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35Application Brochure
Excellence Line Titrators
Selected Applicationsfor METTLER TOLEDO Titration Excellence Line
METTLER TOLEDO
I
Contents Method Electrode Title Page
M361 DGi112-Pro Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl 1
M362 DGi112-Pro Buffer Capacity of Coca Cola 4
M363-A DGi116-
Solvent Acid Number in Used Motor Oil According to ASTM D664-07 7
M363-B DGi116-
Solvent
Blank Value of Acid Number Solvent
According to ASTM D664-07 10
M363-C DGi116-
Solvent
Blank Value for Strong Acid Number 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
Buffer Value pH 4 for Acid Number
According to ASTM D664-07 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
II
M368 DMi145-SC Titer Determination of 0.01 mol/L AgNO3 in 2-Propanol 46
M369 DMi147-SC Peroxide Value of edible Oils and Fats 49
M370 DMi147-SC Titer Determination of 0.01 mol/L Na2S2O3 52
M371 DMi148-SC Chloride Determination in Ethanol 55
M372 DMi148-SC Titer Determination of 0,001 mol/L AgNO3 58
M373 DM405-SC Mercaptan Sulfur Content in Kerosine
According to ASTM D3227-04a 61
M374-A InLab®718 Base Number Determination in Fresh Oils
by Conductometric Titration According to IP400-1994 64
M374-B InLab®718 Base Number Determination in Used Oils
by Conductometric Titration According to IP400-1994 67
M375 InLab®718 Titer Determination of 0.1 mol/L HCl in 2-Propanol
by Conductometric Titration 70
M376 DS800 -
TwoPhase
Anionic Content in Shower Gels by Potentiometric Two-Phase
Titration According to DIN EN 14480 73
M377 DS800-
TwoPhase
Anionic Content in Cutting Oils by Potentiometric Two-Phase
Titration According to DIN EN 14480 76
M378 DS800-
TwoPhase
Titer Determination of 0.004 mol/L Hyamine by Potentiometric
Two-Phase Titration According to DIN EN 14480 79
M379 DGi102-Mini
DMi102-Mini Acid and Chloride Content in Wine 81
III
Titration Probes: An Overview
DGi101-SC DGi102-Mini DGi111-SC DGi112-Pro DGi114-SC DGi115-SC DGi117-Water
DGi113-SC DGi116-Solvent DG300-SC Half-Cell pH sensor
DX200 Glass reference sensor
DX202-SC Plastic reference sensor
IV
DMi102-SC DMi141-SC DMi145-SC DMi148-SC DM405-SC
DMi101-SC DMi140-SC DMi144-SC
Sensor for Rondo 20 COD set 149.5 mm
DMi147-SC DM143-SC Sb850-S7/120
InLab®717 Conductometric
titration
Conductivity range: 10 μS/cm – 500 mS/cm
InLab®718 Conductometric
titration
Conductivity range: 0.1 – 200 μS/cm
DS500 Surfactant Titration
Medium:: Aqueous solutions
DS800-TwoPhase Surfactant Titration
Medium: Mixed two-phase system (water, MIBK)
V
pH electrodes for aqueous media Product name Electrolyte
Combined micro pH electrode for direct pH measurements and acid/base titrations in aqueous solutions:
- For very small sample volumes (min. volume 1 mL)
- pH range: 0-14
- Temperature range: 0-100°C
- 3 mm shaft
- ceramic junction
- ARGENTHALTM reference system (increased life span and heat resistance)
- Silver ion trap (avoid precipitation of e.g. silver sulfide at the ceramic junction)
- U glass bulb
-
DGi101-SC
3 mol/L KCl
Combined semi micro pH electrode for direct pH measurements and acid/base titrations in aqueous solutions
- For small sample volumes 1) 10-25 mL, suitable for micro-titration beaker ME-23516 2) Automation with Rondo 30 and Rondo 60 plus
- pH range: 0-14
- Temperature range: 0-100°C
- 6 mm shaft
- Ceramic junction
- ARGENTHALTM reference system (increased life span and heat resistance)
- Silver ion trap (avoid precipitation of e.g. silver sulfide at the ceramic frit)
- U glass bulb
DGi102-Mini
3 mol/L KCl
Combined pH electrode for general direct pH measurements and acid/base titrations:
- Standard aqueous solutions
- pH range: 0-14
- Temperature range: 0-80°C
- 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: 0-60°C
- 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: 0-60°C
- Movable PTFE-sleeve junction
- ARGENTHALTM reference system
- Tubular HA glass membrane
DGi114-SC
3 mol/L KCl
Combined pH electrode for direct pH measurements and acid/base titrations:
- Low ionic strength media (e.g. pure water, organic solvents such as alcohols)
- pH range: 0-14
- Temperature range: 0-100°C
- 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: 0-100°C
- ARGENTHALTM reference system, gold shielding
- Double junction with 3 M KCl-based reference gel electrolyte
- Fixed ground glass sleeve junction (higher electrolyte flow)
- Spherical LoT glass membrane with low resistance
DGi117-Water
Bridge electrolyte:
1 mol/L KCl
VII
pH electrodes for non-aqueous media Product name Electrolyte
Combined glass pH electrode for non-aqueous media with moderate electrostatic effects
- Acid/base titrations in standard organic solvents such as alcohols and acetic acid
- pH range: 0-12
- Temperature range: 0-60°C
- ARGENTHALTM reference system
- Movable PTFE-sleeve junction
- Tubular A41 glass membrane with low resistance (Membrane glass with excellent chemical resistance)
DGi113-SC
1 mol/L LiCl in ethanol
Combined glass pH electrode for non-aqueous matrices with strong electrostatic effects
- High performance titrations that require fast response times and quick equilibration of measured values
- Applications: 1. TAN/TBN determinations in oil products according to oil standards 2. Perchloric acid titrations 3. Cyclohexylamine and alcoholic HCl as titrants 4. Titrations using alcoholic KOH, NaOH, TBAOH and Na-Methylate as titrants, 5. Epoxy number in epoxy resins 6. Acid value and numbers (AN) in polymers 7. Free fatty acids (FFA) in oil or fat 8. Saponification number in resins
- pH range: 0-12
- Temperature range: 0-60°C
- 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
DGi116-Solvent
1 mol/L LiCl in ethanol
Silver ring electrodes
Combined semi micro silver ring electrode for argentometric precipitation titration in aqueous media
- For small sample volumes: 1) 10-25 mL, suitable for micro-titration beaker ME-23516 2) Automation with Rondo 30 and Rondo 60 plus
- Determination of e.g. chlorides, bromides, iodides, cyanides and thiocyanides
- Sulfidation is possible: titration of sulfides, hydrogen sulfides and mercaptans, in particular in petroleum and oil products
- Temperature range: 0-80°C
- 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: 0-80°C
- 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: 0-80°C
- 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: 0-80°C
- 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: 0-80°C
- 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: 0-80°C
- 6 mm shaft
- Ceramic junction, Ag/AgCl reference system
DMi101-Mini
3 mol/L KCl saturated with
AgCl
Combined platinum ring electrode for redox titration in aqueous media
- Oxidation with potassium permanganate
- Cerium sulfate (e.g. gold determination)
- Iodine (e.g. copper determination)
- Reduction with sodium thiosulfate (back titration reagent for iodometric determinations)
- Ammonium ferrous sulfate (back titration reagent)
- Temperature range: 0-80°C
- Ceramic junction
- Ag/AgCl reference system
DMi140-SC
3 mol/L KCl saturated with
AgCl
Combined platinum ring electrode for redox titration in aqueous media
- Dedicated electrode for automatic COD determinations on the Rondo 20 COD rack
- Temperature range: 0-80°C
- 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: 0-80°C
- Junction-free bulb pH glass reference, no electrolyte
DMi147-SC
--
X
XI
Double pin platinum electrode
- Voltametric titration 1. Karl Fischer titration 2. Vitamin C determination (Voltam. det. with DPI as a titrant) 3. Sulphur dioxide in wine 4. Bromine number and Bromine index (Petroleum products)
- Amperometric titration 1. Vitamin C determination (Amperom. det. with DPI as a titrant)
- No junction, no reference electrolyte
DM143-SC
--
Half-cell electrodes
Double junction glass half-cell reference electrode
- Ion selective measurements with ISE half-cell
- In combination with pH half cell electrodes in aqueous or non aqueous media
- In combination with metal half cell electrodes in aqueous or non aqueous media
- Temperature range: 0-80°C
- pH range: 0-14
- Fixed 4 mm banana plug cable
- Ag/AgCl reference system
- Movable glass sleeve junction
DX200
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
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: 0-80°C
- pH range: 0-14
- S7-screw cap connection
- Internal Ag/AgCl reference system
- Porous plastic junction
DX202-SC
Internal Ag/AgCl
reference system
(not refillable)
Bridge electrolyte: selectable
Standard delivery:
3 mol/L KCl 1 mol/L KNO3
Half cell pH electrode
- for direct pH measurements and acid/base titrations
- for difficult aqueous and non-aqueous matrices in conjunction with reference electrode DX200
- Temperature range: 0-100°C
- pH range: 0-13
- S7-Screw cap connection
DG300-SC
--
M361
Hydrochloric acid (HCl), Acetic acid (HOAc),
Ammonium chloride (NH4Cl), all approx. 0.1 mol/L
40 mL deionized waterpH 4, 7 and 9 buffer solutions
Sodium hydroxide (NaOH)c(NaOH) = 0.1 mol/L
Titration Excellence Line T70/T90Rondolino Sample Changer withPowerShowe and pump
pH 2.8-5.0:HCl+NaOH = Na++Cl-+H2OpH 5.0-9.0:HOAc+NaOH = -OAc+Na++H2OpH 9.0-11.5:NH4Cl+NaOH = Na++Cl-+NH3+H2O
Titration beaker ME-101974LabX Titration Software
METTLER TOLEDO
Neutralize the sample before finaldisposal as aqueous solution
Wastedisposal
Preparation and Procedures3 mL acidic mixture (1 mL of eachacid)
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi112-ProIndication
Buffer Capacity of the Acidic Mixture HCl, CH3COOH and NH4Cl
1) The electrode is calibrated using METTLER TOLEDO pH 4, 7and 9 buffer solutions.
2) The acidic mixture is prepared by adding 1 mL of each acidsolution into the titration beaker.
3) The mixture is diluted with 40 mL deionized water beforetitration. Since 3 mL acidic mixture is used , the total samplevolume is 43 mL.
4) After each sample, the electrode is rinsed with water during 2s and conditioned during 10 s (Rondolino mode: 6).
A mixture of three different acids (HCl, HOAc, NH4Cl) with clearlydifferent pKa values (HCl: -7, HOAc: 4.75, NH4Cl: 9.25) istitrated with 0.1 mol/L NaOH. The buffer capacity is used todescribe this complex mixture. Since three EQPs are found threedifferent half neutralization values can be calculated (HNV1-HNV3, see titration curve).
Three different series (6 samples) have been performed. Thestatistics of one series is shown below:
R1 HCl 0.1088 mol/L 0.00143 1.318R2 HOAc 0.08263 mol/L 0.00151 1.827R3 NH4Cl 0.09374 mol/L 0.00084 0.896
R4 BETAHNV1 3.47 mmol/(L*pH) 0.15824 4.56R5 BETAHNV2 1.18667 mmol/(L*pH) 0.00516 0.435R6 BETAHNV3 1.21333 mmol/(L*pH) 0.01033 0.851R7 BETAHNV1+2 4.65667 mmol/(L*pH) 0.15908 3.416R8 BETAHNV1+2+3 5.87 mmol/(L*pH) 0.15849 2.7
In the following the mean value range and the srel-rangeobtained for these three different series are shown:
R1: 0.1081 - 0.10939 0.7 - 2.4R2: 0.08263 - 0.08344 1.8 - 3.3R3: 0.09374 - 0.09455 0.9 - 1.5R4: 3.47 - 3.53833 3.0 - 8.8R5: 1.175 - 1.195 0.4 - 3.2R6: 1.21333 - 1.225 0.8 - 3.0R7: 4.65667 - 4.73333 1.7 - 6.2R8: 5.87 - 5.95833 1.5 - 4.8
Remarks
R1=Q1*C/1, C=1/z (HCl in mol/L)R2=Q2*C/1, C=1/z (HOAc in mol/L)R3=Q3*C/1, C=1/z (NH4Cl in mol/L)R4=BETAHNV1, unit: mmol/(L*pH)R5=BETAHNV2, unit: mmol/(L*pH)R6=BETAHNV3, unit: mmol/(L*pH)R7=BETAHNV1+BETAHNV2, unit: mmol/(L*pH)R8=BETAHNV1+BETAHNV2+BETAHNV3, unit:mmol/(L*pH)
Calculation
Titration Excellence Line: The buffer capacity of the acidic mixture HCl, CH3COOH and NH4Cl and theconcentration of each acid was determined by potentiometric titration with the DG112-Pro electrode.
Standard Potassium hydrogen phthalate, 80 mg
Thomas HitzAuthor
Wastedisposal
1
HNV1
HNV2 HNV3
HNV1
HNV2 HNV3
Table of measured values
No. Comment / ID Rx Result Unit Name 1/6 -- R1 = 0.109 mol/L HCl
R2 = 0.07941 mol/L HOAc R3 = 0.09244 mol/L NH4Cl R4 = 3.71 mmol/(L*pH) BETAHNV1 R5 = 1.15 mmol/(L*pH) BETAHNV2 R6 = 1.19 mmol/(L*pH) BETAHNV3 R7 = 4.86 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 6.05 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3
2/6 -- R1 = 0.10712 mol/L HCl R2 = 0.08107 mol/L HOAc R3 = 0.09558 mol/L NH4Cl R4 = 3.52 mmol/(L*pH) BETAHNV1 R5 = 1.17 mmol/(L*pH) BETAHNV2 R6 = 1.24 mmol/(L*pH) BETAHNV3 R7 = 4.69 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 5.93 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3
3/6 -- R1 = 0.10798 mol/L HCl R2 = 0.08468 mol/L HOAc R3 = 0.09327 mol/L NH4Cl R4 = 3.4 mmol/(L*pH) BETAHNV1 R5 = 1.26 mmol/(L*pH) BETAHNV2 R6 = 1.22 mmol/(L*pH) BETAHNV3 R7 = 4.66 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 5.88 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3
4/6 -- R1 = 0.10756 mol/L HCl R2 = 0.08358 mol/L HOAc R3 = 0.0955 mol/L NH4Cl R4 = 3.47 mmol/(L*pH) BETAHNV1 R5 = 1.19 mmol/(L*pH) BETAHNV2 R6 = 1.21 mmol/(L*pH) BETAHNV3 R7 = 4.66 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 5.87 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3
5/6 -- R1 = 0.10756 mol/L HCl R2 = 0.0863 mol/L HOAc R3 = 0.09445 mol/L NH4Cl R4 = 3.53 mmol/(L*pH) BETAHNV1 R5 = 1.19 mmol/(L*pH) BETAHNV2 R6 = 1.2 mmol/(L*pH) BETAHNV3 R7 = 4.72 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 5.92 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3
6/6 -- R1 = 0.10886 mol/L HCl R2 = 0.08557 mol/L HOAc R3 = 0.09606 mol/L NH4Cl R4 = 3.6 mmol/(L*pH) BETAHNV1 R5 = 1.21 mmol/(L*pH) BETAHNV2 R6 = 1.29 mmol/(L*pH) BETAHNV3 R7 = 4.81 mmol/(L*pH) BETAHNV1+BETAHNV2 R8 = 6.1 mmol/(L*pH) BETAHNV1+BETAHNV2+BETAHNV3
Titration curve
Results
2
Method: m361 Buffer Capacity 08.01.2008User: Thomas Hitz
001 Title Typ General titration Compatible with T70/T90 ID m361 Titel Buffer Capacity Author Thomas Hitz Date / Time 08.01.2008 Modified at 08.01.2008 Protect No SOP None002 Sample
Number of IDs 1 ID 1 -- Entry Type Fixed volume Volume [mL] 43 Density [g/ml] 1 Correction factor 1.0 Temperature [°C] 25.0°C003 Titration stand (Rondolino TTL) Typ Rondolino TTL Titration stand Rondolino TTL 1004 Stir Speed 50 % Duration 20 s Condition No005 Titration (EQP) [1]
Titrant Titrant NaOH Concentration [mol/L] 0.1
Sensor Type pH Sensor DG112-SC Unit pH
Temperature acquisition Temperature acquisition No
Stir Speed [%] 30
PredispenseMode None
Wait time [s] 0Control
Control Normal Mode Acid/base Show parameters Yes Titrant addition Dynamic dE(set value) 10 dV(min) [mL] 0.005 dV(max) [mL] 0.2 Mode Equilibrium controlled dE 0.5 dt [s] 2.0 t(min)[s] 3.0 t(max)[s] 30.0
Evaluation and recognitionProcedure Standard
Threshold [pH/mL] 1.5 Tendency None Ranges 0 Add. EQP criteria No Buffer capacity Yes
TerminationAt Vmax [mL] 5
At potential No At Slope No After numbered of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating No
Condition Condition No006 Calculation R1 Result HCl Result unit mol/L Formula R1=Q1*C/1 Constant C= 1/z M M[Hydrochloric acid] z z[Hydrochloric acid] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No007 Calculation R2 Result HOAc Result unit mol/L Formula R2=Q2*C/1 Constant C= 1/z M M[Acetic acid] z z[Acetic acid] Decimal places 5 Result limits No Record statistics Yes
Extra statistical functions No Send to buffer No Condition No
Method008 Calculation R3 Result NH4Cl Result unit mol/L Formula R3=Q3*C/1 Constant C= 1/z M M[Ammonium chloride] z z[Ammonium chloride] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No009 Calculation R4 Result Buffer capacity HCl Result unit mmol/(L*pH) Formula R4=BETAHNV1 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No010 Calculation R5 Result Buffer capacity HOAc Result unit mmol/(L*pH) Formula R5=BETAHNV2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No011 Calculation R6 Result Buffer capacity NH4Cl Result unit mmol/(L*pH) Formula R6=BETAHNV3 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Calculation R7 Result Buffer capacity sum1 Result unit mmol/(L*pH) Formula R7=BETAHNV1+BETAHNV2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No013 Calculation R8 Result Buffer capacity sum2 Result unit mmol/(L*pH) Formula R8=BETAHNV1+BETAHNV2+BETAHNV3 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No014 Record Summary No Results Per sample Raw results Per sample Table of measured values No Sample data No Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - V Last titration function E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No
3
M362
Acidic components
pH 4, 7 and 9 buffer solutions
Sodium hydroxide, NaOHc(NaOH) = 0.1 mol/L
Titration Excellence Line T70/T90Rondolino Sample Changer withPowerShower and pump
HX + NaOH = NaX + H2O
Olivetti JobJet 210 PrinterLabX Titration Software
METTLER TOLEDO
Neutralization before final disposal asaqueous solution.
Wastedisposal
Preparation and ProceduresCoca Cola, 50 mLSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi112-ProIndication
Buffer Capacity of Coca Cola
- 1 L of Coca Cola is added to an Erlenmeyer flask anddegassed by stirring and while heating for 1 hour.
- The degassed Coca Cola is stored in a sealed bottle, which isonly opened for sample aliquotation.
2) 50 mL of degassed Coca Cola are dispensed into a titrationbeaker.
3) The titration is started.
4) After each sample, the electrode is rinsed with water during 2s and conditioned during 10 s (Rondolino mode: 6).
The determination of the buffer capacity represents an alternativeway to analyze the general behaviour of e.g. an acid solution.
In particular, it can be used to describe complex acid/basemixtures that can be found in electroplating baths, in beveragesas well as in saliva.
Remarks to the graph:- HNV stands for half neutralization value.- HNV1 indicates the half neutralization value of the 1 EQP(EQP1).- HNV2 indicates the half neutralization value of the second EQP(EQP2).- The dashed line represents the buffer capacity curve (unit:mmol/(L*pH)).
Remarks
R1 = BETAHNV1R2 = BETAHNV2R3 = BETAHNV1+BETAHNV2
Units: mmol/(L*pH)
Calculation
Titration Excellence Line: The buffer capacity of Coca Cola is determined by titration with sodium hydroxide
Standard Potassium hydrogen phthalate (KHP)
Thomas HitzAuthor
Wastedisposal
4
HNV1
HNV2
HNV1
HNV2
Table of measured values
No. Comment / ID Start time Rx Result Unit
1/5 CocaCola 10.09.2007 15:54:43 R1 = 5.24 mmol/(L*pH) R2 = 3.62 mmol/(L*pH) R3 = 8.86 mmol/(L*pH)
2/5 CocaCola 10.09.2007 16:00:04 R1 = 5.17 mmol/(L*pH) R2 = 3.64 mmol/(L*pH) R3 = 8.81 mmol/(L*pH)
3/5 CocaCola 10.09.2007 16:05:15 R1 = 5.22 mmol/(L*pH) R2 = 3.63 mmol/(L*pH) R3 = 8.85 mmol/(L*pH)
4/5 CocaCola 10.09.2007 16:10:22 R1 = 5.16 mmol/(L*pH) R2 = 3.51 mmol/(L*pH) R3 = 8.67 mmol/(L*pH)
5/5 CocaCola 10.09.2007 16:15:35 R1 = 5.16 mmol/(L*pH) R2 = 3.46 mmol/(L*pH) R3 = 8.62 mmol/(L*pH)
Statistics
Rx n Mean value Unit s srel[%]
R1 5 5.19000 mmol/(L*pH) 0.03742 0.721R2 5 3.57200 mmol/(L*pH) 0.08167 2.286R3 5 8.76200 mmol/(L*pH) 0.10986 1.254
Titration curve
Results
5
Method: m362 Buffer Capacity Coca Cola 10.09.2007User: Thomas Hitz
001 Title Typ General titration Compatible with T50/T70/T90 ID m362 Titel Buffer Capacity Coca Cola Author Thomas Hitz Date / Time 01.09.2007 Modified at 10.09.2007 Protect No SOP None
002 Sample Number of IDs 1 ID 1 Coca Cola Entry Type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature [°C] 25.0
003 Titration stand (Rondolino TTL) Typ Rondolino TTL Titration stand Rondolino TTL 1
004 Stir Speed 30 % Duration 10 s Condition No
005 Titration (EQP) Titrant Titrant NaOH Concentration [mol/L] 0.1 mol/L Sensor Type pH Sensor DG112-SC Unit pH Temperature acquisition Temperature acquisition No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 12 dV (min) 0.005 dV (max) 0.5 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and recognition Procedure Standard Threshold 0.7 pH/mL Tendency Positive Ranges 0 Add. EQP criteria No Buffer capacity Yes Termination At Vmax 15 mL At potential No At Slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating
Accompanying stating No Condition
Condition No006 Calculation
Result BufferCapacity Result Unit mmol/(L*pH) Formula R1 = BETAHNV1 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No
Method007 Calculation
Result BufferCapacity Result Unit mmol/(L*pH) Formula R2 = BETAHNV2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No
008 CalculationResult BufferCapacity
Result Unit mmol/(L*pH) Formula R3 = BETAHNV1+BETAHNV2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No
009 RecordSummary No
Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration functions dE/dV - V Last titration functions log dE/dV - V No d2E/dV2 - V No Beta-V Last titration function E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No Condition No
010 End of sample
6
M363-A
Acid components as mg KOH/gsample, M=56.1 g/mol, z=1
60 mL ASTM D664-07 solvent:Toluene:2-propanol:deion. water500 mL : 495 mL : 5 mL
Potassium hydroxide in 2-propanolKOH, c(KOH) = 0.1 mol/L
Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software
KOH + HA = KA + H2O
HA: Acid components
DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer
METTLER TOLEDO
Dispose as aromatic organic solvent(toluene)
Wastedisposal
Preparation and ProceduresUsed motor oil,approx. 3 g for AN 5 -10
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Acid Number in Used Motor Oil According to ASTM D664-07
1) The titer is determined using potassium hydrogen phthalate(KHP): add approx. 80 mg KHP into a glass titration beakerand dissolve it with 60 mL deion. water (See M363-F).
2) The buffer potential 1 (pH 4) and the buffer potential 2(pH 11) are determined using aqueous pH buffers.These values are stored as auxiliary values H[Buffer pH4] andH[Buffer pH11]. See M363-D (pH 11) and M363-E (pH 4).
3) A blank value is determined for every new batch of solventmixture and stored as B[ASTM 664 AN] and B[ASTM 664 SAN]See applications M363-B for AN and M363-C for SAN.
4) Depending on the AN of the sample, different sampleamounts are requested:AN / mg KOH/g Sample size/g0.05 - <1.0 20.0 +/- 2.01.0 - <5.0 5.0 +/- 0.55 - <20 1.0 +/- 0.120 - <100 0.25 +/- 0.02100 - <260 0.1 +/- 0.01
5) After each sample titration the DG116-Solvent electrode isrinsed and conditioned in a chloroform/toluene 1:1 mixtureduring 5 minutes. Subsequently, it is conditioned in deionizedwater during additional 5 minutes.
1) This application does not replace the ASTM standard.
2) The method parameters have been optimised for the sampleused in this application. Thus, it may be necessary to slightlyadapt the method to your specific sample.
3) The acid number indicates the amount of base as mg KOH/gsample needed to titrate the acidic constituents in a sampleunder specific conditions, i.e. specified solvent and endpoint.
4) The sample is titrated using an EQP method function. If noinflection point is detected, endpoints are taken at meter readingscorresponding to those found for aqueous acidic and basicbuffer solutions for SAN at pH 4 and AN at pH 11
5) CalculationsR1 = AN to EQP in mg KOH/gR2 = mmol consumption to buffer potential pH 11R3 = AN to buffer potential pH 11 in mg KOH/gR4 = mmol consumption to buffer potential pH 4R5 = SAN to buffer potential pH 4 in mg KOH/g
Literature:- ASTM D664-07, see www.astm.org- METTLER TOLEDO Appl. brochure 34, ME-51 725 066- METTLER TOLEDO Appl. brochure 20, ME-51 725 020
Remarks
R1= (Q-B[ASTM 664 AN])*C/mC = M/zR2= QE(H[Buffer pH11])R3= (R2-B[ASTM 664 AN])*C/mC = M/zR4 = QE(H[Buffer pH4])R5= (R4+B[ASTM 664 SAN])*C/mC = M/z
Calculation
Titration Excellence Line: Method for the determination of the Acid Number (AN) and Strong Acid Number(SAN) in used motor oil by potentiometric titration with potassium hydroxide in 2-propanol according toASTM D664-07.
Standard Potassium hydrogen phthalate, 80 mg
Albert AichertAuthor
Wastedisposal
7
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C
0 NaN 187 NaN NaN 0 250.05 0.05 181.1 -5.9 NaN 5 250.1 0.05 174.4 -6.7 NaN 10 25
0.153 0.053 167.3 -7.1 NaN 15 250.214 0.061 159.5 -7.8 NaN 20 250.278 0.064 151 -8.5 -131.19 25 250.337 0.059 143.4 -7.6 -130.39 30 25
0.4 0.063 135 -8.4 -131.91 36 250.46 0.06 127.3 -7.7 -133.33 41 25
0.521 0.061 118.9 -8.4 -135.08 46 250.578 0.057 111.3 -7.6 -137.04 51 250.639 0.061 102.6 -8.7 -138.96 56 250.692 0.053 95.5 -7.1 -140.91 61 250.754 0.062 86.5 -9 -142.71 66 250.806 0.052 79.2 -7.3 -145.46 71 250.865 0.059 70.5 -8.7 -146.73 76 250.916 0.051 63 -7.5 -147.09 81 250.972 0.056 54.7 -8.3 -145.08 86 251.023 0.051 47.2 -7.5 -141.58 91 251.08 0.057 39.5 -7.7 -137.1 97 25
1.144 0.064 30.8 -8.7 -131.48 102 251.204 0.06 23 -7.8 -127.32 108 251.266 0.062 15.4 -7.6 -124.03 114 251.336 0.07 6.7 -8.7 -120.47 119 251.399 0.063 -0.6 -7.3 -117.37 124 251.476 0.077 -9.8 -9.2 -113.94 130 251.538 0.062 -16.7 -6.9 -111.36 136 251.616 0.078 -25.2 -8.5 -109.72 142 251.693 0.077 -33.6 -8.4 -108.28 147 251.764 0.071 -41.1 -7.5 -106.87 152 251.844 0.08 -49.8 -8.7 -106.95 157 251.914 0.07 -57.5 -7.7 -104.32 163 251.987 0.073 -64.6 -7.1 -102.22 169 252.08 0.093 -74.3 -9.7 -100.26 174 25
2.149 0.069 -81.4 -7.1 -99.8 179 252.232 0.083 -88.7 -7.3 -98.69 184 252.334 0.102 -99.4 -10.7 -97.91 189 25
2.4 0.066 -105.9 -6.5 -96.27 194 252.484 0.084 -114 -8.1 -94.33 200 252.57 0.086 -121.5 -7.5 -91.47 205 252.67 0.1 -131 -9.5 -86.83 210 252.75 0.08 -137.5 -6.5 -85.12 215 252.86 0.11 -146.8 -9.3 -82.14 220 25
2.952 0.092 -154.2 -7.4 -80.26 225 253.059 0.107 -162.5 -8.3 -77.69 230 253.164 0.105 -171.1 -8.6 -76.36 235 253.257 0.093 -177.6 -6.5 -74.67 240 253.39 0.133 -187.7 -10.1 -73.03 245 25
3.488 0.098 -194.5 -6.8 -71.37 250 253.614 0.126 -203.7 -9.2 -70.21 255 253.717 0.103 -210.7 -7 -69.31 260 253.845 0.128 -219.5 -8.8 -66.44 266 253.957 0.112 -226.6 -7.1 -64.23 271 254.098 0.141 -236.1 -9.5 -60.27 276 254.21 0.112 -242.2 -6.1 -57.67 282 254.39 0.18 -252 -9.8 -53.15 288 25
4.536 0.146 -259.9 -7.9 -49.99 294 254.686 0.15 -266.7 -6.8 -46.27 300 254.886 0.2 -276 -9.3 -41.8 305 255.051 0.165 -282.3 -6.3 -37.81 310 255.251 0.2 -289.7 -7.4 -33.28 315 255.451 0.2 -295.5 -5.8 -29.4 320 255.651 0.2 -301.3 -5.8 -25.75 325 255.851 0.2 -306.1 -4.8 -23 330 256.051 0.2 -310.4 -4.3 -20.38 336 256.251 0.2 -314.3 -3.9 NaN 341 256.451 0.2 -317.7 -3.4 NaN 346 256.651 0.2 -320.9 -3.2 NaN 351 256.851 0.2 -323.6 -2.7 NaN 356 257.051 0.2 -326.2 -2.6 NaN 361 25
Table of measured values
Summary Method-ID m363ASample No. ID Sample size and results 1 Used oil 3.04742 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.376 mmol R3 (TAN BP) 6.849 mg KOH/g R4 (Consumption SAN) 0.011 mmol R5 (SAN BP) 0.312 mg KOH/g 2 Used oil 3.31062 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.405 mmol R3 (TAN BP) 6.796 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.355 mg KOH/g 3 Used oil 3.27543 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.402 mmol R3 (TAN BP) 6.817 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.359 mg KOH/g 4 Used oil 3.09854 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.381 mmol R3 (TAN BP) 6.826 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.379 mg KOH/g 5 Used oil 3.16791 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.388 mmol R3 (TAN BP) 6.801 mg KOH/g R4 (Consumption SAN) 0.016 mmol R5 (SAN BP) 0.389 mg KOH/g 6 Used oil 3.27816 g R1 (TAN EQP) ----- mg KOH/g R2 (Consumption BP) 0.401 mmol R3 (TAN BP) 6.794 mg KOH/g R4 (Consumption SAN) 0.015 mmol R5 (SAN BP) 0.358 mg KOH/gStatistics R3 TAN BP Samples 6 Mean 6.814 mg KOH/g s 0.021311 mg KOH/g srel 0.313 % R5 SAN BP Samples 6 Mean 0.359 mg KOH/g s 0.026553 mg KOH/g srel 7.403 %
Titration curve
Results
8
Method m363 SAN & AN ASTM D664 29.01.2008Author Albert Aichert
001 Title Type General titration Compatible with T50 / T70 / T90 ID m363 Title SAN & AN ASTM D664 Author Albert Aichert Date/Time 29.01.2008 10:12:42 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Used oil Entry type Weight Lower limit 1.0 g Upper limit 10.0 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 Pump Auxiliary reagent ASTM 664 solvent Volume 60 mL Condition No005 Stir Speed 35 % Duration 60 s Condition No
006 Titration (EQP) [1] Titrant Titrant KOH in 2-Propanol Concentration 0.1 mol/L
Sensor Type pH Sensor DG116-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 30 %
Predispense Mode None Wait time 0 s
Control Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.05 mL dV(max) 0.2 mL Meas. value acquisition Equilibrium controlled dE 0.5 mV dt 1 s t(min) 5 s t(max) 60 s
Evaluation and recognition Procedure Standard Threshold 150 mV/mL Tendency None Ranges 1 Lower limit -400.0 mV Upper limit 0.0 mV Add. EQP criteria No
Termination At Vmax 15.0 mL At potential Yes Potential H[Buffer pH11]-100 mV Termination tendency None At slope No After number of recognized EQPs No Number of EQPs No Combined termination criteria No
Accompanying stating Accompanying stating No
Condition Condition No
007 Conditioning Type Fix Interval 1 Position Special beaker 1 Time 180 s Speed 100 % Condition no
Method008 Conditioning Type Fix Interval 1 Position Conditioning beaker Time 300 s Speed 30 % Condition no009 Calculation R1 Result TAN (EQP) Result unit mg KOH/g Formula R1=(Q-B[ASTM 664 AN])*C/m Constant C z/M M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No010 Calculation R2 Result Consumption EP Result unit mmol Formula R2=QE(H[Buffer pH11]) Constant C 1 M M[none] z z[none] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No011 Calculation R3 Result TAN (BP) Result unit mg KOH/g Formula R3=(R2-B[ASTM 664 AN])*C/m Constant C z/M M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Calculation R4 Result Consumption SAN Result unit mmol Formula R4=QE(H[Buffer pH4]) Constant C 1 M M[none] z z[none] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No013 Calculation R5 Result SAN (BP) Result unit mg KOH/g Formula R5=(R4+B[ASTM 664 SAN])*C/m Constant C z/M M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No014 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No015 End of sample
016 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No 014 Record Summary Yes Results No Raw results No Table of meas. value No E - V No dE/dV - V No Condition No
9
M363-B
--
--
Potassium hydroxide in 2-propanolKOH, c(KOH) = 0.1 mol/L
Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software
KOH + HA = KA + H2O
HA: Acid components
DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer
METTLER TOLEDO
Dispose as aromatic organic solvent(toluene)
Wastedisposal
Preparation and Procedures60 mL solvent ASTM 664-07mixture of 2-propanol/toluene/water inthe ratio 495 mL : 500 mL : 5 mL
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Blank Value for Acid Number According to ASTM D664-07
1) Use the empty beaker for the blank determination. Add thesolvent by means of the first membrane pump of Rondo 20.
2) For the blank determination, an EQP titration is used and theresult is calculated at the potential value obtained for pH 11buffer, i.e. QE(H[Buffer pH11]).This value was previously determined with application M363-Dand stored as auxiliary value H[Buffer pH11].
3) Finally, the result QE(H[Buffer pH11]) in mmol is stored asblank value B[ASTM 664 AN]
1) This application does not replace the ASTM standard.
2) The method parameters have been optimised for the sampleused in this application. Thus, it may be necessary to slightlyadapt the method to your specific sample.
3) The titrant has to be protected against the uptake of CO2 fromthe air. NaOH on carrier (e.g. "Sodium hydroxide on support",MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKANr. 03350) is an effective medium to avoid such formation ofcarbonate.
Literature:- ASTM D664-07, see www.astm.org- METTLER TOLEDO Appl. brochure 34, ME-51 725 066- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
R1= QE(H[Buffer pH11])Calculation
Titration Excellence Line: Method for the blank value determination to pH 11 of the acid number in thesolvent ASTM D664-07 with potassium hydroxide in 2-propanol.
Standard Potassium hydrogen phthalate, 80 mg
Albert AichertAuthor
Wastedisposal
10
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C
0 NaN -189.2 NaN NaN 0 250.002 0.002 -177.9 11.3 NaN 10 250.004 0.002 -171.9 6 NaN 20 250.009 0.005 -169 2.9 NaN 31 250.019 0.01 -168.7 0.3 NaN 41 250.029 0.01 -172.8 -4.1 NaN 52 250.039 0.01 -189.4 -16.6 NaN 62 250.044 0.005 -256.5 -67.1 NaN 87 25
Table of measured values
Summary Method-ID T202Sample No. ID Sample size and results 1 Solvent 664 60 mL R1 (Blank pH11) 0.003970 2 Solvent 664 60 mL R1 (Blank pH11) 0.003941 3 Solvent 664 60 mL R1 (Blank pH11) 0.004210Statistics R1 Blank pH11 Samples 3 Mean 0.004040 mmol s 0.000148 mg KOH/g srel 3.654 %
Titration curve
Results
11
Method T202 Blank AN pH11 ASTM D664 07.12.2007Author Albert Aichert
001 Title Type General titration Compatible with T50 / T70 / T90 ID T202 Title Blank AN pH11 ASTM D664 Author Albert Aichert Date/Time 07.12.2007 10:12:42 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Solvent 664 Entry type Fixed volume Volume 60 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 Pump Auxiliary reagent ASTM 664 solvent Volume 60 mL Condition No
005 Stir Speed 35 % Duration 60 s Condition No
006 Titration (EQP) [1] Titrant Titrant KOH in 2-Propanol Concentration 0.1 mol/L
Sensor Type pH Sensor DG116-SC Unit mV
Temperature acquisition Temperature acquisition NoStir Speed 30 %
Predispense Mode None Wait time 0 s
Control Control User Titrant addition Dynamic dE(set value) 12.0 mV dV(min) 0.002 mL dV(max) 0.01 mL Meas. value acquisition Equilibrium controlled dE 0.5 mV dt 1 s t(min) 10 s t(max) 60 s
Evaluation and recognition Procedure Standard Threshold 200 mV/mL Tendency Negative Ranges 0 Add. EQP criteria No
Termination At Vmax 15.0 mL At potential Yes Potential H[Buffer pH11]-30 mV Termination tendency None At slope No After number of recognized EQPs No Number of EQPs No Combined termination criteria No
Accompanying stating Accompanying stating No
Condition Condition No007 Rinse Auxiliary reagent ASTM 664 solvent Rinse cycles 1 Vol. per cycle 15 mL Position Actual sample Drain No Condition No
Method008 Calculation R1 Result Blank pH11 Result unit mmol Formula R1=QE(H[Buffer pH11]) Constant C 1 M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No009 Blank Name ASTM 664 AN Value B= Mean[R1] Unit mmol Limits No Condition No010 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No011 End of sample
012 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No 013 Record Summary Yes Results No Raw results No Table of meas. value No E - V No dE/dV - V No Condition No
12
M363-C
--
--
Hydrochloric acid in 2-PropanolHCl, c(HCl) = 0.1 mol/L
Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software
KOH + HA = KA + H2O
HA: Acid components
DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer
METTLER TOLEDO
Dispose as aromatic organic solvent(toluene)
Wastedisposal
Preparation and Procedures60 mL solvent ASTM 664-07mixture of 2-propanol/toluene/water inthe ratio 495 mL : 500 mL : 5 mL
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Blank Value for Strong Acid Number According to ASTM D664-07
1) Use the empty beaker for the blank determinaton. Add thesolvent by means of the first membrane pump of Rondo 20.
2) For the blank determination, an EQP titration is used and theresult is calculated at the potential value obtained for pH 4buffer, i.e. QE(H[Buffer pH4]).This value was previously determined with application M363-Eand stored as auxiliary value H[Buffer pH4]
3) Finally, the result QE(H[Buffer pH4]) in mmol is stored asblank value B[ASTM 664 SAN].
1) This application does not replace the ASTM standard.
2) The method parameters have been optimised for the sampleused in this application. Thus, it may be necessary to slightlyadapt the method to your specific sample.
Literature:- ASTM D664-07, see www.astm.org- METTLER TOLEDO Appl. brochure 34, ME-51 725 066- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
R1= QE(H[Buffer pH4])Calculation
Titration Excellence Line: Method for the blank value determination to pH 4 in the solvent ASTM D664-07with hydrochloric acid in 2-propanol.
Standard Tris-(hydroxymethyl)-aminomethane, 80 mg
Albert AichertAuthor
Wastedisposal
13
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C
0 NaN 44.5 NaN NaN 0 250.002 0.002 67.8 23.3 NaN 10 250.004 0.002 80 12.2 NaN 20 250.008 0.004 92.6 12.6 NaN 30 250.016 0.008 107.1 14.5 NaN 41 250.026 0.01 120.8 13.7 997.3 51 250.036 0.01 133.2 12.4 1010.34 62 250.046 0.01 146.5 13.3 1673.72 72 250.054 0.008 161.2 14.7 2863.48 82 250.06 0.006 175.6 14.4 NaN 92 25
0.062 0.002 187.1 11.5 NaN 103 250.064 0.002 197.4 10.3 NaN 113 250.066 0.002 210.7 13.3 NaN 124 250.068 0.002 227.6 16.9 NaN 134 25
Table of measured values
Summary Method-ID T212Sample No. ID Sample size and results 1 solvent 664 60 mL R1 (Blank pH4) 0.006157 2 solvent 664 60 mL R1 (Blank pH4) 0.005933 3 solvent 664 60 mL R1 (Blank pH4) 0.005929 4 solvent 664 60 mL R1 (Blank pH4) 0.005733Statistics R1 Blank pH4 Samples 4 Mean 0.005938 mmol s 0.000173 mg KOH/g srel 2.918 %
Titration curve
Results
14
Method T212 Blank SAN pH4 ASTM D664 17.01.2008Author Albert Aichert
001 Title Type General titration Compatible with T50 / T70 / T90 ID T212 Title Blank SAN pH4 ASTM D664 Author Albert Aichert Date/Time 17.01.2008 10:12:42 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Solvent 664 Entry type Fixed volume Volume 60 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 Pump Auxiliary reagent ASTM 664 solvent Volume 60 mL Condition No005 Stir Speed 35 % Duration 60 s Condition No
006 Titration (EQP) [1] Titrant Titrant HCl in 2-propanol Concentration 0.1 mol/L
Sensor Type pH Sensor DG116-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 30 %
Predispense Mode None Wait time 0 s
Control Control User Titrant addition Dynamic dE(set value) 12.0 mV dV(min) 0.002 mL dV(max) 0.01 mL Meas. value acquisition Equilibrium controlled dE 0.5 mV dt 1 s t(min) 10 s t(max) 60 s
Evaluation and recognition Procedure Standard Threshold 200 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No
Termination At Vmax 15.0 mL At potential Yes Potential H[Buffer pH4]+50 mV Termination tendency None At slope No After number of recognized EQPs No Number of EQPs No Combined termination criteria No
Accompanying stating Accompanying stating No
Condition Condition No
007 Rinse Auxiliary reagent ASTM 664 solvent Rinse cycles 1 Vol. per cycle 15 mL Position Actual sample Drain No Condition No
Method008 Calculation R1 Result Blank pH4 Result unit mmol Formula R1=QE(H[Buffer pH4]) Constant C 1 M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No009 Blank Name ASTM 664 SAN Value B= Mean[R1] Unit mmol Limits No Condition No010 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No011 End of sample
012 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No 013 Record Summary Yes Results No Raw results No Table of meas. value No E - V No dE/dV - V No Condition No
15
M363-D
--
--
--
Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software
--
DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer
METTLER TOLEDO
Neutralize before final disposal asqueous solution.
Wastedisposal
Preparation and Procedures50 mL pH 11 buffer solutionSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Buffer Value pH 11 for Acid Number According to ASTM D664-07
1) Always use fresh pH 11 buffer solution. The buffer pH 11 isnot stable when exposed to air.
2) 50 mL pH 11 buffer solution are added into a titrationbeaker.
3) Before measure the buffer potential, the electrode shouldconditioned in aquous media (water pH 5-6) for 3 - 5 minutes.
4) The measured potential value for buffer pH 11 is stored asauxilliary value H[Buffer pH11].
5) Finally, the electrode is parked in the condioning beakercontaining slightly acidic water (pH 5-6).
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 theair is strongly improved.For instance, the potential value (mV) in an open beaker withbuffer pH 11.can change of 0.1 mV/minThe potential value of an opened bottle of pH 11 buffer solutioncan rapidly change.Thus, it is very important to use fresh pH 11 buffer solution everytime a new value has to be determined
Literature:- ASTM D664-07, see www.astm.org- METTLER TOLEDO Appl. brochure 34, ME-51 725 066- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
R1= ECalculation
Titration Excellence Line: Determination of the potential value for pH 11 buffer (AN, Acid Number) acccordingto ASTM D 664-07.
Standard --
Albert AichertAuthor
Wastedisposal
16
Table of measured values
Method-ID T102
Data / Time 07.01.2008 03:12:05 pm
All results Sample 1/1 Buffer pH11 R1(Buffer pH11) -222.400 mV
Titration curve
Results
17
Method T102 Buffer value AN pH11 ASTM D664 17.12.2007Author Albert Aichert
001 Title Type General titration Compatible with T50 / T70 / T90 ID T102 Title Buffer value AN pH11 ASTMD664 Author Albert Aichert Date/Time 17.12.2007 10:12:42 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Buffer pH11 Entry type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 Stir Speed 35 % Duration 300 s Condition No
005 Measure (normal) [1] Sensor
Type pH Sensor DG116-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 30 %
Acquisition of the measured value Acquisition Fix Time 30 s Mean value No t(min) 10 s t(max) 60 s
Condition Condition No
006 Calculation R1 Result Buffer pH11 Result unit mV Formula R1=E Constant C 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No
007 Auxiliary value Name Buffer pH11 Value B= R1 Unit mV Limits No Condition No
008 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V No dE/dV - V No Condition No
009 End of sample
010 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No
Method
18
M363-E
--
--
--
Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software
--
DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer
METTLER TOLEDO
Neutralize before final disposal asqueous solution.
Wastedisposal
Preparation and Procedures50 mL pH 4 buffer solutionSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Buffer Value pH4 for Strong Acid Number According to ASTM D664-07
1) Always use fresh pH 4 buffer solution.
2) 50 mL pH 4 buffer solution are added into a titration beaker.
3) Before measure the buffer potential, the electrode shouldconditioned in aquous media (water pH 5-6) for 3 - 5 minutes.
4) The measured potential value for buffer pH 4 is stored asauxilliary value H[Buffer pH4].
5) Finally, the electrode is parked in the condioning beakercontaining slightly acidic water (pH 5-6).
1) This application does not replace the ASTM standard.
2) Before measure the buffer potential, the electrode shouldconditioned in aqueous media (water pH 5-6) for 3 - 5minutes.
Literature:- ASTM D664-07, see www.astm.org- METTLER TOLEDO Appl. brochure 34, ME-51 725 066- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
R1= ECalculation
Titration Excellence Line: Determination of the potential value for pH 4 buffer (SAN, Strong Acid Number)acccording to ASTM D 664-07.
Standard --
Albert AichertAuthor
Wastedisposal
19
Table of measured values
Method-ID T112
Data / Time 17.01.2008 11:12:05 pm
All results Sample 1/1 Buffer pH4 R1(Buffer pH4) 169.200 mV
Titration curve
Results
20
Method T112 Buffer value SAN pH4 ASTM D664 16.01.2008Author Albert Aichert
001 Title Type General titration Compatible with T70 / T90 ID T112 Title Buffer value SAN pH4 ASTMD664 Author Albert Aichert Date/Time 16.01.2008 10:12:42 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Buffer pH4 Entry type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 Stir Speed 35 % Duration 300 s Condition No
005 Measure (normal) [1] Sensor
Type pH Sensor DG116-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 30 %
Acquisition of the measured value Acquisition Fix Time 30 s Mean value No t(min) 10 s t(max) 60 s
Condition Condition No
006 Calculation R1 Result Buffer pH4 Result unit mV Formula R1=E Constant C 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No
007 Auxiliary value Name Buffer pH4 Value B= R1 Unit mV Limits No Condition No
008 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V No dE/dV - V No Condition No
009 End of sample
010 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No
Method
21
M363-F
Potassium hydrogen phthalateM=204.23 g/mol z=1
50 mL CO2-free, deionized water
Potassium hydroxide in 2-propanolKOH, c(KOH) = 0.1 mol/L
Titration Excellence T50/T70/T90Rondo20 with two membrane pumpsLabX Titration Software
KOH + K2HPO3 = H2O + 3K+ + PO43-
DV1010 BuretteGlass titration beaker ME-101446XS205 BalanceOlivetti JobJet 210 Printer
METTLER TOLEDO
Neutralize before final disposal asaqueous solution.
Wastedisposal
Preparation and ProceduresPrimary standardPotassium hydrogen phthalate,70 - 100 mg
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Titer Determination of 0.1 mol/L KOH in 2-Propanol (ASTM D664-07)
1) Weigh the primary standard into the glass titration beaker toavoid electrostatic influence.
2) Add 50 mL CO2-free deionized water to dissolve the sample.
3) After each sample titration, the eelctrode is rinsed with water
4) At the end of the titration, the electrode is parked in thecondioning beaker containing slightly acidic water (pH 5-6).
1) This application does not replace the ASTM standard.
2) The titrant has to be protected against the uptake of CO2 fromthe air. NaOH on carrier (e.g. "Sodium hydroxide on support",MERCK no. 101564, or "Sodium hydroxide on carrier", FLUKANr. 03350) is an effective medium to avoid such formation ofcarbonate.
Literature:- ASTM D664-07, see www.astm.org- METTLER TOLEDO Appl. brochure 34, ME-51 725 066- METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
R1= m/(VEQ*c*C)C=(10*p*z)
p: purity of standard
Calculation
Titration Excellence Line:Method for the titer determination of 0.1 mol/L KOH in 2-Propanol according to ASTM D664-07.
Standard Potassium hydrogen phthalate, 80 mg
Albert AichertAuthor
Wastedisposal
22
Table of measured values
Summary Method-ID T001
Sample No. ID Sample size and results 1 KHP 0.11936 g R1 (Titer) 0.961720 2 KHP 0.12372 g R1 (Titer) 0.961095 3 KHP 0.11054 g R1 (Titer) 0.960251 4 KHP 0.11502 g R1 (Titer) 0.960945
Statistics R1 Titer Samples 4 Mean 0.961003 s 0.000603 srel 0.063 %
Titer Titrant KOH in 2-Propanol New titer 0.96100
Titration curve
Results
23
Method m363F Titer of KOH in 2-propanol 02.10.2007Author Albert Aichert
001 Title Type General titration Compatible with T50 / T70 / T90 ID m363F Title Titer of KOH in 2-propanol Author Albert Aichert Date/Time 02.10.2007 10:51:42 Modified -- Modified by -- Protect No SOP None
002 Sample (Titer) Titrant KOH in 2-Propanol Concentration 0.1 mol/L Standard KHP Type of standard solid Entry type Weight Lower limit 0.07 g Upper limit 0.12 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 Pump Auxiliary reagent Water Volume 60 mL Condition No005 Stir Speed 60 % Duration 60 s Condition No
006 Titration (EQP) [1] Titrant Titrant KOH in 2-Propanol Concentration 0.1 mol/L
Sensor Type pH Sensor DG116-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 30 %
Predispense Mode Volume Volume 1.0 mL Wait time 5 s
Control Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.005 mL dV(max) 0.5 mL Meas. value acquisition Equilibrium controlled dE 1.0 mV dt 1 s t(min) 3 s t(max) 60 s
Evaluation and recognition Procedure Standard Threshold 3.0 pH/mL Tendency Positive Ranges 0 Add. EQP criteria No
Termination At Vmax 10.0 mL At potential No Tendency None At slope No After number of recognized EQPs Yes Number of EQP's 1 Number of EQPs No Combined termination criteria No
Accompanying stating Accompanying stating No
Condition Condition No
007 Rinse Auxiliary reagent Water Rinse cycles 1 Vol. per cycle 15 mL Position Actual sample Drain No Condition No
Method008 Calculation R1 Result Titer Result unit -- Formula R1=(m/(VEQ*c*C) Constant C M/(10*p*z) M M[Potassium hydroxid] z z[Potassium hydroxid] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
009 Record Summary No Results Per sample Raw results Per sample Table of meas. value No E - V Last titration function dE/dV - V Last titration function Condition No010 End of sample
011 Titer Titrant KOH in 2-Propanol Concentration 0.1 mol/L TITER= Mean[R1] Limits No Condition No
012 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No
013 Record Summary Yes Results No Raw results No Table of meas. value No E - V No dE/dV - V No Condition No
24
M364-A
Alkaline components in oil expressedas KOH, M=56.1 g/mol , z=1
60 mL ASTM D4739-06a solvent(see Preparation and Procedures)pH 3 and pH 10 buffer solutions
HCl in 2-propanol, c(HCl)=0.1 mol/LKOH in 2-propanol, c(HCl)=0.1 mol/L
Titration Excellence T70/T90Rondo 20 Sample changer1 additional dosing unit (20 mL)
HCl + KOH = Cl- + K+ + H2O
KOH represents the alkalinecomponents.
DV1010 and DV1020 BurettesTitration beakers ME-101974XS205 Balance, SP250 pumpPC with LabX Software
METTLER TOLEDO
Dispose of as halogenated organicwaste
Wastedisposal
Preparation and ProceduresUsed Motor oil, ~2.5 gSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Base Number in Used Motor Oil According to ASTM D4739-06a
1) Solvent preparation: ASTM D4739-06a solvent is preparedby mixing 2-propanol, toluene, chloroform and water in thefollowing ratio: 10:10:10:0.3 (v/v).
2) The titer is determined by titration of previously standardizedKOH in 2-propanol solution. The latter has been standardizedusing potassium hydrogen phthalate (KHP), see M364-D.
3) The acidic (pH 3) and the alkaline (pH 10) aqueous bufferpotentials are measured and stored as auxiliary values pH 3 (H[Buffer pH3] ) and ( H[Buffer pH10] ).
4) Blank values for the base number (BN) are determined forevery new batch of solvent mixture by titration with HCl in 2-propanol to the buffer pH 3 potential.For strong base number (SBN), the solvent is titrated with KOHin 2-propanol to pH 10 pot. value. The result is stored as blankvalue ASTM D4739 (M364-B).
5) Add the oil sample into the titration beaker. The appropriatesample size is calculated according to the following formula:sample size (g) = 7/expected BN
6) 60 mL ASTM D4739-06a solvent are added using anadditional dosing unit. This step can be performed manuallyusing a dispenser or a graduated cylinder.
This method allows a fully automated procedure using asample changer and an additional dosing unit. It can bemodified for manual operation. Select "Manual stand" in themethod function "Titration stand".
1) This application does not replace the ASTM standard.The method parameters have been optimised for the sampleused in this application. Thus, it may be necessary to slightlyadapt the method to your specific sample.
2) The base number BN is defined as the consumption ofhydrochloric acid to a specific endpoint to neutralize the alkalinecomponents of the oil. It is expressed as mg KOH/g sample:- If an EQP is found between the acidic buffer potential value anda point 100 mV past this potential, then this will be the BN.- If no EQP is found in this region, then the result is evaluated atthe potential value of the acidic buffer.
3) Between each sample it is necessary to condition theelectrode under stirring during 300 s in deion. water. Theelectrode is parked in buffer pH 4 (Rinse beaker).
Literature:1) ASTM D4739-06a and draft next version, see www.astm.org2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
Base number mg KOH/g:R1=(Q-B[ASTM D4739])*C/mC=M/z
Base number mg KOH/g at acidic potential:R2=(QE(H[Buffer pH3])-B[ASTM D4739])*C/mC=M/z
Calculation
Titration Excellence Line: Method for the determination of the base number (BN) in oil by titration withhydrochloric acid in 2-propanol according to ASTM D4739-06a.
Standard KOH in 2-propanol 0.1 mol/L / KHP
Melanie NijmanAuthor
Wastedisposal
25
Table of measured values
Mettler Toledo T90 Titrator Mettler Toledo AGMarket Support Laboratory17.01.2008
Method M364_A Base Number According to ASTM D4739-06a
RESULTS with DG116-Solvent electrodeNo. ID Sample size and results1 Used Motor Oil 2.54656 g
R1 = 3.50 mg KOH/g Content (EQP)R2 = 1.87 mg KOH/g Content (Buffer Potential)
2 Used Motor Oil 2.67162 gR1 = 3.48 mg KOH/g Content (EQP)R2 = 1.80 mg KOH/g Content (Buffer Potential)
3 Used Motor Oil 2.48459 gR1 = 3.46 mg KOH/g Content (EQP)R2 = 1.80 mg KOH/g Content (Buffer Potential)
4 Used Motor Oil 2.54055 gR1 = 3.49 mg KOH/g Content (EQP)R2 = 1.84 mg KOH/g Content (Buffer Potential)
5 Used Motor Oil 2.4121 gR1 = 3.45 mg KOH/g Content (EQP)R2 = 1.81 mg KOH/g Content (Buffer Potential)
6 Used Motor Oil 2.53271 gR1 = 3.44 mg KOH/g Content (EQP)R2 = 1.83 mg KOH/g Content (Buffer Potential)
STATISTICSNumber results R1 n = 6Mean value x = 3.47 mg KOH/g Content (EQP)Standard deviation s = 0.02 mg KOH/g Content (EQP)Relative standard deviation srel = 0.682 %
Number results R2 n = 6Mean value x = 1.82 mg KOH/g Content (Buffer Potential)Standard deviation s = 0.03 mg KOH/g Content (Buffer Potential)Relative standard deviation srel = 1.501 %
RESULTS with DG113-SC electrode
STATISTICSNumber results R1 n = 6Mean value x = 3.46 mg KOH/g Content (EQP)Standard deviation s = 0.06 mg KOH/g Content (EQP)Relative standard deviation srel = 1.659 %
Number results R2 n = 6Mean value x = 1.71 mg KOH/g Content (Buffer Potential)Standard deviation s = 0.05 mg KOH/g Content (Buffer Potential)Relative standard deviation srel = 3.072 %
Titration curve
Results
26
Method: m364A Base number ASTM D4739 17.01.2008User: Melanie Nijman
001 Title Type General titration Compatible with T70/ T90 ID m364A Title Base number ASTM D4739 Author Melanie Nijman Date / Time 17.01.2008 Modified at 11.01.2008 Modified by Administrator Protect No SOP None LabX SOP None
002 Conditioning Titration stand Rondo60/1A Position Conditioning beaker Time [s] 20 Speed [%] 30 Condition No
003 Sample Number of IDs 1 ID 1 Motor Oil Entry Type Weight Lower limit [g] 0.0 Upper limit [g] 10.0 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0 Entry Arbitrary
004 Titration stand Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No
005 Dispense (normal) [1]Titrant ASTM D4739 solvent
Concentration [mol/L] 1 Volume [mL] 60 Dosing rate [mL/min] 60.0 Condition No
006 Stir Speed [%] 35 Duration [s] 60 Condition No
007 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG116-Solvent Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 35 Predispense Mode Volume Volume 0.5 Wait time [s] 60 Predispense Mode Volume Volume [mL] 0.2 Wait time [s] 5 Control Control User Titrant addition Incremental dV (mL) 0.1 Mode Fixed time dt [s] 90 Evaluation and Recognition Procedure Standard Threshold [mV/mL] 80.0 Tendency None Ranges 1 Lower limit 1 [mV] H[Buffer pH3] Upper limit 1 [mV] H[Buffer pH3]+100 Add. EQP criteria No Termination At Vmax [mL] 5.0 At potential Yes Potential H[Buffer pH3]+140 Termination tendency Positive At Slope No After number of recognized EQPs No Combined termination criteria No
Accompanying stating Accompanying stating No Condition Condition No
Method008 Calculation R1 Result Content EQP Result Unit mg KOH/g Formula R1=(Q-B[ASTM D4739])*C/m Constant C= M/z M M[Potassium hydroxide] z z[Potassium hydroxide] Decimal places 2 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
009 Calculation R2 Result Content (Buffer Potential) Result Unit mg KOH/g Formula R1=(QE(H[Buffer pH3]) -B[ASTM D4739])*C/m Constant C= M/z M M[Potassium hydroxide] z z[Potassium hydroxide] Decimal places 2 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
010 RinseAuxiliary reagent ASTM D4739
Rinse cycles 3 Vol. per cycle [mL] 20.0 Position Actual position Drain Yes Drain pump SP250 Condition No
011 Conditioning Type Fix Interval 1 Position Conditioning beaker Time [s] 300 Speed [%] 30 Condition No
012 Record Summary No Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No
013 End of sample
014 Park Titration stand Rondo60/1A Position Rinse beaker
Condition No
27
M364-B
--
pH 3 and pH 10 buffer solutions
HCl in 2-propanol, c(HCl)=0.1 mol/LKOH in 2-propanol, c(HCl)=0.1 mol/L
Titration Excellence T70/T90Rondo 20 Sample changer1 additional dosing unit (20 mL)
--
DV1010 and DV1020 BurettesTitration beakers ME-101974XS205 Balance, SP250PC with LabX Software
METTLER TOLEDO
Dispose of as halogenated organicwaste
Wastedisposal
Preparation and Procedures60 mL solvent ASTM D4739-06aSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi116-SolventIndication
Blank Value of Base Number Solvent According to ASTM D4739-06a
1) Solvent preparation:ASTM D4739-06a solvent is prepared by mixing 2-propanol,toluene, chloroform and water in the following ratio:10 : 10 : 10 : 0.3 (v/v).
2) The titer is determined by titration of standardized KOH in 2-propanol solution. The latter is standardized using potassiumhydrogen phthalate (KHP).
3) The acidic and the alkaline aqueous buffers are measuredand stored as auxiliary values H[Buffer pH3] (BN) and H[BuffferpH10] (SBN, Strong Base Number). The values are then usedfor the EQP termination and the calculation R1.
4) 60 mL ASTM D4739-06a solvent are added using anadditional dosing unit. This step can be performed manuallyusing a dispenser or a graduated cylinder.
5) Blank value determinations are performed for every newbatch of solvent by titration with HCl in 2-propanol to pH 3potential value. The result is stored as blank B[ASTM D4739].
6) For SBN, the solvent is titrated with KOH in 2-propanol to pH10 buffer potential value and stored as B[ASTM D4739 pH10].
This method allows a fully automated procedure using a samplechanger and an additional dosing unit. It can be modified formanual operation. Select "Manual stand" in the method function"Titration stand".
1) This application does not replace the ASTM standard.
2) The base number BN is defined as the consumption ofhydrochloric acid to a specific endpoint to neutralize the alkalinecomponents of the oil. It is expressed as mg KOH/g sample:- If an EQP is found between the acidic buffer potential value anda point 100 mV past this potential, then this will be the BN.- If no EQP is found in this region, then the result is evaluated atthe potential value of the acidic buffer pH3.
3) Between each sample it is necessary to condition theelectrode under stirring during 300 s in deion. water. Theelectrode is parked in buffer pH 4 (Rinse beaker).
Literature:1) ASTM D4739-06a and draft next version, see www.astm.org2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
Consumption of HCl in 2-Propanol up toEQP or acidic potential value:R1=Q (mmol) orR1=QE(H[Buffer pH3])SBN blank: Consumption of KOH in 2-Propanol up to EQP/potential value:R1=Q (mmol) orR1=QE(H[Buffer pH10])
Calculation
Titration Excellence Line: Blank value determination of the base number BN solvent by titration withhydrochloric acid or potassium hydroxide in 2-propanol according to ASTM D4739-06a.
Standard KOH in 2-propanol 0.1 mol/L / KHP
Melanie NijmanAuthor
Wastedisposal
28
Table of measured values
Mettler Toledo T90 Titrator Mettler Toledo AGMarket Support Laboratory17.01.2008
Method m364B Blank Base Number According to ASTM D4739-06a
Measured 17.01.2007
RESULTSNo. ID Sample size and results1 ASTM D4739 Solvent 60.0 mL
R1 = 0.00478 mmol Consumption (Buffer potential)R3 = 0.00469 mmol Consumption (EQP)
2 ASTM D4739 Solvent 60.0 mLR1 = 0.00487 mmol Consumption (Buffer potential)R3 = 0.00478 mmol Consumption (EQP)
3 ASTM D4739 Solvent 60.0 mLR1 = 0.00484 mmol Consumption (Buffer potential)R3 = 0.00474 mmol Consumption (EQP)
4 ASTM D4739 Solvent 60.0 mLR1 = 0.00481 mmol Consumption (Buffer potential)R3 = 0.00472 mmol Consumption (EQP)
5 ASTM D4739 Solvent 60.0 mLR1 = 0.00482 mmol Consumption (Buffer potential)R3 = 0.00474 mmol Consumption (EQP)
STATISTICSNumber results R1 n = 5Mean value x = 0.00482 mmol Consumption (Buffer potential)Standard deviation s = 0.00003 mmol Consumption (Buffer potential)Relative standard deviation srel = 0.697 %
Number results R3 n = 5Mean value x = 0.00473 mmol Consumption (EQP)Standard deviation s = 0.00003 mmol Consumption (EQP)Relative standard deviation srel = 0.694 %
Titration curve
Results
29
Method: m364B Blank BN According to ASTM 17.01.2008User: Nijman
001 Title Type General titration Compatible with T70/ T90 ID M364_B Title Blank ASTM D4739 Author Mettler Toledo Date / Time 17.01.2008 Modified at 17.01.2008 Modified by Administrator Protect No SOP None LabX SOP002 Conditioning Titration stand Rondo60/1A
Position Conditioning beaker Time [s] 20 Speed [%] 30 Condition No003 Sample Number of IDs 1
ID 1 ASTM D4739 Solvent Entry Type Fixed volume Volume [mL] 60.0 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0004 Titration stand
Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No005 Dispense (normal) [1] Titrant ASTM D4739 solvent Concentration [mol/L] 1 Volume [mL] 60 Dosing rate [mL/min] 60.0 Condition No006 Stir Speed [%] 30
Duration [s] 10 Condition No007 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG116-Solvent Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode Volume Volume 0.02 Wait time [s] 10 Predispense Mode Volume Volume [mL] 0.2 Wait time [s] 5 Control Control User Titrant addition Incremental dV (mL) 0.002 Mode Fixed time dt [s] 30 Evaluation and Recognition Procedure Standard Threshold [mV/mL] 7500.0 Tendency Positive Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 1.0 At potential Yes Potential H[Buffer pH3]+100 Termination tendency Positive At Slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No008 Calculation R1
Result Consumption (Buffer potential) Result Unit mmol Formula R1=QE(H[Buffer pH3]) Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No
Method009 Calculation R3
Result Consumption (EQP) Result Unit mmol Formula R3=Q Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No010 Record Summary No Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No011 Conditioning
Type Fix Interval 1 Position Conditioning beaker Time [s] 300 Speed [%] 30 Condition No012 End of sample013 Park
Titration stand Rondo60/1A Position Rinse beaker
Condition No014 Blank
Name ASTM D4739 Value B= Mean[R1] Unit mmol Limits No Condition Yes
Formula Mean[R1]>0015 Blank
Name ASTM D4739 Value B= Mean[R3] Unit mmol Limits No Condition Yes Formula Mean[R3]>0016 Calculation R2
Result Mean Consumption (Buffer potential) Result Unit mmol Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Send to buffer No Condition No017 Calculation R4
Result Mean Consumption (EQP) Result Unit mmol Formula R4=Mean[R3] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Send to buffer No Condition No018 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No
30
M364-C
Potassium hydroxide, KOHM(KOH)=56.1 g/mol, z=1
50 mL deionized water
HCl in 2-propanol,c(HCl)=0.1 mol/L
Titration Excellence T50/T70/T90Rondo 20 Sample changer1 additional dosing unit
HCl + KOH = Cl- + K+ + H2O
DV1010 BurettesTitration beakers ME-101974PC with LabX Software
METTLER TOLEDO
Disposal as halogenated organic wasteWastedisposal
Preparation and ProceduresStandardized KOH in 2-Propanolc(KOH) = 0.1 mol/L, 8.00 mL
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi111-SCIndication
Titer Determination of 0.1 mol/L HCl in 2-Propanol (ASTM D4739-06a)
1) Add 50 ml deionized into the titration beaker
2) 8 mL KOH in 2-propanol are added automaticlayy by menasot an additional dosing unit. If this is not available, the samplecan be added manaully using a pipette.
3) The mean value of the titer determinations is savedautomatically as the titer for the titrant by means of the functionTITER in the method.
Literature:1) ASTM D4739-06a and draft next version, see www.astm.org2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
Titer HCl:
R1=VENDDi/(VEQ*c*C)C=1/(cst*H[KOH Titer]*z)
The real value for the KOH concentrationdetermined in M364_D is used for the titerdetermination of HCl in 2-Propanol.
Calculation
Titration Excellence Line: Method for the titer determination of hydrochloric acid in 2-propanol according toASTM D4739-06a.
Standard KOH in 2-propanol 0.1 mol/L(via KHP)
Melanie NijmanAuthor
Wastedisposal
31
Table of measured values
Mettler Toledo T90 Titrator Mettler Toledo AGMarket Support Laboratory07.03.2008
Method m364C Titer HCl in 2-PropanolMeasured 07.03.2008
RESULTSNo. ID Sample size and results1 KOH in 2-Propanol 8.0 mL
R1 = 0.99689 -- Titer HCl2 KOH in 2-Propanol 8.0 mL
R1 = 0.99622 -- Titer HCl3 KOH in 2-Propanol 8.0 mL
R1 = 0.99649 -- Titer HCl4 KOH in 2-Propanol 8.0 mL
R1 = 0.99674 -- Titer HCl5 KOH in 2-Propanol 8.0 mL
R1 = 0.99613 -- Titer HCl6 KOH in 2-Propanol 8.0 mL
R1 = 0.99626 -- Titer HCl7 KOH in 2-Propanol 8.0 mL
R1 = 0.99694 -- Titer HCl
STATISTICSNumber results R1 n = 7Mean value x = 0.99652 -- Titer HClStandard deviation s = 0.00033 -- Titer HClRelative standard deviation srel = 0.034 %
Titration curve
Results
32
Method: m364C Titer of HCl in 2-Propanol 07.03.2008User: Melanie Nijman
001 Title Type Titer determination Compatible with T50 / T70 / T90 ID M364_C Title Titer of HCl in 2-Propanol Author melanie Nijman Date / Time 26.02.2008 Modified at 07.03.2008 Modified by Administrator Protect No SOP None LabX SOP
002 Sample (Titer) Titrant HCl in 2-Propanol Concentration 0.1 Standard KOH in 2-Propanol Type of standard liquid Entry type Fixed volume Volume [mL] 8.0 Correction factor 1.0 Temperature [°C] 25.0
003 Titration stand Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No
004 Dispense (normal) [1] Titrant KOH in 2-Propanol
Concentration [mol/L] 0.1 Volume [mL] 8.0 Dosing rate [mL/min] 60.0 Condition No
005 Stir Speed [%] 30
Duration [s] 10 Condition No
006 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG111-SC Unit pH Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 8.0 dV(min) [mL] 0.01 dV(max) [mL] 0.5 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold [pH/mL] 3.0 Tendency None Ranges 0 Add. EQP criteria No Buffer capacity No Termination At Vmax [mL] 10.0 At potential No At Slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No
007 Calculation R1 Result Titer Result Unit -- Formula R1=VENDDi/(VEQ*c*C) Constant C= 1/(cst*H[KOH Titer]*z) M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No
Method008 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No
009 End of sample
010 Titer Titrant HCl in 2-Propanol Concentration [mol/L] 0.1 TITER= Mean[R1] Limits No
Condition No
011 ParkTitration stand Rondo60/1A
Position Conditioning beaker Condition No
012 Calculation R2 Result Mean Titer Result Unit -- Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Send to buffer No Condition No
013 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No
Condition No
33
M364-D
Potassium hydrogen phthalateM = 204.23 g/mol; z=1
50 mL deionized water
KOH in 2-propanolc(KOH) = 0.1 mol/L
Titration Excellence T50/T70/T90Rondo 20 Sample changer
KHC8H4O4 + KOH = H20 + K2C8H4O4
DV1010 BurettesTitration beakers ME-101974PC with LabX Software
METTLER TOLEDO
Disposal as halogenated organic wasteWastedisposal
Preparation and ProceduresPrimary standard KHPm = ~ 0.11 g
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi111-SCIndication
Titer Determination of 0.1 mol/L KOH in 2-Propanol (ASTM D4739-06a)
1) weigh the standard into the glass titration beaker in order toavoid electrostatic interferences.
2) Add 50 ml deionized into the titration beaker.
3) The mean value of the titer determinations is savedautomatically as the titer for the titrant by means of the functionTITER in the method.
1) The titrant has to be protected against the uptake of CO2 fromthe air.NaOH on carrier (e.g. "Sodium hydroxide on support", MERCKno. 101564, or "Sodium hydroxide on carrier", FLUKA Nr.03350) is an effective medium to avoid such formation ofcarbonate.
Literature:1) ASTM D4739-06a and draft next version, see www.astm.org2) METTLER TOLEDO Appl. brochure 34, ME-51 725 066.3) METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
Titer KOH:
R1=m/(VEQ*c*C)C=M/(10*p*z)
Calculation
Titration Excellence Line: Method for the titer determination of potassium hydroxide in 2-propanol accordingto ASTM D4739-06a.
Standard --
Melanie NijmanAuthor
Wastedisposal
34
Table of measured values
Mettler Toledo T90 Titrator Mettler Toledo AGMarket Support Laboratory28.02.2008
Method m364D Titer of KOH in 2-propanolMeasured 28.02.2008
RESULTSNo. ID Sample size and results1 KHP 0.1057 g
R1 = 0.9870 -- Titer KOH2 KHP 0.1030 g
R1 = 0.9920 -- Titer KOH3 KHP 0.1018 g
R1 = 0.9960 -- Titer KOH4 KHP 0.1209 g
R1 = 0.9900 -- Titer KOH5 KHP 0.1183 g
R1 = 0.9920 -- Titer KOH6 KHP 0.1205 g
R1 = 0.9930 -- Titer KOH
STATISTICSNumber results R1 n = 6Mean value x = 0.992 -- Titer KOHStandard deviation s = 0.003 -- Titer KOHRelative standard deviation srel = 0.304 %
Titration curve
Results
35
Method: m364D Titer of KOH in 2-Propanol 28.02.2008User: Melanie Nijman
001 Title Type Titer determination Compatible with T50 / T70 / T90 ID M364_D Title Titer of KOH in 2-Propanol Author Melanie Nijman Date / Time 26.02.2008 Modified at 28.02.2008 Modified by Administrator Protect No SOP None LabX SOP
002 Sample (Titer) Titrant KOH in 2-Propanol Concentration 0.1 Standard Potassium hydrogen phthalate Type of standard solid Entry type Weight Lower limit 0.0 Upper limit 0.5 Correction factor 1.0 Temperature [°C] 25.0 Input Arbitrary
003 Titration stand Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No
004 Stir Speed [%] 30
Duration [s] 30 Condition No
005 Titration (EQP) [1] Titrant Titrant KOH in 2-Propanol Concentration [mol/L] 0.1 Sensor Type pH Sensor DG111-SC Unit pH Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 8.0 dV(min) [mL] 0.01 dV(max) [mL] 0.5 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold [pH/mL] 3.0 Tendency None Ranges 0 Add. EQP criteria No Buffer capacity No Termination At Vmax [mL] 10.0 At potential No At Slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No
006 Calculation R1 Result Titer Result Unit -- Formula R1=m/(VEQ*c*C) Constant C= M/(10*p*z) M M[Potassium hydrogen phthalate] z z[Potassium hydrogen phthalate] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
Method007 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No d2E/dV2 - V No BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No
008 End of sample
009 Titer Titrant KOH in 2-Propanol Concentration [mol/L] 0.1 TITER= Mean[R1] Limits No
Condition No
010 ParkTitration stand Rondo60/1A
Position Conditioning beaker Condition No
011 Calculation R2 Result Mean Titer Result Unit -- Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Send to buffer No Condition No
012 Auxiliary value Name KOH Titer Formula H= R2 Limits No Condition No
013 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No
Condition No
36
M365
--
--
Hydrochloric acid, HClc(HCl) = 0.1 mol/L
Titration Excellence T50/T70/T90Rondolino Sample changer
HCl + NaOH = NaCl + H2O
HCl + CO32- = HCO3
- + Cl-
HCl + HCO3- = CO2 + H2O + Cl-
LabX Titration Software1 DV1010 buretteTitration beakers ME-101974Cable MultiPinTM-Lemo/Pt1000
METTLER TOLEDO
Neutralization of the acidic waste beforefinal disposal.
Wastedisposal
Preparation and Procedures50 mL tap waterSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi117-SC with internal temperaturesensor Pt1000
Indication
m-Value of Tap Water with Automatic Temperature Compensation
Note: This method allows a fully automated analysis procedureby using a Rondolinos sample changer. The method can beeasily modified for manual operation. Select "Manual stand" inthe method function "Titration stand".
1) Before the analysis an electrode calibration was performedusing METTLER TOLEDO buffers of pH 4.01, 7.00 and 9.21.
2) Fill a (preferably) PE bottle to the brim with the water to beanalyzed. Keep it closed and at sampling temperature.
3) Pipette 50 mL into the beaker shortly before titration.
4) The samples were analysed using a Rondolino samplechanger. The electrode was rinsed during 2 s and conditionedduring 10 s (Rondolino settings: 6). In this way, the electrode iscleaned with deionised water before starting the subsequentsample.
5) The automatic temperature compensation was achievedusing the new DG117-SC titration electrode with theMultiPinTM-Lemo/Pt1000 cable, connected to the analogueboard of the T50.
See also: Application M415, Brochure 34, ME-51 725 066
1) The method parameters have been optimised for the sampleused in this application. It may be necessary to slightly adaptthe method to your specific sample.
2) Automatic temperature compensation during titrationincreases the accuracy of the analysis (smaller limit of error),since temperature fluctuations are taken into consideration.
3) Comparison with the DG115-SC (no internal T-sensor).The following result was obtained from 8 samples:m-value: 2.650 +/- 0.005 mmol/L , srel: 0.188%.The slightly higher value probably arises from the missingtemperature correction. However the obtained m-valuesdetermined with both sensors are, as expected, rather similar.
4) The m-value (total alkalinity) represents the acid neutralizingcapacity and is determined in e.g. drinking water. Acidity canaffect corrosion, soil leaching and aquatic life in general. Thename originates from the methyl orange color indicator (red toyellow-orange at pH 4.3) formerly used. The acid capacitydepends on the equilibrium of free CO2, bicarbonate HCO3
-, andcarbonate CO3
2- in the on its temperature.Mineral weathering buffers groundwaters, e.g. limestone rockCaCO3 (s) + CO2 (g) = Ca2+ (aq) + 2 HCO3
- (aq)The bicarbonate ion then acts as a base to neutralize acids:HCO3
- (aq) + H+ (aq) = CO2 (g) + H2O (l)
Remarks
Total alkalinity or methyl orangealkalinity (m-value) is expressed asmmol/L or mg/L CaCO3
Calculation
Titration Excellence Line: The m-value of tap water is determined by endpoint titration to pH 4.3 with theDG117-SC sensor, which allows automatic temperature compensation during titration.
Standard Tris(hydroxymethyl)-aminomethane, 50-100 mg
Thomas HitzAuthor
Wastedisposal
37
EP-titraion (m-value of tap water)
3
4
5
6
7
8
9
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6
Volume (mL)
pH-v
alue
Table of measured values
All results Method-ID m365 Sample Tap water (1/8) R1 (Content) 2.62200 mmol/L Sample Tap water (2/8) R1 (Content) 2.61534 mmol/L Sample Tap water (3/8) R1 (Content) 2.61600 mmol/L Sample Tap water (4/8) R1 (Content) 2.61250 mmol/L Sample Tap water (5/8) R1 (Content) 2.62000 mmol/L Sample Tap water (6/8) R1 (Content) 2.61800 mmol/L Sample Tap water (7/8) R1 (Content) 2.61600 mmol/L Sample Tap water (8/8) R1 (Content) 2.63200 mmol/L
Statistics Method-ID m365 Content R1 Samples 8 Mean 2.61898 mmol/L s 0.00602 mmol/L srel 0.230 %
Titration curve
Results
38
Method m365 m-Value of tap water 10.08.2007Author Thomas Hitz
001 Title Type General titration Compatible with T50 / T70 / T90 ID m365 Title m-Value of tap water Author Thomas Hitz Date/Time 10.08.2007 10:00:00 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Tap water Entry type Fixed volume Volume 50 mL Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C
003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1
004 Stir Speed 50 % Duration 10 s
005 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L
Sensor Type pH Sensor DG117 Unit pH
Temperature acquisition Temperature acquisition Yes Temerature sensor interner Sensor 1 Unit °C
Stir Speed 50 %
Predispense Mode None Wait time 0 s
Control Control User End point type Absolute Tendency Negative Endpoint value 4.30 pH Control band 3.0 pH Dosing rate (max) 10 mL/min Dosing rate (min) 10 mL/min
Termination At EP Yes Tuermination delay 10 s At Vmax 10.0 mL Max. time Infinity
006 Calculation R1 Result Content Result unit mmol/L Formula R1=Q*C/m Constant C=1000 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
Method007 Record Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No d2E/dV2 - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No
008 End of sample
39
M366
Na2O, SiO2
KF solution, 25%
HCl, 2.0 mol/L (hydrochloric acid)NaOH, 1.0 mol/L (sodium hydroxide)
Titration Excellence T70/T902 additional dosing units
Na2SiO3 + 2HCl -> 2NaCl + SiO2 + H2OSiO2+6KF+2H2O -> Na2SiF6 + 4NaOHHCl + NaOH -> NaCl + H2O
Titration beakers ME-101974LabX Titration SoftwareRondo 20 Sample Changer
METTLER TOLEDO
Dilute and non-acidic fluoride solutionsdo not have to be treated as specialwaste.
Wastedisposal
Preparation and ProceduresWaterglass ~1.0 gSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
Sb850-S7/120 (pH sensor input)DX202-SC (ref. electrode)
Indication
Na2O and SiO2 in Waterglass
Determination of Na2O with HCl in Titration (EQP) [1]:Na2SiO3 + 2 HCl -> 2 NaCl + SiO2 + H2O
Add excess KF to form NaOH from SiO2:SiO2 + 6 KF + 2 H2O -> Na2SiF6 + 4 NaOH
Neutralise NaOH formed with excess HCl, back-titrate remainingHCl with NaOH in Titration (EQP) [2]:HCl + NaOH -> NaCl + H2O
1) Because of the high fluoride content in acidic environmentglass electrodes and titration beakers cannot be used for thedetermination of Na2O and SiO2 in waterglass.
2) For this reason only the polypropylene titration beakers canbe used. Care needs to be taken when weighing in thewaterglass samples in the polypropylene beakers that staticelectricity is avoided as much as possible.
3) Also, no glass sensors may be used for this determination asthese will be the corroded as well.All fluoride solutions should be kept in plastic bottles.
The titration curve for the first EQP titration shows clearly thatmore than one site is present for the alkali metal oxide (mainlyNa2O) component of waterglass.
Waterglass is used in a wide variety of application areas as e.g.,filler, additive, flame retardant, etc.
Order number for Sb850-S7/120:Available from MT-PRO, old Ingold no. 10 850 3074
Order no. for DX202 ref. electrode: ME-51 109 295
Remarks
R1: Na2O content (%)R2: SiO2 content (%)R3: Relative amounts Na2O/SiO2 (-)
Calculation
Titration Excellence Line: Method for the determination of Na2O and SiO2 in waterglass
Standard TRIS/THAM for HCl, KHP for NaOH
Melanie NijmanAuthor
Wastedisposal
40
Table of measured values
Method m366 Na2O and SiO2 in waterglass
RESULTSNo. ID Sample size and results
1 Waterglass 0.9365 gR1 = 49.91661 % ContentR2 = 44.05010 % ContentR3 = 1.13318 -
2 Waterglass 0.9843 gR1 = 49.92277 % ContentR2 = 44.32853 % ContentR3 = 1.12620 -
3 Waterglass 0.9806 gR1 = 49.85243 % ContentR2 = 44.21881 % ContentR3 = 1.12740 -
4 Waterglass 0.9521 gR1 = 49.90093 % ContentR2 = 44.02595 % ContentR3 = 1.13344 -
5 Waterglass 0.9843 gR1 = 49.88776 % ContentR2 = 44.25015 % ContentR3 = 1.12740 -
6 Waterglass 1.0449 gR1 = 49.89149 % ContentR2 = 44.35087 % ContentR3 = 1.12493 -
7 Waterglass 1.0130 gR1 = 49.95810 % ContentR2 = 44.25864 % ContentR3 = 1.12878 -
STATISTICSNumber results R1 n = 7Mean value x = 49.9043 % ContentStandard deviation s = 0.03298 ContentRelative standard deviation srel = 0.066 %
Number results R2 n = 7Mean value x = 44.21186 % ContentStandard deviation s = 0.12739 ContentRelative standard deviation srel = 0.288 %
Number results R3 n = 7Mean value x = 1.12876 -Standard deviation s = 0.00333 -Relative standard deviation srel = 0.295 %
Titration curve
Results
41
Method: m366 Na2O and SiO2 in waterglass 08.08.2007User: Melanie Nijman
001 Title Type General titration Compatible with T70/ T90 ID m366 Titel Na2O/SiO2 in Waterglass Author Melanie Nijman Date / Time 03.08.2007 Modified at 08.08.2007 Protect No SOP None LabX SOP002 Sample Number of IDs 1
ID 1 Waterglass Entry Type Weight Lower limit [g] 0.8 Upper limit [g] 1.2 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0 Entry Arbitrary003 Titration stand Type Rondo60/Tower A Titration stand Rondo60/1A Lid handling No004 Stir Speed [%] 50 Duration [s] 60 Condition No005 Titration (EQP)
Titrant Titrant HCl Concentration [mol/L] 2.0 Sensor Type mV Sensor Sb-850 Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 9.0 dV (min) 0.008 dV (max) 0.4 Mode Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold 1500 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 10 At potential No At Slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No
Accompanying stating Accompanying stating No Condition Condition No006 Calculation R1 Result Na2O Content Result Unit % Formula R1=Q*C/m Constant C= M/(10*z) M M[Sodium oxide] z z[Sodium oxide] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No007 Dispense (normal) Titrant 25% KF Concentration [mol/L] 25 Volume [mL] 10.0 Dosing rate [mL/min] 60.0 Condition No008 Dispense (normal) Titrant HCl Concentration [mol/L] 2.0 Volume [mL] 16.0 Dosing rate [mL/min] 60.0 Condition No
Method009 Stir Speed [%] 30 Duration [s] 30 Condition No010 Titration (EQP)
Titrant Titrant NaOH Concentration [mol/L] 1.0 Sensor Type mV Sensor Sb-850 Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Control User Titrant addition Dynamic dE (set value) 5 dV (min) 0.002 dV (max) 0.4 Mode Equilibrium controlled dE 1 dt [s] 1.0 t(min) [s] 3 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold 150 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 15 At potential No At Slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No
Accompanying stating Accompanying stating No Condition Condition No011 Calculation R2 Result SiO2 Content Result Unit % Formula R2=(QEX[1]+QENDDi[2]-Q[2])*C/m Constant C= M/(10*z) M M[Silicon dioxide] z z[Silicon dioxide] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No012 Calculation R3 Result Na2O/SiO2 Result Unit - Formula R2=R1/R2 Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Condition No013 Conditioning Type Fix Interval 1 Position Conditioning beaker Time [s] 20 Speed [%] 50 Condition No014 Record Summary No Results Per sample Raw results Per sample Table of measured values No Sample data No Resource data No E - V All titration functions dE/dV - V All titration functions ... E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No Condition No015 End of sample
42
M367
Chloride, Cl-,M = 35.45 g/mol, z = 1
50 mL Solvent (ASTM 3227)2-Propanol p.a.Toluene p.a.Sodium acetate (anhydrous)
Silver nitrate (AgNO3) in 2-Propanolc(AgNO3) = 0.01 mol/L
Titration Excellence T70/T90Rondo 20 Sample Changer withPowerShowerTM
NaCl + AgNO3 = AgCl + NaNO3
1 DV1005 BuretteGlass titration beaker ME-101446XS205 BalanceLabX Titration Software
METTLER TOLEDO
Filtration. The precipitate (AgCl) has tobe classified as special waste. Theliquid phase has to be disposed asorganic waste.
Wastedisposal
Preparation and ProceduresUsed motor oil, approx. 10 gSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DMi145-SC (with 1 mol/L KNO3)Indication
Chloride Content in Used Motor Oil
1) 10 g of sample is added into a glass titration beaker.
2) 2.5 mL 0.01mol/L NaCl standard solution are added tospike the sample since the chloride content is too low(Standard-Addition).
3) 50 mL Solvent ASTM 3227 will be added automatically withthe Rondo membrane pump.
4) The sample serie is analysed using a Rondo 20 samplechanger. Special beaker 1 and 2 are filled with toluene andthe condition beaker with solvent ASTM 3227.
Preparation of 0.01 mol/L NaCl- Dissolve 0.2922 g NaCl p.a. in deionized water- transfer quantitatively in a 500 volumetric flask and fill up to 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)
- The method parameters have been developed and optimisedfor the above mentioned sample. It may be necessary toslightly adapt the method to your specific sample. The weightof the sample can vary from 0.5 to 30 g (depending on thekind of oil).
- Sulfides interfere with the analysis. If necessary, they have tobe oxidised to sulfates by adding 10 mL 30% H2O2 previousto the analysis. In this application, this was not the case.
Literature:1) METTLER TOLEDO Application brochure 20, ME-51 725 0202) METTLER TOLEDO Application brochure 34, ME-51 725 066
Remarks
R1: Content (mg/L Chloride)
R1 = (Q-H[NaCl Std])*C/m,C = M*1000/z
1 mL AgNO3 (0.01 mol/l) is equal to0.354 mg Chloride
Calculation
Titration Excellence Line: Inorganic chloride content in used motor oil is determined by precipitation titrationin non aqueous solvent with silver nitrate. The content is expressed as chloride, Cl-.
Standard c(NaCl) = 0.01 mol/L, 2.5 mL
Claudia SchreinerAuthor
Wastedisposal
43
Table of measured values
Start time: 04.12.2007
Sample Data Note / ID Sample size No. 1/6 Motor Oil 10.0318 g No. 2/6 Motor Oil 10.1953 g No. 3/6 Motor Oil 10.0720 g No. 4/6 Motor Oil 10.1120 g No. 5/6 Motor Oil 10.1386 g No. 6/6 Motor Oil 10.1322 g
Results Note / ID Rx Result Unit No. 1/6 Motor Oil R1= 28.25 mg/L No. 2/6 Motor Oil R1= 27.80 mg/L No. 3/6 Motor Oil R1= 26.33 mg/L No. 4/6 Motor Oil R1= 27.35 mg/L No. 5/6 Motor Oil R1= 27.28 mg/L No. 6/6 Motor Oil R1= 26.38 mg/L
Statistics Rx Name n Mean Value Unit s srel[%] R1 Chloride 6 27.23 mg/L 0.76 2.8
Titration curve
Results
44
Method 367 Chloride content in motor oil 04.12.2007Author Claudia Schreiner
001 Title Type General titration Compatible with T70 / T90 ID 367 Title Chloride in motor oil Author Claudia Schreiner Date/Time 04.12.2007 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Motor oil Entry type Weight Lower limit 0 g Upper limit 15 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 PumpAuxiliary reagent ASTM D3227 solvent
Volume 50.0 mL
005 Stir Speed 60% Duration 120 s
006 Titration (EQP) [1]Titrant
Titrant AgNO3 Concentration 0.01 mol/L
Sensor Type mV Sensor DMi145-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 40%
Predispense Mode None Wait time 0 s
Control Control User Titrant addition Incremental dV 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t(min) 5 s t(max) 30 s
Evaluation and Recognition Procedure Standard Threshold 100 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No
Termination At Vmax 5 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No
Method007 Calculation R1 Result Chloride Result unit mg/L Formula R=(Q-H[Std NaCl])*C/m Constant C= M*1000/z M M[Chloride] z z[Chloride] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
008 RinseAuxiliary reagent ASTM D3227 solventRinse cycles 1Vol. per cycle [mL] 15Position Actual positionDrain NoCondition No
009 ConditioningType FixInterval 1Position Special beaker 1Time 120sSpeed 60%
010 ConditioningType FixInterval 1Position Special beaker 2Time 300sSpeed 60%
011 ConditioningType FixInterval 1Position Conditioning beakerTime 120sSpeed 60%
012 End of sample
45
M368
Chloride, Cl-,M = 35.45 g/mol, z = 1
50 mL Solvent (ASTM 3227)2-Propanol p.a.Toluene p.a.Sodium acetate (anhydrous)
Silver nitrate (AgNO3) in 2-Propanolc(AgNO3) = 0.01 mol/L
Titration Excellence T50/T70/T90Rondo 20 Sample Changer withPowerShowerTM
NaCl + AgNO3 = AgCl + NaNO3
1 DV1005 BuretteGlass titration beaker ME-101446XS205 BalanceLabX Titration Software
METTLER TOLEDO
Filtration. The precipitate (AgCl) has tobe classified as special waste. Theliquid phase has to be disposed asorganic waste.
Wastedisposal
Preparation and ProceduresPrimary standardSodium chloride solution (0.01 mol/L),2.5 mL
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DMi145-SC (with 1 mol/L KNO3)Indication
Titer Determination of 0.01 mol/L AgNO3 in 2-Propanol
1) Pipette 2.5 mL 0.01mol/L NaCl standard solution in atitration beaker
2) 50 mL Solvent ASTM 3227 will be added automatically withthe Rondo membrane pump.
3) The sample serie is analysed using a Rondo 20 samplechanger. The condition beaker is filled with solvent ASTM3227.
Preparation of 0.01 mol/L NaCl- Dissolve 0.2922 g NaCl p.a. in deionized water- transfer quantitatively in a 500 volumetric flask and fill up to 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)
- This method is used to standardize the silver nitrate solutionwhich is used in the method M367 (Chloride in motor oil).
Remarks
R1: Titer
R1 = m/(VEQ*c*C)C = 1/(cst*z)
1 mL AgNO3 (0.01 mol/l) is equal to0.584 mg sodium chloride
Calculation
Titration Excellence Line: Method for the titer determination of 0.01 mol/L AgNO3 by precipitation titration withsodium chloride as a primary standard.
Standard c(NaCl) = 0.01 mol/L, 2.5 mL
Claudia SchreinerAuthor
Wastedisposal
46
Table of measured values
Start time: 04.12.2007
Sample Data Note / ID Sample size No. 1/6 NaCl solution 2.5 mL No. 2/6 NaCl solution 2.5 mL No. 3/6 NaCl solution 2.5 mL No. 4/6 NaCl solution 2.5 mL No. 5/6 NaCl solution 2.5 mL No. 6/6 NaCl solution 2.5 mL
Results Note / ID Rx Result Unit No. 1/6 NaCl solution R1= 0.9694 mg/L No. 2/6 NaCl solution R1= 0.9684 mg/L No. 3/6 NaCl solution R1= 0.9704 mg/L No. 4/6 NaCl solution R1= 0.9690 mg/L No. 5/6 NaCl solution R1= 0.9708 mg/L No. 6/6 NaCl solution R1= 0.9711 mg/L
Statistics Rx Name n Mean Value Unit s srel[%] R1 Titer 6 0.9698 mg/L 0.0011 0.11
Titration curve
Results
47
Method 368 Titer 0.01 mol/L AgNO3 04.12.2007Author Claudia Schreiner
001 Title Type General titration Compatible with T50 / T70 / T90 ID 368 Title Titer 0.01 mol/L AgNO3 Author Claudia Schreiner Date/Time 04.12.2007 Modified -- Modified by -- Protect No SOP None
002 Sample (Titer) Titrant AgNO3 Concentration 0.01 mol/L Standard NaCl Type of standard liquid Entry type Fixed volume Volume 2.5 mL Correction factor 1.0 Temperature 25.0°C
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A
004 PumpAuxiliary reagent ASTM D3227 solvent
Volume 50.0 mL
005 Stir Speed 40% Duration 120 s
006 Titration (EQP) [1]Titrant
Titrant AgNO3 Concentration 0.01 mol/L
Sensor Type mV Sensor DMi145-SC Unit mV
Temperature acquisition Temperature acquisition No
Stir Speed 40%
Predispense Mode Volume Volume 1.5 mL Wait time 15 s
Control Control User Titrant addition Incremental dV 0.1 mL Mode Equilibrium controlled dE 1.0 mV dt 3 s t(min) 5 s t(max) 30 s
Evaluation and Recognition Procedure Standard Threshold 100 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No
Termination At Vmax 5 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No
Method007 Calculation R1 Result Titer Result unit --- Formula R= m/(VEQ*c*C) Constant C= 1/(cst*z) M M[Sodium chloride] z z[Sodium chloride] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
008 RinseAuxiliary reagent ASTM D3227 solventRinse cycles 1Vol. per cycle [mL] 15Position Actual positionDrain NoCondition No
009 ConditioningType FixInterval 1Position Conditioning beakerTime 120sSpeed 60%
010 End of sample
011 Titer Titrant AgNO3 Concentration 0.01 mol/L Titer = Mean[R1] Limits No
48
M369
Peroxide functional group, R-OOH
20 mL acetic acid/chloroform (3:2)1 mL saturated KI solution50 mL deion. water
Sodium thiosulfate, Na2S2O3
c(Na2S2O3)= 0.01mol/L
Titration Excellence T70/T90Rondo 20 Sample Changer withPowerShowerTM
R-OOH + 2 I- + 2 H3O+ =
R-OH + I2 + 3 H2O
I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6
2 additional dosing units1 DV1020 and 2 DV1010 BurettesGlass titration beaker ME-101446XS205 Balance, LabX 2.6
METTLER TOLEDO
The waste contains halogenatedorganic solvents and has to bedisposed of accordingly.
Wastedisposal
Preparation and ProceduresSunflower oil, 4-5 gOlive oil, 1 gMargarine, 2 g
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DMi147-SCIndication
Peroxide Value of Edible Oils and Fats
1) Beakers have to be cleaned very well. Invisible fat residues ormetal traces can strongly affect the result.
2) About 3 g of sample were dissolved in 20 mL of acetic acid/chloroform (3:2) The acetic acid/chloroform mixture was addedby the function DISPENSE.
3) 1 mL saturated KI solution is added by an additional burette.The reaction takes place and iodine is formed.
4) 50 mL deionized water are added by the membrane pump ofRondo 20.
5) Iodine is titrated with sodium thiosulphate.
127 g KI were dissolved in 100 mL water to obtain thesaturated KI solution. The solution has to be kept in the dark.
Impurities of the solvent are taken into account by a blank valuedetermination. The blank value determination is done under thesame conditions as the peroxide value determination itself. Thevalue is stored under B[1].
1) Fats and oils undergo changes during storage due tooxidation with air (oxidative rancidity). The compounds formedreact as peroxides. Their content is commonly expressed as the"peroxide value" in milliequivalents peroxidic oxygen per kg ofsample.
2) Peroxide values higher than 10 to 20 meq O2/kg arecommonly interpreted as rancidity. Unrefined oils have higherperoxide values. They are usually in the range between 5 to 20meq O2/kg.
1) Exactly 60 seconds were allowed for the generation of iodine,as is requested by the official method (AOAC No. 28.022).
2) Earlier studies, however, had indicated that the generation isnot complete yet at this time. 200 to 300 seconds were foundto yield the highest results. Longer generation times resulted inlow results (secondary reactions between iodine and the oil).
3) The duration of the generation time (time between 'adding theKI solution' and 'adding the water + starting the titration') is thecritical point for repeatable results.
Remarks
R = (Q-B[1])*C/mC = 1000, meq/kg
B[1]: Solvent blank value, mmol
Calculation
Titration Excellence Line: Method for the determination of the peroxide value in oil, fat and margarine byiodometric titration with sodium thiosulphate of released iodine.
Standard Potassium iodate, KIO3
Maria-José SchmidAuthor
Wastedisposal
49
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN -16.7 NaN NaN 0 250.057 0.057 -8 8.7 NaN 3 250.086 0.029 -11.3 -3.3 NaN 8 250.1 0.014 -11.2 0.1 NaN 13 250.135 0.035 -10.9 0.3 NaN 18 250.222 0.087 -10.4 0.5 5.85 23 250.322 0.1 -10.1 0.3 4.51 28 250.422 0.1 -9.6 0.5 4.57 33 250.522 0.1 -9.1 0.5 4.98 38 250.622 0.1 -8.6 0.5 5.57 43 250.722 0.1 -8.1 0.5 6.12 48 250.822 0.1 -7.3 0.8 6.4 53 250.922 0.1 -6.7 0.6 6.84 58 251.022 0.1 -6 0.7 7.31 64 251.122 0.1 -5.3 0.7 7.76 69 251.222 0.1 -4.5 0.8 8.08 74 251.322 0.1 -3.6 0.9 8.42 79 251.422 0.1 -2.7 0.9 8.92 84 251.522 0.1 -1.8 0.9 9.72 89 251.622 0.1 -0.9 0.9 10.58 94 251.722 0.1 0.2 1.1 12.06 99 251.822 0.1 1.7 1.5 13.44 104 251.922 0.1 3.1 1.4 15.57 109 252.022 0.1 4.7 1.6 17.35 114 252.122 0.1 6.8 2.1 16.96 120 252.222 0.1 8.9 2.1 22.42 125 252.322 0.1 12.2 3.3 36.29 130 252.422 0.1 15.7 3.5 64.9 135 252.522 0.1 21.7 6 129.96 142 252.622 0.1 35.3 13.6 311.23 158 252.642 0.02 42.2 6.9 520.27 169 252.648 0.006 46.4 4.2 822.53 180 252.654 0.006 50 3.6 1165.65 190 252.661 0.007 57.2 7.2 1330.43 202 252.666 0.005 66.2 9 1635.55 217 252.671 0.005 78.3 12.1 1915.47 232 25
EQP1 2.671216 NaN 78.8 NaN 1916.21 NaN NaN2.676 0.005 89.8 11.5 1536.17 247 252.681 0.005 97.7 7.9 1263.43 262 252.686 0.005 104 6.3 1191.38 277 252.694 0.008 109.9 5.9 774.71 292 252.704 0.01 114.2 4.3 NaN 303 252.728 0.024 120.3 6.1 NaN 318 252.772 0.044 125.3 5 NaN 330 252.872 0.1 130 4.7 NaN 342 252.972 0.1 132.5 2.5 NaN 351 25
Table of measured values
Method: DM1471 Peroxide number 10/25/2007 11:27:34 AMStart time: 25.10.2007 1:53:24 PM___________________________________________________________________________________________
Sample Data Comment / ID Sample size No. 1/5 Olive oil 0.8164 g No. 2/5 Olive oil 0.8523 g No. 3/5 Olive oil 0.815 g No. 4/5 Olive oil 0.8149 g No. 5/5 Olive oil 0.8235 g
Results No. Comment / ID Start time Rx Result Unit Name 1/5 Olive oil 10/25/2007 1:53:25 PM R1= 0.024 mmol Consumption R2= 25.601 meq/kg Content 2/5 Olive oil 10/25/2007 2:05:29 PM R1= 0.025 mmol Consumption R2= 25.795 meq/kg Content 3/5 Olive oil 10/25/2007 2:17:32 PM R1= 0.024 mmol Consumption R2= 26.013 meq/kg Content 4/5 Olive oil 10/25/2007 2:29:19 PM R1= 0.024 mmol Consumption R2= 25.888 meq/kg Content 5/5 Olive oil 10/25/2007 2:41:10 PM R1= 0.024 mmol Consumption R2= 26.074 meq/kg ContentSQC/Statistics
Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________
R1 Consumption 5 0.024 mmol 0.000 1.848 R2 Content 5 25.874 meq/kg 0.187 0.724
Additional results
Sample Size n Mean value Unit s srel[%] ____________________________________________________________________________________________
Sunflower oil 4-5 g 5 0.028 mmol 0.000 1.609 5.583 meq/kg 0.044 0.791
Margarine 2 g 6 0.022 mmol 0.001 4.624 11.759 meq/kg 0.578 4.918
Mais oil 4-5 g 5 0.021 mmol 0.000 2.150 3.980 meq/kg 0.043 1.087
Titration curve
Results
50
Method DM1471 Peroxide number 25.10.2007Author schmid
001 Title Type General titration Compatible with T70 / T90 ID DM1471 Title Peroxide number Author schmid Date/Time 10/16/2007 12:37:42 pm Modified 10/25/2007 11.27:34 am Modified by Administrator Protect No SOP None002 Sample Number of IDs 1 ID 1 Olive oil Entry type Weight Lower limit 0.5 g Upper limit 20 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant AA/Chloroform Concentration 32 Volume 20 mL Dosing rate 60.0 mL/min Condition No005 Stir Speed 40 % Duration 30 s Condition No006 Dispense (normal) [2] Titrant KI Concentration 63.5 Volume 1 mL Dosing rate 60.0 mL/min Condition No007 Stir Speed 30 % Duration 30 s Condition No008 Stir Speed 0 % Duration 60 s Condition No009 Pump
Auxiliary reagent Water Volume 50.0 mL Condition No010 Titration (EQP) [1]Titrant
Titrant Na2S2O3
Concentration 0.01 mol/LSensor
Type mV Sensor DM147 Unit mVTemperature acquisition
Temperature acquisition NoStir
Speed 30%Predispense
Mode Volume Volume 0.1 mL Wait time 0 s Control Control Cautious Mode Redox Show parameters Yes Titrant addition Dynamic dE(set value) 6.0 mV dV(min) 0.005 mL dV(max) 0.1 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 5.0 s t(max) 15.0 s
MethodEvaluation and Recognition
Procedure Standard Threshold 200.0 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination
At Vmax 20 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria NoAccompanying stating
Accompanying stating NoCondition
Condition No011 Calculation R1 Result Consumption Result unit mmol Formula R1=Q Constant 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Calculation R2 Result Content Result unit meq/kg Formula R2=(Q-B[1])*C/m Constant 1000 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No013 Record ......014 Rinse
Auxiliary reagent WaterRinse cycles 1Vol. per cycle [mL] 10 mLPosition Actual positionDrain NoCondition No
015 ConditioningType FixInterval 1Position According to intervalTime 60 sSpeed 30%
Condition No016 Rinse
Auxiliary reagent WaterRinse cycles 1Vol. per cycle [mL] 10 mLPosition Actual positionDrain NoCondition No
017 ConditioningType FixInterval 1Position Conditioning beakerTime 10 sSpeed 30 %
Condition No 018 End of sample019 Park Titration stand Rondo60/1A Position Conditioning beaker Condition No
51
M370
Potassium iodate, KIO3
M=213.99 g/mol ; z = 6
40 mL HCl 0.1 mol/L1 mL saturated KI solution
Sodium thiosulfate, Na2S2O3
c(Na2S2O3)= 0.01mol/L
Titration Excellence T70/T90Rondo 20 Sample Changer withPowerShowerTM
IO3- + 5 I- + 6 H+ = 3 I2 + 3 H2O
I2 + 2 Na2S2O3 = 2 NaI + Na2S4O6
2 additional dosing units1 DV1020 and 2 DV1010 BurettesGlass titration beaker ME-101446XS205 Balance, LabX 2.6
METTLER TOLEDO
Inorganic salt solutionWastedisposal
Preparation and Procedures1 mL potassium iodate standardsolution, KIO3
c(KIO3) = 0.01 mol/L
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DMi147-SCIndication
Titer Determination of 0.01 mol/L Na2S2O3
1) Beakers have to be cleaned very well. Fat residues or metaltraces can strongly affect the result.
2) About 3 g of sample were dissolved in 20 mL of acetic acid/chloroform (3:2) The acetic acid/chloroform mixture was addedby the function DISPENSE.
3) 1 mL saturated KI solution is added by an additional burette.The reaction takes place and iodine is formed.
4) 50 mL deionized water are added by the membrane pump ofRondo 20.
5) Iodine is titrated with sodium thiosulphate.
127 g KI were dissolved in 100 mL water to obtain thesaturated KI solution. The solution has to be kept in the dark.
Impurities of the solvent are taken into account by a blank valuedetermination. The blank value determination is done under thesame conditions as the peroxide value determination itself. Thevalue is stored under B[1].
1) Fats and oils undergo changes during storage due tooxidation with air (oxidative rancidity). The compounds formedreact as peroxides. Their content is commonly expressed as the"peroxide value" in milliequivalents peroxidic oxygen per kg ofsample.
2) Peroxide values higher than 10 to 20 meq O2/kg arecommonly interpreted as rancidity. Unrefined oils have higherperoxide values. They are usually in the range between 5 to 20meq O2/kg.
1) Exactly 60 seconds were allowed for the generation of iodine,as is requested by the official method (AOAC No. 28.022).
2) Earlier studies, however, had indicated that the generation isnot complete yet at this time. 200 to 300 seconds were foundto yield the highest results. Longer generation times resulted inlow results (secondary reactions between iodine and the oil).
3) The duration of the generation time (time between 'adding theKI solution' and 'adding the water + starting the titration') is thecritical point for repeatable results.
Remarks
R1=m/(VEQ*c*C)
C=1/(cst*z)
cst = concentration of standard solution
Calculation
Titration Excellence Line: Method for the titer determination of 0.01 mol/L Na2S2O3 by redox titration withpotassium iodate as a primary standard.
Standard ---
Maria-José SchmidAuthor
Wastedisposal
52
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN 18.4 NaN NaN 0 251.143 1.143 19.6 1.2 NaN 6 251.714 0.571 20.6 1 NaN 11 252 0.286 21.1 0.5 NaN 16 252.1 0.1 21.3 0.2 NaN 21 252.2 0.1 21.4 0.1 1.86 26 252.3 0.1 21.6 0.2 1.83 31 252.4 0.1 21.8 0.2 1.89 36 252.5 0.1 22 0.2 2.1 41 252.6 0.1 22.2 0.2 2.2 46 252.7 0.1 22.4 0.2 2.2 51 252.8 0.1 22.7 0.3 2.36 56 252.9 0.1 22.9 0.2 2.44 62 253 0.1 23.1 0.2 2.5 67 253.1 0.1 23.4 0.3 2.56 72 253.2 0.1 23.7 0.3 2.64 77 253.3 0.1 23.9 0.2 2.8 82 253.4 0.1 24.2 0.3 2.8 87 253.5 0.1 24.5 0.3 2.9 92 253.6 0.1 24.8 0.3 3.05 97 253.7 0.1 25.1 0.3 3.2 102 253.8 0.1 25.4 0.3 3.3 107 253.9 0.1 25.8 0.4 3.5 112 254 0.1 26.1 0.3 3.64 117 254.1 0.1 26.5 0.4 3.86 122 254.2 0.1 26.9 0.4 4 128 254.3 0.1 27.3 0.4 4.08 133 254.4 0.1 27.7 0.4 4.36 138 254.5 0.1 28.2 0.5 4.54 143 254.6 0.1 28.6 0.4 4.84 148 254.7 0.1 29.1 0.5 5.1 153 254.8 0.1 29.7 0.6 5.4 158 254.9 0.1 30.2 0.5 5.69 163 255 0.1 30.8 0.6 6.1 168 255.1 0.1 31.4 0.6 6.44 173 255.2 0.1 32.1 0.7 6.88 178 255.3 0.1 32.8 0.7 7.5 183 255.4 0.1 33.6 0.8 7.99 188 255.5 0.1 34.4 0.8 8.58 194 255.6 0.1 35.3 0.9 9.23 199 255.7 0.1 36.3 1 10.07 204 255.8 0.1 37.3 1 11.05 209 255.9 0.1 38.5 1.2 12.35 214 256 0.1 39.8 1.3 13.82 219 256.1 0.1 41.3 1.5 15.51 224 256.2 0.1 43 1.7 17.1 229 256.3 0.1 45 2 18.16 234 256.4 0.1 47.3 2.3 23.2 239 256.5 0.1 50.2 2.9 36.4 244 256.6 0.1 54.1 3.9 64.74 250 256.7 0.1 60.4 6.3 131.13 258 256.79 0.09 71.4 11 293.52 272 256.815 0.025 79.3 7.9 480.39 285 256.822 0.007 83.3 4 710.68 294 256.829 0.007 87.6 4.3 987.73 304 256.836 0.007 95.1 7.5 1151.71 319 256.841 0.005 103.2 8.1 1337.28 334 256.846 0.005 111.9 8.7 1610.88 349 25
EQP1 6.846215 NaN 112.3 NaN 1611.06 NaN NaN6.851 0.005 120.2 8.3 1474.04 364 256.856 0.005 127.6 7.4 1174.26 379 256.861 0.005 134.1 6.5 1070.14 394 256.866 0.005 139.3 5.2 881.97 408 256.875 0.009 144.3 5 NaN 420 256.892 0.017 150.4 6.1 NaN 434 256.919 0.027 155.5 5.1 NaN 445 256.981 0.062 161 5.5 NaN 456 257.081 0.1 165.3 4.3 NaN 466 25
Table of measured values
Method: T147 Titer Na2S2O3 09.10.2007 13:39:16Start time: 09.10.2007 13:42:03___________________________________________________________________________________________
Results
No. Comment / ID Start time Rx Result Unit Name 1/5 Potassium iodate 09.10.2007 13:42:03 R1= 0.901 -- Titer 2/5 Potassium iodate 09.10.2007 13:55:31 R1= 0.909 -- Titer 3/5 Potassium iodate 09.10.2007 14:08:40 R1= 0.910 -- Titer 4/5 Potassium iodate 09.10.2007 14:21:55 R1= 0.908 -- Titer 5/5 Potassium iodate 09.10.2007 14:35:14 R1= 0.908 -- Titer
SQC/Statistics
Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________
R1 Titer 5 0.906 -- 0.004 0.437
Titration curve
Results
53
Method T147 Titer Na2S2O3 09.10.2007Author schmid
001 Title Type Titer determination Compatible with T70 / T90 ID T147 Title Titer Na2S2O3
Author schmid Date/Time 09.10.2007 13:39:16 Modified 09.10.2007 13:39:16 Modified by Administrator Protect No SOP None LabX SOP002 Sample (Titer) Titrant Na2S2O3
Concentration [mol/L] 0.01 Standard Potassium iodate
Type of standard liquid Entry type Fixed weight Volume 1.0 mL Correction factor 1.0 Temperature 25.0°C003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant HCl Concentration 0.1 mol/L Volume 40.0 mL Dosing rate 60.0 mL/min Condition No005 Dispense (normal) [2] Titrant KI Concentration 63.5 mol/L Volume 1.0 mL Dosing rate 60.0 mL/min Condition No006 Stir Speed 30 % Duration 30 s Condition No007 Stir Speed [%] 0 % Duration [s] 60 s Condition No008 Titration (EQP) [1]Titrant
Titrant Na2S2O3
Concentration 0.01 mol/LSensor
Type mV Sensor DM147 Unit mVTemperature acquisition
Temperature acquisition NoStir
Speed 30 %Predispense
Mode Volume Volume 2.0 mL Wait time 0 s Control Control Cautious Mode Redox Show parameters Yes Titrant addition Dynamic dE(set value) 6.0 mV dV(min) 0.005 mL dV(max) 0.1 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 5.0 s t(max) 15.0 s
MethodEvaluation and Recognition
Procedure Standard Threshold 200.0 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination
At Vmax 10 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria NoAccompanying stating
Accompanying stating NoCondition
Condition No009 Rinse
Auxiliary reagent WaterRinse cycles 1Vol. per cycle [mL] 10 mLPosition Actual positionDrain NoCondition No
010 Calculation R1 Result Titer Result unit -- Formula R1=m/(VEQ*c*C) Constant 1/(cst*z) M M[Potassium iodate] z z[Potassium iodate] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No011 Record Summary No Results Per sample Raw results Per sample Table of meas. values Last titration function Sample data No ............... Method No Series data No Condition No012 End of sample013 Titer Titrant Na2S2O3
Concentration 0.01 mol/L TITER= Mean[R1] Limits No Condition No014 Park
Titration stand Rondo60/1A Position Conditioning beaker Condition No015 Calculation R2 Result Mean Titer Result unit -- Formula R2=Mean[R1] Constant 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No016 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No
54
M371
Chloride ions, Cl-
M(Cl) = 35.45 g/mol, z = 1
Perchloric acid, HClO4 (0.1 mol/L)Sodium chloride, NaCl (0.001 mol/L)
Silver nitrate, AgNO3
c(AgNO3)= 0.001mol/L
Titration Excellence T50/T70/T90Rondo 20 Sample Changer withPowerShowerTM
NaCl + AgNO3 = AgCl + NaNO3
1 additional dosing unit2 DV1010 BurettesTitration beaker ME-101974XS205 Balance, LabX 2.6
METTLER TOLEDO
Neutralization before final disposal asheavy metal aqueous solutions.
Wastedisposal
Preparation and ProceduresEthanol, 40 g(approx. 60 mL)
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DMi148-SCIndication
Chloride Determination in Ethanol
The samples have been prepared by spiking high purity ethanolwith NaCl solution in order to achieve different chorideconcentrations. In this way, several NaCl ethanolic solutionshave been prepared.General procedure:1) Weigh accurately ethanolic NaCl solution into the beaker.2) Add 1 mL 0.001 mol/L NaCl standard solution to spike thesample.3) The sample is acidified by adding 1 mL 0.1 mol/L HClO4
using an additional dosing unit. If this is not available,perchloric acid is added with a manual pipette.4) Place the beaker on the Rondo sample rack and start thedetermination.
1) Weigh accurately 40 g ethanol into the titration beaker.2) Add 1 mL 0.001 mol/L NaCl standard solution to spike theblank sample.3) 1 mL 0.1 mol/L HClO4 is added to the blank solution usingan additional dosing unit. if this is not available, perchloric acidis added using a manual pipette.4) Place the beaker on the Rondo sample rack and start theblank value determination.
Literature:
1. "Standard Tests Methods for Chloride Ion in Water"ASTM D512-04
2. METTLER TOLEDO Titration Application M359,"Chloride content determination in ethanol based on ASTM D512-04".
3. "Selected METTLER TOLEDO Methods for Biofuel Analysis"Application Brochure 36, May 2007, ME-51725070
Remarks
R = (Q-B[Blank EtOH])*C/mC = M*100/z, mg/kg
B[Blank EtOH]:Solvent blank value, mmol
Calculation
Titration Excellence Line: Method for the determination of the chloride content in ethanol by precipitationtitration with silver nitrate.
Standard NaCl solution, 1 mL 0.001 mol/L
Maria-José SchmidAuthor
Wastedisposal
55
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN 161 NaN NaN 0 250.057 0.057 160.9 -0.1 NaN 3 250.086 0.029 160.4 -0.5 NaN 6 250.1 0.014 160.2 -0.2 NaN 9 250.135 0.035 160.3 0.1 NaN 27 250.222 0.087 158.7 -1.6 -15.74 31 250.422 0.2 154.4 -4.3 -22.1 36 250.622 0.2 149.4 -5 -28.41 42 250.822 0.2 143 -6.4 -37.69 48 250.943 0.121 137.9 -5.1 -45.94 56 251.032 0.089 133.8 -4.1 -54.77 62 251.135 0.103 128.3 -5.5 -68.8 68 251.213 0.078 122.9 -5.4 -85.4 75 251.269 0.056 118 -4.9 -102.81 82 251.314 0.045 113.3 -4.7 -124.84 89 251.355 0.041 108.2 -5.1 -154.59 97 251.388 0.033 103.1 -5.1 -189.02 106 251.415 0.027 97.9 -5.2 -231.57 115 251.435 0.02 93.2 -4.7 -278.49 124 251.452 0.017 88.1 -5.1 -335.6 135 251.466 0.014 83.7 -4.4 -401.04 145 251.479 0.013 78.3 -5.4 -491.7 157 251.49 0.011 72.9 -5.4 -606.1 170 251.497 0.007 68.3 -4.6 -704.71 183 251.504 0.007 63.3 -5 -839.84 196 251.51 0.006 58 -5.3 -977.31 212 251.514 0.004 53.5 -4.5 -1090.51 225 251.519 0.005 47.8 -5.7 -1234.77 243 251.523 0.004 42.6 -5.2 -1364.69 259 251.527 0.004 36.7 -5.9 -1472.06 278 251.531 0.004 30.7 -6 -1517.89 296 25
EQP1 1.533123 NaN 27.7 NaN -1552.6 NaN NaN1.535 0.004 25 -5.7 -1545.86 314 251.539 0.004 17.9 -7.1 -1427.73 336 251.543 0.004 12.7 -5.2 -1302.62 352 251.548 0.005 6.6 -6.1 -1135.67 369 251.552 0.004 1.3 -5.3 -1019.34 386 251.557 0.005 -2 -3.3 NaN 392 251.568 0.011 -10.7 -8.7 NaN 411 251.574 0.006 -14.9 -4.2 NaN 423 251.582 0.008 -19.3 -4.4 NaN 435 251.592 0.01 -24.2 -4.9 NaN 447 25
Table of measured values
Method: 148 Chloride content in EtOH 12/18/2007 12:17:35 PMStart time: 12/18/2007 12:17:35 AM___________________________________________________________________________________________
Sample Data Comment / ID Sample size No. 1/5 Ethanol 38.672 g No. 2/5 Ethanol 38.4992 g No. 3/5 Ethanol 38.791 g No. 4/5 Ethanol 38.983 g No. 5/5 Ethanol 38.9095 g
Results No. Comment / ID Start time Rx Result Unit Name 1/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.45 mg/kg Content
2/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.48 mg/kg Content
3/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.45 mg/kg Content
4/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.45 mg/kg Content
5/5 Ethanol 12/18/2007 12:17:35 PM R1= 0.45 mg/kg Content
SQC/Statistics
Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________
R1 Content 5 0.46 mg/kg 0.01 2.942
Additional results
Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________
R1 Content 3 4.61 mg/kg 0.06 1.253 R1 Content 5 12.15 mg/kg 0.04 0.291 R1 Content 5 23.60 mg/kg 0.08 0.318
DM140 electrode results
Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________
R1 Content 3 0.43 mg/kg 0.07 16.279 R1 Content 3 5.60 mg/kg 0.55 9.749
Titration curve
Results
56
Method 148 Chloride content in EtOH 18.12.2007 12:16:30Author schmid
001 Title Type General titration Compatible with T50 / T70 / T90 ID 148 Title Chloride content in EtOH Author schmid Date/Time 22.11.2007 12:09:49 Modified 18.12.2007 12:16:30 Modified by schmid Protect No SOP None002 Sample Number of IDs 1 ID 1 Ethanol Entry type Weight Lower limit 1 g Upper limit 60 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0°C Entry Arbitrary003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant HClO4 Concentration 0.1 mol/L Volume 1 mL Dosing rate 60.0 mL/min Condition No005 Stir Speed 40 % Duration 15 s Condition No006 Titration (EQP) [1]Titrant
Titrant AgNO3 Concentration 0.001 mol/LSensor
Type mV Sensor DM148-SC Unit mVTemperature acquisition
Temperature acquisition NoStir
Speed 30%Predispense
Mode Volume Volume 0.1 mL Wait time 15 s Control Control Cautious Mode Precipitation Show parameters Yes Titrant addition Dynamic dE(set value) 5.0 mV dV(min) 0.004 mL dV(max) 0.2 mL Meas. val. acquisition Equilibrium controlled dE 0.5 mV dt 2.0 s t(min) 3.0 s t(max) 30.0 sEvaluation and Recognition
Procedure Standard Threshold 200.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria NoTermination
At Vmax 15 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria NoAccompanying stating
Accompanying stating NoCondition
Condition No
Method007 Calculation R1 Result Content Result unit mg/kg Formula R1=(Q-B[Blank EtOH])*C/m Constant M*1000/z M M[Chloride] z z[Chloride] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No008 Record Summary No Results Per sample Raw results Per sample Table of meas. values Last titration function Sample data Per series Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No
d2E/dV2 - V No BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No009 Rinse
Auxiliary reagent WaterRinse cycles 1Vol. per cycle [mL] 10 mLPosition Actual positionDrain NoCondition No
010 ConditioningType FixInterval 1Position Conditioning beakerTime 10 sSpeed 30%
Condition No 011 End of sample
-------------------------------------------------------Blank Titration.......Predispense
Mode Volume Volume 0 mL Wait time 0 s.......007 Calculation R1 Result Blank Ethanol Result unit mmol Formula R1=Q Constant 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No.......014 Blank Name Blank EtOH Result unit mmol Formula R2=Mean[R1] .....
57
M372
Sodium chloride, NaClM=58.44 g/mol ; z = 1
50 mL deionized waterPerchloric acid, HClO4 (0.1 mol/L)1 mL
Silver nitrate, AgNO3
c(AgNO3)= 0.01mol/L
Titration Excellence T50/T70/T90Rondo 20 Sample Changer withPowerShowerTM
NaCl + AgNO3 = AgCl + NaNO3
1 additional dosing units2 DV1010 BurettesGlass titration beaker ME-101446XS205 Balance, LabX 2.6
METTLER TOLEDO
Neutralization before final disposal asheavy metal aqueous solutions.
Wastedisposal
Preparation and Procedures5 mL sodium chloride iodate standardsolution, NaClc(NaCl) = 0.001 mol/L
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DMi148-SCIndication
Titer Determination of 0.001 mol/L AgNO3
1) Beakers have to be cleaned very well.
2) Add 5 mL 0.001 mol/L NaCl standard solution.
3) 1 mL 0.1 mol/L HClO4 is added to the solution using anadditional dosing unit. If this is not available, perchloric acid isadded using a manual pipette.
4) Place the beaker on the Rondo sample rack and start thedetermination.
Remarks
R1=m/(VEQ*c*C)
C=1/(cst*z)
cst = concentration of standard solution
Calculation
Titration Excellence Line: Method for the titer determination of 0.001 mol/L AgNO3 by precipitation reactionwith sodium chloride as a primary standard.
Standard ---
Maria-José SchmidAuthor
Wastedisposal
58
Volume Increment Signal Change 1st deriv. Time Temperature mL mL mV mV mV/mL s °C0 NaN 116.3 NaN NaN 0 250.571 0.571 113.9 -2.4 NaN 6 250.857 0.286 112.4 -1.5 NaN 10 251 0.143 111.6 -0.8 NaN 13 251.2 0.2 110.4 -1.2 NaN 18 251.4 0.2 109.1 -1.3 -6.44 22 251.6 0.2 107.8 -1.3 -6.64 26 251.8 0.2 106.5 -1.3 -6.8 30 252 0.2 105.1 -1.4 -7.05 35 252.2 0.2 103.6 -1.5 -7.34 39 252.4 0.2 102.2 -1.4 -7.66 43 252.6 0.2 100.6 -1.6 -8.05 48 252.8 0.2 98.9 -1.7 -8.44 52 253 0.2 97.2 -1.7 -8.85 57 253.2 0.2 95.4 -1.8 -9.36 62 253.4 0.2 93.4 -2 -9.93 66 253.6 0.2 91.4 -2 -10.72 71 253.8 0.2 89.2 -2.2 -11.64 76 254 0.2 86.7 -2.5 -12.73 82 254.2 0.2 84 -2.7 -14 87 254.4 0.2 81 -3 -15.66 93 254.6 0.2 77.7 -3.3 -17.84 98 254.8 0.2 73.8 -3.9 -20.92 104 255 0.2 69.3 -4.5 -25.48 111 255.2 0.2 63.7 -5.6 -32.7 118 255.362 0.162 58.1 -5.6 -41.67 125 255.479 0.117 53.1 -5 -51.27 132 255.571 0.092 48.4 -4.7 -62.11 140 255.655 0.084 43 -5.4 -76.65 147 255.716 0.061 38.3 -4.7 -91.36 155 255.771 0.055 33.4 -4.9 -110.67 163 255.818 0.047 27.9 -5.5 -134.94 172 255.852 0.034 23.2 -4.7 -159.1 181 255.88 0.028 18.3 -4.9 -185.61 191 255.906 0.026 13.7 -4.6 -218.32 200 255.93 0.024 8.1 -5.6 -257.57 212 255.947 0.017 3.4 -4.7 -292.97 223 255.963 0.016 -1.4 -4.8 -334.94 234 255.978 0.015 -6.8 -5.4 -383.1 247 255.99 0.012 -11.6 -4.8 -420.6 259 256 0.01 -16.4 -4.8 -456.08 272 256.01 0.01 -21 -4.6 -478.18 285 25
EQP1 6.014073 NaN -23.1 NaN -479.1 NaN NaN6.021 0.011 -26.6 -5.6 -476.74 300 256.03 0.009 -30.8 -4.2 -454.01 312 256.042 0.012 -36 -5.2 -411.03 326 256.054 0.012 -41 -5 -369.07 340 256.066 0.012 -45.3 -4.3 -331.99 352 256.084 0.018 -50.6 -5.3 NaN 365 256.104 0.02 -55.5 -4.9 NaN 377 256.128 0.024 -60.7 -5.2 NaN 389 256.154 0.026 -65.3 -4.6 NaN 401 256.19 0.036 -70.5 -5.2 NaN 412 25
Table of measured values
Method: 148T Titer of AgNO3 11.12.2007 14:27:36Start time: 11.12.2007 14:27:51___________________________________________________________________________________________
Results
No. Comment / ID Start time Rx Result Unit Name 1/3 NaCl 11.12.2007 14:27:51 R1= 0.986 -- Titer 2/3 NaCl 11.12.2007 14:37:29 R1= 0.993 -- Titer 3/3 NaCl 11.12.2007 14:47:01 R1= 0.993 -- Titer -/- R2= 0.991 -- Mean Titer Titer 0.991
SQC/Statistics
Rx Name n Mean Value Unit s srel[%] ____________________________________________________________________________________________
R1 Titer 3 0.991 -- 0.004 0.408 R2 Mean Titer 1 0.991 -- NaN NaN
Titration curve
Results
59
Method 148T Titer of AgNO3 11.12.2007Author schmid
001 Title Type Titer determination Compatible with T50 / T70 / T90 ID 148T Title Titer of AgNO3 Author schmid Date/Time 26.11.2007 12:46:07 Modified 11.12.2007 14:27:36 Modified by Administrator Protect No SOP None LabX SOP002 Sample (Titer) Titrant AgNO3
Concentration [mol/L] 0.001 Standard NaCl
Type of standard liquid Entry type Fixed weight Volume 5.0 mL Correction factor 1.0 Temperature 25.0°C003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No004 Dispense (normal) [1] Titrant HClO4 Concentration 0.1 mol/L Volume 1.0 mL Dosing rate 60.0 mL/min Condition No005 Stir Speed 30 % Duration 10 s Condition No006 Titration (EQP) [1]Titrant
Titrant AgNO3 Concentration 0.001 mol/LSensor
Type mV Sensor DM148-SC Unit mVTemperature acquisition
Temperature acquisition NoStir
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 sEvaluation and Recognition
Procedure Standard Threshold 200.0 mV/mL Tendency Negative Ranges 0 Add. EQP criteria NoTermination
At Vmax 10 mL At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria NoAccompanying stating
Accompanying stating NoCondition
Condition No
Method007 Calculation R1 Result Titer Result unit -- Formula R1=m/(VEQ*c*C) Constant 1/(cst*z) M M[Sodium chloride] z z[Sodium chloride] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No008 Rinse
Auxiliary reagent WaterRinse cycles 1Vol. per cycle [mL] 10 mLPosition Actual positionDrain NoCondition No
009 Record Summary No Results Per sample Raw results Per sample Table of meas. values Last titration function Sample data No E - V Last titration function dE/dV - V No log dE/dV - V No
d2E/dV2 - V No BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Method No Series data No Condition No Method No Series data No Condition No010 Conditioning
Type FixInterval 1Position Conditioning beakerTime 10 sSpeed 30%
Condition No011 End of sample012 Titer Titrant AgNO3 Concentration 0.001 mol/L TITER= Mean[R1] Limits No Condition No013 Calculation R2 Result Mean Titer Result unit -- Formula R2=Mean[R1] Constant 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No014 Record Summary Yes Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No
60
M373
Mercaptan sulfur, R-S-,M = 32.06 g/mol, z = 1
25 mL solvent ASTM D3227-04a2 mL Ethyl mercaptan standard solve.(see remarks)
Silver nitrate, AgNO3 , in 2-Propanolc(AgNO3) = 0.01 mol/L
Titration Excellence T50/T70/T902 additional dosing unitsRondo 20 Sample Changer
R-SH + AgNO3 = R-S-Ag + HNO3
2 DV1010 and 1 DV1020 BurettesGlass titration beaker ME-101446XS205 BalanceOlivetti Printer JobJet 210
METTLER TOLEDO
Filtration. The precipitate has to beclassified as special waste. The liquidphase has to be disposed as organicwaste.
Wastedisposal
Preparation and Procedures25 mL, kerosineSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DM405-SCIndication
Mercaptan Sulfur Content in Kerosine According to ASTM D3227-04a
1) Dissolved oxygen is removed by purging the solvent and thetitrant solutions with nitrogen gas for at least 10 min prior touse. The solutions must be kept protected from atmosphere.
2) Before sample analysis a blank value titration is determined(result is stored as B[ASTM D 3227]).
3) Reagents addition:- 25 mL solvent ASTM D3227-04a are added into the beaker.
4) A Rondo sample changer with a diaphragm pump was used.
5) For accurate sampling, kerosene was added with a pipetteinstead of weighing (volatility). Thus, its density must be takeninto account. The density of flight petrol was measured using aMETTLER TOLEDO DR45 density meter (d = 0.7905 g/cm3 ,25°C)
6) The electrode was rinsed and conditioned using the ASTMD3227 solvent (Functions RINSE, CONDITIONING in specialbeaker 2, and CONDITIONING in conditioning beaker).
1) The method parameters have been optimised for the abovementioned sample. It may be necessary to slightly adapt themethod to your specific sample.
2) A fully automated procedure is performed by using twoadditional burette drives and a sample changer. It can be easilymodified for manual operation. Select "Manual stand" in themethod function "Titration stand".
3) ASTM D3227-04a alkaline solvent:Dissolve 1.6 g anhydrous sodium acetate (NaC2H3O2) in 25 mLof deion. water and pour into 1 L flask. Fill up to the mark with2-propanol. This solvent allows a good dissolution of the oil.
4) The 0.02 mol/L mercaptan standard is prepared bydissolving approx. 1.24 g ethyl mercaptan in a 1 L volumetricflask and filling up with the ASTM D3227 solvent.Literature:ASTM D3227-04a, see www.astm.orgMETTLER TOLEDO Appl. brochure 34, ME-51 725 066METTLER TOLEDO Appl. brochure 20, ME-51 725 020.
Remarks
R1: Mercaptan content (mg/kg)
R1 = (Q-B[ASTM D 3227])*C/(m*d),C = M*1000/z
B[ASTM D3227]: Blank value ofmercaptan standard solution
Calculation
Titration Excellence Line: The content of (thiol mercaptan) sulfur in kerosine is determined by precipitationtitration in non aqueous solvent using silver nitrate in 2-propanol. The content is expressed as sulfur, S2-.
Standard NaCl, c(NaCl) = 0.01 mol/L , 5 mL
Claudia SchreinerAuthor
Wastedisposal
61
Table of measured values
Start time: 27.10.2007
Sample Data Note / ID Sample size No. 1/6 Kerosene 25 mL No. 2/6 Kerosene 25 mL No. 3/6 Kerosene 25 mL No. 4/6 Kerosene 25 mL No. 5/6 Kerosene 25 mL No. 6/6 Kerosene 25 mL
Results Note / ID Rx Result Unit No. 1/6 Kerosene R1= 14.794 mg/L No. 2/6 Kerosene R1= 14.768 mg/L No. 3/6 Kerosene R1= 14.696 mg/L No. 4/6 Kerosene R1= 14.676 mg/L No. 5/6 Kerosene R1= 14.616 mg/L No. 6/6 Kerosene R1= 14.623 mg/L
Statistics Rx Name n Mean Value Unit s srel[%] R1 Mercaptans 6 14.70 mg/L 0.07 0.50
Titration curve
Results
62
Method m373 Mercaptan sulfur ASTM D3227 27.08.2007Author METTLER TOLEDO
001 Title Type General titration Compatible with T50 / T70 / T90 ID m373 Title Mercaptan sulfur ASTM D3227 Author METTLER TOLEDO Date/Time 27.08.2007 Modified -- Modified by -- Protect No SOP None
002 Sample Number of IDs 1 ID 1 Kerosene Entry type Fixed volume Volume 25.0 mL Density 0.8 g/mL Correction factor 1.0 Temperature 25.0°C
003 Titration stand Type Rondo/Tower A Titration stand Rondo60/1A
004 PumpAuxiliary reagent ASTM D3227 solvent
Volume 25 mL
005 Dispense (normal) [1]Titrant Kerosene
Concentration 1 Volume 25 mL Dosing rate 60.0 mL/min
006 Stir Speed 30% Duration 480 s
007 Titration (EQP) [1]Titrant
Titrant AgNO3 in 2-Propanol Concentration 0.01 mol/L
Sensor Type mV Sensor DM405-SC Unit mV
Temperature acquisition Temperature acquisition No
Stirrer Speed 30%
Predispense Mode None Wait time 0 s
Control Control User Titrant addition Dynamic dE(set value) 4.0 dV(min) 0.005 mL dV(max) 0.05 mL Meas. val. acquisition Equilibrium controlled dE 1.0 mV dt 2 s t(min) 10 s t(max) 30 s
Evaluation and Recognition Procedure Standard Threshold 1000 mV/mL Tendency Positive Ranges 0 Add. EQP criteria No
Method Termination At Vmax [mL] 3 At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No
008 Calculation R1 Result Content Result unit mg/kg Formula R1=(Q-B[ASTM D3227])*C/(m*d) Constant C=M*1000/z M M[Mercaptan sulfur] z z[Mercaptan sulfur] Decimal place 3 Result limits No Record statistics No Extra statistical functions No Condition No
009 Record Results Per series Raw results Per series Table of measured values Last titration function Sample data Per series Resource data No E - V Last titration functions dE/dV - V Last titration functions log dE/dV - V No d2E/dV2 - V No E - t No V - t No dV/dt - t No T - t No E - V & dE/dV - V No V - t & dV/dt - t No Calibration curve No Method No Series data No
010 Rinse Auxiliary reagent ASTM D3227 solvent Rinse cycles 1 Vol. per cycle [mL] 15 Position Actual position Drain No
011 Conditioning Type Fix Interval 1 Position Special beaker 2 Time [s] 30 Speed [%] 50
012 Conditioning Type Fix Interval 1 Position Conditioning Time [s] 30 Speed [%] 50
013 End of sample
63
M374-A
Alkaline components B,expressed as mg KOH/g sample
55 mL solvent mixtureToluene:isopropanol:distilled water(50% (v/v):49.5%(v/v):0.5%(v/v) )
HCl in 2-propanol:c(HCl) = 0.1 mol/L
Titration Excellence Line, T50/70/90Conductivity board ME-51109840Rondo 20 with PowerShower
Neutralization of all basic componentsin oil.General neutralization reactions:1) HCl + NaOH = NaCl + H2O
2) HCl + B = HB+ + Cl-
Glass titration beaker ME-1014462 x SP250 Peristaltic pumpsME-51108016Printer, XP205 balance
METTLER TOLEDO
Organic solvent waste(aromatic solvents)
Wastedisposal
Preparation and ProceduresFresh oils, 0.2-1 gSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
InLab718 conductivity probeIndication
Base Number Determination in Fresh Oils by Conductometric Titration
1) Titrant preparation:If not commercially available, the titrant can be prepared byadding 9 mL 37% v/v HCl and filling up to 1 L with 2-propanol(isopropanol).
2) Depending on the BN number, 0.2-1 g oil are weighed into aglass titration bealer. The higher the BN, the lower the samplesize.
3) 60 mL solvent are added automatically by a peristalticpump.
4) The titration is started after 60 s stirring time at 50% in orderto achieve a complete dissolution of the sample.
1) To ensure a complete rinsing of the probe, the followingcleaning procedure was defined (see method):1.1 Drain: The sample beaker is emptied1.2 Pump: 35 mL of solvent are dosed1.3 Stir:To remove all residuals, the solvent is stirred 20 s at 70%.1.4 Drain: The solvent is pumped out.1.5 Rinse: Finally, the titration stand is rinsed two times aftereach sample using the rinsing cycles defined in the methodfunction "Rinse".
Literature:
1) IP400/94 Standard, British Institute of Petroleum(Now: Energy Institute, http://www.energyinst.org.uk/)
2) METTLER TOLEDO Applications M252/M253. and M099/M100.
3) This application does not replace the standard.
Remarks
Base number (mg KOH/g)R1= (Q-B[IP400])*C1/mC1= 56.1
B[IP400]: solvent blank value
Calculation
Titration Excellence Line: Determination of the base number of freshmotor and cutting oils by titration with0.1 mol/L hydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe (IP400/94).
Standard TRIS (THAM), 50 mg
Hans-Joachim MuhrAuthor
Wastedisposal
64
Table of measured values
Method ID: IP400B Sample series ID 13 Date / Time: 09/20/2006 01:43:12 pm User name Administrator
Samples Nr. ID Sample size and results
1 13 0.2584 g R1(BN) 38.798 mg KOH/g R2(Titration time) 2.570 min 2 13 0.2535 g R1(BN) 38.309 mg KOH/g R2(Titration time) 2.470 min
3 13 0.2511 g R1(BN) 38.490 mg KOH/g R2(Titration time) 2.470 min 4 13 0.2541 g R1(BN) 38.380 mg KOH/g R2(Titration time) 2.570 min
5 13 0.2521 g R1(BN) 38.560 mg KOH/g R2(Titration time) 2.470 min 6 13 0.2 g R1(BN) 38.263 mg KOH/g R2(Titration time) 2.570 min
Statistics R1(BN) Number of samples 6 Mean value 38.467 mg KOH/g s 0.196 mg KOH/g srel 0.511 %
TBN according to ASTM D4739: 40.4 mg KOH/g---------------------------------------------------------------------------------------------
Different samples of fresh oils
Sample Size / g n Base number s srel TBN ASTM D4739 mg KOH/g mg KOH/g % mg KOH/g
CF15 0.5 6 18.947 0.106 0.559 20.0
58420 1.0 6 10.886 0.034 0.316 10.8
Titration curve
Results
65
Method IP400B Conductometric BNVersion 09/20/2006 01:43:12 pm
001 Title Type General titration Compatible with T50/T70/T90 ID IP400B Titel Conductometric BN Author Administrator Date / Time 08/28/2006 03:09:17 pm Modified at 09/20/2006 01:43:12 pm Modified by Administrator Protect No SOP None
002 Sample Number of IDs 1 ID 1 13 Entry Type Weight Lower limit 0.0 g Upper limit 5.0 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0 °C Entry Before
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No
004 PumpAuxiliary reagent IP400 Solvent
Volume 55 mL Condition No
005 Stir Speed 50 % Duration 60 s Condition No
006 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration 0.1 mol/L Sensor Type Conductivity Sensor InLab 718
Unit STemperature aquisition
Temperature measurement NoStir
Speed 30 %Predispense
Mode None Wait time 0 s Control Control User Titrant addition Incremental dV 0.1 mL Meas. val. acquisition Equilibrium controlled
dE 0.5 S dt 1.0 s t(min) 10 s t(max) 20 s Evaluation and Recognition Procedure Segmented
Threshold 0.5 S mL2
Ranges 0 Add. EQP criteria Steepest jump Steepest jumps 1 Termination At Vmax 4 mL
At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No
Method007 Calculation R1 Result BN Result unit mg KOH/g Formula R1=(Q-B[IP400])*C/m Constant C= 56.1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Condition No
008 Calculation R2 Result Titration time Result Unit min Formula R2=t Constant C= -- M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Condition No
009 Record Summary Per sample Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Per sample Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No
d2E/dV2 - V Last titration function BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & DE/dV - V No V - t & dV/dt - V No Method No Series data No Condition No
010 Drain Drain pump SP250 Drain volume 60 mL Condition No
011 Pump Auxiliary reagent IP400 Solvent Volume 35 mL Condition No
012 Stir Speed 70 % Duration 20 s Condition No
013 Drain Drain pump SP250 Drain volume 40 mL Condition No
014 Rinse Auxiliary reagent IP400 Solvent Rinse cycles 2 Vol. per cycle 10 mL Position Actual position Drain Yes Drain pump SP250 Condition No
015 End of sample
66
M374-B
Alkaline components B,expressed as mg KOH/g sample
60 mL solvent mixtureToluene:isopropanol:distilled water(50% (v/v):49.5%(v/v):0.5%(v/v) )
HCl in 2-propanol:c(HCl) = 0.1 mol/L
Titration Excellence Line, T50/70/90Conductivity board ME-51109840Rondo 20 Sample Changer
Neutralization of all basic componentsin oil.General neutralization reactions:1) HCl + NaOH = NaCl + H2O
2) HCl + B = HB+ + Cl-
Glass titration beaker ME-101446SP250 Peristaltic pump ME-51108016Printer, XP205 balance
METTLER TOLEDO
Organic solvent waste(aromatic solvents)
Wastedisposal
Preparation and ProceduresUsed oils, 2-5 gSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
InLab718 conductivity probeIndication
Base Number Determination in Used Oils by Conductometric Titration
1) Titrant preparation:If not commercially available, the titrant can be preparedmanually by adding 9 mL 37% v/v HCl and filling up to 1 Lwith 2-propanol (isopropanol).
2) 2-4 g oil are weighed into a glass titration bealer.
3) 60 mL solvent are added automatically by a peristalticpump.
4) The titration is started after 300 s stirring time at 50% inorder to achieve a complete dissolution of the sample.
1) The conductivity probe is conditioned during 10 s in the fixedconditioning beaker of the Rondo 20 sample changer.
2) Most oil samples may create sticky residues. In this case, itis necessary to additionally clean the conductivity probe with apaper tissue soaked in solvent mixture. Afterwards, the probe isrinsed again with solvent mixture to remove the last impurities.
Literature:
1) IP400/94 Standard, British Institute of Petroleum(Now: Energy Institute, http://www.energyinst.org.uk/)
2) METTLER TOLEDO Applications M252/M253, and M099/M100.
3) This application does not replace the standard.
Remarks
Base number (mg KOH/g)R1= (Q-B[IP400])*C1/mC1= 56.1
B[IP400]: solvent blank value
Calculation
Titration Excellence Line: Determination of the base number of various used oils by titration with 0.1 mol/Lhydrochloric acid in 2-propanol. The titration is monitored with a conductivity probe according to IP400/94.
Standard TRIS (THAM), 50 mg
Tobias Beckmann, MT-DAuthor
Wastedisposal
67
Table of measured values
Method ID: AIP400 Sample series ID -- Date / Time: 14/08/2007 12:00:28 User name Administrator
Summary
Samples Nr. ID Sample size and results
1 WC 433591 2.0134 g R1(BN) 6.373 mg KOH/g R2(Titration time) 5.070 min
2 WC 433591 2.0717 g R1(BN) 6.396 mg KOH/g R2(Titration time) 5.230 min
3 WC 433591 2.2171 g R1(BN) 6.438 mg KOH/g R2(Titration time) 5.500 min
Statistics R1(BN) Number of samples 3 Mean value 6.402 mg KOH/g s 0.033 mg KOH/g srel 0.515 %
---------------------------------------------------------------------------------------------
Different samples of used oilsSample Size / g n Base number s srel mg KOH/g %
WC 529913 2.2 3 5.780 0.062 1.068
WC 526402 2.2 3 4.599 0.299 4.974
WC 471807 2.3 3 4.571 0.290 6.349
WC 457700 2.2 3 3.250 0.101 3.095
WC 541628 2.1 3 1.820 0.007 0.405
Titration curve
Results
68
Method AIP400 Conductometric BNVersion 14/08/2007 12:00:28
001 Title Type General titration Compatible with T50/T70/T90 ID AIP400 Titel Conductometric BN Author Administrator Date / Time 14/08/2007 09:19:49 Modified at 14/08/2007 12:00:28 Modified by Administrator Protect No SOP None
002 Sample Number of IDs 1 ID 1 WC 433591 Entry Type Weight Lower limit 0.0 g Upper limit 5.0 g Density 1.0 g/mL Correction factor 1.0 Temperature 25.0 °C Entry Before
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No
004 PumpAuxiliary reagent IP400
Volume 60 mL Condition No
005 Stir Speed 50 % Duration 300 s Condition No
006 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration 0.1 mol/L Sensor Type Conductivity Sensor InLab 718
Unit STemperature aquisition
Temperature measurement NoStir
Speed 30 %Predispense
Mode None Wait time 0 s Control Control User Titrant addition Incremental dV 0.05 mL Meas. val. acquisition Equilibrium controlled
dE 1.0 S dt 2 s t(min) 3 s t(max) 15 s Evaluation and Recognition Procedure Segmented
Threshold 10 S mL2
Ranges 0 Add. EQP criteria Steepest jump Steepest jumps 1 Termination At Vmax 10 mL
At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No
Method007 Conditioning Type Fix Interval 1 Positioning Conditioning beaker Time 10 s Speed 30 % Condition No
008 Calculation R1 Result BN Result unit mg KOH/g Formula R1=(Q-B[IP400])*C/m Constant C= 56.1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
009 Calculation R2 Result Titration time Result Unit min Formula R2=t Constant C= -- M M[None] z z[None] Decimal places 3 Result limits No Record statistics No Extra statistical functions No Send to buffer No Condition No
010 Record Summary Per series Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Per sample Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No
d2E/dV2 - V Last titration function BETA - V No E - t No V - t No dV/dt - t No T - t No E - V & DE/dV - V No V - t & dV/dt - V No Method No Series data No Condition No
011 End of sample
----------------------------------------------------
Blank value determination and storage as B[IP400]...... Control Control User Titrant addition Incremental dV 0.01 mL Meas. val. acquisition Equilibrium controlled
dE 0.5 S dt 1.0 s t(min) 10 s t(max) 20 s Evaluation and Recognition Procedure Segmented
Threshold 0.5 S mL2 Ranges 0 Add. EQP criteria Steepest jump Steepest jumps 1 Termination At Vmax 1.5 mL
At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1
69
M375
TRIS, Tris-hydroxymethyl-aminomethaneM=121.14, z=1
60 mL solvent mixtureToluene:isopropanol:distilled water(50% (v/v):49.5%(v/v):0.5%(v/v) )
HCl in 2-propanol:c(HCl) = 0.1 mol/L
Titration Excellence Line, T50/70/90Conductivity board ME-51109840Rondo 20 Sample Changer
Neutralization of all basic componentsin oil.General neutralization reactions:1) HCl + NaOH = NaCl + H2O
2) HCl + B = HB+ + Cl-
Glass titration beaker ME-101446SP250 Peristaltic pump ME-51108016Printer, XP205 balance
METTLER TOLEDO
Organic solvent waste(aromatic solvents)
Wastedisposal
Preparation and ProceduresPrimary standard:TRIS (THAM), 50-80 mg
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
InLab718 conductivity probeIndication
Titer of 0.1 mol/L HCl in 2-Propanol by Conductometric Titration (IP400)
1) Titrant preparation:If not commercially available, the titrant can be preparedmanually by adding 9 mL 37% v/v HCl and filling up to 1 Lwith 2-propanol (isopropanol).
2) 50-80 mg TRIS are weighed into a glass titration bealer.
3) 60 mL solvent are added automatically by a peristalticpump.
4) The titration is started after 120 s stirring in order to achievea complete dissolution of TRIS.
1) The conductivity probe is conditioned during 10 s in the fixedconditioning beaker of the Rondo 20 sample changer.
Literature:
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.
Remarks
Titer determinationR = m/(VEQ*c*C)C = M/(10*p*z)
p: purity of solid primary standard [%]
Calculation
Titration Excellence Line: Titer determination of 0.1 mol/L hydrochloric acid in 2-propanol (isopropanol, IPA)by conductometric titration using TRIS (Tris-hydroxymethyl-aminomethane, THAM) as a primary standard.
Standard --
Tobias Beckmann, MT-DAuthor
Wastedisposal
70
Table of measured values
Method ID: AIP8014 Sample series ID -- Date / Time: 14/08/2007 10:01:04 User name Administrator
All resultsMethod ID AIP8014
Sample 1/3 TRIS R1 0.986 Sample 2/3 TRIS R1 0.993 Sample 3/3 TRIS R1 0.995
Statistics Method ID AIP8014 R1 (Titer) Number of samples 3 Mean value 0.991 s 0.005 srel 0.477
All results R2(mean Titer) 0.991
Titration curve
Results
71
Method AIPB8014 Titer HCl in 2-PropanolVersion 14/08/2007 10:01:04
001 Title Type General titration Compatible with T50/T70/T90 ID AIP8014 Titel Titer HCl in 2-Propanol Author Administrator Date / Time 14/08/2007 09:19:49 Modified at 14/08/2007 10:01:04 Modified by Administrator Protect No SOP None
002 Sample (Titer) Titrant HCl in 2-Propanol
Concentration 0.1 mol/L Standard TRIS Type of standard Solid Entry Type Weight Low limit 0.05 g Upper limit 0.08 g Correction factor 1.0 Temperature 25.0 °C Entry Arbitrary
003 Titration stand (Rondo/Tower A) Type Rondo/Tower A Titration stand Rondo60/1A Lid handling No
004 PumpAuxiliary reagent IP400
Volume 60 mL Condition No
005 Stir Speed 40 % Duration 120 s Condition No
006 Titration (EQP) [1] Titrant Titrant HCl in 2-Propanol Concentration 0.1 mol/L Sensor Type Conductivity Sensor InLab 718
Unit STemperature aquisition
Temperature measurement NoStir
Speed 30 %Predispense
Mode None Wait time 0 s Control Control User Titrant addition Incremental dV 0.1 mL Meas. val. acquisition Equilibrium controlled
dE 1.0 S dt 2 s t(min) 3 s t(max) 30 s Evaluation and Recognition Procedure Segmented
Threshold 10 S mL2
Ranges 0 Add. EQP criteria No Termination At Vmax 10.0 mL
At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating No Condition Condition No
Method007 Conditioning Type Fix Interval 1 Positioning Conditioning beaker Time 10 s Speed 30 % Condition No
008 Calculation R1 Result Titer Result unit -- Formula R1=m/(VEQ*c*C) Constant C= M/(10*p*z) M M[TRIS] z z[TRIS] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
009 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V No log dE/dV - V No
d2E/dV2 - V Last titration function ........... Method No Series data No Condition No
010 End of sample
011 Titer Titrant HCl in 2-Propanol Concentration 0.1 mol/L TITER= Mean[R1] Limits No Condition No
012 Calculation R2 Result Mean Titer Result Unit -- Formula R2=Mean[R1] Constant C= 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No
013 Record Summary No Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No
72
M376
Anionics as Na-dodecylsulfate, C12H25NaO4SM(SDS)=288.38 g/mol, z=1
40 mL deion water20 mL MIBK:EtOH 1:1 solvent
Hyamine 1622, c(Hyamine)=0.004 MHydrochloric acid, HCl, c(HCl)=0.1 M
Titration Excellence Line T70/T902 additional dosing unitsRondolino Sample Changer
SDS- + Hyamine+ = SDS-Hyamine
Titration beaker ME-101974
METTLER TOLEDO
Neutralize the sample solution beforefinal disposal as organic solvent.
Wastedisposal
Preparation and Procedures5 mL aliquots of aqueous solutionsprepared with shower gels andshampoo.
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DS800 TwoPhase surfactant electrode,InLabRReference , DG111-SC
Indication
Anionic Content in Shower Gels by Potentiometric Two-Phase Titration
Note: MIBK is an organic solvent which is strongly andintensively smelling. It is recommended to work in a fume hood.
1) 40 mL of deionised water are added to the 5 mL sample.2) The titration beaker is placed on the Rondolino samplechanger.3) The pH value is first adjusted to pH 3 with HCl by means ofthe second titration burette (EN DIN 14480).4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensedby means of an additional dosing unit.MIBK: Methylisobutylketone (4-Methylpentan-2-one)EtOH: Ethanol5) To obtain a homogeneous emulsion the solution is stirred ata high speed (80%).6) The anionic surfactant content is expressed as SDS content, i.e. the molecular mass of SDS is used for the calculation.
DS800 TwoPhase surfactant sensitive electrode:1) Fill the DS800 TwoPhase and the electrode tip with theelectrolyte.2) Screw the electrode tip onto the shaft.3) Shake the electrode 2-3 times to avoid the presence of airbubbles into the electrode tip. Rinse it with deion. water.4) Condition the electrode first in deionised water for e.g. 15minutes, and then perform 1-2 test titrations with the sample.
1) The determination of anionic surfactants is performed at pH 3according to DIN EN 14480. This is perfomed to avoidinterference due to the presence of free fatty acids (FFA) in theproducts, otherwise the result will be higher. In fact, at pH 3 theFFA are fully protonated, therefore they can not be titrated withhyamine.
2) Standard solutions of the different products are prepared bydissolving in 1 L volumetric flask approx. 5-10 g of theproducts. The resulting concentration in g/L = mg/mL is storedas auxiliary value e.g. H[Anionic] in the titrator.
3) The electrode is cleaned and conditioned after each sample indeionised water in the conditioning beaker of Rondolino(Position 5: 120 s).
4) When working with the LabX Software, select "RondolinoMode" in the LabX window at the PC and activate it.
Literature:1) DIN EN 14480-20042) METTLER TOLEDO Application brochure 34,"Selected METTLER TOLEDO methods for Titration ExcellenceLine", ME-51 725 066.3) METTLER TOLEDO Application brochure 22,"Surfactant titration", ME-51 725 015.
Remarks
R1=Q[2]*C/mC= M/(10*z)
Calculation
Titration Excellence Line: Determination of anionic surfactant content in shower gels by titration with 0.004mol/L Hyamine 1622 in a two-phase mixed system using a DS800 TwoPhase electrode according to DINEN 14480-2004.
Standard SDS (for Hyamine), THAM (for HCl)
C. De CaroAuthor
Wastedisposal
73
Table of measured values
Method ID: 0214 Sample series ID -- Date / Time: 09/07/2007 07:50:32 User name Administrator
All resultsMethod ID 0214LAS
Sample 1/5 0214 R1 24.726 % Sample 2/5 0214 R1 24.677 % Sample 3/5 0214 R1 24.669 % Sample 4/5 0214 R1 24.622 % Sample 5/5 0214 R1 24.641 %
Statistics Method ID 0214LAS R1 (Content) Number of samples 5 Mean value 24.667 % s 0.040 % srel 0.161 %
----------------------------------------------------------------------------------------------Different samplesSample type exp./%SDS n Result s srel content /%SDS /%SDS /%
0214 viscous 24 5 24.667 0.040 0.161 pH 3 H[0214]=0.005056 g/L 8 24.494 0.033 0.136 pH 5.5
0273 viscous 25 8 25.290 0.034 0.136 pH 3 H[0273]=0.005019 g/L 7 25.291 0.031 0.123 pH 3
0411 powder 20 3 20.274 0.055 0.273 pH 3 H[0411]=0.010012 g/L 5 20.303 0.073 0.359 pH 3
0193 formulation 8-9 5 9.303 0.031 0.332 pH 3 H[0193]=0.010033 g/L 6 9.253 0.048 0.521 pH 3
0Liq liquid det. 5-15 6 7.317 0.060 0.817 pH 3 H[0Liq]=0.00805 g/L 9 7.365 0.080 1.092 pH 3
Titration curve
Results
74
Method 0214 SDS content potentiometricVersion 09/07/2007 07:50:32
001 Title Type General titration Compatible with T70/ T90 ID 0214 Titel SDS content potentiometric Author Administrator Date / Time 06/07/2007 17:56:59 Modified at 09/07/2007 07:50:32 Protect No SOP None
002 Sample Number of IDs 1
ID 1 0214 Entry Type Fixed volume Volume 5 mL Density 1.0 Correction factor 1.0 Temperature [°C] 25.0
003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1
004 Stir Speed 35 % Duration 45 s Condition No
005 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L Sensor Type pH Sensor DG111-SC Unit pHTemperature aquisition
Temperature measurement NoStir
Speed 30 %Predispense
Mode None Wait time [s] 0Control
End point type Absolute Tendency Negative End point value 3 pH Control band 2.0 pH Dosing rate (max) 10.0 mL/min
Dosing rate (min) 500 L/minTermination
At EP Yes Termination delay 0 s At Vmax 10.0 mL Max. time InfiniteAccompanying stating
Accompanying stating NoCondition
Condition No
006 Dispense (normal) [1] Titrant MIBK-EtOH 1:1 Concentration 1 Volume 20 mL Dosing rate 60.0 mL/min Condition No
007 Stir Speed 80 % Duration 60 s Condition No
Method008 Titration (EQP) [2] Titrant
Titrant Hyamine 1622 Concentration [mol/L] 0.004 mol/L Sensor Type mV
Sensor DS800 Unit mV Temperature aquisition Temperature measurement No
Stir Speed 80 % Predispense
Mode Volume Volume 1.5 mL Wait time [s] 15 sControl
Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.01 mL dV(max) 0.4 mL Mode Equilibrium controlled dE 1.0 mV dt 1 s t(min) 5 s t(max) 30 sEvaluation and Recognition
Procedure Standard Threshold 100 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination
At Vmax [mL] 8 At potential No At slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating NoCondition
Condition No
009 Calculation R1 Result Content Result unit % Formula R1=Q[2]*C/(m*H[0214]) Constant C= M/(10*z) M M[Sodium dodecylsulfate] z z[Sodium dodecylsulfate] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Condition No
010 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Yes Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No
d2E/dV2 - V No .... Method No Series data No Condition No
011 End of sample
012 Record Summary Yes Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No
75
M377
Anionics as Na-dodecylsulfate, C12H25NaO4SM(SDS)=288.38 g/mol, z=1
40 mL deion water20 mL MIBK:EtOH 1:1 solvent
Hyamine 1622, c(Hyamine)=0.004 MHydrochloric acid, HCl, c(HCl)=1 MSodium hydroxide, c(NaOH)=1 M
Titration Excellence Line T70/T902 additional dosing unitsRondolino Sample Changer
SDS- + Hyamine+ = SDS-Hyamine
Titration beaker ME-101974
METTLER TOLEDO
Neutralize the sample solution beforefinal disposal as organic solvent.
Wastedisposal
Preparation and Procedures0.1-0.3 g cutting oil, depending onanionic surfactant content.
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DS800 TwoPhase surfactant electrode,InLabRReference , DG111-SC
Indication
Anionic Content in Cutting Oils by Potentiometric Two-Phase Titration
Note: MIBK is an organic solvent which is strongly andintensively smelling. It is recommended to work in a fume hood.
1) 40 mL of deionised water are added to the 5 mL sample.2) The titration beaker is placed on the Rondolino samplechanger.3) The pH value is adjusted to pH 3 (DIN EN 14480) with HClor to pH 11 with NaOH by means of the second titration burette.4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensedby means of an additional dosing unit.MIBK: Methylisobutylketone (4-Methylpentan-2-one)EtOH: Ethanol5) To obtain a homogeneous emulsion the solution is stirred ata high speed (80%).6) The anionic surfactant content is expressed as SDS content, i.e. the molecular mass of SDS is used for the calculation.
DS800 TwoPhase surfactant sensitive electrode:1) Fill the DS800 TwoPhase and the electrode tip with theelectrolyte.2) Screw the electrode tip onto the shaft.3) Shake the electrode 2-3 times to avoid the presence of airbubbles into the electrode tip. Rinse it with deion. water.4) Condition the electrode first in deionised water for e.g. 15minutes, and then perform 1-2 test titrations with the sample.
1) The determination of anionic surfactants is performed at pH 3according to DIN EN 14480. This is done in order to avoidinterference due to the presence of free fatty acids (FFA) in theproducts, otherwise the result will be higher. In fact, at pH 3 theFFA are fully protonated, therefore they can not be titrated withhyamine.
2) In the case where samples contain anionic surfactants withR-COOH end groups, it is necessary to titrate the sample at analkaline pH value of e.g. pH 11 (see also DIN EN 14669) to beable to precipitate them with Hyamine.
3) The electrode is cleaned and conditioned after each sample indeionised water in the conditioning beaker of Rondolino(Position 5: 120 s).
4) When working with the LabX Software, select "RondolinoMode" in the LabX window at the PC and activate it.
Literature:1) DIN EN 14480-2004 and 14669-20052) METTLER TOLEDO Application brochure 34,"Selected METTLER TOLEDO methods for Titration ExcellenceLine", ME-51 725 066.3) METTLER TOLEDO Application brochure 22,"Surfactant titration", ME-51 725 015.
Remarks
R1=Q[2]*C/mC= M/(10*z)
Calculation
Titration Excellence Line: Determination of anionic surfactant content in cutting oils by titration with 0.004mol/L Hyamine 1622 in a two-phase mixed system using a DS800 TwoPhase electrode according to DINEN 14480-2004 (pH 3).
Standard SDS (for Hyamine)
C. De CaroAuthor
Wastedisposal
76
Table of measured values
Method ID: m377 Sample series ID -- Date / Time: 11/12/2007 09:02:23 am User name AdministratorSummary Samples No. ID Sample size and results
1 00883-03 0.1773 g R1(Anionics Content) 4.91 %
2 00883-03 0.1873 g R1(Anionics Content) 4.88 %
3 00883-03 0.1537 g R1(Anionics Content) 4.82 %
4 00883-03 0.2101 g R1(Anionics Content) 4.86 %
5 00883-03 0.1782 g R1(Anionics Content) 4.86 %
6 00883-03 0.1624 g R1(Anionics Content) 4.88 %Statistics
R1 (Anionics Content) Number of samples 6 Mean value 4.87 % s 0.03 % srel 0.636 %===========================================================================================Various samples n Result/%SDS s/%SDS srel/%-------------------------------------------------------------------00883-03 6 4.87 0.03 0.576 pH 3
01325-01 3 2.73 0.02 0.559 pH 3 5 2.66 0.02 0.734 pH 3
02800-01 6 2.01 0.01 0.733 pH 3
C93 18656 6 61.07 0.47 0.764 pH 3 6 61.14 0.31 0.506 pH 3 6 61.48 0.48 0.783 pH 3
V43 18571 6 30.93 0.05 0.155 pH 3 6 30.96 0.08 0.256 pH 3 6 30.92 0.04 0.141 pH 3
11675-01 4 13.57 0.17 1.228 pH 11 0.004 M Hyamine 6 13.61 0.20 1.486 pH 11 0.01 M CPC01125-02 4 4.49 0.05 1.155 pH 11 0.004 M Hyamine 6 4.55 0.01 0.231 pH 11 0.01 M CPC
Titration curve
Results
77
Method m377 SDS content potentiometricVersion 11/12/2007 09:02:23 am
001 Title Type General titration Compatible with T70/ T90 ID m377 Titel SDS content potentiometric Author Administrator Date / Time 11/12/2007 07:22:42 am Modified at 11/12/2007 09:02:23 am Protect No SOP None
002 Sample Number of IDs 1
ID 1 00883-03 Entry Type Weight Lower limit 0 g Upper limit 5 g Density 1.0 g/mL Correction factor 1.0 Temperature [°C] 25.0°C Entry Before
003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1
004 Stir Speed 35 % Duration 60 s Condition No
005 Titration (EP) [1] Titrant Titrant HCl Concentration 1 mol/L Sensor Type pH Sensor DG111-SC Unit pHTemperature aquisition
Temperature measurement NoStir
Speed 35 %Predispense
Mode None Wait time [s] 0Control
End point type Absolute Tendency Negative End point value 3 pH Control band 2.0 pH Dosing rate (max) 10.0 mL/min
Dosing rate (min) 500 L/minTermination
At EP Yes Termination delay 0 s At Vmax 10.0 mL Max. time InfiniteAccompanying stating
Accompanying stating NoCondition
Condition No
006 Dispense (normal) [1] Titrant MIBK-EtOH 1:1 Concentration 1 Volume 20 mL Dosing rate 60.0 mL/min Condition No
007 Stir Speed 80 % Duration 60 s Condition No
Method008 Titration (EQP) [2] Titrant
Titrant Hyamine 1622 Concentration [mol/L] 0.004 mol/L Sensor Type mV
Sensor DS800 Unit mV Temperature aquisition Temperature measurement No
Stir Speed 80 % Predispense
Mode None Wait time [s] 0 sControl
Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.1 mL dV(max) 0.5 mL Mode Equilibrium controlled dE 0.5 mV dt 2 s t(min) 8 s t(max) 45 sEvaluation and Recognition
Procedure Standard Threshold 30 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination
At Vmax [mL] 20 mL At potential No At slope No After number of recognized EQPs No Combined termination criteria No Accompanying stating Accompanying stating NoCondition
Condition No
009 Calculation R1 Result Anionics Content Result unit % Formula R1=Q[2]*C/m Constant C= M/(10*z) M M[Sodium dodecylsulfate] z z[Sodium dodecylsulfate] Decimal places 2 Result limits No Record statistics Yes Extra statistical functions No Condition No
010 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data Yes Resource data No E - V Last titration function dE/dV - V Last titration function log dE/dV - V No
d2E/dV2 - V No .... Method No Series data No Condition No
011 End of sample
012 Record Summary Yes Results Yes Raw results No Resource data No Calibration curve No Method No Series data No Condition No
78
M378
Sodium dodecylsulfate, C12H25NaO4SM(SDS)=288.38 g/mol, z=1
40 mL deion water20 mL MIBK:EtOH 1:1 solvent
Hyamine 1622, c(Hyamine)=0.004 MHydrochloric acid, HCl, c(HCl)=0.1 M
Titration Excellence Line T70/T902 additional dosing unitsRondolino Sample Changer
SDS- + Hyamine+ = SDS-Hyamine
Rondolino Sample ChangerTitration beaker ME-101974
METTLER TOLEDO
Organic solventWastedisposal
Preparation and Procedures5 mL 0.004 SDSSDS: Sodium dodecylsulfate
Sample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DS800 TwoPhase surfactant electrode,InLabRReference , DG111-SC
Indication
Titer Determination of Hyamine by Potentiometric Two-Phase Titration
Note: MIBK is an organic solvent which is strongly andintensively smelling. It is recommended to work in a fume hood.
1) 40 mL of deionised water are added to the 5 mL sample.2) The titration beaker is placed on the Rondolino samplechanger.3) The pH value is first adjusted to pH 3 with HCl by means ofthe second titration burette (EN DIN 14480).4) 20 mL MIBK-EtOH 1:1 solvent are automatically dispensedby means of an additional dosing unit.MIBK: Methylisobutylketone (4-Methylpentan-2-one)EtOH: Ethanol5) To obtain a homogeneous emulsion the solution is stirred ata high speed (80%).
DS800 TwoPhase surfactant sensitive electrode:1) Fill the DS800 TwoPhase and the electrode tip with theelectrolyte.2) Screw the electrode tip onto the shaft.3) Shake the electrode 2-3 times to avoid the presence of airbubbles into the electrode tip. Rinse it with deion. water.4) Condition the electrode first in deionised water for e.g. 15minutes, and then perform 1-2 test titrations with the sample.
Rondolino:
1) The electrode is cleaned and conditioned after each sample indeionised water in the conditioning beaker of Rondolino(Position 5: 120 s).
2) When working with the LabX Software, select "RondolinoMode" 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 Excellenceline", ME-51 725 066.
3) METTLER TOLEDO Application brochure 22,"Surfactant titration", ME-51 725 015.
Remarks
Titer:R=m/(VEQ[2]*c[2]*C)C=1/(cst*z)
Note: "cst" is the concentration of theSDS standard solution.
Calculation
Titration Excellence Line: Titer determination of 0.004 mol/L Hyamine 1622 with sodium dodecylsulfate(SDS) as a standard in a two-phase mixed system using a DS800 TwoPhase surfactant sensitive electrodeaccording to DIN EN 14480-2004.
Standard For HCl: THAM (TRIS)
C. De CaroAuthor
Wastedisposal
79
Table of measured values
Method ID: 414Titer Sample series ID -- Date / Time: 06/07/2007 17:15:16 User name Administrator
Summary
Samples No. ID Sample size and results
1 SDSTiter414 5 mL R1 (Titer) = 1.002013 2 SDSTiter414 5 mL R1 (Titer) = 1.001679 3 SDSTiter414 5 mL R1 (Titer) = 1.000487 4 SDSTiter414 5 mL R1 (Titer) = 0.997958 5 SDSTiter414 5 mL R1 (Titer) = 0.998080 6 SDSTiter414 5 mL R1 (Titer) = 0.998976
Statistics R1 (Titer) Number of samples 6 Mean value 0.999866 s 0.001784 srel 0.178%
Titer Titrant Hyamine 1622 New titer 0.99987
Results R2 (Hyamine) 0.999866
Titration curve
Results
80
Method 414Titer Titer Hyamine 1622Version 06/07/2007 17:15:16
001 Title Type General titration Compatible with T70/ T90 ID 414Titer Titel Titer Hyamine 1622 Author Administrator Date / Time 28/08/2006 14:53:19 Modified at 06/07/2007 17:15:16 Protect No SOP None002 Sample (Titer) Titrant Hyamine 1622
Concentration 0.004 mol/L Standard SDSTiter414 Type of standard liquid Entry Type Fixed volume Volume 5 mL Correction factor 1.0 Temperature [°C] 25.0003 Titration stand (Rondolino TTL) Type Rondolino TTL Titration stand Rondolino TTL 1004 Stir Speed 30 % Duration 45 s Condition No005 Titration (EP) [1] Titrant Titrant HCl Concentration 0.1 mol/L Sensor Type pH Sensor DG111-SC Unit pHTemperature aquisition
Temperature measurement NoStir
Speed 35 %Predispense
Mode None Wait time [s] 0Control
End point type Absolute Tendency Negative End point value 3 pH Control band 2.0 pH Dosing rate (max) 0.2 mL/min
Dosing rate (min) 50 L/minTermination
At EP Yes Termination delay 0 s At Vmax 10.0 mL Max. time InfiniteAccompanying stating
Accompanying stating NoCondition
Condition No006 Dispense (normal) [1] Titrant MIBK-EtOH 1:1 Concentration 1 Volume 20 mL Dosing rate 60.0 mL/min Condition No007 Stir Speed 80 % Duration 60 s Condition No008 Titration (EQP) [2] Titrant
Titrant Hyamine 1622 Concentration [mol/L] 0.004 mol/L Sensor Type mV
Sensor DS800 Unit mV Temperature aquisition Temperature measurement No
Stir Speed 80 % Predispense
Mode Volume Volume 1.5 mL Wait time [s] 15 s
MethodControl
Control User Titrant addition Dynamic dE(set value) 8.0 mV dV(min) 0.01 mL dV(max) 0.5 mL Mode Equilibrium controlled dE 1.0 mV dt 1 s t(min) 5 s t(max) 30 sEvaluation and Recognition
Procedure Standard Threshold 100 mV/mL Tendency Positive Ranges 0 Add. EQP criteria NoTermination
At Vmax [mL] 10 At potential No At slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No Accompanying stating Accompanying stating NoCondition
Condition No009 Calculation R1 Result Titer Result unit Formula R=m/(VEQ[2]*c[2]*C Constant C= M/(cst*z) M M[Sodium dodecylsulfate] z z[Sodium dodecylsulfate] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Condition No010 Record Summary No Results Per sample Raw results Per sample Table of measured values Last titration function Sample data No Resource data No E - V Last titration function dE/dV - V No ... Calibration curve No Method No Series data No Condition No011 End of sample012 Titer Titrant Hyamine 1622 Concentration 0.004 mol/L TITER= Mean[R] Limits No Condition No013 Calculation R2 Result Titer Hyamine Result Unit Formula R2=Mean[R1] Constant C= M M[None] z z[None] Decimal places 6 Result limits No Record statistics Yes Extra statistical functions No Condition No014 Record Summary Yes Results No Raw results No Resource data No Calibration curve No Method No Series data No Condition No
81
M379
Tartaric acid ((CHOH)2(COOH)2)
Chloride (Cl-)
H2SO4 (10%)
NaOH, 1.0 mol/L (sodium hydroxide)AgNO3, 0.02 mol/L (silver nitrate)
Titration Excellence T70/T902 additional dosing units
EP titration:C4H6O6 + 2NaOH = Na2C4H4O6 +2H2OEQP titration:Cl- + Ag+ + NO3
- = AgCl + NO3-
LabX Pro Titration ME-51106500Rondo30 sample changer (51108004)with sample beakers (51108030)
METTLER TOLEDO
AgCl has to be disposed of as specialwaste.
Wastedisposal
Preparation and ProceduresWine, 40 mLSample
Substance
Chemicals
Titrant
Instruments
Results
Chemistry
Accessories
DGi102-Mini (pH sensor)DMi102-SC (silver electrode)
Indication
Acid and Chloride Content in Wine
Before the acid content analysis is performed the pH electrodeneeds to be adjusted by use of the METTLER TOLEDO buffers4.01, 7.00 and 9.21 and method M436.
When working with Rondo30 and two mini electrodes lowersample volumes can be used for two consecutive titrations in thesame sample.
In this method conditioning in the conditioning beaker is used forelectrode cleaning, alternatively, rinsing with the Rondo30 powershower can be used.
When automation with Rondo30 is not required, microtitrationbeakers can also be used when wanting to use smaller samplevolumes.
Remarks
R1: Consumption NaOH (mL)R2: Measurement pH value (pH)R3: Chloride content (mg/L)
Calculation
Titration Excellence Line: Method for the determination of tartaric acid and chloride in wine
Standard NaCl for AgNO3, KHP for NaOH
Melanie NijmanAuthor
Wastedisposal
82
Table of measured values
Mettler Toledo T90 Titrator Mettler Toledo AGMarket Support Laboratory15.10.2007
Method m379 Acid and Chloride Content in WineMeasured 11.10.2007
RESULTSNo. ID Sample size and results1 Wine 40.0 ml
R1 = 3.0744 ml ContentR2 = 1.660 pH pH valueR3 = 33.6713 mg/L Chloride content
2 Wine 40.0 mlR1 = 3.0925 ml ContentR2 = 1.662 pH pH valueR3 = 33.7785 mg/L Chloride content
3 Wine 40.0 mlR1 = 3.1120 ml ContentR2 = 1.670 pH pH valueR3 = 33.8016 mg/L Chloride content
4 Wine 40.0 mlR1 = 3.0839 ml ContentR2 = 1.669 pH pH valueR3 = 33.7493 mg/L Chloride content
5 Wine 40.0 mlR1 = 3.0739 ml ContentR2 = 1.669 pH pH valueR3 = 33.7564 mg/L Chloride content
6 Wine 40.0 mlR1 = 3.0859 ml ContentR2 = 1.671 pH pH valueR3 = 33.8069 mg/L Chloride content
STATISTICSNumber results R1 n = 6Mean value x = 3.0871 ml ConsumptionStandard deviation s = 0.0141 ConsumptionRelative standard deviation srel = 0.4570 %
Number results R2 n = 6Mean value x = 1.667 pH pH valueStandard deviation s = 0.005 pH valueRelative standard deviation srel = 0.277 %
Number results R3 n = 6Mean value x = 33.7607 mg/L Chloride contentStandard deviation s = 0.0495 Chloride contentRelative standard deviation srel = 0.1470 %
Titration curve
Results
83
Method: m379 Acid and Chloride Content in Wine 10.10.2007User: Nijman
001 Title Type General titration Compatible with T70/ T90 ID MxxxMN2 Titel Acid and Chloride Content in Wine Author Mettler Toledo Date / Time 10.10.2007 Modified at 10.10.2007 Protect No SOP None LabX SOP002 Sample Number of IDs 1
ID 1 Wine Entry Type Fixed volume Volume [mL] 40.0 Density [g/mL] 1.0 Correction factor 1.0 Temperature [°C] 25.0003 Titration stand Type Rondo60/Tower A Titration stand Rondo60/1A Lid handling No004 Stir Speed [%] 30 Duration [s] 10 Condition No005 Titration (EP) [1]
Titrant Titrant NaOH Concentration [mol/L] 1.0 Sensor Type pH Sensor DG102-Mini Unit pH Temperature aquisition Temperature measurement No Stir Speed [%] 30 Predispense Mode None Wait time [s] 0 Control Mode Absolute Tendency None End point value 7.0 Control band 0.2 Dosing rate (max) [mL/min] 20 Dosing rate (min) [mL/min] 300 Termination At EP Yes Termination delay [s] 0 At Vmax [mL] 5 Max. time[s] 20000
Accompanying stating Accompanying stating No Condition Condition No006 Dispense (normal) [1] Titrant H2SO4 10% Concentration [mol/L] 1 Volume [mL] 2.0 Dosing rate [mL/min] 60.0 Condition No007 Measure (normal) [1] Sensor Type pH Sensor DG102-Mini Unit pH Temperature acquisition Temperature measurement No Stir Speed [%] 30 Aquisition of measured values Aquisition Equilibrium controlled dE 0.5 dt [s] 1 t(min) [s] 10 t(max) [s] 30 Mean value No Condition Condition No008 Titration (EQP) [2]
Titrant Titrant AgNO3 Concentration [mol/L] 0.02 Sensor Type mV Sensor DM102-SC Unit mV Temperature aquisition Temperature measurement No Stir Speed [%] 30
Method Predispense Mode Volume Volume [mL] 0.2 Wait time [s] 5 Control Control User Titrant addition Dynamic dE (set value) 6 dV (min) 0.02 dV (max) 0.2 Mode Equilibrium controlled dE 1.0 dt [s] 2 t(min) [s] 10 t(max) [s] 30 Evaluation and Recognition Procedure Standard Threshold 150 Tendency None Ranges 0 Add. EQP criteria No Termination At Vmax [mL] 6.0 At potential No At Slope No After number of recognized EQPs Yes Number of EQPs 1 Combined termination criteria No
Accompanying stating Accompanying stating No Condition Condition No009 Calculation R1 Result Consumption Result Unit mL Formula R1=VEQ[1] Constant C= 1 M M[None] z z[None] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No010 Calculation R2 Result pH value Result Unit pH Formula R2=E Constant C= 1 M M[None] z z[None] Decimal places 3 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No011 Calculation R3 Result Chloride content Result Unit mg/L Formula R3=Q[2]*C/m Constant C= M*1000/z M M[Chloride] z z[Chloride] Decimal places 5 Result limits No Record statistics Yes Extra statistical functions No Send to buffer No Condition No012 Conditioning Type Fix Interval 1 Position Conditioning beaker Time [s] 20 Speed [%] 35 Condition No013 Record Summary No Results Per sample Raw results Per sample Table of measured values No Sample data No Resource data No E - V All titration functions dE/dV - V All titration functions ...... Condition No014 End of sample
84
The methods in this brochure represent selected, possible application examples. These have been tested with all possible care with the analytical instruments mentioned in the brochure. The experiments were conducted and the resulting data evaluated based on our current state of knowledge. However, the applications do not absolve you from personally testing their suitability for your intended methods, instruments and purposes. As the use and transfer of an application example are beyond our control, we cannot accept responsibility therefore. When chemicals and solvents are used, the general safety rules and the directions of the manufacturer must be observed.
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Application Brochure 35
A Choice of Methods for Various Probes
The models of the Titration Excellence line of METTLER TOLEDO
are an ideal base to build fully automated titration systems.
Thanks to the method concept and the color touch screen,
operation is made easy. A single sample or an entire series of samples can be started with a touch to the shortcut:
True One Click Titration™.
This Application Brochure contains a selection of methods
illustrating the applicative power or METTLER TOLEDO.
Titration Excellence
LineT70 Terminal, Rondo 20 with
PowerShower™ and LabX titration
Plug
& Play ElectrodesReliable
and secure
handling