E and stored as auxiliary value H[Buffer pH4] 3) Finally, the result QE(H[Buffer pH4]) in mmol is stored as blank value B[ASTM 664 SAN].
Substance Chemicals
--
Titrant
Hydrochloric acid in 2-Propanol HCl, c(HCl) = 0.1 mol/L
Tris-(hydroxymethyl)-aminomethane, 80 mg
Titration Excellence T50/T70/T90 Rondo20 with two membrane pumps LabX Titration Software DV1010 Burette Glass titration beaker ME-101446 XS205 Balance Olivetti JobJet 210 Printer DGi116-Solvent
Accessories
Remarks
1) This application does not replace the ASTM standard. 2) The method parameters have been optimised for the sample used in this application. Thus, it may be necessary to slightly adapt the method to your specific sample.
Calculation
R1= QE(H[Buffer pH4])
Literature: - ASTM D664-07, see www.astm.org - METTLER TOLEDO Appl. brochure 34, ME-51 725 066 - METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Results
Dispose as aromatic organic solvent (toluene)
Author
Albert Aichert
13
Results
Method-ID T212 Summary Sample No. ID Sample size and results 1 solvent 664 60 mL R1 (Blank pH4) 0.006157 2 solvent 664 60 mL R1 (Blank pH4) 0.005933 3 solvent 664 60 mL R1 (Blank pH4) 0.005929 4 solvent 664 60 mL R1 (Blank pH4) 0.005733 Statistics R1 Blank pH4 Samples 4 Mean 0.005938 mmol s 0.000173 mg KOH/g srel 2.918 %

Volume mL 0 0.002 0.004 0.008 0.016 0.026 0.036 0.046 0.054 0.06 0.062 0.064 0.066 0.068 Increment Signal Change 1st deriv. Time mL mV mV mV/mL s NaN 44.5 NaN NaN 0.002 67.8 23.3 NaN 0.002 80 12.2 NaN 0.004 92.6 12.6 NaN 0.008 107.1 14.5 NaN 0.01 120.8 13.7 997.3 0.01 133.2 12.4 1010.34 0.01 146.5 13.3 1673.72 0.008 161.2 14.7 2863.48 0.006 175.6 14.4 NaN 0.002 187.1 11.5 NaN 0.002 197.4 10.3 NaN 0.002 210.7 13.3 NaN 0.002 227.6 16.9 NaN 0 10 20 30 41 51 62 72 82 92 103 113 124 134 Temperature C 25 25 25 25 25 25 25 25 25 25 25 25 25 25
Titration curve
14
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Volume Density Correction factor Temperature Entry General titration T50 / T70 / T90 T212 Blank SAN pH4 ASTM D664 Albert Aichert 17.01.2008 10:12:42 --No None T212 Blank SAN pH4 ASTM D664 Albert Aichert 17.01.2008 008 Calculation R1 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 009 Blank Name Value B= Unit Limits Condition 010 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition 011 End of sample 012 Park Titration stand Position Condition 013 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition Rondo60/1A Conditioning beaker No Yes No No No No No No Blank pH4 mmol R1=QE(H[Buffer pH4]) 1 M[None] z[None] 6 No Yes No No No ASTM 664 SAN Mean[R1] mmol No No No Per sample Per sample No Last titration function Last titration function No
1 Solvent 664 Fixed volume 60 mL 1.0 g/mL 1.0 25.0C Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Pump Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Predispense Mode Wait time Control Control Titrant addition dE(set value) dV(min) dV(max) Meas. value acquisition dE dt t(min) t(max) Evaluation and recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential Potential Termination tendency At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 007 Rinse Auxiliary reagent Rinse cycles Vol. per cycle Position Drain Condition ASTM 664 solvent 1 15 mL Actual sample No No 35 % 60 s No ASTM 664 solvent 60 mL No
HCl in 2-propanol 0.1 mol/L pH DG116-SC mV No 30 % None 0 s User Dynamic 12.0 mV 0.002 mL 0.01 mL Equilibrium controlled 0.5 mV 1 s 10 s 60 s Standard 200 mV/mL Positive 0 No 15.0 mL Yes H[Buffer pH4]+50 mV None No No No No No No
15
METTLER TOLEDO
M363-D

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

1) Always use fresh pH 11 buffer solution. The buffer pH 11 is not stable when exposed to air.
Substance Chemicals
--
2) 50 mL pH 11 buffer solution are added into a titration beaker. 3) Before measure the buffer potential, the electrode should conditioned in aquous media (water pH 5-6) for 3 - 5 minutes. 4) The measured potential value for buffer pH 11 is stored as auxilliary value H[Buffer pH11].
--
Titrant
--
5) Finally, the electrode is parked in the condioning beaker containing slightly acidic water (pH 5-6).
-Titration Excellence T50/T70/T90 Rondo20 with two membrane pumps LabX Titration Software DV1010 Burette Glass titration beaker ME-101446 XS205 Balance Olivetti JobJet 210 Printer DGi116-Solvent
Accessories
Remarks
1) This application does not replace the ASTM standard. 2) The buffer pH 11 is not stable when exposed to air. In fact, due to the high alkaline pH value, the absorption of CO2 from the air is strongly improved. For instance, the potential value (mV) in an open beaker with buffer pH 11.can change of 0.1 mV/min The potential value of an opened bottle of pH 11 buffer solution can rapidly change. Thus, it is very important to use fresh pH 11 buffer solution every time a new value has to be determined
--
Calculation
R1= E
Results
Neutralize before final disposal as queous solution.
Author
Albert Aichert
16
Results
Method-ID Data / Time T102 07.01.2008 03:12:05 pm
All results Sample 1/1 R1(Buffer pH11)
Buffer pH11 -222.400 mV
Titration curve
17
Method
Method Author 001 Title Type Compatible with ID Title D664 Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Volume Density Correction factor Temperature Entry Albert Aichert 17.12.2007 10:12:42 --No None General titration T50 / T70 / T90 T102 Buffer value AN pH11 ASTM T102 Buffer value AN pH11 ASTM D664 Albert Aichert 17.12.2007
1 Buffer pH11 Fixed volume 50 mL 1.0 g/mL 1.0 25.0C Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Stir Speed Duration Condition 005 Measure (normal) [1] Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Acquisition of the measured Acquisition Time Mean value t(min) t(max) Condition Condition 006 Calculation R1 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 007 Auxiliary value Name Value B= Unit Limits Condition 008 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition 009 End of sample 010 Park Titration stand Position Condition Rondo60/1A Conditioning beaker No 35 % 300 s No
pH DG116-SC mV No 30 % value Fix 30 s No 10 s 60 s No
Buffer pH11 mV R1=E 1 M[None] z[None] 3 No No No No No
Buffer pH11 R1 mV No No
No Per sample Per sample No No No No
18
METTLER TOLEDO
M363-E
Buffer Value pH4 for Strong Acid Number According to ASTM D664-07
Titration Excellence Line: Determination of the potential value for pH 4 buffer (SAN, Strong Acid Number) acccording to ASTM D 664-07. Sample
50 mL pH 4 buffer solution

1) Always use fresh pH 4 buffer solution. 2) 50 mL pH 4 buffer solution are added into a titration beaker.
Substance Chemicals
--
3) Before measure the buffer potential, the electrode should conditioned in aquous media (water pH 5-6) for 3 - 5 minutes. 4) The measured potential value for buffer pH 4 is stored as auxilliary value H[Buffer pH4]. 5) Finally, the electrode is parked in the condioning beaker containing slightly acidic water (pH 5-6).
--
Titrant
--
-Titration Excellence T50/T70/T90 Rondo20 with two membrane pumps LabX Titration Software DV1010 Burette Glass titration beaker ME-101446 XS205 Balance Olivetti JobJet 210 Printer DGi116-Solvent
Accessories
Remarks
1) This application does not replace the ASTM standard. 2) Before measure the buffer potential, the electrode should conditioned in aqueous media (water pH 5-6) for 3 - 5 minutes.
--
Calculation
R1= E
Results
Neutralize before final disposal as queous solution.
Author
Albert Aichert
19
Results
Method-ID Data / Time T112 17.01.2008 11:12:05 pm
All results Sample 1/1 R1(Buffer pH4)
Buffer pH4 169.200 mV
Titration curve
20
Method
Method Author 001 Title Type Compatible with ID Title D664 Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Volume Density Correction factor Temperature Entry Albert Aichert 16.01.2008 10:12:42 --No None General titration T70 / T90 T112 Buffer value SAN pH4 ASTM T112 Buffer value SAN pH4 ASTM D664 Albert Aichert 16.01.2008
1 Buffer pH4 Fixed volume 50 mL 1.0 g/mL 1.0 25.0C Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Stir Speed Duration Condition 005 Measure (normal) [1] Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Acquisition of the measured Acquisition Time Mean value t(min) t(max) Condition Condition 006 Calculation R1 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 007 Auxiliary value Name Value B= Unit Limits Condition 008 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition 009 End of sample 010 Park Titration stand Position Condition Rondo60/1A Conditioning beaker No 35 % 300 s No
pH DG116-SC mV No 30 % value Fix 30 s No 10 s 60 s No
Buffer pH4 mV R1=E 1 M[None] z[None] 3 No No No No No
Buffer pH4 R1 mV No No
No Per sample Per sample No No No No
21
METTLER TOLEDO
M363-F
Titer Determination of 0.1 mol/L KOH in 2-Propanol (ASTM D664-07)

Titration Excellence Line: Method for the titer determination of 0.1 mol/L KOH in 2-Propanol according to ASTM D664-07. Sample
Primary standard Potassium hydrogen phthalate, 70 - 100 mg Potassium hydrogen phthalate M=204.23 g/mol z=1 50 mL CO 2-free, deionized water

1) Weigh the primary standard into the glass titration beaker to avoid electrostatic influence. 2) Add 50 mL CO 2-free deionized water to dissolve the sample. 3) After each sample titration, the eelctrode is rinsed with water 4) At the end of the titration, the electrode is parked in the condioning beaker containing slightly acidic water (pH 5-6).
Substance Chemicals
Titrant
Potassium hydroxide in 2-propanol KOH, c(KOH) = 0.1 mol/L
Potassium hydrogen phthalate, 80 mg Titration Excellence T50/T70/T90 Rondo20 with two membrane pumps LabX Titration Software DV1010 Burette Glass titration beaker ME-101446 XS205 Balance Olivetti JobJet 210 Printer DGi116-Solvent
Accessories
Remarks
1) This application does not replace the ASTM standard. 2) The titrant has to be protected against the uptake of CO2 from the air. NaOH on carrier (e.g. "Sodium hydroxide on support", MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKA Nr. 03350) is an effective medium to avoid such formation of carbonate.
KOH + K2HPO3 = H2O + 3K+ + PO43-
Calculation
R1= m/(VEQ*c*C) C=(10*p*z) p: purity of standard
Results
Neutralize before final disposal as aqueous solution.
Author
Albert Aichert
22
Results
Summary Method-ID T001
Sample No. 1 2 3 4
ID KHP KHP KHP KHP
Sample size and results 0.11936 g R1 (Titer) 0.961720 0.12372 g R1 (Titer) 0.961095 0.11054 g R1 (Titer) 0.960251 0.11502 g R1 (Titer) 0.960945
Statistics R1 Samples Mean s srel Titer Titrant New titer
Titer 4 0.961003 0.000603 0.063 %
KOH in 2-Propanol 0.96100
Titration curve
23
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample (Titer) Titrant Concentration Standard Type of standard Entry type Lower limit Upper limit Density Correction factor Temperature Entry General titration T50 / T70 / T90 m363F Titer of KOH in 2-propanol Albert Aichert 02.10.2007 10:51:42 --No None m363F Titer of KOH in 2-propanol Albert Aichert 02.10.2007 008 Calculation R1 Result Result unit Formula Constant C M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 009 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition 010 End of sample 011 Titer Titrant Concentration TITER= Limits Condition 012 Park Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Predispense Mode Volume Wait time Control Control Titrant addition dE(set value) dV(min) dV(max) Meas. value acquisition dE dt t(min) t(max) Evaluation and recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential Tendency At slope After number of recognized EQPs Number of EQP's Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 007 Rinse Auxiliary reagent Rinse cycles Vol. per cycle Position Drain Condition Water 1 15 mL Actual sample No No 60 % 60 s No 013 Record Summary Results Raw results Table of meas. value E - V dE/dV - V Condition Yes No No No No No No Water 60 mL No Titration stand Position Condition Rondo60/1A Conditioning beaker No KOH in 2-Propanol 0.1 mol/L Mean[R1] No No Titer -R1=(m/(VEQ*c*C) M/(10*p*z) M[Potassium hydroxid] z[Potassium hydroxid] 6 No Yes No No No
KOH in 2-Propanol 0.1 mol/L KHP solid Weight 0.07 g 0.12 g 1.0 g/mL 1.0 25.0C Arbitrary
No Per sample Per sample No Last titration function Last titration function No
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Pump
KOH in 2-Propanol 0.1 mol/L pH DG116-SC mV No 30 % Volume 1.0 mL 5 s User Dynamic 8.0 mV 0.005 mL 0.5 mL Equilibrium controlled 1.0 mV 1 s 3 s 60 s Standard 3.0 pH/mL Positive 0 No 10.0 mL No None No Yes 1 No No No No
24
METTLER TOLEDO
M364-A
Base Number in Used Motor Oil According to ASTM D4739-06a

Titration Excellence Line: Method for the determination of the base number (BN) in oil by titration with hydrochloric acid in 2-propanol according to ASTM D4739-06a. Sample
Used Motor oil, ~2.5 g

1) Solvent preparation: ASTM D4739-06a solvent is prepared by mixing 2-propanol, toluene, chloroform and water in the following ratio: 10:10:10:0.3 (v/v).
Substance Chemicals
Alkaline components in oil expressed as KOH, M=56.1 g/mol , z=1 60 mL ASTM D4739-06a solvent (see Preparation and Procedures) pH 3 and pH 10 buffer solutions HCl in 2-propanol, c(HCl)=0.1 mol/L KOH in 2-propanol, c(HCl)=0.1 mol/L
2) The titer is determined by titration of previously standardized KOH in 2-propanol solution. The latter has been standardized using potassium hydrogen phthalate (KHP), see M364-D. 3) The acidic (pH 3) and the alkaline (pH 10) aqueous buffer potentials are measured and stored as auxiliary values pH 3 (H [Buffer pH3] ) and ( H[Buffer pH10] ). 4) Blank values for the base number (BN) are determined for every new batch of solvent mixture by titration with HCl in 2propanol to the buffer pH 3 potential. For strong base number (SBN), the solvent is titrated with KOH in 2-propanol to pH 10 pot. value. The result is stored as blank value ASTM D4739 (M364-B). 5) Add the oil sample into the titration beaker. The appropriate sample size is calculated according to the following formula: sample size (g) = 7/expected BN 6) 60 mL ASTM D4739-06a solvent are added using an additional dosing unit. This step can be performed manually using a dispenser or a graduated cylinder.
Titrant
KOH in 2-propanol 0.1 mol/L / KHP Titration Excellence T70/T90 Rondo 20 Sample changer 1 additional dosing unit (20 mL) DV1010 and DV1020 Burettes Titration beakers ME-101974 XS205 Balance, SP250 pump PC with LabX Software DGi116-Solvent
Accessories
Remarks
This method allows a fully automated procedure using a sample changer and an additional dosing unit. It can be modified for manual operation. Select "Manual stand" in the method function "Titration stand". 1) This application does not replace the ASTM standard. The method parameters have been optimised for the sample used in this application. Thus, it may be necessary to slightly adapt the method to your specific sample. 2) The base number BN is defined as the consumption of hydrochloric acid to a specific endpoint to neutralize the alkaline components of the oil. It is expressed as mg KOH/g sample: - If an EQP is found between the acidic buffer potential value and a point 100 mV past this potential, then this will be the BN. - If no EQP is found in this region, then the result is evaluated at the potential value of the acidic buffer. 3) Between each sample it is necessary to condition the electrode under stirring during 300 s in deion. water. The electrode is parked in buffer pH 4 (Rinse beaker). Literature: 1) ASTM D4739-06a and draft next version, see www.astm.org 2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066. 3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
HCl + KOH = Cl - + K+ + H 2O KOH represents the alkaline components.
Calculation
Base number mg KOH/g: R1=(Q-B[ASTM D4739])*C/m C=M/z Base number mg KOH/g at acidic potential:
R2=(QE(H[Buffer pH3])-B[ASTM D4739])*C/m
C=M/z
Results
Dispose of as halogenated organic waste
Author
Melanie Nijman
25
Results
Mettler Toledo T90 Titrator Mettler Toledo AG Market Support Laboratory 17.01.2008
Method
M364_A
Base Number According to ASTM D4739-06a
RESULTS with DG116-Solvent electrode No. ID Sample size and results 1 Used Motor Oil 2.54656 g R1 = 3.50 mg KOH/g R2 = 1.87 mg KOH/g 2 Used Motor Oil 2.67162 g R1 = 3.48 mg KOH/g R2 = 1.80 mg KOH/g 3 Used Motor Oil 2.48459 g R1 = 3.46 mg KOH/g R2 = 1.80 mg KOH/g 4 Used Motor Oil 2.54055 g R1 = 3.49 mg KOH/g R2 = 1.84 mg KOH/g 5 Used Motor Oil 2.4121 g R1 = 3.45 mg KOH/g R2 = 1.81 mg KOH/g 6 Used Motor Oil 2.53271 g R1 = 3.44 mg KOH/g R2 = 1.83 mg KOH/g STATISTICS Number results Mean value Standard deviation Relative standard deviation Number results Mean value Standard deviation Relative standard deviation RESULTS with DG113-SC electrode STATISTICS Number results Mean value Standard deviation Relative standard deviation Number results Mean value Standard deviation Relative standard deviation
Content (EQP) Content (Buffer Potential) Content (EQP) Content (Buffer Potential) Content (EQP) Content (Buffer Potential) Content (EQP) Content (Buffer Potential) Content (EQP) Content (Buffer Potential) Content (EQP) Content (Buffer Potential)
R1
n = x = s = srel = n = x = s = srel =
6 3.47 0.02 0.682 6 1.82 0.03 1.501
mg KOH/g Content (EQP) mg KOH/g Content (EQP) %
R2
mg KOH/g Content (Buffer Potential) mg KOH/g Content (Buffer Potential) %
R1
n = x = s = srel = n = x = s = srel =
6 3.46 0.06 1.659 6 1.71 0.05 3.072
mg KOH/g Content (EQP) mg KOH/g Content (EQP) %
R2
mg KOH/g Content (Buffer Potential) mg KOH/g Content (Buffer Potential) %
Titration curve
26
Method
Method: User: m364A Base number ASTM D4739 Melanie Nijman 17.01.2008
008 Calculation R1 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 009 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 010 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Drain pump Condition 011 Conditioning Type Interval Position Time [s] Speed [%] Condition 012 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d2 E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition 013 End of sample 014 Park Titration stand Position Condition Content EQP mg KOH/g R1=(Q-B[ASTM D4739])*C/m M/z M[Potassium hydroxide] z[Potassium hydroxide] 2 No Yes No No No
001 Title Type Compatible with ID Title Author Date / Time Modified at Modified by Protect SOP LabX SOP 002 Conditioning Titration stand Position Time [s] Speed [%] Condition 003 Sample Number of IDs ID 1 Entry Type Lower limit [g] Upper limit [g] Density [g/mL] Correction factor Temperature [C] Entry 004 Titration stand Type Titration stand Lid handling 005 Dispense (normal) [1] Titrant Concentration [mol/L] Volume [mL] Dosing rate [mL/min] Condition 006 Stir Speed [%] Duration [s] Condition 007 Titration (EQP) [1] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Volume Wait time [s] Predispense Mode Volume [mL] Wait time [s] Control Control Titrant addition dV (mL) Mode dt [s] Evaluation and Recognition Procedure Threshold [mV/mL] Tendency Ranges Lower limit 1 [mV] Upper limit 1 [mV] Add. EQP criteria Termination At Vmax [mL] At potential Potential Termination tendency At Slope After number of recognized EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition
General titration T70/ T90 m364A Base number ASTM D4739 Melanie Nijman 17.01.2008 11.01.2008 Administrator No None None
Rondo60/1A Conditioning beaker 20 30 No
1 Motor Oil Weight 0.0 10.0 1.0 1.0 25.0 Arbitrary
Content (Buffer Potential) mg KOH/g R1=(QE(H[Buffer pH3]) -B[ASTM D4739])*C/m M/z M[Potassium hydroxide] z[Potassium hydroxide] 2 No Yes No No No
Rondo/Tower A Rondo60/1A No
ASTM D4739 3 20.0 Actual position Yes SP250 No
ASTM D4739 solvent 1 60 60.0 No
Fix 1 Conditioning beaker 300 30 No
35 60 No
HCl in 2-Propanol 0.1 pH DG116-Solvent mV No 35 Volume 0.5 60 Volume 0.2 5 User Incremental 0.1 Fixed time 90 Standard 80.0 None 1 H[Buffer pH3] H[Buffer pH3]+100 No 5.0 Yes H[Buffer pH3]+140 Positive No No No No No
No Per series Per series Last titration function Per series No Last titration function Last titration function No No No No No No No No No No No No
Rondo60/1A Rinse beaker No
27
METTLER TOLEDO
M364-B
Blank Value of Base Number Solvent According to ASTM D4739-06a

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

1) Solvent preparation: ASTM D4739-06a solvent is prepared by mixing 2-propanol, toluene, chloroform and water in the following ratio: 10 : 10 : 10 : 0.3 (v/v). 2) The titer is determined by titration of standardized KOH in 2propanol solution. The latter is standardized using potassium hydrogen phthalate (KHP). 3) The acidic and the alkaline aqueous buffers are measured and stored as auxiliary values H[Buffer pH3] (BN) and H[Bufffer pH10] (SBN, Strong Base Number). The values are then used for the EQP termination and the calculation R1. 4) 60 mL ASTM D4739-06a solvent are added using an additional dosing unit. This step can be performed manually using a dispenser or a graduated cylinder. 5) Blank value determinations are performed for every new batch of solvent by titration with HCl in 2-propanol to pH 3 potential value. The result is stored as blank B[ASTM D4739]. 6) For SBN, the solvent is titrated with KOH in 2-propanol to pH 10 buffer potential value and stored as B[ASTM D4739 pH10].
Substance Chemicals
--
pH 3 and pH 10 buffer solutions
Titrant
HCl in 2-propanol, c(HCl)=0.1 mol/L KOH in 2-propanol, c(HCl)=0.1 mol/L
KOH in 2-propanol 0.1 mol/L / KHP Titration Excellence T70/T90 Rondo 20 Sample changer 1 additional dosing unit (20 mL) DV1010 and DV1020 Burettes Titration beakers ME-101974 XS205 Balance, SP250 PC with LabX Software DGi116-Solvent
Accessories
Remarks
This method allows a fully automated procedure using a sample changer and an additional dosing unit. It can be modified for manual operation. Select "Manual stand" in the method function "Titration stand". 1) This application does not replace the ASTM standard. 2) The base number BN is defined as the consumption of hydrochloric acid to a specific endpoint to neutralize the alkaline components of the oil. It is expressed as mg KOH/g sample: - If an EQP is found between the acidic buffer potential value and a point 100 mV past this potential, then this will be the BN. - If no EQP is found in this region, then the result is evaluated at the potential value of the acidic buffer pH3. 3) Between each sample it is necessary to condition the electrode under stirring during 300 s in deion. water. The electrode is parked in buffer pH 4 (Rinse beaker). Literature: 1) ASTM D4739-06a and draft next version, see www.astm.org 2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066. 3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
--
Calculation
Results
Consumption of HCl in 2-Propanol up to EQP or acidic potential value: R1=Q (mmol) or R1=QE(H[Buffer pH3]) SBN blank: Consumption of KOH in 2Propanol up to EQP/potential value: R1=Q (mmol) or R1=QE(H[Buffer pH10])
Dispose of as halogenated organic waste
Author
Melanie Nijman
28
Results
Method Measured RESULTS No. 1
m364B
Blank Base Number According to ASTM D4739-06a
17.01.2007
ID ASTM D4739 Solvent
ASTM D4739 Solvent
ASTM D4739 Solvent
ASTM D4739 Solvent
ASTM D4739 Solvent
Sample size and results 60.0 mL R1 = 0.00478 mmol R3 = 0.00469 mmol 60.0 mL R1 = 0.00487 mmol R3 = 0.00478 mmol 60.0 mL R1 = 0.00484 mmol R3 = 0.00474 mmol 60.0 mL R1 = 0.00481 mmol R3 = 0.00472 mmol 60.0 mL R1 = 0.00482 mmol R3 = 0.00474 mmol
Consumption (Buffer potential) Consumption (EQP) Consumption (Buffer potential) Consumption (EQP) Consumption (Buffer potential) Consumption (EQP) Consumption (Buffer potential) Consumption (EQP) Consumption (Buffer potential) Consumption (EQP)
STATISTICS Number results Mean value Standard deviation Relative standard deviation Number results Mean value Standard deviation Relative standard deviation
R1
n = x = s = srel = n = x = s = srel =
5 0.00482 mmol 0.00003 mmol 0.697 % 5 0.00473 mmol 0.00003 mmol 0.694 %
Consumption (Buffer potential) Consumption (Buffer potential)
R3
Consumption (EQP) Consumption (EQP)
Titration curve
29
Method
Method: User: m364B Blank BN According to ASTM Nijman 17.01.2008
009 Calculation R3 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 010 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d2 E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition 011 Conditioning Type Interval Position Time [s] Speed [%] Condition 012 End of sample 013 Park Titration stand Position Condition 014 Blank Name Value B= Unit Limits Condition Formula 015 Blank Name Value B= Unit Limits Condition Formula 016 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Send to buffer Condition 017 Calculation R4 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Send to buffer Condition 018 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition Consumption (EQP) mmol R3=Q 1 M[None] z[None] 5 No Yes No No No No Per series Per series Last titration function Per series No Last titration function Last titration function No No No No No No No No No No No No Fix 1 Conditioning beaker 300 30 No
001 Title Type Compatible with ID Title Author Date / Time Modified at Modified by Protect SOP LabX SOP 002 Conditioning Titration stand Position Time [s] Speed [%] Condition 003 Sample Number of IDs ID 1 Entry Type Volume [mL] Density [g/mL] Correction factor Temperature [C] 004 Titration stand Type Titration stand Lid handling 005 Dispense (normal) [1] Titrant Concentration [mol/L] Volume [mL] Dosing rate [mL/min] Condition 006 Stir Speed [%] Duration [s] Condition 007 Titration (EQP) [1] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Volume Wait time [s] Predispense Mode Volume [mL] Wait time [s] Control Control Titrant addition dV (mL) Mode dt [s] Evaluation and Recognition Procedure Threshold [mV/mL] Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential Potential Termination tendency At Slope After number of recognized EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 008 Calculation R1 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer
General titration T70/ T90 M364_B Blank ASTM D4739 Mettler Toledo 17.01.2008 17.01.2008 Administrator No None
Rondo60/1A Conditioning beaker 20 30 No 1 ASTM D4739 Solvent Fixed volume 60.0 1.0 1.0 25.0 Rondo/Tower A Rondo60/1A No ASTM D4739 solvent 1 60 60.0 No 30 10 No
Rondo60/1A Rinse beaker No ASTM D4739 Mean[R1] mmol No Yes Mean[R1]>0 ASTM D4739 Mean[R3] mmol No Yes Mean[R3]>0 Mean Consumption (Buffer potential) mmol R2=Mean[R1] 1 M[None] z[None] 5 No Yes No No Mean Consumption (EQP) mmol R4=Mean[R3] 1 M[None] z[None] 5 No Yes No No No Yes No No No No No No
HCl in 2-Propanol 0.1 pH DG116-Solvent mV No 30 Volume 0.02 10 Volume 0.2 5 User Incremental 0.002 Fixed time 30 Standard 7500.0 Positive 0 No 1.0 Yes H[Buffer pH3]+100 Positive No No No No No Consumption (Buffer potential) mmol R1=QE(H[Buffer pH3]) 1 M[None] z[None] 5 No Yes No No
30
METTLER TOLEDO
M364-C
Titer Determination of 0.1 mol/L HCl in 2-Propanol (ASTM D4739-06a)

Titration Excellence Line: Method for the titer determination of hydrochloric acid in 2-propanol according to ASTM D4739-06a. Sample
Standardized KOH in 2-Propanol c(KOH) = 0.1 mol/L, 8.00 mL

1) Add 50 ml deionized into the titration beaker 2) 8 mL KOH in 2-propanol are added automaticlayy by menas ot an additional dosing unit. If this is not available, the sample can be added manaully using a pipette. 3) The mean value of the titer determinations is saved automatically as the titer for the titrant by means of the function TITER in the method.
Substance Chemicals
Potassium hydroxide, KOH M(KOH)=56.1 g/mol, z=1 50 mL deionized water
Titrant
HCl in 2-propanol, c(HCl)=0.1 mol/L
KOH in 2-propanol 0.1 mol/L(via KHP) Titration Excellence T50/T70/T90 Rondo 20 Sample changer 1 additional dosing unit DV1010 Burettes Titration beakers ME-101974 PC with LabX Software
Accessories

DGi111-SC
Literature: 1) ASTM D4739-06a and draft next version, see www.astm.org 2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066. 3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
HCl + KOH = Cl - + K+ + H 2O
Calculation
Titer HCl: R1=VENDDi/(VEQ*c*C) C=1/(cst*H[KOH Titer]*z) The real value for the KOH concentration determined in M364_D is used for the titer determination of HCl in 2-Propanol.
Results
Disposal as halogenated organic waste
Author
Melanie Nijman
31
Results
Method Measured RESULTS No. 1 2 3 4 5 6 7
m364C Titer HCl in 2-Propanol 07.03.2008
ID Sample size and KOH in 2-Propanol 8.0 mL R1 = 0.99689 -KOH in 2-Propanol 8.0 mL R1 = 0.99622 -KOH in 2-Propanol 8.0 mL R1 = 0.99649 -KOH in 2-Propanol 8.0 mL R1 = 0.99674 -KOH in 2-Propanol 8.0 mL R1 = 0.99613 -KOH in 2-Propanol 8.0 mL R1 = 0.99626 -KOH in 2-Propanol 8.0 mL R1 = 0.99694 --
results Titer HCl Titer HCl Titer HCl Titer HCl Titer HCl Titer HCl Titer HCl
STATISTICS Number results Mean value Standard deviation Relative standard deviation
R1 x = s = srel =
n = 7 0.99652 -0.00033 -0.034 %
Titer HCl Titer HCl
Titration curve
32
Method
Method: User: m364C Titer of HCl in 2-Propanol Melanie Nijman 07.03.2008
008 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d2 E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition 009 End of sample 010 Titer Titrant Concentration [mol/L] TITER= Limits Condition 011 Park Titration stand Position Condition 012 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Send to buffer Condition 013 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition No Per sample Per sample Last titration function No No Last titration function Last titration function No No No No No No No No No No No No
001 Title Type Compatible with ID Title Author Date / Time Modified at Modified by Protect SOP LabX SOP 002 Sample (Titer) Titrant Concentration Standard Type of standard Entry type Volume [mL] Correction factor Temperature [C] 003 Titration stand Type Titration stand Lid handling 004 Dispense (normal) [1] Titrant Concentration [mol/L] Volume [mL] Dosing rate [mL/min] Condition 005 Stir Speed [%] Duration [s] Condition 006 Titration (EQP) [1] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Wait time [s] Control Control Titrant addition dE (set value) dV(min) [mL] dV(max) [mL] Mode dE dt [s] t(min) [s] t(max) [s] Evaluation and Recognition Procedure Threshold [pH/mL] Tendency Ranges Add. EQP criteria Buffer capacity Termination At Vmax [mL] At potential At Slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 007 Calculation R1 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions
Titer determination T50 / T70 / T90 M364_C Titer of HCl in 2-Propanol melanie Nijman 26.02.2008 07.03.2008 Administrator No None
HCl in 2-Propanol 0.1 KOH in 2-Propanol liquid Fixed volume 8.0 1.0 25.0
HCl in 2-Propanol 0.1 Mean[R1] No No
KOH in 2-Propanol 0.1 8.0 60.0 No
Rondo60/1A Conditioning beaker No
30 10 No
HCl in 2-Propanol 0.1 pH DG111-SC pH No 30 None 0 User Dynamic 8.0 0.01 0.5 Equilibrium controlled 0.5 1 3 30 Standard 3.0 None 0 No No 10.0 No No Yes 1 No No No
Mean Titer -R2=Mean[R1] 1 M[None] z[None] 5 No Yes No No
No Yes No No No No No No
Titer -R1=VENDDi/(VEQ*c*C) 1/(cst*H[KOH Titer]*z) M[None] z[None] 5 No Yes No
33
METTLER TOLEDO
M364-D
Titer Determination of 0.1 mol/L KOH in 2-Propanol (ASTM D4739-06a)

Titration Excellence Line: Method for the titer determination of potassium hydroxide in 2-propanol according to ASTM D4739-06a. Sample
Primary standard KHP m = ~ 0.11 g

1) weigh the standard into the glass titration beaker in order to avoid electrostatic interferences. 2) Add 50 ml deionized into the titration beaker. 3) The mean value of the titer determinations is saved automatically as the titer for the titrant by means of the function TITER in the method.
Substance Chemicals
Potassium hydrogen phthalate M = 204.23 g/mol; z=1 50 mL deionized water
Titrant
KOH in 2-propanol c(KOH) = 0.1 mol/L
-Titration Excellence T50/T70/T90 Rondo 20 Sample changer
Accessories
DV1010 Burettes Titration beakers ME-101974 PC with LabX Software

DGi111-SC
1) The titrant has to be protected against the uptake of CO2 from the air. NaOH on carrier (e.g. "Sodium hydroxide on support", MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKA Nr. 03350) is an effective medium to avoid such formation of carbonate.
KHC8H4O4 + KOH = H20 + K 2C 8H4O4
Calculation
Titer KOH: R1=m/(VEQ*c*C) C=M/(10*p*z)
Literature: 1) ASTM D4739-06a and draft next version, see www.astm.org 2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066. 3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Results
Disposal as halogenated organic waste
Author
Melanie Nijman
34
Results
Method Measured RESULTS No. 1 2 3 4 5 6
m364D Titer of KOH in 2-propanol 28.02.2008
ID KHP KHP KHP KHP KHP KHP
Sample size and results 0.1057 g R1 = 0.9870 -0.1030 g R1 = 0.9920 -0.1018 g R1 = 0.9960 -0.1209 g R1 = 0.9900 -0.1183 g R1 = 0.9920 -0.1205 g R1 = 0.9930 --
Titer KOH Titer KOH Titer KOH Titer KOH Titer KOH Titer KOH
STATISTICS Number results Mean value Standard deviation Relative standard deviation
R1 x = s = srel =
n = 6 0.992 0.003 0.304
--%
Titer KOH Titer KOH
Titration curve
35
Method
Method: User: m364D Titer of KOH in 2-Propanol Melanie Nijman 28.02.2008
007 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d2 E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition 008 End of sample 009 Titer Titrant Concentration [mol/L] TITER= Limits Condition 010 Park Titration stand Position Condition 011 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Send to buffer Condition 012 Auxiliary value Name Formula H= Limits Condition 013 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition No Per sample Per sample Last titration function No No Last titration function Last titration function No No No No No No No No No No No No
001 Title Type Compatible with ID Title Author Date / Time Modified at Modified by Protect SOP LabX SOP 002 Sample (Titer) Titrant Concentration Standard Type of standard Entry type Lower limit Upper limit Correction factor Temperature [C] Input 003 Titration stand Type Titration stand Lid handling 004 Stir Speed [%] Duration [s] Condition 005 Titration (EQP) [1] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Wait time [s] Control Control Titrant addition dE (set value) dV(min) [mL] dV(max) [mL] Mode dE dt [s] t(min) [s] t(max) [s] Evaluation and Recognition Procedure Threshold [pH/mL] Tendency Ranges Add. EQP criteria Buffer capacity Termination At Vmax [mL] At potential At Slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 006 Calculation R1 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition
Titer determination T50 / T70 / T90 M364_D Titer of KOH in 2-Propanol Melanie Nijman 26.02.2008 28.02.2008 Administrator No None
KOH in 2-Propanol 0.1 Potassium hydrogen phthalate solid Weight 0.0 0.5 1.0 25.0 Arbitrary
KOH in 2-Propanol 0.1 Mean[R1] No No
30 30 No
KOH in 2-Propanol 0.1 pH DG111-SC pH No 30 None 0 User Dynamic 8.0 0.01 0.5 Equilibrium controlled 0.5 1 3 30 Standard 3.0 None 0 No No 10.0 No No Yes 1 No No No
Mean Titer -R2=Mean[R1] 1 M[None] z[None] 3 No Yes No No
KOH Titer R2 No No
Titer -R1=m/(VEQ*c*C) M/(10*p*z) M[Potassium hydrogen phthalate] z[Potassium hydrogen phthalate] 3 No Yes No No No
36
METTLER TOLEDO
M365
m-Value of Tap Water with Automatic Temperature Compensation

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

Note: This method allows a fully automated analysis procedure by using a Rondolinos sample changer. The method can be easily modified for manual operation. Select "Manual stand" in the method function "Titration stand". 1) Before the analysis an electrode calibration was performed using METTLER TOLEDO buffers of pH 4.01, 7.00 and 9.21. 2) Fill a (preferably) PE bottle to the brim with the water to be analyzed. Keep it closed and at sampling temperature.
Substance Chemicals
--
--
Titrant
3) Pipette 50 mL into the beaker shortly before titration.
Hydrochloric acid, HCl c(HCl) = 0.1 mol/L
Tris(hydroxymethyl)-aminomethane, 50-100 mg
4) The samples were analysed using a Rondolino sample changer. The electrode was rinsed during 2 s and conditioned during 10 s (Rondolino settings: 6). In this way, the electrode is cleaned with deionised water before starting the subsequent sample. 5) The automatic temperature compensation was achieved using the new DG117-SC titration electrode with the MultiPinTM-Lemo/Pt1000 cable, connected to the analogue board of the T50. See also: Application M415, Brochure 34, ME-51 725 066
Titration Excellence T50/T70/T90 Rondolino Sample changer
Accessories
LabX Titration Software 1 DV1010 burette Titration beakers ME-101974 Cable MultiPinTM-Lemo/Pt1000 DGi117-SC with internal temperature sensor Pt1000 HCl + NaOH = NaCl + H2O HCl + CO32- = HCO3- + ClHCl + HCO3- = CO2 + H 2O + Cl-
Remarks
1) The method parameters have been optimised for the sample used in this application. It may be necessary to slightly adapt the method to your specific sample. 2) Automatic temperature compensation during titration increases the accuracy of the analysis (smaller limit of error), since temperature fluctuations are taken into consideration. 3) Comparison with the DG115-SC (no internal T-sensor). The following result was obtained from 8 samples: m-value: 2.650 +/- 0.005 mmol/L , srel: 0.188%. The slightly higher value probably arises from the missing temperature correction. However the obtained m-values determined with both sensors are, as expected, rather similar. 4) The m-value (total alkalinity) represents the acid neutralizing capacity and is determined in e.g. drinking water. Acidity can affect corrosion, soil leaching and aquatic life in general. The name originates from the methyl orange color indicator (red to yellow-orange at pH 4.3) formerly used. The acid capacity depends on the equilibrium of free CO2, bicarbonate HCO3 , and 2carbonate CO3 in the on its temperature. Mineral weathering buffers groundwaters, e.g. limestone rock 2+ CaCO3 (s) + CO2 (g) = Ca (aq) + 2 HCO3 (aq) The bicarbonate ion then acts as a base to neutralize acids: + HCO3 (aq) + H (aq) = CO2 (g) + H2O (l)
Calculation
Total alkalinity or methyl orange alkalinity (m-value) is expressed as mmol/L or mg/L CaCO3
Results
Neutralization of the acidic waste before final disposal.
Author
Thomas Hitz
37
Results
All results Method-ID Sample R1 (Content) Sample R1 (Content) Sample R1 (Content) Sample R1 (Content) Sample R1 (Content) Sample R1 (Content) Sample R1 (Content) Sample R1 (Content) Statistics Method-ID Samples Mean s srel m365 Content R1 8 2.61898 mmol/L 0.00602 mmol/L 0.230 % m365 Tap water 2.62200 Tap water 2.61534 Tap water 2.61600 Tap water 2.61250 Tap water 2.62000 Tap water 2.61800 Tap water 2.61600 Tap water 2.63200 (1/8) mmol/L (2/8) mmol/L (3/8) mmol/L (4/8) mmol/L (5/8) mmol/L (6/8) mmol/L (7/8) mmol/L (8/8) mmol/L
Titration curve
EP-titraion (m-value of tap water)
9 8 7 pH-value 6 5 4 3 0 0.2 0.4 0.6 0.8 Volume (mL) 1 1.2 1.4 1.6
38
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Volume Density Correction factor Temperature 003 Titration stand (Rondolino TTL) Type Titration stand 004 Stir Speed Duration 005 Titration (EP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Temerature sensor Unit Stir Speed Predispense Mode Wait time Control Control End point type Tendency Endpoint value Control band Dosing rate (max) Dosing rate (min) Termination At EP Tuermination delay At Vmax Max. time 50 % 10 s General titration T50 / T70 / T90 m365 m-Value of tap water Thomas Hitz 10.08.2007 10:00:00 --No None m365 m-Value of tap water Thomas Hitz 10.08.2007 007 Record Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d2E/dV2 - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Calibration curve Method Series data 008 End of sample Per series Per series Last titration function Per series No Last titration function No No No No No No No No No No No No
1 Tap water Fixed volume 50 mL 1.0 g/mL 1.0 25.0C
Rondolino TTL Rondolino TTL 1
HCl 0.1 mol/L pH DG117 pH Yes interner Sensor 1 C 50 % None 0 s User Absolute Negative 4.30 pH 3.0 pH 10 mL/min 10 mL/min Yes 10 s 10.0 mL Infinity
006 Calculation R1 Result Content Result unit mmol/L Formula R1=Q*C/m Constant C=1000 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
39
METTLER TOLEDO
M366
Na2O and SiO2 in Waterglass

Titration Excellence Line: Method for the determination of Na2O and SiO2 in waterglass
Sample
Waterglass ~1.0 g

Determination of Na2O with HCl in Titration (EQP) [1]: Na2SiO3 + 2 HCl -> 2 NaCl + SiO2 + H2O
Substance Chemicals
Na2O, SiO2
KF solution, 25%
Add excess KF to form NaOH from SiO2: SiO2 + 6 KF + 2 H2O -> Na2SiF6 + 4 NaOH Neutralise NaOH formed with excess HCl, back-titrate remaining HCl with NaOH in Titration (EQP) [2]: HCl + NaOH -> NaCl + H2O 1) Because of the high fluoride content in acidic environment glass electrodes and titration beakers cannot be used for the determination of Na2O and SiO2 in waterglass. 2) For this reason only the polypropylene titration beakers can be used. Care needs to be taken when weighing in the waterglass samples in the polypropylene beakers that static electricity is avoided as much as possible. 3) Also, no glass sensors may be used for this determination as these will be the corroded as well. All fluoride solutions should be kept in plastic bottles.
Titrant
HCl, 2.0 mol/L (hydrochloric acid) NaOH, 1.0 mol/L (sodium hydroxide)
TRIS/THAM for HCl, KHP for NaOH Titration Excellence T70/T90 2 additional dosing units
Accessories
Titration beakers ME-101974 LabX Titration Software Rondo 20 Sample Changer

Sb850-S7/120 (pH sensor input) DX202-SC (ref. electrode) Na2SiO3 + 2HCl -> 2NaCl + SiO2 + H 2O SiO2+6KF+2H2O -> Na2SiF 6 + 4NaOH HCl + NaOH -> NaCl + H2O
The titration curve for the first EQP titration shows clearly that more than one site is present for the alkali metal oxide (mainly Na2O) component of waterglass. Waterglass is used in a wide variety of application areas as e.g., filler, additive, flame retardant, etc. Order number for Sb850-S7/120: Available from MT-PRO, old Ingold no. 10 850 3074
Calculation
R1: Na2O content (%) R2: SiO2 content (%) R3: Relative amounts Na2O/SiO2 (-)
Order no. for DX202 ref. electrode: ME-51 109 295
Results
Dilute and non-acidic fluoride solutions do not have to be treated as special waste.
Author
Melanie Nijman
40
Results
Method RESULTS No. ID Sample size and results m366 Na2O and SiO2 in waterglass
Waterglass R1 R2 R3 Waterglass R1 R2 R3 Waterglass R1 R2 R3 Waterglass R1 R2 R3 Waterglass R1 R2 R3 Waterglass R1 R2 R3 Waterglass R1 R2 R3
= = = = = = = = = = = = = = = = = = = = =
0.9365 49.91661 44.05010 1.13318 0.9843 49.92277 44.32853 1.12620 0.9806 49.85243 44.21881 1.12740 0.9521 49.90093 44.02595 1.13344 0.9843 49.88776 44.25015 1.12740 1.0449 49.89149 44.35087 1.12493 1.0130 49.95810 44.25864 1.12878
g % % g % % g % % g % % g % % g % % g % %
Content Content Content Content Content Content Content Content Content Content Content Content Content Content -
STATISTICS Number results R1 Mean value Standard deviation Relative standard deviation Number results R2 Mean value Standard deviation Relative standard deviation Number results R3 Mean value Standard deviation Relative standard deviation
n = x = s = srel = n = x = s = srel = n = x = s = srel =
7 49.9043 % 0.03298 0.066 % 7 44.21186 % 0.12739 0.288 % 7 1.12876 0.00333 0.295 %
Content Content
Content Content
Titration curve
41
Method
Method: User: m366 Na2O and SiO2 in waterglass Melanie Nijman 08.08.2007
009 Stir Speed [%] Duration [s] Condition 010 Titration (EQP) Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Wait time [s] Control Control Titrant addition dE (set value) dV (min) dV (max) Mode dE dt [s] t(min) [s] t(max) [s] Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential At Slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 011 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 012 Calculation R3 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 013 Conditioning Type Interval Position Time [s] Speed [%] Condition 014 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V ... E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Calibration curve Method Series data Condition 015 End of sample 30 30 No
001 Title Type Compatible with ID Titel Author Date / Time Modified at Protect SOP LabX SOP 002 Sample Number of IDs ID 1 Entry Type Lower limit [g] Upper limit [g] Density [g/mL] Correction factor Temperature [C] Entry 003 Titration stand Type Titration stand Lid handling 004 Stir Speed [%] Duration [s] Condition 005 Titration (EQP) Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Wait time [s] Control Control Titrant addition dE (set value) dV (min) dV (max) Mode dE dt [s] t(min) [s] t(max) [s] Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential At Slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 006 Calculation R1 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 007 Dispense (normal) Titrant Concentration [mol/L] Volume [mL] Dosing rate [mL/min] Condition 008 Dispense (normal) Titrant Concentration [mol/L] Volume [mL] Dosing rate [mL/min] Condition
General titration T70/ T90 m366 Na2O/SiO2 in Waterglass Melanie Nijman 03.08.2007 08.08.2007 No None
NaOH 1.0 mV Sb-850 mV No 30 None 0 User Dynamic 5 0.002 0.4 Equilibrium controlled 1 1.0 3 30 Standard 150 None 0 No 15 No No Yes 1 No No No SiO2 Content % R2=(QEX[1]+QENDDi[2]-Q[2])*C/m M/(10*z) M[Silicon dioxide] z[Silicon dioxide] 5 No Yes No No Na2O/SiO2 R2=R1/R2 1 M[None] z[None] 5 No Yes No No Fix 1 Conditioning beaker 20 50 No No Per Per No No No All All No No No No No No No No No No
1 Waterglass Weight 0.8 1.2 1.0 1.0 25.0 Arbitrary Rondo60/Tower A Rondo60/1A No 50 60 No
HCl 2.0 mV Sb-850 mV No 30 None 0 User Dynamic 9.0 0.008 0.4 Equilibrium controlled 0.5 1 3 30 Standard 1500 None 0 No 10 No No Yes 1 No No No Na2O Content % R1=Q*C/m M/(10*z) M[Sodium oxide] z[Sodium oxide] 5 No Yes No No 25% KF 25 10.0 60.0 No HCl 2.0 16.0 60.0 No
sample sample
titration functions titration functions
42
METTLER TOLEDO
M367
Chloride Content in Used Motor Oil

Titration Excellence Line: Inorganic chloride content in used motor oil is determined by precipitation titration in non aqueous solvent with silver nitrate. The content is expressed as chloride, Cl . Sample
Used motor oil, approx. 10 g

1) 10 g of sample is added into a glass titration beaker. 2) 2.5 mL 0.01mol/L NaCl standard solution are added to spike the sample since the chloride content is too low (Standard-Addition). 3) 50 mL Solvent ASTM 3227 will be added automatically with the Rondo membrane pump. 4) The sample serie is analysed using a Rondo 20 sample changer. Special beaker 1 and 2 are filled with toluene and the condition beaker with solvent ASTM 3227. Preparation of 0.01 mol/L NaCl - Dissolve 0.2922 g NaCl p.a. in deionized water - transfer quantitatively in a 500 volumetric flask and fill up to the mark with deionized water Preparation of Solvent ASTM 3227 - Dissolve 1.6 g sodium acetate anhydrous (NaC2H3O2) in 25 mL of deionized water and pour into 1 L flask - Fill up to the mark with 2-Propanol Preparation of 0.01 mol/L AgNO3 - Dissolve 8.494 g AgNO3 p.a. in 50 mL deionized water - transfer it quantitatively into a 500 mL volumetric flask and fill up to the mark with 2-Propanol (c=0.1 mol/L) - take 100.0 mL of this solution and dilute it with 2- Propanol to 1L in a volumetric flask (c=0.01 mol/L)
Substance Chemicals
Chloride, Cl -, M = 35.45 g/mol, z = 1

50 mL Solvent (ASTM 3227) 2-Propanol p.a. Toluene p.a. Sodium acetate (anhydrous)
Titrant
Silver nitrate (AgNO 3) in 2-Propanol c(AgNO 3) = 0.01 mol/L c(NaCl) = 0.01 mol/L, 2.5 mL Titration Excellence T70/T90 Rondo 20 Sample Changer with PowerShowerTM 1 DV1005 Burette Glass titration beaker ME-101446 XS205 Balance LabX Titration Software DMi145-SC (with 1 mol/L KNO3) NaCl + AgNO 3 = AgCl + NaNO3
Accessories
Remarks
- The method parameters have been developed and optimised for the above mentioned sample. It may be necessary to slightly adapt the method to your specific sample. The weight of the sample can vary from 0.5 to 30 g (depending on the kind of oil). - Sulfides interfere with the analysis. If necessary, they have to be oxidised to sulfates by adding 10 mL 30% H2O2 previous to the analysis. In this application, this was not the case.
Calculation
R1: Content (mg/L Chloride) R1 = (Q-H[NaCl Std])*C/m, C = M*1000/z 1 mL AgNO 3 (0.01 mol/l) is equal to 0.354 mg Chloride Filtration. The precipitate (AgCl) has to be classified as special waste. The liquid phase has to be disposed as organic waste. Claudia Schreiner
Literature: 1) METTLER TOLEDO Application brochure 20, ME-51 725 020 2) METTLER TOLEDO Application brochure 34, ME-51 725 066
Results
Author
43
Results
Start time: Sample Data No. 1/6 No. 2/6 No. 3/6 No. 4/6 No. 5/6 No. 6/6 04.12.2007 Note / ID Motor Oil Motor Oil Motor Oil Motor Oil Motor Oil Motor Oil Sample size 10.0318 g 10.1953 g 10.0720 g 10.1120 g 10.1386 g 10.1322 g
Results No. 1/6 No. 2/6 No. 3/6 No. 4/6 No. 5/6 No. 6/6
Note / ID Motor Oil Motor Oil Motor Oil Motor Oil Motor Oil Motor Oil
Rx R1= R1= R1= R1= R1= R1=
Result 28.25 27.80 26.33 27.35 27.28 26.38
Unit mg/L mg/L mg/L mg/L mg/L mg/L
Statistics Rx R1
Name Chloride
n 6
Mean Value 27.23
Unit mg/L
s 0.76
srel[%] 2.8
Titration curve
44
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Lower limit Upper limit Density Correction factor Temperature Entry General titration T70 / T90 367 Chloride in motor oil Claudia Schreiner 04.12.2007 --No None 367 Chloride content in motor oil Claudia Schreiner 04.12.2007 007 Calculation R1 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 008 Rinse 1 Motor oil Weight 0 g 15 g 1.0 g/mL 1.0 25.0C Arbitrary Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 009 Conditioning Type Interval Position Time Speed 010 Conditioning Type Interval Position Time Speed 011 Conditioning Type Interval Position Time Speed 012 End of sample ASTM D3227 solvent 1 15 Actual position No No Chloride mg/L R=(Q-H[Std NaCl])*C/m C= M*1000/z M[Chloride] z[Chloride] 3 No Yes No No No
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Pump Auxiliary reagent Volume 005 Stir Speed Duration 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Predispense Mode Wait time Control Control Titrant addition dV Mode dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria 60% 120 s ASTM D3227 solvent 50.0 mL
Fix 1 Special beaker 1 120s 60%
Fix 1 Special beaker 2 300s 60%
AgNO 3 0.01 mol/L mV DMi145-SC mV No 40% None 0 s User Incremental 0.1 mL Equilibrium controlled 1.0 mV 3 s 5 s 30 s Standard 100 mV/mL Positive 0 No 5 mL No No Yes 1 No
Fix 1 Conditioning beaker 120s 60%
45
METTLER TOLEDO
M368
Titer Determination of 0.01 mol/L AgNO3 in 2-Propanol

Titration Excellence Line: Method for the titer determination of 0.01 mol/L AgNO 3 by precipitation titration with sodium chloride as a primary standard. Sample
Primary standard Sodium chloride solution (0.01 mol/L), 2.5 mL Chloride, Cl -, M = 35.45 g/mol, z = 1
50 mL Solvent (ASTM 3227) 2-Propanol p.a. Toluene p.a. Sodium acetate (anhydrous)

1) Pipette 2.5 mL 0.01mol/L NaCl standard solution in a titration beaker 2) 50 mL Solvent ASTM 3227 will be added automatically with the Rondo membrane pump. 3) The sample serie is analysed using a Rondo 20 sample changer. The condition beaker is filled with solvent ASTM 3227.
Preparation of 0.01 mol/L NaCl - Dissolve 0.2922 g NaCl p.a. in deionized water - transfer quantitatively in a 500 volumetric flask and fill up to the mark with deionized water Preparation of Solvent ASTM 3227 - Dissolve 1.6 g sodium acetate anhydrous (NaC2H3O2) in 25 mL of deionized water and pour into 1 L flask - Fill up to the mark with 2-Propanol Preparation of 0.01 mol/L AgNO3 - Dissolve 8.494 g AgNO3 p.a. in 50 mL deionized water - transfer it quantitatively into a 500 mL volumetric flask and fill up to the mark with 2-Propanol (c=0.1 mol/L) - take 100.0 mL of this solution and dilute it with 2- Propanol to 1L in a volumetric flask (c=0.01 mol/L)
Substance Chemicals
Titrant
Silver nitrate (AgNO 3) in 2-Propanol c(AgNO 3) = 0.01 mol/L c(NaCl) = 0.01 mol/L, 2.5 mL Titration Excellence T50/T70/T90 Rondo 20 Sample Changer with PowerShowerTM 1 DV1005 Burette Glass titration beaker ME-101446 XS205 Balance LabX Titration Software DMi145-SC (with 1 mol/L KNO3) NaCl + AgNO 3 = AgCl + NaNO3
Accessories
Remarks
- This method is used to standardize the silver nitrate solution which is used in the method M367 (Chloride in motor oil).
Calculation
R1: Titer R1 = m/(VEQ*c*C) C = 1/(cst*z) 1 mL AgNO 3 (0.01 mol/l) is equal to 0.584 mg sodium chloride Filtration. The precipitate (AgCl) has to be classified as special waste. The liquid phase has to be disposed as organic waste. Claudia Schreiner
Results
Author
46
Results
Start time: Sample Data No. 1/6 No. 2/6 No. 3/6 No. 4/6 No. 5/6 No. 6/6 04.12.2007 Note NaCl NaCl NaCl NaCl NaCl NaCl / ID solution solution solution solution solution solution Sample size 2.5 mL 2.5 mL 2.5 mL 2.5 mL 2.5 mL 2.5 mL
Note NaCl NaCl NaCl NaCl NaCl NaCl
/ ID solution solution solution solution solution solution
Rx R1= R1= R1= R1= R1= R1=
Result 0.9694 0.9684 0.9704 0.9690 0.9708 0.9711
Statistics Rx R1
Name Titer
n 6
Mean Value 0.9698
Unit mg/L
s 0.0011
srel[%] 0.11
Titration curve
47
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample (Titer) Titrant Concentration Standard Type of standard Entry type Volume Correction factor Temperature General titration T50 / T70 / T90 368 Titer 0.01 mol/L AgNO3 Claudia Schreiner 04.12.2007 --No None 368 Titer 0.01 mol/L AgNO 3 Claudia Schreiner 04.12.2007 007 Calculation R1 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 008 Rinse AgNO 3 0.01 mol/L NaCl liquid Fixed volume 2.5 mL 1.0 25.0C Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 009 Conditioning Type Interval Position Time Speed 010 End of sample 011 Titer 005 Stir Speed Duration 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stir Speed Predispense Mode Volume Wait time Control Control Titrant addition dV Mode dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria 40% 120 s Titrant Concentration Titer = Limits AgNO3 0.01 mol/L Mean[R1] No ASTM D3227 solvent 1 15 Actual position No No Titer --R= m/(VEQ*c*C) C= 1/(cst*z) M[Sodium chloride] z[Sodium chloride] 5 No Yes No No No
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A 004 Pump Auxiliary reagent Volume ASTM D3227 solvent 50.0 mL
Fix 1 Conditioning beaker 120s 60%
AgNO 3 0.01 mol/L mV DMi145-SC mV No 40% Volume 1.5 mL 15 s User Incremental 0.1 mL Equilibrium controlled 1.0 mV 3 s 5 s 30 s Standard 100 mV/mL Positive 0 No 5 mL No No Yes 1 No
48
METTLER TOLEDO
M369
Peroxide Value of Edible Oils and Fats

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

1) Beakers have to be cleaned very well. Invisible fat residues or metal traces can strongly affect the result. 2) About 3 g of sample were dissolved in 20 mL of acetic acid/ chloroform (3:2) The acetic acid/chloroform mixture was added by the function DISPENSE. 3) 1 mL saturated KI solution is added by an additional burette. The reaction takes place and iodine is formed. 4) 50 mL deionized water are added by the membrane pump of Rondo 20.
Substance Chemicals
20 mL acetic acid/chloroform (3:2) 1 mL saturated KI solution 50 mL deion. water
Titrant
Sodium thiosulfate, Na2S2O3 c(Na2S2O3)= 0.01mol/L Potassium iodate, KIO 3 Titration Excellence T70/T90 Rondo 20 Sample Changer with PowerShowerTM 2 additional dosing units 1 DV1020 and 2 DV1010 Burettes Glass titration beaker ME-101446 XS205 Balance, LabX 2.6 DMi147-SC
5) Iodine is titrated with sodium thiosulphate.
127 g KI were dissolved in 100 mL water to obtain the saturated KI solution. The solution has to be kept in the dark.
Accessories
Impurities of the solvent are taken into account by a blank value determination. The blank value determination is done under the same conditions as the peroxide value determination itself. The value is stored under B[1].
Remarks
1) Fats and oils undergo changes during storage due to oxidation with air (oxidative rancidity). The compounds formed react as peroxides. Their content is commonly expressed as the "peroxide value" in milliequivalents peroxidic oxygen per kg of sample. 2) Peroxide values higher than 10 to 20 meq O2/kg are commonly interpreted as rancidity. Unrefined oils have higher peroxide values. They are usually in the range between 5 to 20 meq O2/kg.
R-OOH + 2 I- + 2 H3O+ = R-OH + I2 + 3 H2O I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6
Calculation
R = (Q-B[1])*C/m C = 1000, meq/kg B[1]: Solvent blank value, mmol
1) Exactly 60 seconds were allowed for the generation of iodine, as is requested by the official method (AOAC No. 28.022). 2) Earlier studies, however, had indicated that the generation is not complete yet at this time. 200 to 300 seconds were found to yield the highest results. Longer generation times resulted in low results (secondary reactions between iodine and the oil). 3) The duration of the generation time (time between 'adding the KI solution' and 'adding the water + starting the titration') is the critical point for repeatable results.
Results
The waste contains halogenated organic solvents and has to be disposed of accordingly.
Author
Maria-Jos Schmid
49
Results
Method: DM1471 Peroxide number 10/25/2007 11:27:34 AM Start time: 25.10.2007 1:53:24 PM ___________________________________________________________________________________________ Sample Data No. 1/5 No. 2/5 No. 3/5 No. 4/5 No. 5/5 Results No. 1/5 2/5 3/5 4/5 5/5 Comment / ID Olive oil Olive oil Olive oil Olive oil Olive oil Sample size 0.8164 g 0.8523 g 0.815 g 0.8149 g 0.8235 g
Comment / ID Olive oil Olive oil Olive oil Olive oil Olive oil
Start time 10/25/2007 1:53:25 PM 10/25/2007 2:05:29 PM 10/25/2007 2:17:32 PM 10/25/2007 2:29:19 PM 10/25/2007 2:41:10 PM
Rx R1= R2= R1= R2= R1= R2= R1= R2= R1= R2=
Result 0.024 25.601 0.025 25.795 0.024 26.013 0.024 25.888 0.024 26.074
Unit mmol meq/kg mmol meq/kg mmol meq/kg mmol meq/kg mmol meq/kg
Name Consumption Content Consumption Content Consumption Content Consumption Content Consumption Content
SQC/Statistics Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________ R1 R2 Consumption Content 5 5 0.024 25.874 mmol meq/kg 0.000 0.187 1.848 0.724
Additional results Sample Size n Mean value Unit s srel[%] ____________________________________________________________________________________________ Sunflower oil 4-5 g 5 0.028 5.583 0.022 11.759 0.021 3.980 mmol meq/kg mmol meq/kg mmol meq/kg 0.000 0.044 0.001 0.578 0.000 0.043 1.609 0.791 4.624 4.918 2.150 1.087
Margarine
2 g
Mais oil
4-5 g

Volume mL 0 0.057 0.086 0.1 0.135 0.222 0.322 0.422 0.522 0.622 0.722 0.822 0.922 1.022 1.122 1.222 1.322 1.422 1.522 1.622 1.722 1.822 1.922 2.022 2.122 2.222 2.322 2.422 2.522 2.622 2.642 2.648 2.654 2.661 2.666 2.671 2.671216 2.676 2.681 2.686 2.694 2.704 2.728 2.772 2.872 2.972 Increment mL NaN 0.057 0.029 0.014 0.035 0.087 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.02 0.006 0.006 0.007 0.005 0.005 NaN 0.005 0.005 0.005 0.008 0.01 0.024 0.044 0.1 0.1 Signal mV -16.7 -8 -11.3 -11.2 -10.9 -10.4 -10.1 -9.6 -9.1 -8.6 -8.1 -7.3 -6.7 -6 -5.3 -4.5 -3.6 -2.7 -1.8 -0.9 0.2 1.7 3.1 4.7 6.8 8.9 12.2 15.7 21.7 35.3 42.2 46.4 50 57.2 66.2 78.3 78.8 89.8 97.7 104 109.9 114.2 120.3 125.3 130 132.5 Change mV NaN 8.7 -3.3 0.1 0.3 0.5 0.3 0.5 0.5 0.5 0.5 0.8 0.6 0.7 0.7 0.8 0.9 0.9 0.9 0.9 1.1 1.5 1.4 1.6 2.1 2.1 3.3 3.5 6 13.6 6.9 4.2 3.6 7.2 9 12.1 NaN 11.5 7.9 6.3 5.9 4.3 6.1 5 4.7 2.5 1st deriv. mV/mL NaN NaN NaN NaN NaN 5.85 4.51 4.57 4.98 5.57 6.12 6.4 6.84 7.31 7.76 8.08 8.42 8.92 9.72 10.58 12.06 13.44 15.57 17.35 16.96 22.42 36.29 64.9 129.96 311.23 520.27 822.53 1165.65 1330.43 1635.55 1915.47 1916.21 1536.17 1263.43 1191.38 774.71 NaN NaN NaN NaN NaN Time s 0 3 8 13 18 23 28 33 38 43 48 53 58 64 69 74 79 84 89 94 99 104 109 114 120 125 130 135 142 158 169 180 190 202 217 232 NaN 247 262 277 292 303 318 330 342 351 Temperature C 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 NaN 25 25 25 25 25 25 25 25 25
Titration curve
EQP1
50
Method
Method Author 001 Title Type General titration Compatible with T70 / T90 ID DM1471 Title Peroxide number Author schmid Date/Time 10/16/2007 12:37:42 pm Modified 10/25/2007 11.27:34 am Modified by Administrator Protect No SOP None 002 Sample Number of IDs 1 ID 1 Olive oil Entry type Weight Lower limit 0.5 g Upper limit 20 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0C Entry Arbitrary 003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant AA/Chloroform Concentration 32 Volume 20 mL Dosing rate 60.0 mL/min Condition No 005 Stir Speed 40 % Duration 30 s Condition No 006 Dispense (normal) [2] Titrant KI Concentration 63.5 Volume 1 mL Dosing rate 60.0 mL/min Condition No 007 Stir Speed 30 % Duration 30 s Condition No 008 Stir Speed 0 % Duration 60 s Condition No 009 Pump Auxiliary reagent Water Volume 50.0 mL Condition No 010 Titration (EQP) [1] Titrant Titrant Na 2S 2O 3 Concentration 0.01 mol/L Sensor Type mV Sensor DM147 Unit mV Temperature acquisition Temperature acquisition No Stir Speed 30% Predispense Mode Volume Volume 0.1 mL Wait time 0 s Control Control Cautious Mode Redox Show parameters Yes Titrant addition Dynamic dE(set value) 6.0 mV dV(min) 0.005 mL dV(max) 0.1 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 5.0 s t(max) 15.0 s DM1471 Peroxide number schmid 25.10.2007 Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 011 Calculation R1 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 012 Calculation R2 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 013 Record ...... 014 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 015 Conditioning Type Interval Position Time Speed Condition 016 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 017 Conditioning Type Interval Position Time Speed Condition 018 End of sample 019 Park Titration stand Position Condition Standard 200.0 mV/mL Positive 0 No 20 mL No No Yes 1 No No No Consumption mmol R1=Q 1 M[None] z[None] 3 No Yes No No No Content meq/kg R2=(Q-B[1])*C/m 1000 M[None] z[None] 3 No Yes No No No
Water 1 10 mL Actual position No No Fix 1 According to interval 60 s 30% No Water 1 10 mL Actual position No No Fix 1 Conditioning beaker 10 s 30 % No
51
METTLER TOLEDO
M370
Titer Determination of 0.01 mol/L Na 2S2O3

Titration Excellence Line: Method for the titer determination of 0.01 mol/L Na2S 2O3 by redox titration with potassium iodate as a primary standard. Sample
1 mL potassium iodate standard solution, KIO 3 c(KIO3) = 0.01 mol/L Potassium iodate, KIO 3 M=213.99 g/mol ; z = 6
40 mL HCl 0.1 mol/L 1 mL saturated KI solution

1) Beakers have to be cleaned very well. Fat residues or metal traces can strongly affect the result. 2) About 3 g of sample were dissolved in 20 mL of acetic acid/ chloroform (3:2) The acetic acid/chloroform mixture was added by the function DISPENSE. 3) 1 mL saturated KI solution is added by an additional burette. The reaction takes place and iodine is formed. 4) 50 mL deionized water are added by the membrane pump of Rondo 20.
Substance Chemicals
Titrant
Sodium thiosulfate, Na2S2O3 c(Na2S2O3)= 0.01mol/L --Titration Excellence T70/T90 Rondo 20 Sample Changer with PowerShowerTM 2 additional dosing units 1 DV1020 and 2 DV1010 Burettes Glass titration beaker ME-101446 XS205 Balance, LabX 2.6 DMi147-SC
5) Iodine is titrated with sodium thiosulphate.
127 g KI were dissolved in 100 mL water to obtain the saturated KI solution. The solution has to be kept in the dark.
Accessories
Impurities of the solvent are taken into account by a blank value determination. The blank value determination is done under the same conditions as the peroxide value determination itself. The value is stored under B[1].
Remarks
1) Fats and oils undergo changes during storage due to oxidation with air (oxidative rancidity). The compounds formed react as peroxides. Their content is commonly expressed as the "peroxide value" in milliequivalents peroxidic oxygen per kg of sample. 2) Peroxide values higher than 10 to 20 meq O2/kg are commonly interpreted as rancidity. Unrefined oils have higher peroxide values. They are usually in the range between 5 to 20 meq O2/kg.
IO3- + 5 I- + 6 H+ = 3 I2 + 3 H2O I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6
Calculation
R1=m/(VEQ*c*C) C=1/(cst*z) cst = concentration of standard solution
1) Exactly 60 seconds were allowed for the generation of iodine, as is requested by the official method (AOAC No. 28.022). 2) Earlier studies, however, had indicated that the generation is not complete yet at this time. 200 to 300 seconds were found to yield the highest results. Longer generation times resulted in low results (secondary reactions between iodine and the oil). 3) The duration of the generation time (time between 'adding the KI solution' and 'adding the water + starting the titration') is the critical point for repeatable results.
Results
Inorganic salt solution
Author
Maria-Jos Schmid
52
Results
Method: T147 Titer Na2S2O3 09.10.2007 13:39:16 Start time: 09.10.2007 13:42:03 ___________________________________________________________________________________________
Results No. 1/5 2/5 3/5 4/5 5/5 Comment / Potassium Potassium Potassium Potassium Potassium ID iodate iodate iodate iodate iodate Start time 09.10.2007 09.10.2007 09.10.2007 09.10.2007 09.10.2007 Rx R1= R1= R1= R1= R1= Result 0.901 0.909 0.910 0.908 0.908 Unit -----Name Titer Titer Titer Titer Titer
13:42:03 13:55:31 14:08:40 14:21:55 14:35:14
SQC/Statistics Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________ R1 Titer 5 0.906 -0.004 0.437

Volume mL 0 1.143 1.714 2 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4 4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9 5 5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 6 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.79 6.815 6.822 6.829 6.836 6.841 6.846 6.846215 6.851 6.856 6.861 6.866 6.875 6.892 6.919 6.981 7.081 Increment mL NaN 1.143 0.571 0.286 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.09 0.025 0.007 0.007 0.007 0.005 0.005 NaN 0.005 0.005 0.005 0.005 0.009 0.017 0.027 0.062 0.1 Signal mV 18.4 19.6 20.6 21.1 21.3 21.4 21.6 21.8 22 22.2 22.4 22.7 22.9 23.1 23.4 23.7 23.9 24.2 24.5 24.8 25.1 25.4 25.8 26.1 26.5 26.9 27.3 27.7 28.2 28.6 29.1 29.7 30.2 30.8 31.4 32.1 32.8 33.6 34.4 35.3 36.3 37.3 38.5 39.8 41.3 43 45 47.3 50.2 54.1 60.4 71.4 79.3 83.3 87.6 95.1 103.2 111.9 112.3 120.2 127.6 134.1 139.3 144.3 150.4 155.5 161 165.3 Change mV NaN 1.2 1 0.5 0.2 0.1 0.2 0.2 0.2 0.2 0.2 0.3 0.2 0.2 0.3 0.3 0.2 0.3 0.3 0.3 0.3 0.3 0.4 0.3 0.4 0.4 0.4 0.4 0.5 0.4 0.5 0.6 0.5 0.6 0.6 0.7 0.7 0.8 0.8 0.9 1 1 1.2 1.3 1.5 1.7 2 2.3 2.9 3.9 6.3 11 7.9 4 4.3 7.5 8.1 8.7 NaN 8.3 7.4 6.5 5.2 5 6.1 5.1 5.5 4.3 1st deriv. mV/mL NaN NaN NaN NaN NaN 1.86 1.83 1.89 2.1 2.2 2.2 2.36 2.44 2.5 2.56 2.64 2.8 2.8 2.9 3.05 3.2 3.3 3.5 3.64 3.86 4 4.08 4.36 4.54 4.84 5.1 5.4 5.69 6.1 6.44 6.88 7.5 7.99 8.58 9.23 10.07 11.05 12.35 13.82 15.51 17.1 18.16 23.2 36.4 64.74 131.13 293.52 480.39 710.68 987.73 1151.71 1337.28 1610.88 1611.06 1474.04 1174.26 1070.14 881.97 NaN NaN NaN NaN NaN Time s 0 6 11 16 21 26 31 36 41 46 51 56 62 67 72 77 82 87 92 97 102 107 112 117 122 128 133 138 143 148 153 158 163 168 173 178 183 188 194 199 204 209 214 219 224 229 234 239 244 250 258 272 285 294 304 319 334 349 NaN 364 379 394 408 420 434 445 456 466 Temperature C 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 NaN 25 25 25 25 25 25 25 25 25
Titration curve
EQP1
53
Method
Method Author 001 Title Type Titer determination Compatible with T70 / T90 ID T147 Title Titer Na2S 2O 3 Author schmid Date/Time 09.10.2007 13:39:16 Modified 09.10.2007 13:39:16 Modified by Administrator Protect No SOP None LabX SOP 002 Sample (Titer) Titrant Na 2S 2O 3 Concentration [mol/L] 0.01 Standard Potassium iodate Type of standard liquid Entry type Fixed weight Volume 1.0 mL Correction factor 1.0 Temperature 25.0C 003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant HCl Concentration 0.1 mol/L Volume 40.0 mL Dosing rate 60.0 mL/min Condition No 005 Dispense (normal) [2] Titrant KI Concentration 63.5 mol/L Volume 1.0 mL Dosing rate 60.0 mL/min Condition No 006 Stir Speed 30 % Duration 30 s Condition No 007 Stir Speed [%] 0 % Duration [s] 60 s Condition No 008 Titration (EQP) [1] Titrant Titrant Na 2S 2O 3 Concentration 0.01 mol/L Sensor Type mV Sensor DM147 Unit mV Temperature acquisition Temperature acquisition No Stir Speed 30 % Predispense Mode Volume Volume 2.0 mL Wait time 0 s Control Control Cautious Mode Redox Show parameters Yes Titrant addition Dynamic dE(set value) 6.0 mV dV(min) 0.005 mL dV(max) 0.1 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 5.0 s t(max) 15.0 s T147 Titer Na2S 2O 3 schmid 09.10.2007 Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 009 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 010 Calculation R1 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 011 Record Summary Results Raw results Table of meas. values Sample data ............... Method Series data Condition 012 End of sample 013 Titer Titrant Concentration TITER= Limits Condition 014 Park Titration stand Position Condition 015 Calculation R2 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 016 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition Standard 200.0 mV/mL Positive 0 No 10 mL No No Yes 1 No No No Water 1 10 mL Actual position No No Titer -R1=m/(VEQ*c*C) 1/(cst*z) M[Potassium iodate] z[Potassium iodate] 3 No Yes No No No No Per sample Per sample Last titration function No No No No
Na2S 2O 3 0.01 mol/L Mean[R1] No No Rondo60/1A Conditioning beaker No Mean Titer -R2=Mean[R1] 1 M[None] z[None] 3 No Yes No No No No Yes No No No No No No
54
METTLER TOLEDO
M371
Chloride Determination in Ethanol

Titration Excellence Line: Method for the determination of the chloride content in ethanol by precipitation titration with silver nitrate. Sample
Ethanol, 40 g (approx. 60 mL)

The samples have been prepared by spiking high purity ethanol with NaCl solution in order to achieve different choride concentrations. In this way, several NaCl ethanolic solutions have been prepared. General procedure: 1) Weigh accurately ethanolic NaCl solution into the beaker. 2) Add 1 mL 0.001 mol/L NaCl standard solution to spike the sample. 3) The sample is acidified by adding 1 mL 0.1 mol/L HClO4 using an additional dosing unit. If this is not available, perchloric acid is added with a manual pipette. 4) Place the beaker on the Rondo sample rack and start the determination.
Substance Chemicals
Chloride ions, ClM(Cl) = 35.45 g/mol, z = 1 Perchloric acid, HClO4 (0.1 mol/L) Sodium chloride, NaCl (0.001 mol/L)
Titrant
Silver nitrate, AgNO 3 c(AgNO 3)= 0.001mol/L NaCl solution, 1 mL 0.001 mol/L Titration Excellence T50/T70/T90 Rondo 20 Sample Changer with PowerShowerTM 1 additional dosing unit 2 DV1010 Burettes Titration beaker ME-101974 XS205 Balance, LabX 2.6 DMi148-SC
Accessories
1) Weigh accurately 40 g ethanol into the titration beaker. 2) Add 1 mL 0.001 mol/L NaCl standard solution to spike the blank sample. 3) 1 mL 0.1 mol/L HClO 4 is added to the blank solution using an additional dosing unit. if this is not available, perchloric acid is added using a manual pipette. 4) Place the beaker on the Rondo sample rack and start the blank value determination.
Remarks
Literature: 1. "Standard Tests Methods for Chloride Ion in Water" ASTM D512-04 2. METTLER TOLEDO Titration Application M359, "Chloride content determination in ethanol based on ASTM D512 -04". 3. "Selected METTLER TOLEDO Methods for Biofuel Analysis" Application Brochure 36, May 2007, ME-51725070
NaCl + AgNO 3 = AgCl + NaNO3
Calculation
R = (Q-B[Blank EtOH])*C/m C = M*100/z, mg/kg B[Blank EtOH]: Solvent blank value, mmol
Results
Neutralization before final disposal as heavy metal aqueous solutions.
Author
Maria-Jos Schmid
55
Results
Method: 148 Chloride content in EtOH 12/18/2007 12:17:35 PM Start time: 12/18/2007 12:17:35 AM ___________________________________________________________________________________________ Sample Data No. 1/5 No. 2/5 No. 3/5 No. 4/5 No. 5/5 Results No. 1/5 2/5 3/5 4/5 5/5 Comment / ID Ethanol Ethanol Ethanol Ethanol Ethanol Sample size 38.672 g 38.4992 g 38.791 g 38.983 g 38.9095 g
Comment / ID Ethanol Ethanol Ethanol Ethanol Ethanol
Start time 12/18/2007 12:17:35 PM 12/18/2007 12:17:35 PM 12/18/2007 12:17:35 PM 12/18/2007 12:17:35 PM 12/18/2007 12:17:35 PM
Rx R1= R1= R1= R1= R1=
Result 0.45 0.48 0.45 0.45 0.45
Unit mg/kg mg/kg mg/kg mg/kg mg/kg
Name Content Content Content Content Content
SQC/Statistics Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________ R1 Content 5 0.46 mg/kg 0.01 2.942
Additional results Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________ R1 R1 R1 Content Content Content 3 5 5 4.61 12.15 23.60 mg/kg mg/kg mg/kg 0.06 0.04 0.08 1.253 0.291 0.318
DM140 electrode results Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________ R1 R1 Content Content 3 3 0.43 5.60 mg/kg mg/kg 0.07 0.55 16.279 9.749

Volume mL 0 0.057 0.086 0.1 0.135 0.222 0.422 0.622 0.822 0.943 1.032 1.135 1.213 1.269 1.314 1.355 1.388 1.415 1.435 1.452 1.466 1.479 1.49 1.497 1.504 1.51 1.514 1.519 1.523 1.527 1.531 1.533123 1.535 1.539 1.543 1.548 1.552 1.557 1.568 1.574 1.582 1.592 Increment mL NaN 0.057 0.029 0.014 0.035 0.087 0.2 0.2 0.2 0.121 0.089 0.103 0.078 0.056 0.045 0.041 0.033 0.027 0.02 0.017 0.014 0.013 0.011 0.007 0.007 0.006 0.004 0.005 0.004 0.004 0.004 NaN 0.004 0.004 0.004 0.005 0.004 0.005 0.011 0.006 0.008 0.01 Signal mV 161 160.9 160.4 160.2 160.3 158.7 154.4 149.4 143 137.9 133.8 128.3 122.9 118 113.3 108.2 103.1 97.9 93.2 88.1 83.7 78.3 72.9 68.3 63.3 58 53.5 47.8 42.6 36.7 30.7 27.7 25 17.9 12.7 6.6 1.3 -2 -10.7 -14.9 -19.3 -24.2 Change mV NaN -0.1 -0.5 -0.2 0.1 -1.6 -4.3 -5 -6.4 -5.1 -4.1 -5.5 -5.4 -4.9 -4.7 -5.1 -5.1 -5.2 -4.7 -5.1 -4.4 -5.4 -5.4 -4.6 -5 -5.3 -4.5 -5.7 -5.2 -5.9 -6 NaN -5.7 -7.1 -5.2 -6.1 -5.3 -3.3 -8.7 -4.2 -4.4 -4.9 1st deriv. mV/mL NaN NaN NaN NaN NaN -15.74 -22.1 -28.41 -37.69 -45.94 -54.77 -68.8 -85.4 -102.81 -124.84 -154.59 -189.02 -231.57 -278.49 -335.6 -401.04 -491.7 -606.1 -704.71 -839.84 -977.31 -1090.51 -1234.77 -1364.69 -1472.06 -1517.89 -1552.6 -1545.86 -1427.73 -1302.62 -1135.67 -1019.34 NaN NaN NaN NaN NaN Time s 0 3 6 9 27 31 36 42 48 56 62 68 75 82 89 97 106 115 124 135 145 157 170 183 196 212 225 243 259 278 296 NaN 314 336 352 369 386 392 411 423 435 447 Temperature C 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 NaN 25 25 25 25 25 25 25 25 25 25
Titration curve
EQP1
56
Method
Method Author 001 Title Type General titration Compatible with T50 / T70 / T90 ID 148 Title Chloride content in EtOH Author schmid Date/Time 22.11.2007 12:09:49 Modified 18.12.2007 12:16:30 Modified by schmid Protect No SOP None 002 Sample Number of IDs 1 ID 1 Ethanol Entry type Weight Lower limit 1 g Upper limit 60 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0C Entry Arbitrary 003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant HClO 4 Concentration 0.1 mol/L Volume 1 mL Dosing rate 60.0 mL/min Condition No 005 Stir Speed 40 % Duration 15 s Condition No 006 Titration (EQP) [1] Titrant Titrant AgNO 3 Concentration 0.001 mol/L Sensor Type mV Sensor DM148-SC Unit mV Temperature acquisition Temperature acquisition No Stir Speed 30% Predispense Mode Volume Volume 0.1 mL Wait time 15 s Control Control Cautious Mode Precipitation Show parameters Yes Titrant addition Dynamic dE(set value) 5.0 mV dV(min) 0.004 mL dV(max) 0.2 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 3.0 s t(max) 30.0 s Evaluation and Recognition Procedure Standard Threshold 200.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria No Termination At Vmax 15 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No 148 Chloride content in EtOH schmid 18.12.2007 12:16:30 007 Calculation R1 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 008 Record Summary Results Raw results Table of meas. values Sample data Resource data E - V dE/dV - V log dE/dV - V d 2E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition 009 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 010 Conditioning Type Interval Position Time Speed Condition 011 End of sample Content mg/kg R1=(Q-B[Blank EtOH])*C/m M*1000/z M[Chloride] z[Chloride] 3 No Yes No No No No Per sample Per sample Last titration function Per series No Last titration function Last titration function No No No No No No No No No No No No Water 1 10 mL Actual position No No Fix 1 Conditioning beaker 10 s 30% No
------------------------------------------------------Blank Titration ....... Predispense Mode Volume Volume 0 mL Wait time 0 s ....... 007 Calculation R1 Result Blank Ethanol Result unit mmol Formula R1=Q Constant 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No ....... 014 Blank Name Blank EtOH Result unit mmol Formula R2=Mean[R1] .....
57
METTLER TOLEDO
M372
Titer Determination of 0.001 mol/L AgNO3

Titration Excellence Line: Method for the titer determination of 0.001 mol/L AgNO 3 by precipitation reaction with sodium chloride as a primary standard. Sample
5 mL sodium chloride iodate standard solution, NaCl c(NaCl) = 0.001 mol/L Sodium chloride, NaCl M=58.44 g/mol ; z = 1 50 mL deionized water Perchloric acid, HClO4 (0.1 mol/L) 1 mL Silver nitrate, AgNO 3 c(AgNO 3)= 0.01mol/L --Titration Excellence T50/T70/T90 Rondo 20 Sample Changer with PowerShowerTM 1 additional dosing units 2 DV1010 Burettes Glass titration beaker ME-101446 XS205 Balance, LabX 2.6 DMi148-SC

1) Beakers have to be cleaned very well. 2) Add 5 mL 0.001 mol/L NaCl standard solution.
Substance Chemicals
3) 1 mL 0.1 mol/L HClO 4 is added to the solution using an additional dosing unit. If this is not available, perchloric acid is added using a manual pipette. 4) Place the beaker on the Rondo sample rack and start the determination.
Titrant
Accessories
Remarks
NaCl + AgNO 3 = AgCl + NaNO3
Calculation
R1=m/(VEQ*c*C) C=1/(cst*z) cst = concentration of standard solution
Results
Neutralization before final disposal as heavy metal aqueous solutions.
Author
Maria-Jos Schmid
58
Results
Method: 148T Titer of AgNO3 11.12.2007 14:27:36 Start time: 11.12.2007 14:27:51 ___________________________________________________________________________________________
Results No. 1/3 2/3 3/3 -/Comment / ID NaCl NaCl NaCl Titer Start time 11.12.2007 14:27:51 11.12.2007 14:37:29 11.12.2007 14:47:01 0.991 Rx R1= R1= R1= R2= Result 0.986 0.993 0.993 0.991 Unit ----Name Titer Titer Titer Mean Titer
SQC/Statistics Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________ R1 R2 Titer Mean Titer 3 1 0.991 0.991 --0.004 NaN 0.408 NaN

Volume mL 0 0.571 0.857 1 1.2 1.4 1.6 1.8 2 2.2 2.4 2.6 2.8 3 3.2 3.4 3.6 3.8 4 4.2 4.4 4.6 4.8 5 5.2 5.362 5.479 5.571 5.655 5.716 5.771 5.818 5.852 5.88 5.906 5.93 5.947 5.963 5.978 5.99 6 6.01 6.014073 6.021 6.03 6.042 6.054 6.066 6.084 6.104 6.128 6.154 6.19 Increment mL NaN 0.571 0.286 0.143 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.162 0.117 0.092 0.084 0.061 0.055 0.047 0.034 0.028 0.026 0.024 0.017 0.016 0.015 0.012 0.01 0.01 NaN 0.011 0.009 0.012 0.012 0.012 0.018 0.02 0.024 0.026 0.036 Signal mV 116.3 113.9 112.4 111.6 110.4 109.1 107.8 106.5 105.1 103.6 102.2 100.6 98.9 97.2 95.4 93.4 91.4 89.2 86.7 84 81 77.7 73.8 69.3 63.7 58.1 53.1 48.4 43 38.3 33.4 27.9 23.2 18.3 13.7 8.1 3.4 -1.4 -6.8 -11.6 -16.4 -21 -23.1 -26.6 -30.8 -36 -41 -45.3 -50.6 -55.5 -60.7 -65.3 -70.5 Change mV NaN -2.4 -1.5 -0.8 -1.2 -1.3 -1.3 -1.3 -1.4 -1.5 -1.4 -1.6 -1.7 -1.7 -1.8 -2 -2 -2.2 -2.5 -2.7 -3 -3.3 -3.9 -4.5 -5.6 -5.6 -5 -4.7 -5.4 -4.7 -4.9 -5.5 -4.7 -4.9 -4.6 -5.6 -4.7 -4.8 -5.4 -4.8 -4.8 -4.6 NaN -5.6 -4.2 -5.2 -5 -4.3 -5.3 -4.9 -5.2 -4.6 -5.2 1st deriv. mV/mL NaN NaN NaN NaN NaN -6.44 -6.64 -6.8 -7.05 -7.34 -7.66 -8.05 -8.44 -8.85 -9.36 -9.93 -10.72 -11.64 -12.73 -14 -15.66 -17.84 -20.92 -25.48 -32.7 -41.67 -51.27 -62.11 -76.65 -91.36 -110.67 -134.94 -159.1 -185.61 -218.32 -257.57 -292.97 -334.94 -383.1 -420.6 -456.08 -478.18 -479.1 -476.74 -454.01 -411.03 -369.07 -331.99 NaN NaN NaN NaN NaN Time s 0 6 10 13 18 22 26 30 35 39 43 48 52 57 62 66 71 76 82 87 93 98 104 111 118 125 132 140 147 155 163 172 181 191 200 212 223 234 247 259 272 285 NaN 300 312 326 340 352 365 377 389 401 412 Temperature C 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 NaN 25 25 25 25 25 25 25 25 25 25
Titration curve
EQP1
59
Method
Method Author 001 Title Type Titer determination Compatible with T50 / T70 / T90 ID 148T Title Titer of AgNO3 Author schmid Date/Time 26.11.2007 12:46:07 Modified 11.12.2007 14:27:36 Modified by Administrator Protect No SOP None LabX SOP 002 Sample (Titer) Titrant AgNO 3 Concentration [mol/L] 0.001 Standard NaCl Type of standard liquid Entry type Fixed weight Volume 5.0 mL Correction factor 1.0 Temperature 25.0C 003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No 004 Dispense (normal) [1] Titrant HClO 4 Concentration 0.1 mol/L Volume 1.0 mL Dosing rate 60.0 mL/min Condition No 005 Stir Speed 30 % Duration 10 s Condition No 006 Titration (EQP) [1] Titrant Titrant AgNO 3 Concentration 0.001 mol/L Sensor Type mV Sensor DM148-SC Unit mV Temperature acquisition Temperature acquisition No Stir Speed 30 % Predispense Mode Volume Volume 1.0 mL Wait time 0 s Control Control Normal Mode Precipitation Show parameters Yes Titrant addition Dynamic dE(set value) 5.0 mV dV(min) 0.004 mL dV(max) 0.2 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 3.0 s t(max) 30.0 s Evaluation and Recognition Procedure Standard Threshold 200.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria No Termination At Vmax 10 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No 148T Titer of AgNO3 schmid 11.12.2007 007 Calculation R1 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 008 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain Condition 009 Record Summary Results Raw results Table of meas. values Sample data E - V dE/dV - V log dE/dV - V d 2E/dV2 - V BETA - V E - t V - t dV/dt - t T - t E - V & dE/dV - V V - t & dV/dt - t Method Series data Condition Method Series data Condition 010 Conditioning Type Interval Position Time Speed Condition 011 End of sample 012 Titer Titrant Concentration TITER= Limits Condition 013 Calculation R2 Result Result unit Formula Constant M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 014 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition Titer -R1=m/(VEQ*c*C) 1/(cst*z) M[Sodium chloride] z[Sodium chloride] 3 No Yes No No No Water 1 10 mL Actual position No No No Per sample Per sample Last titration function No Last titration function No No No No No No No No No No No No No No No No Fix 1 Conditioning beaker 10 s 30% No
AgNO3 0.001 mol/L Mean[R1] No No Mean Titer -R2=Mean[R1] 1 M[None] z[None] 3 No Yes No No No Yes Yes No No No No No No
60
METTLER TOLEDO
M373
Mercaptan Sulfur Content in Kerosine According to ASTM D3227-04a

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

1) Dissolved oxygen is removed by purging the solvent and the titrant solutions with nitrogen gas for at least 10 min prior to use. The solutions must be kept protected from atmosphere.
Substance Chemicals
Mercaptan sulfur, R-S-, M = 32.06 g/mol, z = 1 25 mL solvent ASTM D3227-04a 2 mL Ethyl mercaptan standard solve. (see remarks) Silver nitrate, AgNO 3 , in 2-Propanol c(AgNO 3) = 0.01 mol/L NaCl, c(NaCl) = 0.01 mol/L , 5 mL Titration Excellence T70/T90 2 additional dosing units Rondo 20 Sample Changer 2 DV1010 and 1 DV1020 Burettes Glass titration beaker ME-101446 XS205 Balance Olivetti Printer JobJet 210 DM405-SC
2) Before sample analysis a blank value titration is determined (result is stored as B[ASTM D 3227]). 3) Reagents addition: - 25 mL solvent ASTM D3227-04a are added into the beaker. 4) A Rondo sample changer with a diaphragm pump was used.
Titrant
5) For accurate sampling, kerosene was added with a pipette instead of weighing (volatility). Thus, its density must be taken into account. The density of flight petrol was measured using a 3 METTLER TOLEDO DR45 density meter (d = 0.7905 g/cm , 25C) 6) The electrode was rinsed and conditioned using the ASTM D3227 solvent (Functions RINSE, CONDITIONING in special beaker 2, and CONDITIONING in conditioning beaker).
Accessories
Remarks
1) The method parameters have been optimised for the above mentioned sample. It may be necessary to slightly adapt the method to your specific sample. 2) A fully automated procedure is performed by using two additional burette drives and a sample changer. It can be easily modified for manual operation. Select "Manual stand" in the method function "Titration stand". 3) ASTM D3227-04a alkaline solvent: Dissolve 1.6 g anhydrous sodium acetate (NaC2H3O2) in 25 mL of deion. water and pour into 1 L flask. Fill up to the mark with 2-propanol. This solvent allows a good dissolution of the oil. 4) The 0.02 mol/L mercaptan standard is prepared by dissolving approx. 1.24 g ethyl mercaptan in a 1 L volumetric flask and filling up with the ASTM D3227 solvent. Literature: ASTM D3227-04a, see www.astm.org METTLER TOLEDO Appl. brochure 34, ME-51 725 066 METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
R-SH + AgNO3 = R-S-Ag + HNO 3
Calculation
R1: Mercaptan content (mg/kg) R1 = (Q-B[ASTM D 3227])*C/(m*d), C = M*1000/z B[ASTM D3227]: Blank value of mercaptan standard solution
Results
Filtration. The precipitate has to be classified as special waste. The liquid phase has to be disposed as organic waste. Claudia Schreiner
Author
61
Results
Start time: Sample Data No. 1/6 No. 2/6 No. 3/6 No. 4/6 No. 5/6 No. 6/6 27.10.2007 Note / ID Kerosene Kerosene Kerosene Kerosene Kerosene Kerosene Sample size 25 mL 25 mL 25 mL 25 mL 25 mL 25 mL
Note / ID Kerosene Kerosene Kerosene Kerosene Kerosene Kerosene
Rx R1= R1= R1= R1= R1= R1=
Result 14.794 14.768 14.696 14.676 14.616 14.623
Statistics Rx R1
Name Mercaptans
n 6
Mean Value 14.70
Unit mg/L
s 0.07
srel[%] 0.50
Titration curve
62
Method
Method Author 001 Title Type Compatible with ID Title Author Date/Time Modified Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry type Volume Density Correction factor Temperature 003 Titration stand Type Titration stand 004 Pump Auxiliary reagent Volume 005 Dispense (normal) [1] Titrant Concentration Volume Dosing rate 006 Stir Speed Duration 007 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature acquisition Temperature acquisition Stirrer Speed Predispense Mode Wait time Control Control Titrant addition dE(set value) dV(min) dV(max) Meas. val. acquisition dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria 30% 480 s ASTM D3227 solvent 25 mL General titration T70 / T90 m373 Mercaptan sulfur ASTM D3227 METTLER TOLEDO 27.08.2007 --No None m373 Mercaptan sulfur ASTM D3227 METTLER TOLEDO 27.08.2007 Termination At Vmax [mL] At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria 008 Calculation R1 Result Result unit Formula Constant M z Decimal place Result limits Record statistics Extra statistical functions Condition 3 No No Yes 1 No
1 Kerosene Fixed volume 25.0 mL 0.8 g/mL 1.0 25.0C
Content mg/kg R1=(Q-B[ASTM D3227])*C/(m*d) C=M*1000/z M[Mercaptan sulfur] z[Mercaptan sulfur] 3 No No No No
Rondo/Tower A Rondo60/1A
Kerosene 1 25 mL 60.0 mL/min
009 Record Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration functions dE/dV - V Last titration functions log dE/dV - V No d2E/dV2 - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No 010 Rinse Auxiliary reagent Rinse cycles Vol. per cycle [mL] Position Drain 011 Conditioning Type Interval Position Time [s] Speed [%] 012 Conditioning Type Interval Position Time [s] Speed [%] 013 End of sample ASTM D3227 solvent 1 15 Actual position No
AgNO 3 in 2-Propanol 0.01 mol/L mV DM405-SC mV No 30% None 0 s User Dynamic 4.0 0.005 mL 0.05 mL Equilibrium controlled 1.0 mV 2 s 10 s 30 s Standard 1000 mV/mL Positive 0 No
Fix 1 Special beaker 2 30 50
Fix 1 Conditioning 30 50
63
METTLER TOLEDO
M374-A
Base Number Determination in Fresh Oils by Conductometric Titration

Titration Excellence Line: Determination of the base number of freshmotor and cutting oils by titration with 0.1 mol/L hydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe (IP400/94). Sample
Fresh oils, 0.2-1 g

1) Titrant preparation: If not commercially available, the titrant can be prepared by adding 9 mL 37% v/v HCl and filling up to 1 L with 2-propanol (isopropanol). 2) Depending on the BN number, 0.2-1 g oil are weighed into a glass titration bealer. The higher the BN, the lower the sample size. 3) 60 mL solvent are added automatically by a peristaltic pump. 4) The titration is started after 60 s stirring time at 50% in order to achieve a complete dissolution of the sample.
Substance Chemicals
Alkaline components B, expressed as mg KOH/g sample 55 mL solvent mixture Toluene:isopropanol:distilled water (50% (v/v):49.5%(v/v):0.5%(v/v) ) HCl in 2-propanol: c(HCl) = 0.1 mol/L
Titrant
TRIS (THAM), 50 mg Titration Excellence Line, T50/70/90 Conductivity board ME-51109840 Rondo 20 with PowerShower Glass titration beaker ME-101446 2 x SP250 Peristaltic pumps ME-51108016 Printer, XP205 balance InLab718 conductivity probe
Accessories
Remarks
1) To ensure a complete rinsing of the probe, the following cleaning procedure was defined (see method): 1.1 Drain: The sample beaker is emptied 1.2 Pump: 35 mL of solvent are dosed 1.3 Stir: To remove all residuals, the solvent is stirred 20 s at 70%. 1.4 Drain: The solvent is pumped out. 1.5 Rinse: Finally, the titration stand is rinsed two times after each sample using the rinsing cycles defined in the method function "Rinse".
Neutralization of all basic components in oil. General neutralization reactions: 1) HCl + NaOH = NaCl + H2O 2) HCl + B = HB+ + ClBase number (mg KOH/g) R1= (Q-B[IP400])*C1/m C1= 56.1 B[IP400]: solvent blank value
Calculation
Literature: 1) IP400/94 Standard, British Institute of Petroleum (Now: Energy Institute, http://www.energyinst.org.uk/) 2) METTLER TOLEDO Applications M252/M253. and M099/ M100.
Results
Organic solvent waste (aromatic solvents)
3) This application does not replace the standard.
Author
Hans-Joachim Muhr
64
Results
Method ID: Date / Time: Samples Nr. 1 2 3 4 5 6 IP400B 09/20/2006 01:43:12 pm Sample series ID User name 13 Administrator
ID 13 13 13 13 13 13
Sample size and results 0.2584 g R1(BN) 38.798 R2(Titration time) 2.570 0.2535 g R1(BN) 38.309 R2(Titration time) 2.470 0.2511 g R1(BN) 38.490 R2(Titration time) 2.470 0.2541 g R1(BN) 38.380 R2(Titration time) 2.570 0.2521 g R1(BN) 38.560 R2(Titration time) 2.470 0.2 g R1(BN) 38.263 R2(Titration time) 2.570
mg KOH/g min mg KOH/g min mg KOH/g min mg KOH/g min mg KOH/g min mg KOH/g min
Statistics R1(BN) Number of samples Mean value s srel
6 38.467 mg KOH/g 0.196 mg KOH/g 0.511 %
TBN according to ASTM D4739: 40.4 mg KOH/g --------------------------------------------------------------------------------------------Different samples of fresh oils Sample Size / g n Base number mg KOH/g 18.947 10.886 s mg KOH/g 0.106 0.034 srel % 0.559 0.316 TBN ASTM D4739 mg KOH/g 20.0 10.8
CF15 58420
0.5 1.0
6 6
Titration curve
65
Method
Method Version IP400B Conductometric BN 09/20/2006 01:43:12 pm 007 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 008 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 009 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V 2 2 d E/dV - V BETA - V E - t V - t dV/dt - t T - t E - V & DE/dV - V V - t & dV/dt - V Method Series data Condition 010 Drain Drain pump Drain volume Condition 011 Pump Auxiliary reagent Volume Condition 012 Stir Speed Duration Condition 013 Drain Drain pump Drain volume Condition 014 Rinse Auxiliary reagent Rinse cycles Vol. per cycle Position Drain Drain pump Condition 015 End of sample BN mg KOH/g R1=(Q-B[IP400])*C/m 56.1 M[None] z[None] 3 No Yes No No
001 Title Type Compatible with ID Titel Author Date / Time Modified at Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry Type Lower limit Upper limit Density Correction factor Temperature Entry 003 Titration stand (Rondo/Tower A) Type Titration stand Lid handling 004 Pump Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time Control Control Titrant addition dV Meas. val. acquisition dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Ranges Add. EQP criteria Steepest jumps Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition
General titration T50/T70/T90 IP400B Conductometric BN Administrator 08/28/2006 03:09:17 pm 09/20/2006 01:43:12 pm Administrator No None
1 13 Weight 0.0 g 5.0 g 1.0 g/mL 1.0 25.0 C Before
Titration time min R2=t -M[None] z[None] 3 No No No No
Per sample Per sample Per sample

Last titration function
IP400 Solvent 55 mL No
Per sample No
No No
50 % 60 s No
HCl in 2-Propanol 0.1 mol/L Conductivity InLab 718 S No 30 % None 0 s User Incremental 0.1 mL Equilibrium controlled 0.5 S 1.0 s 10 s 20 s Segmented 0.5 S mL2 0 Steepest jump 1 4 mL No No Yes 1 No No No
No No No No No No No No No No
SP250 60 mL No
IP400 Solvent 35 mL No
70 % 20 s No
SP250 40 mL No
IP400 Solvent 2 10 mL Actual position Yes SP250 No
66
METTLER TOLEDO
M374-B
Base Number Determination in Used Oils by Conductometric Titration

Titration Excellence Line: Determination of the base number of various used oils by titration with 0.1 mol/L hydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe according to IP400/94. Sample
Used oils, 2-5 g

1) Titrant preparation: If not commercially available, the titrant can be prepared manually by adding 9 mL 37% v/v HCl and filling up to 1 L with 2-propanol (isopropanol). 2) 2-4 g oil are weighed into a glass titration bealer. 3) 60 mL solvent are added automatically by a peristaltic pump. 4) The titration is started after 300 s stirring time at 50% in order to achieve a complete dissolution of the sample.
Substance Chemicals
Alkaline components B, expressed as mg KOH/g sample 60 mL solvent mixture Toluene:isopropanol:distilled water (50% (v/v):49.5%(v/v):0.5%(v/v) ) HCl in 2-propanol: c(HCl) = 0.1 mol/L
Titrant
TRIS (THAM), 50 mg Titration Excellence Line, T50/70/90 Conductivity board ME-51109840 Rondo 20 Sample Changer Glass titration beaker ME-101446 SP250 Peristaltic pump ME-51108016 Printer, XP205 balance
Accessories

InLab718 conductivity probe
1) The conductivity probe is conditioned during 10 s in the fixed conditioning beaker of the Rondo 20 sample changer. 2) Most oil samples may create sticky residues. In this case, it is necessary to additionally clean the conductivity probe with a paper tissue soaked in solvent mixture. Afterwards, the probe is rinsed again with solvent mixture to remove the last impurities.
Neutralization of all basic components in oil. General neutralization reactions: 1) HCl + NaOH = NaCl + H2O 2) HCl + B = HB+ + ClBase number (mg KOH/g) R1= (Q-B[IP400])*C1/m C1= 56.1 B[IP400]: solvent blank value
Literature:
Calculation
1) IP400/94 Standard, British Institute of Petroleum (Now: Energy Institute, http://www.energyinst.org.uk/) 2) METTLER TOLEDO Applications M252/M253, and M099/ M100. 3) This application does not replace the standard.
Results
Author
Tobias Beckmann, MT-D
67
Results
Method ID: Date / Time: Summary Samples Nr. 1 AIP400 14/08/2007 12:00:28 Sample series ID User name -Administrator
ID WC 433591
WC 433591
WC 433591
Sample size and results 2.0134 g R1(BN) 6.373 R2(Titration time) 5.070 2.0717 g R1(BN) 6.396 R2(Titration time) 5.230 2.2171 g R1(BN) 6.438 R2(Titration time) 5.500
mg KOH/g min mg KOH/g min mg KOH/g min
Statistics R1(BN) Number of samples Mean value s srel
3 6.402 mg KOH/g 0.033 mg KOH/g 0.515 %
--------------------------------------------------------------------------------------------Different samples of used oils Sample Size / g n Base number mg KOH/g WC 529913 WC 526402 WC 471807 WC 457700 WC 541628 2.2 2.2 2.3 2.2 2.1 3 3 3 3 3 5.780 4.599 4.571 3.250 1.820
srel % 1.068 4.974 6.349 3.095 0.405
0.062 0.299 0.290 0.101 0.007
Titration curve
68
Method
Method Version AIP400 Conductometric BN 14/08/2007 12:00:28 007 Conditioning Type Interval Positioning Time Speed Condition 008 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 009 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 010 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V 2 2 d E/dV - V BETA - V E - t V - t dV/dt - t T - t E - V & DE/dV - V V - t & dV/dt - V Method Series data Condition 011 End of sample ---------------------------------------------------Blank value determination and storage as B[IP400] ...... Control Control User Titrant addition Incremental dV 0.01 mL Meas. val. acquisition Equilibrium controlled dE 0.5 S dt 1.0 s t(min) 10 s t(max) 20 s Evaluation and Recognition Procedure Segmented Threshold 0.5 S mL2 Ranges 0 Add. EQP criteria Steepest jump Steepest jumps 1 Termination At Vmax 1.5 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Fix 1 Conditioning beaker 10 s 30 % No
001 Title Type Compatible with ID Titel Author Date / Time Modified at Modified by Protect SOP 002 Sample Number of IDs ID 1 Entry Type Lower limit Upper limit Density Correction factor Temperature Entry 003 Titration stand (Rondo/Tower A) Type Titration stand Lid handling 004 Pump Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time Control Control Titrant addition dV Meas. val. acquisition dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Ranges Add. EQP criteria Steepest jumps Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition
General titration T50/T70/T90 AIP400 Conductometric BN Administrator 14/08/2007 09:19:49 14/08/2007 12:00:28 Administrator No None
1 WC 433591 Weight 0.0 g 5.0 g 1.0 g/mL 1.0 25.0 C Before
BN mg KOH/g R1=(Q-B[IP400])*C/m 56.1 M[None] z[None] 3 No Yes No No No
IP400 60 mL No
Titration time min R2=t -M[None] z[None] 3 No No No No No
50 % 300 s No
Per series Per sample Per sample

Per sample No
HCl in 2-Propanol 0.1 mol/L Conductivity InLab 718 S No 30 % None 0 s User Incremental 0.05 mL Equilibrium controlled 1.0 S 2 s 3 s 15 s Segmented 2 10 S mL 0 Steepest jump 1 10 mL No No Yes 1 No No No
No No
No No No No No No No No No No
69
METTLER TOLEDO
M375
Titer of 0.1 mol/L HCl in 2-Propanol by Conductometric Titration (IP400)

Titration Excellence Line: Titer determination of 0.1 mol/L hydrochloric acid in 2-propanol (isopropanol, IPA) by conductometric titration using TRIS (Tris-hydroxymethyl-aminomethane, THAM) as a primary standard. Sample
Primary standard: TRIS (THAM), 50-80 mg

1) Titrant preparation: If not commercially available, the titrant can be prepared manually by adding 9 mL 37% v/v HCl and filling up to 1 L with 2-propanol (isopropanol). 2) 50-80 mg TRIS are weighed into a glass titration bealer. 3) 60 mL solvent are added automatically by a peristaltic pump. 4) The titration is started after 120 s stirring in order to achieve a complete dissolution of TRIS.
Substance Chemicals
TRIS, Tris-hydroxymethyl-aminomethane M=121.14, z=1 60 mL solvent mixture Toluene:isopropanol:distilled water (50% (v/v):49.5%(v/v):0.5%(v/v) ) HCl in 2-propanol: c(HCl) = 0.1 mol/L
Titrant
-Titration Excellence Line, T50/70/90 Conductivity board ME-51109840 Rondo 20 Sample Changer Glass titration beaker ME-101446 SP250 Peristaltic pump ME-51108016 Printer, XP205 balance
Accessories

InLab718 conductivity probe
1) The conductivity probe is conditioned during 10 s in the fixed conditioning beaker of the Rondo 20 sample changer.
Neutralization of all basic components in oil. General neutralization reactions: 1) HCl + NaOH = NaCl + H2O 2) HCl + B = HB+ + ClTiter determination R = m/(VEQ*c*C) C = M/(10*p*z) p: purity of solid primary standard [%]
Literature: 1) IP400/94 Standard, British Institute of Petroleum (Now: Energy Institute, http://www.energyinst.org.uk/) 2) METTLER TOLEDO Applications M099/M100, M253 3) This application does not replace the standard.
Calculation
Results
Author
Tobias Beckmann, MT-D
70
Results
Method ID: Date / Time: AIP8014 14/08/2007 10:01:04 Sample series ID User name -Administrator
All results Method ID Sample 1/3 R1 Sample 2/3 R1 Sample 3/3 R1 Statistics Method ID R1 (Titer) Number of samples Mean value s srel All results R2(mean Titer)
AIP8014 TRIS 0.986 TRIS 0.993 TRIS 0.995
AIP8014 3 0.991 0.005 0.477
0.991
Titration curve
71
Method
Method Version AIPB8014 Titer HCl in 2-Propanol 14/08/2007 10:01:04 007 Conditioning Type Interval Positioning Time Speed Condition 008 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 009 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d E/dV - V ........... Method Series data Condition 010 End of sample 011 Titer Titrant Concentration TITER= Limits Condition 012 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition 013 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition
2 2
001 Title Type Compatible with ID Titel Author Date / Time Modified at Modified by Protect SOP 002 Sample (Titer) Titrant Concentration Standard Type of standard Entry Type Low limit Upper limit Correction factor Temperature Entry 003 Titration stand (Rondo/Tower A) Type Titration stand Lid handling 004 Pump Auxiliary reagent Volume Condition 005 Stir Speed Duration Condition 006 Titration (EQP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time Control Control Titrant addition dV Meas. val. acquisition dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Ranges Add. EQP criteria Termination At Vmax At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition
General titration T50/T70/T90 AIP8014

Titer HCl in 2-Propanol
Fix 1 Conditioning beaker 10 s 30 % No
Administrator 14/08/2007 09:19:49 14/08/2007 10:01:04 Administrator No None
HCl in 2-Propanol 0.1 mol/L TRIS Solid Weight 0.05 g 0.08 g 1.0 25.0 C Arbitrary
Titer -R1=m/(VEQ*c*C) M/(10*p*z) M[TRIS] z[TRIS] 3 No Yes No No No
No Per sample Per sample

No No
No No
IP400 60 mL No
No No No
40 % 120 s No
HCl in 2-Propanol 0.1 mol/L Conductivity InLab 718 S No 30 % None 0 s User Incremental 0.1 mL Equilibrium controlled 1.0 S 2 s 3 s 30 s Segmented 10 S mL2 0 No 10.0 mL No No Yes 1 No No No
HCl in 2-Propanol 0.1 mol/L Mean[R1] No No
Mean Titer -R2=Mean[R1] 1 M[None] z[None] 3 No Yes No No No
72
METTLER TOLEDO
M376
Anionic Content in Shower Gels by Potentiometric Two-Phase Titration

Titration Excellence Line: Determination of anionic surfactant content in shower gels by titration with 0.004 mol/L Hyamine 1622 in a two-phase mixed system using a DS800 TwoPhase electrode according to DIN EN 14480-2004. Sample
5 mL aliquots of aqueous solutions prepared with shower gels and shampoo.
Anionics as Na-dodecylsulfate, C12 H25 NaO4S

Note: MIBK is an organic solvent which is strongly and intensively smelling. It is recommended to work in a fume hood. 1) 40 mL of deionised water are added to the 5 mL sample. 2) The titration beaker is placed on the Rondolino sample changer. 3) The pH value is first adjusted to pH 3 with HCl by means of the second titration burette (EN DIN 14480). 4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensed by means of an additional dosing unit. MIBK: Methylisobutylketone (4-Methylpentan-2-one) EtOH: Ethanol 5) To obtain a homogeneous emulsion the solution is stirred at a high speed (80%). 6) The anionic surfactant content is expressed as SDS content, i. e. the molecular mass of SDS is used for the calculation. DS800 TwoPhase surfactant sensitive electrode: 1) Fill the DS800 TwoPhase and the electrode tip with the electrolyte. 2) Screw the electrode tip onto the shaft. 3) Shake the electrode 2-3 times to avoid the presence of air bubbles into the electrode tip. Rinse it with deion. water. 4) Condition the electrode first in deionised water for e.g. 15 minutes, and then perform 1-2 test titrations with the sample.
Substance Chemicals
M(SDS)=288.38 g/mol, z=1 40 mL deion water 20 mL MIBK:EtOH 1:1 solvent
Titrant
Hyamine 1622, c(Hyamine)=0.004 M Hydrochloric acid, HCl, c(HCl)=0.1 M
SDS (for Hyamine), THAM (for HCl) Titration Excellence Line T70/T90 2 additional dosing units Rondolino Sample Changer Titration beaker ME-101974
Accessories

DS800 TwoPhase surfactant electrode, InLab RReference , DG111-SC SDS- + Hyamine + = SDS-Hyamine
1) The determination of anionic surfactants is performed at pH 3 according to DIN EN 14480. This is perfomed to avoid interference due to the presence of free fatty acids (FFA) in the products, otherwise the result will be higher. In fact, at pH 3 the FFA are fully protonated, therefore they can not be titrated with hyamine. 2) Standard solutions of the different products are prepared by dissolving in 1 L volumetric flask approx. 5-10 g of the products. The resulting concentration in g/L = mg/mL is stored as auxiliary value e.g. H[Anionic] in the titrator. 3) The electrode is cleaned and conditioned after each sample in deionised water in the conditioning beaker of Rondolino (Position 5: 120 s). 4) When working with the LabX Software, select "Rondolino Mode" in the LabX window at the PC and activate it. Literature: 1) DIN EN 14480-2004 2) METTLER TOLEDO Application brochure 34, "Selected METTLER TOLEDO methods for Titration Excellence Line", ME-51 725 066. 3) METTLER TOLEDO Application brochure 22, "Surfactant titration", ME-51 725 015.
Calculation
R1=Q[2]*C/m C= M/(10*z)
Results
Neutralize the sample solution before final disposal as organic solvent.
Author
C. De Caro
73
Results
Method ID: Date / Time: All results Method ID Sample 1/5 R1 Sample 2/5 R1 Sample 3/5 R1 Sample 4/5 R1 Sample 5/5 R1 Statistics Method ID R1 (Content) Number of samples Mean value s srel 0214 09/07/2007 07:50:32 Sample series ID User name -Administrator
0214LAS 0214 24.726 % 0214 24.677 % 0214 24.669 % 0214 24.622 % 0214 24.641 %
0214LAS 5 24.667 % 0.040 % 0.161 %
---------------------------------------------------------------------------------------------Different samples Sample type exp./%SDS n Result s srel content /%SDS /%SDS /% 0214 0273 0411 0193 0Liq viscous viscous powder 24 25 20 5 8 8 7 3 5 5 6 6 9 24.667 24.494 25.290 25.291 20.274 20.303 9.303 9.253 7.317 7.365 0.040 0.033 0.034 0.031 0.055 0.073 0.031 0.048 0.060 0.080 0.161 0.136 0.136 0.123 0.273 0.359 0.332 0.521 0.817 1.092 pH 3 pH 5.5 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 H[0214]=0.005056 g/L H[0273]=0.005019 g/L H[0411]=0.010012 g/L H[0193]=0.010033 g/L H[0Liq]=0.00805 g/L
formulation 8-9 liquid det. 5-15
Titration curve
74
Method
Method Version 0214 SDS content potentiometric 09/07/2007 07:50:32 008 Titration (EQP) [2] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Volume Wait time [s] Control Control Titrant addition dE(set value) dV(min) dV(max) Mode dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential At slope After number of recognized EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 009 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 010 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d 2E/dV2 - V .... Method Series data Condition 011 End of sample 012 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition Hyamine 1622 0.004 mol/L mV DS800 mV No 80 % Volume 1.5 mL 15 s User Dynamic 8.0 mV 0.01 mL 0.4 mL Equilibrium controlled 1.0 mV 1 s 5 s 30 s Standard 100 mV/mL Positive 0 No 8 No No No No No No
001 Title Type Compatible with ID Titel Author Date / Time Modified at Protect SOP 002 Sample Number of IDs ID 1 Entry Type Volume Density Correction factor Temperature [C] 003 Titration stand (Rondolino TTL) Type Titration stand 004 Stir Speed Duration Condition 005 Titration (EP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time [s] Control End point type Tendency End point value Control band Dosing rate (max) Dosing rate (min) Termination At EP Termination delay At Vmax Max. time Accompanying stating Accompanying stating Condition Condition 006 Dispense (normal) [1] Titrant Concentration Volume Dosing rate Condition 007 Stir Speed Duration Condition
General titration T70/ T90 0214

SDS content potentiometric
Administrator 06/07/2007 17:56:59 09/07/2007 07:50:32 No None
1 0214 Fixed volume 5 mL 1.0 1.0 25.0
35 % 45 s No
HCl 0.1 mol/L pH DG111-SC pH No 30 % None 0 Absolute Negative 3 pH 2.0 pH 10.0 mL/min 500 L/min Yes 0 s 10.0 mL Infinite No No
Content % R1=Q[2]*C/(m*H[0214]) M/(10*z) M[Sodium dodecylsulfate] z[Sodium dodecylsulfate] 3 No Yes No No

Yes No
Last titration function Last titration function
MIBK-EtOH 1:1 1 20 mL 60.0 mL/min No
No No No No No
80 % 60 s No
Yes Yes No No No No No No
75
METTLER TOLEDO
M377
Anionic Content in Cutting Oils by Potentiometric Two-Phase Titration

Titration Excellence Line: Determination of anionic surfactant content in cutting oils by titration with 0.004 mol/L Hyamine 1622 in a two-phase mixed system using a DS800 TwoPhase electrode according to DIN EN 14480-2004 (pH 3). Sample
0.1-0.3 g cutting oil, depending on anionic surfactant content.

Note: MIBK is an organic solvent which is strongly and intensively smelling. It is recommended to work in a fume hood. 1) 40 mL of deionised water are added to the 5 mL sample. 2) The titration beaker is placed on the Rondolino sample changer. 3) The pH value is adjusted to pH 3 (DIN EN 14480) with HCl or to pH 11 with NaOH by means of the second titration burette. 4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensed by means of an additional dosing unit. MIBK: Methylisobutylketone (4-Methylpentan-2-one) EtOH: Ethanol 5) To obtain a homogeneous emulsion the solution is stirred at a high speed (80%). 6) The anionic surfactant content is expressed as SDS content, i. e. the molecular mass of SDS is used for the calculation. DS800 TwoPhase surfactant sensitive electrode: 1) Fill the DS800 TwoPhase and the electrode tip with the electrolyte. 2) Screw the electrode tip onto the shaft. 3) Shake the electrode 2-3 times to avoid the presence of air bubbles into the electrode tip. Rinse it with deion. water. 4) Condition the electrode first in deionised water for e.g. 15 minutes, and then perform 1-2 test titrations with the sample.
Substance Chemicals
Anionics as Na-dodecylsulfate, C12 H25 NaO4S
M(SDS)=288.38 g/mol, z=1 40 mL deion water 20 mL MIBK:EtOH 1:1 solvent
Titrant
Hyamine 1622, c(Hyamine)=0.004 M Hydrochloric acid, HCl, c(HCl)=1 M Sodium hydroxide, c(NaOH)=1 M SDS (for Hyamine) Titration Excellence Line T70/T90 2 additional dosing units Rondolino Sample Changer Titration beaker ME-101974
Accessories

DS800 TwoPhase surfactant electrode, InLab RReference , DG111-SC SDS- + Hyamine + = SDS-Hyamine
1) The determination of anionic surfactants is performed at pH 3 according to DIN EN 14480. This is done in order to avoid interference due to the presence of free fatty acids (FFA) in the products, otherwise the result will be higher. In fact, at pH 3 the FFA are fully protonated, therefore they can not be titrated with hyamine. 2) In the case where samples contain anionic surfactants with R-COOH end groups, it is necessary to titrate the sample at an alkaline pH value of e.g. pH 11 (see also DIN EN 14669) to be able to precipitate them with Hyamine. 3) The electrode is cleaned and conditioned after each sample in deionised water in the conditioning beaker of Rondolino (Position 5: 120 s). 4) When working with the LabX Software, select "Rondolino Mode" in the LabX window at the PC and activate it. Literature: 1) DIN EN 14480-2004 and 14669-2005 2) METTLER TOLEDO Application brochure 34, "Selected METTLER TOLEDO methods for Titration Excellence Line", ME-51 725 066. 3) METTLER TOLEDO Application brochure 22, "Surfactant titration", ME-51 725 015.
Calculation
R1=Q[2]*C/m C= M/(10*z)
Results
Neutralize the sample solution before final disposal as organic solvent.
Author
C. De Caro
76
Results
Method ID: m377 Date / Time: 11/12/2007 09:02:23 am Summary Samples No. ID 1 00883-03 2 3 4 5 6 00883-03 00883-03 00883-03 00883-03 00883-03 Sample series ID User name -Administrator
Content) 4.88 % Statistics R1 (Anionics Content) Number of samples 6 Mean value 4.87 % s 0.03 % srel 0.636 % =========================================================================================== Various samples n Result/%SDS s/%SDS srel/% ------------------------------------------------------------------00883-03 6 4.87 0.03 0.576 pH 3 01325-01 02800-01 C93 18656 3 5 6 6 6 6 6 6 6 4 6 4 6 2.73 2.66 2.01 61.07 61.14 61.48 30.93 30.96 30.92 13.57 13.61 4.49 4.55 0.02 0.02 0.01 0.47 0.31 0.48 0.05 0.08 0.04 0.17 0.20 0.05 0.01 0.559 0.734 0.733 0.764 0.506 0.783 0.155 0.256 0.141 1.228 1.486 1.155 0.231 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 pH 3 pH pH pH pH 11 11 11 11 0.004 0.01 0.004 0.01 M M M M Hyamine CPC Hyamine CPC
Sample size 0.1773 g R1(Anionics 0.1873 g R1(Anionics 0.1537 g R1(Anionics 0.2101 g R1(Anionics 0.1782 g R1(Anionics 0.1624 g R1(Anionics
and results Content) Content) Content) Content) Content) 4.91 % 4.88 % 4.82 % 4.86 % 4.86 %
V43 18571
11675-01 01125-02
Titration curve
77
Method
Method Version m377 SDS content potentiometric 11/12/2007 09:02:23 am 008 Titration (EQP) [2] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time [s] Control Control Titrant addition dE(set value) dV(min) dV(max) Mode dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential At slope After number of recognized EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 009 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 010 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V log dE/dV - V d 2E/dV2 - V .... Method Series data Condition 011 End of sample 007 Stir Speed Duration Condition 80 % 60 s No 012 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition Hyamine 1622 0.004 mol/L mV DS800 mV No 80 % None 0 s User Dynamic 8.0 mV 0.1 mL 0.5 mL Equilibrium controlled 0.5 mV 2 s 8 s 45 s Standard 30 mV/mL Positive 0 No 20 mL No No No No No No
001 Title Type Compatible with ID Titel Author Date / Time Modified at Protect SOP 002 Sample Number of IDs ID 1 Entry Type Lower limit Upper limit Density Correction factor Temperature [C] Entry 003 Titration stand (Rondolino TTL) Type Titration stand 004 Stir Speed Duration Condition 005 Titration (EP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time [s] Control End point type Tendency End point value Control band Dosing rate (max) Dosing rate (min) Termination At EP Termination delay At Vmax Max. time Accompanying stating Accompanying stating Condition Condition 006 Dispense (normal) [1] Titrant Concentration Volume Dosing rate Condition
General titration T70/ T90 m377

SDS content potentiometric
Administrator 11/12/2007 07:22:42 am 11/12/2007 09:02:23 am No None
1 00883-03 Weight 0 g 5 g 1.0 g/mL 1.0 25.0C Before
35 % 60 s No
HCl 1 mol/L pH DG111-SC pH No 35 % None 0 Absolute Negative 3 pH 2.0 pH 10.0 mL/min 500 L/min Yes 0 s 10.0 mL Infinite No No
Anionics Content % R1=Q[2]*C/m M/(10*z) M[Sodium dodecylsulfate] z[Sodium dodecylsulfate] 2 No Yes No No

Yes No
Last titration function Last titration function
No No No No No
MIBK-EtOH 1:1 1 20 mL 60.0 mL/min No
Yes Yes No No No No No No
78
METTLER TOLEDO
M378
Titer Determination of Hyamine by Potentiometric Two-Phase Titration

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

Note: MIBK is an organic solvent which is strongly and intensively smelling. It is recommended to work in a fume hood. 1) 40 mL of deionised water are added to the 5 mL sample. 2) The titration beaker is placed on the Rondolino sample changer. 3) The pH value is first adjusted to pH 3 with HCl by means of the second titration burette (EN DIN 14480). 4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensed by means of an additional dosing unit. MIBK: Methylisobutylketone (4-Methylpentan-2-one) EtOH: Ethanol 5) To obtain a homogeneous emulsion the solution is stirred at a high speed (80%).
Substance Chemicals
Sodium dodecylsulfate, C12 H25 NaO4S M(SDS)=288.38 g/mol, z=1 40 mL deion water 20 mL MIBK:EtOH 1:1 solvent
Titrant
Hyamine 1622, c(Hyamine)=0.004 M Hydrochloric acid, HCl, c(HCl)=0.1 M
For HCl: THAM (TRIS) Titration Excellence Line T70/T90 2 additional dosing units Rondolino Sample Changer Rondolino Sample Changer Titration beaker ME-101974
Accessories
DS800 TwoPhase surfactant sensitive electrode: 1) Fill the DS800 TwoPhase and the electrode tip with the electrolyte. 2) Screw the electrode tip onto the shaft. 3) Shake the electrode 2-3 times to avoid the presence of air bubbles into the electrode tip. Rinse it with deion. water. 4) Condition the electrode first in deionised water for e.g. 15 minutes, and then perform 1-2 test titrations with the sample.

DS800 TwoPhase surfactant electrode, InLab RReference , DG111-SC SDS + Hyamine + = SDS-Hyamine
-
Rondolino: 1) The electrode is cleaned and conditioned after each sample in deionised water in the conditioning beaker of Rondolino (Position 5: 120 s). 2) When working with the LabX Software, select "Rondolino Mode" in the LabX window at the PC and activate it.
Calculation
Titer: R=m/(VEQ[2]*c[2]*C) C=1/(cst*z) Note: "cst" is the concentration of the SDS standard solution.
Literature: 1) DIN EN 14480-2004 2) METTLER TOLEDO Application brochure 34, "Selected METTLER TOLEDO methods for Titration Excellence line", ME-51 725 066. 3) METTLER TOLEDO Application brochure 22, "Surfactant titration", ME-51 725 015.
Results
Organic solvent
Author
C. De Caro
79
Results
Method ID: Date / Time: Summary Samples No. 1 2 3 4 5 6 414Titer 06/07/2007 17:15:16 Sample series ID User name -Administrator
ID SDSTiter414 SDSTiter414 SDSTiter414 SDSTiter414 SDSTiter414 SDSTiter414
Sample size and results 5 mL R1 (Titer) 5 mL R1 (Titer) 5 mL R1 (Titer) 5 mL R1 (Titer) 5 mL R1 (Titer) 5 mL R1 (Titer) = = = = = = 1.002013 1.001679 1.000487 0.997958 0.998080 0.998976
Statistics R1 (Titer) Number of samples Mean value s srel Titer Titrant New titer Results R2 (Hyamine)
6 0.999866 0.001784 0.178%
Hyamine 1622 0.99987
0.999866
Titration curve
80
Method
Method Version 414Titer Titer Hyamine 1622 06/07/2007 17:15:16 Control Control Titrant addition dE(set value) dV(min) dV(max) Mode dE dt t(min) t(max) Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential At slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition 009 Calculation R1 Result Result unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 010 Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V ... Calibration curve Method Series data Condition 011 End of sample 012 Titer Titrant Concentration TITER= Limits Condition 013 Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Condition 014 Record Summary Results Raw results Resource data Calibration curve Method Series data Condition User Dynamic 8.0 mV 0.01 mL 0.5 mL Equilibrium controlled 1.0 mV 1 s 5 s 30 s Standard 100 mV/mL Positive 0 No 10 No No Yes 1 No No No Titer R=m/(VEQ[2]*c[2]*C) 1/(cst*z) M[None] z[None] 6 No Yes No No No Per sample Per sample
001 Title Type Compatible with ID Titel Author Date / Time Modified at Protect SOP 002 Sample (Titer) Titrant Concentration Standard Type of standard Entry Type Volume Correction factor Temperature [C] 003 Titration stand (Rondolino TTL) Type Titration stand 004 Stir Speed Duration Condition 005 Titration (EP) [1] Titrant Titrant Concentration Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Wait time [s] Control End point type Tendency End point value Control band Dosing rate (max) Dosing rate (min) Termination At EP Termination delay At Vmax Max. time Accompanying stating Accompanying stating Condition Condition 006 Dispense (normal) [1] Titrant Concentration Volume Dosing rate Condition 007 Stir Speed Duration Condition 008 Titration (EQP) [2] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed Predispense Mode Volume Wait time [s]
General titration T70/ T90 414Titer Titer Hyamine 1622 Administrator 28/08/2006 14:53:19 06/07/2007 17:15:16 No None Hyamine 1622 0.004 mol/L SDSTiter414 liquid Fixed volume 5 mL 1.0 25.0 Rondolino TTL Rondolino TTL 1 30 % 45 s No
HCl 0.1 mol/L pH DG111-SC pH No 35 % None 0 Absolute Negative 3 pH 2.0 pH 0.2 mL/min 50 L/min Yes 0 s 10.0 mL Infinite No No MIBK-EtOH 1:1 1 20 mL 60.0 mL/min No 80 % 60 s No
No No
No No No No No
Hyamine 1622 0.004 mol/L Mean[R] No No Titer Hyamine R2=Mean[R1] M[None] z[None] 6 No Yes No No Yes No No No No No No No
Hyamine 1622 0.004 mol/L mV DS800 mV No 80 % Volume 1.5 mL 15 s
81
METTLER TOLEDO
M379
Acid and Chloride Content in Wine

Titration Excellence Line: Method for the determination of tartaric acid and chloride in wine
Sample
Wine, 40 mL

Before the acid content analysis is performed the pH electrode needs to be adjusted by use of the METTLER TOLEDO buffers 4.01, 7.00 and 9.21 and method M436.
Substance Chemicals
Tartaric acid ((CHOH) 2(COOH)2) Chloride (Cl -)

H2SO4 (10%)
Titrant
NaOH, 1.0 mol/L (sodium hydroxide) AgNO3, 0.02 mol/L (silver nitrate)
NaCl for AgNO 3, KHP for NaOH Titration Excellence T70/T90 2 additional dosing units
Accessories
LabX Pro Titration ME-51106500 Rondo30 sample changer (51108004) with sample beakers (51108030)

DGi102-Mini (pH sensor) DMi102-SC (silver electrode) EP titration: C 4H6O6 + 2NaOH = Na2C 4H4O6 +2H2O EQP titration: Cl- + Ag + + NO3- = AgCl + NO3When working with Rondo30 and two mini electrodes lower sample volumes can be used for two consecutive titrations in the same sample. In this method conditioning in the conditioning beaker is used for electrode cleaning, alternatively, rinsing with the Rondo30 power shower can be used. When automation with Rondo30 is not required, microtitration beakers can also be used when wanting to use smaller sample volumes.
Calculation
R1: Consumption NaOH (mL) R2: Measurement pH value (pH) R3: Chloride content (mg/L)
Results
AgCl has to be disposed of as special waste.
Author
Melanie Nijman
82
Results
Method Measured RESULTS No. 1
m379 Acid and Chloride Content in Wine 11.10.2007
ID Wine
Wine
Wine
Wine
Wine
Wine
Sample size and results 40.0 ml R1 = 3.0744 ml R2 = 1.660 pH R3 = 33.6713 mg/L 40.0 ml R1 = 3.0925 ml R2 = 1.662 pH R3 = 33.7785 mg/L 40.0 ml R1 = 3.1120 ml R2 = 1.670 pH R3 = 33.8016 mg/L 40.0 ml R1 = 3.0839 ml R2 = 1.669 pH R3 = 33.7493 mg/L 40.0 ml R1 = 3.0739 ml R2 = 1.669 pH R3 = 33.7564 mg/L 40.0 ml R1 = 3.0859 ml R2 = 1.671 pH R3 = 33.8069 mg/L
Content pH value Chloride content Content pH value Chloride content Content pH value Chloride content Content pH value Chloride content Content pH value Chloride content Content pH value Chloride content
STATISTICS Number results R1 Mean value Standard deviation Relative standard deviation Number results R2 Mean value Standard deviation Relative standard deviation Number results R3 Mean value Standard deviation Relative standard deviation
n = x = s = srel = n = x = s = srel = n = x = s = srel =
6 3.0871 0.0141 0.4570 6 1.667 0.005 0.277
ml %
Consumption Consumption
pH %
pH value pH value
6 33.7607 mg/L 0.0495 0.1470 %
Chloride content Chloride content
Titration curve
83
Method
Method: User: m379 Acid and Chloride Content in Wine 10.10.2007 Nijman
Predispense Mode Volume [mL] Wait time [s] Control Control Titrant addition dE (set value) dV (min) dV (max) Mode dE dt [s] t(min) [s] t(max) [s] Evaluation and Recognition Procedure Threshold Tendency Ranges Add. EQP criteria Termination At Vmax [mL] At potential At Slope After number of recognized EQPs Number of EQPs Combined termination criteria Accompanying stating Accompanying stating Condition Condition Calculation R1 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition Calculation R2 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition Calculation R3 Result Result Unit Formula Constant C= M z Decimal places Result limits Record statistics Extra statistical functions Send to buffer Condition Conditioning Type Interval Position Time [s] Speed [%] Condition Record Summary Results Raw results Table of measured values Sample data Resource data E - V dE/dV - V ...... Condition End of sample Volume 0.2 5 User Dynamic 6 0.02 0.2 Equilibrium controlled 1.0 2 10 30 Standard 150 None 0 No 6.0 No No Yes 1 No No No Consumption mL R1=VEQ[1] 1 M[None] z[None] 5 No Yes No No No pH value pH R2=E 1 M[None] z[None] 3 No Yes No No No Chloride content mg/L R3=Q[2]*C/m M*1000/z M[Chloride] z[Chloride] 5 No Yes No No No Fix 1 Conditioning beaker 20 35 No No Per Per No No No All All No
001 Title Type Compatible with ID Titel Author Date / Time Modified at Protect SOP LabX SOP 002 Sample Number of IDs ID 1 Entry Type Volume [mL] Density [g/mL] Correction factor Temperature [C] 003 Titration stand Type Titration stand Lid handling 004 Stir Speed [%] Duration [s] Condition 005 Titration (EP) [1] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%] Predispense Mode Wait time [s] Control Mode Tendency End point value Control band Dosing rate (max) [mL/min] Dosing rate (min) [mL/min] Termination At EP Termination delay [s] At Vmax [mL] Max. time[s] Accompanying stating Accompanying stating Condition Condition 006 Dispense (normal) [1] Titrant Concentration [mol/L] Volume [mL] Dosing rate [mL/min] Condition 007 Measure (normal) [1] Sensor Type Sensor Unit Temperature acquisition Temperature measurement Stir Speed [%] Aquisition of measured values Aquisition dE dt [s] t(min) [s] t(max) [s] Mean value Condition Condition 008 Titration (EQP) [2] Titrant Titrant Concentration [mol/L] Sensor Type Sensor Unit Temperature aquisition Temperature measurement Stir Speed [%]
General titration T70/ T90 MxxxMN2 Acid and Chloride Content in Wine Mettler Toledo 10.10.2007 10.10.2007 No None
1 Wine Fixed volume 40.0 1.0 1.0 25.0 Rondo60/Tower A Rondo60/1A No 30 10 No
NaOH 1.0 pH DG102-Mini pH No 30 None 0
009
010 Absolute None 7.0 0.2 20 300 Yes 0 5 20000 No No H2 SO4 10% 1 2.0 60.0 No 011
pH DG102-Mini pH No 30 Equilibrium controlled 0.5 1 10 30 No No
012
013
sample sample
titration functions titration functions
AgNO3 0.02 014 mV DM102-SC mV No 30
84
The methods in this brochure represent selected, possible application examples. These have been tested with all possible care with the analytical instruments mentioned in the brochure. The experiments were conducted and the resulting data evaluated based on our current state of knowledge. However, the applications do not absolve you from personally testing their suitability for your intended methods, instruments and purposes. As the use and transfer of an application example are beyond our control, we cannot accept responsibility therefore. When chemicals and solvents are used, the general safety rules and the directions of the manufacturer must be observed.
Application Brochure 35 A Choice of Methods for Various Probes

The models of the Titration Excellence line of METTLER TOLEDO are an ideal base to build fully automated titration systems. Thanks to the method concept and the color touch screen, operation is made easy. A single sample or an entire series of samples can be started with a touch to the shortcut: True One Click Titration. This Application Brochure contains a selection of methods illustrating the applicative power or METTLER TOLEDO.
Titration Excellence Line T70 Terminal, Rondo 20 with PowerShower and LabX titration
Plug & Play Electrodes Reliable and secure handling
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Mettler-Toledo AG, Analytical Sonnenbergstrasse 74 CH-8603 Schwerzenbach, Switzerland Tel +41-44 806 77 11 Fax +41-44 806 73 50 Subjet to technical changes. 12/2009 Mettler-Toledo AG Market Support AnaChem
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Selected Applications

Excellence Line Titrators

Selected Applications for METTLER TOLEDO Titration Excellence Line

Buffer Capacity of Coca Cola

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

Blank Value of Acid Number Solvent According to ASTM D664-07

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

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

Buffer Value pH 4 for Acid Number According to ASTM D664-07

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

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

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

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

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

m-Value of Tap Water with Automatic Temperature Compensation

Na2O and SiO2 in Waterglass

Chloride Content in Used Motor Oil

Peroxide Value of edible Oils and Fats

Titer Determination of 0.01 mol/L Na2S2O3

Chloride Determination in Ethanol

Titer Determination of 0,001 mol/L AgNO3

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

Base Number Determination in Fresh Oils by Conductometric Titration According to IP400-1994

Base Number Determination in Used Oils by Conductometric Titration According to IP400-1994

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

Titration Probes: An Overview

InLab717 Conductometric titration Conductivity range:

InLab718 Conductometric titration Conductivity range:

DS500 Surfactant Titration Medium:: Aqueous solutions

DS800-TwoPhase Surfactant Titration Medium: Mixed two-phase system (water, MIBK)

pH electrodes for aqueous media

Electrolyte 3 mol/L KCl

3 mol/L KCl saturated with AgCl

Reference electrolyte: 3 mol/L KCl

Bridge electrolyte: selectable (standard delivery : 3 mol/L KCl)

Bridge electrolyte: 1 mol/L KCl

pH electrodes for non-aqueous media

Electrolyte 1 mol/L LiCl in ethanol

1 mol/L LiCl in ethanol

Silver ring electrodes

Platinum ring electrode

3 mol/L KCl saturated with AgCl

Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl

Preparation and Procedures

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

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

Remarks Indication Chemistry

Waste Waste disposal disposal

Neutralize the sample before final disposal as aqueous solution

Table of measured values

Buffer Capacity of Coca Cola

Preparation and Procedures

pH 4, 7 and 9 buffer solutions

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

Remarks Indication Chemistry

HX + NaOH = NaX + H2O

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

Waste Waste disposal disposal

Neutralization before final disposal as aqueous solution.

Table of measured values

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

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

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

R1= m/(VEQcC) C=(10pz) p: purity of standard