METTLER TOLEDO M592

Base Number ASTM D 2896-92

Method for the determination of the base number in oils according to ASTM D 2896.

Sample Oil sample, sample size 0.1 - 10 g Preparation and Procedures

(see table under remarks).
Substance Alkaline contents in the oil.
Chemicals ASTM 2896 solvent (Acetic
acid:Chlorobenzene 1:2)
Titrant HClO4 in acetic acid;
c(HClO4) = 0.1 mol/L;
The well homogenized (very important!) oil sample is weighed
into the titration beaker and then placed on the sample changer
ST20A. Used oils have to be warmed up to 50 °C and shaken
strongly if necessary.
Many used oils also contain insoluble solids. Their presence is
normal and does not disturb the titration. If necessary the
solution can also be filtered.
The 60 mL of solvent are added automatically by means of the
connected pump (e.g. function RINSE). The solvent for rinsing
and conditioning is added automatically with this pump.
Samples of low solubility are first dissolved in 40 mL of
chlorobenzene. 20 mL acetic acid are added afterwards. In this
case the automatic dosing of solvent 2896 must be deactivated.

Standard KHP

Instruments DL55; Sample changer ST20A,

METTLER TOLEDO AT261, HP Deskjet
or EPSON LX/FX

Accessories Glass beaker ME-101446,

Pump ME-65241

Remarks
Indication DG113 with NaClO4, saturated in acetic For many products the results obtained for the BN with this
acid, as electrolyte. method are very similar to those from ASTM D 4739.

Chemistry Yet some products containing special compounds like strongly

over-alkalized oil additives and polymers containing nitrogen
can yield higher results than with the standard ASTM D 4739.

Calculation

Results

Waste The resulting solution is a mixture of

disposal water and organic solvents. The water
has to be separated off before
disposing of as organic solvent.

Author D. Rehwald, A. Logean

1
Results
Oil type ASTM D 2896 ASTM D 4739 (standard)

Amount BN (EQP) time BN (buffer) BN (EQP) time

x RSD Min x RSD x RSD Min

Standard oil (2g) 10.93 0.1 9 6.56 0.9 -- -- 135

GTX3 high perf. (2g) 11.94 3.6 13 8.60 1.9 -- -- 67
Synthetic oil (2g) 13.52 0.1 12 12.19 0.9 13.46 0.3 35
Light oil 10.11 4.4 9 7.03 2.2 -- -- 136
Used oil (tractor) (2g) 10.15 0.1 10 3.69 4.7 -- -- 121
Used oil (diesel) (2g) 6.81 0.8 13 2.27 2.1 -- -- 21

The analysis consisted of series of five samples per oil type. The dashed lines indicate that no EQP was found
in this titration.

METTLER TOLEDO DL55 Titrator V2.0 Mettler-Toledo GmbH

Market Support Laboratory

Method MT086 BN ASTM D 2896 18-Aug-1995 13:46

Measured 30-Aug-1995 16:40
User

RESULTS

No. ID Sample size and results

1 Oil 1.9918 g
R1 = 13.53 mg KOH/g BN
2 Oil 2.0019 g
R1 = 13.51 mg KOH/g BN
3 Oil 2.0086 g
R1 = 13.55 mg KOH/g BN
4 Oil 1.9978 g
R1 = 13.51 mg KOH/g BN
5 Oil 1.9989 g
R1 = 13.52 mg KOH/g BN

STATISTICS
Number of results R1 n = 5
Mean value x = 13.52 mg KOH/g BN
Standard deviation s = 0.01544 mg KOH/g BN
Rel. standard deviation srel = 0.114 %

Table of measured values Titration curve

2
Method
Method MT086 BN ASTM D 2896 Calculation
Version 18-Aug-1995 13:46 Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . .
Title Decimal places . . . . . . . . . . . 0
Method ID . . . . . . . . . . . . . MT086 Result unit . . . . . . . . . . . .
Title . . . . . . . . . . . . . . . BN ASTM D 2896 Result name . . . . . . . . . . . .
Date/time . . . . . . . . . . . . . 18-Aug-1995 13:46 Statistics . . . . . . . . . . . . . No
Sample
Sample ID . . . . . . . . . . . . . Oil Report
Entry type . . . . . . . . . . . . . Weight Output unit . . . . . . . . . . . . Printer
Lower limit [g] . . . . . . . . . 0.1 Results . . . . . . . . . . . . . . No
Upper limit [g] . . . . . . . . . 10.0 All results . . . . . . . . . . . . Yes
Molar mass M . . . . . . . . . . . . 56.1 Raw results . . . . . . . . . . . . Yes
Equivalent number z . . . . . . . . 1 Table of measured values . . . . . . Yes
Titration stand . . . . . . . . . . ST20A Sample data . . . . . . . . . . . . No
Pump . . . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . . Solvent 2896 dE/dV - V curve . . . . . . . . . . No
Volume [mL] . . . . . . . . . 60.0 d2E/dV2 - V curve . . . . . . . . . No
Stir . . . . . . . . . . . . . Yes log dE/dV - V curve . . . . . . . . No
Pump . . . . . . . . . . . . . . No E - t curve . . . . . . . . . . . . No
Rinse . . . . . . . . . . . . . . Yes V - t curve . . . . . . . . . . . . No
Solvent . . . . . . . . . . . Solvent 2896 dV/dt - t curve . . . . . . . . . .
Volume [mL] . . . . . . . . . 20.0
Conditioning . . . . . . . . . . Yes Parameters of titration
Time [s] . . . . . . . . . . . 60 The mode of operation according to the standard allows a dosing
Rinse . . . . . . . . . . . . Yes rate of maximal 1.0 mL/min and a potential change (dEnom) of 30
Solvent . . . . . . . . . . Solvent 2896 mV.
Volume [mL] . . . . . . . . 20.0 If dE is < 30mV per 0.1mL, then the increment size is 0.1 mL.
Temperature sensor . . . . . . . . . Manual With dE > 30 mV per 0.1 mL the increment size is only 0.05 mL.
Stir The titration can be terminated as soon as an EQP is found. If
Speed [%] . . . . . . . . . . . . . 60 no EQP is detected a subsequent back titration has to be
Time [s] . . . . . . . . . . . . . . 60 performed. For more information see method MT087 in this
EQP titration brochure.
Titrant/Sensor Sample size
Titrant . . . . . . . . . . . . . HClO4 The sample size depends on the expected value of the BN:
Concentration [mol/L] . . . . . . 0.1 Amount (g) = 28/BN (expected)
Sensor . . . . . . . . . . . . . DG113
Unit of meas. . . . . . . . . . . mV According to the standard (procedure B) a minimum of 0.1g and a
Predispensing . . . . . . . . . . . to volume maximum of 10 g of sample are intended. The standard describes
Volume [mL] . . . . . . . . . . . 0.2 a procedure A with a maximal sample volume of 120 mL and a
Titrant addition . . . . . . . . . . Dynamic procedure B with a maximum of 60 mL, which allows an analysis
dE(set) [mV] . . . . . . . . . . 30.0 of half the sample size. A ring test with fresh and with used
dV(min) [mL] . . . . . . . . . . 0.05 oils and additive concentrates showed both procedures (A and B)
dV(max) [mL] . . . . . . . . . . 0.1 to deliver statistically equal results. Considering economy as
Measure mode . . . . . . . . . . . . Equilibrium controlled well as ecology the use of smaller quantities is preferable.
dE [mV] . . . . . . . . . . . . . 0.5 However with only 0.1 g sample a weighing accuracy of 0.0005 g
dt [s] . . . . . . . . . . . . . 6.0 (500 µg) has to be ensured.
t(min) [s] . . . . . . . . . . . 10.0 The standard demands the following repeatability and
t(max) [s] . . . . . . . . . . . 60.0 reproducibility for the determination of the BN:
Recognition a: repeatability
Threshold . . . . . . . . . . . . 80.0 Two results, same operator, same instrument, same sample,
Steepest jump only . . . . . . . No longtime routine operation under normal conditions:
Range . . . . . . . . . . . . . . No one value out of 20 is allowed to differ more than 5 % from
Tendency . . . . . . . . . . . . Positive the mean of the two. With the back titration of used oils up to
Termination 32 % are allowed.
at maximum volume [mL] . . . . . 10.0 b: reproducibility
at potential . . . . . . . . . . No Two independent individual results, different operators,
at slope . . . . . . . . . . . . No different instruments, the same
after number EQPs . . . . . . . . Yes sample, longtime routine operation under normal conditions:
n = . . . . . . . . . . . . . 1 one value out of 20 is allowed to differ more than 7 % from the
comb. termination conditions . . No mean of the two.
Evaluation - total base number > 59.9 5 %
Procedure . . . . . . . . . . . . Standard - used oils, direct titration 5 %
Potential 1 . . . . . . . . . . . No - used oils, back titration 24 %
Potential 2 . . . . . . . . . . . No DIN ISO 3771
Stop for reevaluation . . . . . . No This standard, which practically corresponds to ASTM D 2896,
Calculation defines the precision of the method even more strictly:
Formula . . . . . . . . . . . . . . R=(Q-H9)*C/m The allowed differences from the mean value of 20
Constant . . . . . . . . . . . . . . C=M/z determinations are:
Decimal places . . . . . . . . . . . 2
Result unit . . . . . . . . . . . . mg KOH/g - total base number up to 59.9 5 %
Result name . . . . . . . . . . . . BN
Statistics . . . . . . . . . . . . . Yes - total base number > 59.9 5 %
Calculation
Formula . . . . . . . . . . . . . . - used oils, direct titration 5 %
Constant . . . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 0 - used oils, back titration 24 %
Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . No