This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D8045 − 17´1

Standard Test Method for

Acid Number of Crude Oils and Petroleum Products by
Catalytic Thermometric Titration1
This standard is issued under the fixed designation D8045; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

ε1 NOTE—Subsections 16.1.1 and 16.1.2 were corrected editorially in July 2018.

1. Scope* 2. Referenced Documents

1.1 This test method covers the determination of acidic 2.1 ASTM Standards:2
components in crude oil and petroleum products including D664 Test Method for Acid Number of Petroleum Products
waxes, bitumen, base stocks, and asphalts that are soluble in by Potentiometric Titration
mixtures of xylenes and propan-2-ol. It is applicable for the D974 Test Method for Acid and Base Number by Color-
determination of acids whose dissociation constants in water Indicator Titration
are larger than 10–9; extremely weak acids whose dissociation D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and
constants are smaller than 10–9 do not interfere. The values
Petroleum Products
obtained by this test method may not be numerically equivalent
D4175 Terminology Relating to Petroleum Products, Liquid
to other acid value measurements. The range of KOH acid
Fuels, and Lubricants
numbers included in the precision statement is 0.1 mg ⁄g to D4177 Practice for Automatic Sampling of Petroleum and
16 mg ⁄g. Petroleum Products
1.2 The values stated in SI units are to be regarded as D5854 Practice for Mixing and Handling of Liquid Samples
standard. No other units of measurement are included in this of Petroleum and Petroleum Products
standard. D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
1.3 This standard does not purport to address all of the Measurement System Performance
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3. Terminology
priate safety, health, and environmental practices and deter-
3.1 For general terminology, refer to Terminology D4175.
mine the applicability of regulatory limitations prior to use.
Some specific hazards statements are given in Section 7 on 3.2 Definitions:
Safety Precautions. 3.2.1 acid number, n—the quantity of a specified base,
expressed in milligrams of potassium hydroxide per gram of
1.4 This international standard was developed in accor-
sample, required to titrate a sample in a specified solvent to a
dance with internationally recognized principles on standard- specified endpoint using a specified detection system.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 3.2.2 catalytic thermometric titration, n—a method to de-
mendations issued by the World Trade Organization Technical termine the end point of a chemical reaction through the use a
temperature measuring device and the addition of a chemical to
Barriers to Trade (TBT) Committee.
enhance the detection of the endpoint.
3.2.3 crude oil, n—a naturally occurring hydrocarbon
mixture, generally in a liquid state, which may also include
compounds of sulfur, nitrogen, oxygen, metals, and other
elements.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2017. Published July 2017. Originally approved contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
in 2016. Last previous edition approved in 2016 as D8045 – 16ɛ1. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D8045-17E01. the ASTM website.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D8045 − 17´1
4. Summary of Test Method 7.2 Consult Safety Data Sheets (SDS) for chemicals listed
4.1 The sample and a fixed mass of paraformaldehyde are in this test method for further information.
dissolved in a mixture of xylenes and propan-2-ol. The mixture 8. Apparatus
is then titrated with potassium hydroxide using a constant rate
of titrant addition. A plot of the temperature of the reaction 8.1 Automatic Titrator, capable of providing a dose rate of
mixture versus the volume of titrant is generated. An exother- 2 mL ⁄min.
mic reaction between the titrant and sample occurs simultane- 8.2 Thermistor, a device capable of measuring the tempera-
ously with the endothermic depolymerization of paraformalde- ture to 0.001 °C. The device should be immersed in the
hyde. After all of the acidic material in the sample has reacted, titration solvent to a depth recommended by the manufacturer
the slope of the plot changes due to the absence of the and have a response time of less than 0.3 s.
competitive exothermic acid-base reaction. The change in 8.3 Analytical Balance, capable of weighing to 60.1 mg.
slope is the inflection point. The depolymerization of para-
formaldehyde is catalytically initiated and does not consume a 8.4 Burette, typically less than 20 mL capacity with a guard
significant quantity of potassium hydroxide. The net change tube containing adsorbent to retard the rate of titrant reaction
(positive or negative) in temperature prior to the consumption with atmospheric carbon dioxide.
of the acidic sample will be dependent upon the relative 8.5 Constant or Variable Speed Propeller Stirrer, sufficient
magnitude of the heats of reaction and environmental influ- to ensure adequate mixing of the sample and titrant.
ences. 8.6 Titration Beaker, with sufficient volume and made of a
material that does not interact with the sample, titrant or
5. Significance and Use
titration solvent.
5.1 Crude oils and oil sands bitumen contain naturally
8.7 Volumetric Dispenser, capable of consistently delivering
occurring acidic species. Acidity of crude oil has been impli-
desired volume of titration solvent.
cated in corrosion of distribution and process systems. The
relative amount of these materials can be determined by 9. Reagents
titrating with bases. The acid number is a measure of this
9.1 Potassium Hydroxide Solution, Standard Alcoholic,
amount of acidic substance in the oil under the conditions of
(0.1 M)—Add 6 g of potassium hydroxide (KOH) to approxi-
the test.
mately 1 L of propan-2-ol. Boil gently for 10 min to dissolve.
5.2 Acid number of crude and distilled petroleum fractions Allow the solution to stand for two days and then filter the
has been measured by Test Method D664. Test Method D664 supernatant liquid through a fine sintered-glass funnel. Store
was developed for the analysis of lubricants and biodiesel. The the solution in a chemically resistant bottle. Dispense in a
titration solvent used in Test Method D664 does not properly manner such that the solution is protected from atmospheric
address dissolving difficult samples such as crude oil, bitumen, carbon dioxide (CO2) by means of a guard tube containing
and high wax samples addressed in this test method. Refer to soda lime or soda non-fibrous silicate absorbents and such that
Appendix X1. it does not come into contact with cork, rubber, or saponifiable
5.3 Test Method D974 is also not applicable to measuring stopcock grease. Commercially prepared reagent is also suit-
acidity of crudes and highly colored samples because the able. Standardize frequently enough to detect concentration
indicator is not visible or it is difficult to discern a color change changes of 0.0005 mol ⁄L by standard industry practices or by
to detect the end point of the titration. thermometric titration of known quantities of benzoic acid
solution dissolved in n-heptane. See Appendix for details.
6. Interferences 9.2 Propan-2-ol (anhydrous, also referred to as isopropyl
6.1 Any material that reacts with potassium hydroxide will alcohol, >99 % purity).
interfere and overestimate the amount of acidic material in the 9.3 Mixed Xylenes—(Warning—Flammable.) A technical
sample. In crude oils, bitumens, synthetic crude oils, and grade of hydrocarbon that includes predominantly o-xylene,
subsequent fractions, the constituents that may be considered m-xylene, p-xylene and lesser quantities of ethyl benzene. The
to have acidic characteristics include inorganic and organic boiling point range is typically 136 °C to 140 °C.
acids, particularly naphthenic acids, phenolic compounds,
resins, salts of heavy metals, and acid salts of polybasic acids. 9.4 Titration Solvent—Add 250 mL 6 10 mL of anhydrous
isopropyl alcohol to 750 mL 6 10 mL of mixed xylenes.
7. Safety Precautions Larger quantities of titration solvent can be prepared using
volumetric ratios (25:75) of the same proportions. Commer-
7.1 Wear chemical resistant gloves. Avoid excessive inha- cially prepared reagent is also suitable.
lation of organic vapors and paraformaldehyde (flammable
solid) by working in a fume hood when possible. Pre-weighed 9.5 Toluene, pre-dissolution solvent (≥99 % purity).
paraformaldehyde packets should be substituted, if possible, to 9.6 Paraformaldehyde (polyoxymethylene)—(Warning—
minimize potential exposures when preparing titration slurry Flammable solid. Harmful if inhaled. Irritant.) Terminated with
solutions. The titrant solution is corrosive and paraformalde- hydroxyl end groups and in fine-powder form. Fine powder
hyde releases small quantities of formaldehyde during depo- mesh is critical to successful and rapid analysis of the material.
lymerization. Too large mesh reacts slowly, resulting in erroneous results. A

2
 D8045 − 17´1
sample of paraformaldehyde with greater than 80 % by mass 12. Quality Control
having a mesh size between 100 and 200 was found suitable. 12.1 Measure a quality control sample each day a sample(s)
Avoid moist, aged, or oxidized reagent. is tested. The quality control sample should be of similar
9.7 Benzoic acid (>99.9 % purity). matrix to sample tested. Control charts shall be established and
9.8 n-heptane (≥99 % purity). maintained according to generally accepted guidelines. Prac-
tice D6299 can be used for this purpose.
9.9 Water—Type 1 deionized, or higher, as defined by
Specification D1193. 13. Procedure
9.10 Titration Slurry with Indicator—17 g 6 0.5 g of para-
13.1 Blank Determination:
formaldehyde are added to one liter of titration solvent.
13.1.1 The blank value must be <0.1 mL. This is generally
10. Sampling the case when high purity propan-2-ol is used. The blank value
can be verified. The blank value is determined indirectly. A
10.1 Sampling is defined as all of the steps required to stable sample with a known acid number is measured using
obtain an aliquot representative of the contents of any pipe, three or more different sample masses. The largest sample size
tank, or other system and to place the sample into a container must not use a volume of titrant greater than the volume of the
for analysis by a laboratory or test facility. Sampling practices burette.
are covered in Practices D4057 and D4177. 13.1.2 The volume of titrant must be ≥0.15 mL for all
10.2 The sample should be well homogenized prior to sample masses.
taking an aliquot for testing. Power mixing per Practice D5854 13.1.3 The sample volume in milliliters (y-axis) is plotted
is advised for crude oils that are fluid at room temperature. versus the sample mass in grams (x-axis). Using the linear
Manual mixing and warming may be required for more viscous equation for the best fit line (R2 value must be 0.98 or greater),
samples. extrapolate to determine the volume of titration solvent that
10.3 For samples that contain more than 10 % entrained corresponds to a sample size of 0.0 g. See example in Fig. 1.
water, it is advised to remove the water prior to testing using 13.1.4 If the blank value exceeds 0.1 mL, prepare fresh
industry accepted methods. If adding toluene or other solvent titration solvent, confirm the titrant concentration and repeat
to aid in water removal, be sure to correct for the solvent the analysis. If the blank is below 0.1 mL, it is not necessary to
dilution in the hydrocarbon sample weight before analysis. apply a blank correction factor provided that the sample masses
shown in Table 1 are used (see 13.2).
11. Preparation of Apparatus 13.2 Sample Analysis:
11.1 If the burette has not been used within the last 12 h 13.2.1 Samples that are very viscous or solid at room
dispense sufficient titrant through the burette to remove air temperature (that is, asphalt) shall be heated in an oven
bubbles from the delivery tubing. Ensure that all of the (≤120 °C) until the material flows and sample can be stirred to
components (that is, stirrer, titrant tubing, thermistor, and so homogenize.
forth) that are to be immersed in the titration solvent are clean 13.2.2 For samples that do not readily dissolve in the slurry,
and free of acidic or basic contamination. it is permissible to pre-dissolve the sample after weighing by

NOTE 1—The above example shows a blank calculation for a sample of crude oil with a KOH acid number of approximately 0.9 mg ⁄g. The blank value
is equal to the value of y when x is set to a value of zero (0.039 mL in this particular example). The software can be configured to calculate the equation
and slope automatically.
FIG. 1 Example Blank Calculation for a Sample of Crude Oil

3
 D8045 − 17´1
TABLE 1 Recommended Sample Weights causing sample or solvent loss. The sample shall be fully
Expected Acid Number Recommended Sample Mass dissolved before titrating. Increase mixing time as needed to
(KOH, mg/g) (g) ± 10 %
completely dissolve the sample. Samples shall stay in solution
0.05 to 0.99 10 to 20
1.00 to 4.99 5
throughout the titration.
5.00 to 15.00 1 13.2.7 Manual Paraformaldehyde Addition—Add 0.50 g 6
0.10 g of paraformaldehyde per 30 mL of titration solvent to
the beaker and start the titration. It is permissible to pause the
adding in up to 10 mL of toluene or xylenes. In this case, stirring temporarily for the addition of the paraformaldehyde
solvent conditions shall be matched if determining the blank powder.
value. 13.2.8 Automated Paraformaldehyde Addition—Use of au-
13.2.3 Weigh the appropriate amount of sample into the tomated delivery systems for the paraformaldehyde addition is
titration beaker. Table 1 shows recommended initial sample permitted if precision and accuracy are not degraded. Such
size based on expected acid number value. This amount used systems may dose solvent with the paraformaldehyde for
may be adjusted to accommodate for solubility limitations and automated delivery such that the same amount of paraformal-
to conduct the blank determination. For unknowns, it is advised dehyde is added as in 13.2.7. The solution should be well
to start with a 5 g sample size, and adjust sample size as needed mixed and undergoing constant stirring during delivery. Follow
for subsequent measurements. The volume of titrant consumed manufacturer’s recommendation.
has to be ≥0.15 mL. Titrant volume ≤0.15 mL indicates that 13.2.9 Titrate the dissolved mixture with 0.1 M KOH at a
additional sample is required, and ≥5.0 mL of titrant suggests suggested rate of 2 mL ⁄min. Ensure that a minimum volume of
less sample is needed. ≥0.15 mL titrant is used.
13.2.4 When using less than the sample masses recom-
mended in Table 1, due to solubility issues (that is, for asphalt, 13.3 End Point Detection:
wax, and bitumen) and/or unavailability of necessary sample 13.3.1 A change in the slope of the plot of temperature
volume, then the blank value shall be determined for the versus volume indicates the endpoint of the titration (Fig. 2).
sample and applied to the calculation of the acid number value. The net change (positive or negative) in temperature may vary
13.2.5 For samples that have been heated in an oven, the from laboratory to laboratory due to the types of samples and
beaker containing the sample and titration solvent (with environmental effects. The use of software to calculate the
pre-dissolution solvent) may be heated (≤65 °C) to ensure full second derivative facilitates the determination of the endpoint.
solubility of the sample prior to the start of the titration. It is 13.3.2 After completion of the titration, verify that all of the
advised to cool the sample to room temperature before testing, sample remains solubilized in the titration solvent. If this is not
provided the sample remains in solution. Analysis at slightly the case, the titration is invalid. Rinse all of the components
elevated temperatures is allowable but the rate of cooling that were immersed in the titration solvent with toluene or
should be minimized. Conditions shall be matched if determin- some other suitable nonacidic solvent. Immersing the probe in
ing the blank value. This approach can affect the precision and solvent with stirring may aid in removal of any visible material
accuracy of the method and is not recommended for samples not removed by solvent rinse. A dip rinse in xylene with
that can be successfully analyzed without heating. stirring has proven to be sufficient for cleaning.
13.2.6 Add titration solvent, typically 30 mL, to the titration
beaker and place the thermistor and titrant delivery line into the 13.4 It is advised that the KOH burette be flushed with Type
sample. Stir the contents for a minimum of 30 s as rapidly as 1 water if the burette is to be idle for an extended period of time
possible without exposing the thermistor to a vortex and to prevent salt deposits from forming.

TET = Thermometric Endpoint Detection

ERC = Endpoint Recognition Criteria
FIG. 2 Example Titration Curve

4
 D8045 − 17´1
14. Calculation Ten cooperators participated in the interlaboratory study which
14.1 Calculate the acid number using Eq 1: included samples of crude oil, asphalt, lubricant base oil,
vacuum gas oil, and bitumen covering an acidity range of
~ A !~ M !~ 56.11! KOH, 0.1 mg ⁄g to 16.0 mg ⁄g. A copy of the research report
~ KOH acid number, mg/g! 5 W
(1)
RR:D02-1842 is available from ASTM.3
where: 16.1.1 Repeatability—The difference between two results
A = volume of titrant at the end point, mL, obtained by the same operator with the same apparatus under
M = titrant concentration, mol/L, and constant operating conditions on identical test material would,
W = sample mass, g. in the long run, in the normal and correct operation of the test
method, exceed only in one case in twenty.
14.1.1 The constant value of 56.11 is the molar mass of
potassium hydroxide in grams per mole. Two unit conversions Repeatability 5 7.399E202 3 X 0.6177 KOH, mg/g
negate each other (grams to milligrams and liters to milliliters). where:
14.1.2 If less than the recommended sample mass was used, X = the average of two results.
then the blank value must be determined and applied to the
calculation of the acid number value (Eq 2): 16.1.2 Reproducibility—The difference between two single
and independent results obtained by the different operators in
~ A 2 B !~ M !~ 56.11! different laboratories on identical test material would, in the
~ KOH acid number, mg/g! 5 W
(2)
long run, in the normal and correct operation of the test
where: method, exceed only in one case in twenty.
A = volume of titrant at the end point, mL, Reproducibility 5 0.3140 3 X 0.6177 KOH, mg/g
B = volume to end point of blank as determined in 13.1,
mL, where:
M = titrant concentration, mol/L, and X = the average of two results.
W = sample mass, g. NOTE 1—The data in Table 2 shows repeatabilities and reproducibilities
acid number values obtained using the formulas given in 16.1.1 and
15. Report 16.1.2.

15.1 Report the acid number in units of KOH, mg/g of 16.2 Bias—The bias of this test method has not been
sample to two (2) decimal places and reference this test determined since no acceptable reference material has been
method. identified.
15.2 If less than 0.15 mL of titrant was consumed, report the 17. Keywords
acid value as KOH, <0.05 mg ⁄g for a 20 g sample size or report 17.1 acid number; corrosion; crude oil; naphthenic acids;
the acid value as KOH, <0.08 mg ⁄g for a 10 g sample size. thermometric titration
16. Precision and Bias
3
Supporting data have been filed at ASTM International Headquarters and may
16.1 Precision—The precision of this test method was be obtained by requesting Research Report RR:D02-1842. Contact ASTM Customer
determined by statistical analysis of interlaboratory test results. Service at [email protected].

5
 D8045 − 17´1
TABLE 2 Calculated Precision Values for Acid Number
Acid Number, Repeatability (r), Reproducibility (R),
mg/g KOH mg/g KOH mg/g KOH
0.50 0.05 0.20
1.00 0.07 0.31
1.50 0.10 0.40
2.00 0.11 0.48
5.00 0.20 0.85
10.00 0.31 1.30

APPENDIXES

(Nonmandatory Information)

X1. CCQTA COMPARISON STUDY BETWEEN TEST METHOD D664 POTENTIOMETRIC TITRATION AND PROPOSED
THERMOMETRIC TITRATION DETERMINATION OF ACID NUMBER OF CRUDE OILS

X1.1 The Canadian Crude Quality Technical Association, NOTE X1.1—Inclusion of the CCQTA study as non-mandatory infor-
CCQTA, conducted studies to compare D8045 thermometric mation is not to be interpreted as endorsement by ASTM of the technical
titration to Test Method D664 potentiometric titration for a merit nor conclusions of the study.
series of crude oil samples. The results of the comparisons can
X1.2 KOH acid numbers in this study ranged from
be found in Research Report RR:D02-1842.3 It is included for
0.02 mg ⁄g to 11 mg ⁄g. Results of these comparative studies are
information only. Some samples were difficult to dissolve in
shown in Figures 2, 3, and 5 of the report. Based on this limited
the Test Method D664 titration solvent. During titration of
these samples, electrodes were found to be coated with waxy study, there appears to be reasonable agreement between the
materials from the crude oils, making the end point difficult to two methods for those samples that were soluble by Test
judge. For the samples in this study, this difficulty was not Method D664.
encountered with the titration solvent used in thermometric
titration.4

4
Permission to use data from Canadian Crude Quality Technical Association
(CCQTA) has been obtained and is on file at ASTM Headquarters.

X2. THERMISTER VALIDATION

X2.1 Temperature Difference Check—Although the accu- five to ten degrees cooler than the initial measurement tem-
racy of the thermistor is not critical to the performance of the perature (that is, 10 °C to 15 °C). Immerse the thermistor and
test, the ability to rapidly detect a temperature change is critical calibrated thermometer in the cooled sample of water. Record
to the test. Immerse a calibrated thermometer (with a resolution the temperature of the thermistor (°C) and the temperature of
of 0.01 °C or lower and an accuracy of <0.5 °C in the the calibrated thermometer (D). Report the temperature differ-
temperature range from 10 °C to 35 °C in a sample of water ential for both the calibrated thermometer and the thermistor.
with a constant temperature of approximately 20 °C 6 5 °C. Replace the thermistor if the ratio of the absolute value of the
Record the temperature of the thermistor (A) and the tempera- temperature difference is greater than 1.1 or less than 0.9.
ture of the calibrated thermometer (B) to the nearest 0.01 °C
after the devices have equilibrated. Cool the sample (that is, Delta Temperature 5
? A 2 C? (X2.1)
using a refrigerator or freezer) to a temperature approximately ? B 2 D?

6
 D8045 − 17´1

X3. VALIDATION OF TITRANT CONCENTRATION

X3.1 Quantitatively add 0.61 g (accurately weighed to X3.1.1 The factor of 122.12 is the molar mass of benzoic
0.1 mg) of high purity benzoic acid to a 250 mL volumetric acid in grams per mole and the factor of 4 is the inverse of
flask. Dilute the sample to approximately 200 mL with 0.25 L.
n-heptane or titration solvent and allow sufficient time for the
X3.2 Pipet 30 mL of the benzoic acid solution into a sample
benzoic acid to dissolve (that is, 60 s on a vortex mixture is titration cup and then add 0.5 g 6 0.10 g of paraformaldehyde.
recommended). Dilute to the 250 mL mark with additional Titrate with 0.1 M KOH solution. Calculate the concentration
n-heptane or titration solvent after dissolution of the benzoic of titrant using Eq X3.2.
acid. Calculate the exact concentration of the benzoic acid
standard using Eq X3.1. ~ Mb !~ Vx!
Mk 5 (X3.2)
Vk
g
Mb 5 34 (X3.1) where:
122.12
Mx = molarity of KOH titrant in moles per liter,
where: Mb = molarity of benzoic acid solution in moles per liter,
Mb = molarity of benzoic acid solution in grams per mole, Vx = volume of benzoic acid solution in liters (0.030 L),
and and
g = sample mass of benzoic acid in grams. Vk = volume of KOH titrant to the endpoint in liters.

SUMMARY OF CHANGES

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D8045 – 16ɛ1) that may impact the use of this standard. (Approved July 1, 2017.)

(1) Revised subsections 7.1, 9.6, and Table 2.

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