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: D5863 − 22

Standard Test Methods for

Determination of Nickel, Vanadium, Iron, and Sodium in
Crude Oils and Residual Fuels by Flame Atomic Absorption
Spectrometry1
This standard is issued under the fixed designation D5863; 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.

1. Scope* mine the applicability of regulatory limitations prior to use.

1.1 These test methods cover the determination of nickel, Specific warning statements are given in 8.1, 9.2, 9.5, 11.2,
vanadium, iron, and sodium in crude oils and residual fuels by 11.4, and 16.1.
flame atomic absorption spectrometry (AAS). Two different 1.8 This international standard was developed in accor-
test methods are presented. dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
1.2 Procedure A, Sections 8–14—Flame AAS is used to Development of International Standards, Guides and Recom-
analyze a sample that is decomposed with acid for the mendations issued by the World Trade Organization Technical
determination of total Ni, V, and Fe. Barriers to Trade (TBT) Committee.
1.3 Procedure B, Sections 15–20—Flame AAS is used to
analyze a sample diluted with an organic solvent for the 2. Referenced Documents
determination of Ni, V, and Na. This test method uses oil- 2.1 ASTM Standards:2
soluble metals for calibration to determine dissolved metals D1193 Specification for Reagent Water
and does not purport to quantitatively determine nor detect D4057 Practice for Manual Sampling of Petroleum and
insoluble particulates. Hence, this test method may underesti- Petroleum Products
mate the metal content, especially sodium, present as inorganic D4175 Terminology Relating to Petroleum Products, Liquid
sodium salts. Fuels, and Lubricants
1.4 The concentration ranges covered by these test methods D4177 Practice for Automatic Sampling of Petroleum and
are determined by the sensitivity of the instruments, the Petroleum Products
amount of sample taken for analysis, and the dilution volume. D6299 Practice for Applying Statistical Quality Assurance
A specific statement is given in Note 1. and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
1.5 For each element, each test method has its own unique
precision. The user can select the appropriate test method based 3. Terminology
on the precision required for the specific analysis.
3.1 Definitions:
1.6 The values stated in SI units are to be regarded as 3.1.1 For definitions of terms used in these test methods,
standard. No other units of measurement are included in this refer to Terminology D4175.
standard, unless specifically stated. Other units that appear in
this standard are included for information purposes only or 4. Summary of Test Method
because they are in embedded pictures that cannot be edited. 4.1 Procedure A—One to twenty grams of sample are
1.7 This standard does not purport to address all of the weighed into a beaker and decomposed with concentrated
safety concerns, if any, associated with its use. It is the sulfuric acid by heating to dryness. The residual carbon is
responsibility of the user of this standard to establish appro- burned off by heating at 525 °C in a muffle furnace. The
priate safety, health, and environmental practices and deter- inorganic residue is digested in dilute nitric acid, evaporated to
incipient dryness, dissolved in dilute nitric and made up to
volume with dilute nitric acid. Interference suppressant is
1
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand are the direct responsibility of
2
Subcommittee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2022. Published January 2023. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1995. Last previous edition approved in 2016 as D5863 – 00a (2016). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5863-22. 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
 D5863 − 22
added to the dilute nitric acid solution. The solution is
nebulized into the flame of an atomic absorption spectrometer.
A nitrous oxide/acetylene flame is used for vanadium and an
air/acetylene flame is used for nickel and iron. The instrument
is calibrated with matrix-matched standard solutions. The
measured absorption intensities are related to concentrations by
the appropriate use of calibration data.
4.2 Procedure B—Sample is diluted with an organic solvent
to give a test solution containing either 5 % (m/m) or 20 %
(m/m) sample. The recommended sample concentration is
dependent on the concentrations of the analytes in the sample.
For the determination of vanadium, interference suppressant is
added to the test solution. The test solution is nebulized into the
flame of an atomic absorption spectrometer. A nitrous oxide/
acetylene flame is used for vanadium and an air/acetylene
flame is used for nickel and sodium. The measured absorption
intensities are related to concentrations by the appropriate use
of calibration data.

5. Significance and Use

FIG. 1 Decomposition Apparatus
5.1 When fuels are combusted, metals present in the fuels
can form low melting compounds that are corrosive to metal
parts. Metals present at trace levels in petroleum can deactivate 7.2 Prior to weighing, stir the sample and then shake the
catalysts during processing. These test methods provide a sample in its container. If the sample does not readily flow at
means of quantitatively determining the concentrations of room temperature, heat the sample to a sufficiently high and
vanadium, nickel, iron, and sodium. Thus, these test methods safe temperature to ensure adequate fluidity.
can be used to aid in determining the quality and value of the
crude oil and residual oil. PROCEDURE A—FLAME ATOMIC ABSORPTION
AFTER ACID DECOMPOSITION OF THE SAMPLE
6. Purity of Reagents
8. Apparatus
6.1 Reagent grade chemicals shall be used for all tests.
Unless otherwise indicated, it is intended that all reagents 8.1 Atomic Absorption Spectrometer, complete instrument
conform to the specifications of the Committee on Analytical with hollow cathode lamps and burners with gas supplies to
Reagents of the American Chemical Society where such support air-acetylene and nitrous oxide-acetylene flames.
specifications are available.3 Other grades may be used, pro- (Warning—Hazardous. Potentially toxic and explosive. Refer
vided it is first ascertained that the reagent is of sufficiently to the manufacturer’s instrument manual for associated safety
high purity to permit its use without lessening the accuracy of hazards.)
the determination. 8.2 Sample Decomposition Apparatus (optional)—This ap-
6.2 When determining metals at concentrations less than paratus is described in Fig. 1. It consists of a borosilicate glass
1 mg ⁄kg, use ultra-pure grade reagents. 400 mL beaker for the test solution, an air bath (Fig. 2) that
rests on a hot plate and a 250 W infrared lamp supported
6.3 Purity of Water—Unless otherwise indicated, reference
2.5 cm above the air bath. A variable transformer controls the
to water shall be understood to mean reagent water conforming
voltage applied to the lamp.
to Type II of Specification D1193.
8.3 Glassware—Borosilicate glass 400 mL beakers, volu-
7. Sampling and Sample Handling metric flasks of various capacities and pipettes of various
7.1 The objective of sampling is to obtain a sample for capacities. When determining concentrations below 1 mg ⁄kg,
testing purposes that is representative of the entire quantity. all glassware must be thoroughly cleaned (or soaked overnight)
Only representative samples obtained as specified in Practices with 5 % HNO3 and rinsed five times with water.
D4057 and D4177 shall be used. Do not fill the sample 8.4 Electric Muffle Furnace, capable of maintaining 525 °C
container more than two-thirds full 6 25 °C and sufficiently large to accommodate 400 mL bea-
kers. The capability of an oxygen bleed is advantageous and
optional.
3
ACS Reagent Chemicals, Specifications and Procedures for Reagents and 8.5 Steam Bath.
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical 8.6 Temperature Controlled Hot Plate, (optional).
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- 8.7 Drying Oven, (optional), explosion-proof, if used to heat
copeial Convention, Inc. (USPC), Rockville, MD. crude oils to obtain fluidity.

2
 D5863 − 22
TABLE 1 AAS Conditions for the Determination of Vanadium,
Nickel, and Iron Following Acid Sample Decomposition
Wavelength, Concentration Interference
Element Flame
nm Range, µg/mL Suppressant
Vanadium 318.4 0.5–20 250 µg/mL Al, N2O-
Al(NO3)3 in 5 % C2H2
(V/V)
HNO3
Nickel 232.0 0.5–20 None Air-C2H2
Iron 248.3 3.0–10 None Air-C2H2

10. Preparation of Standards

10.1 Multi-Element Standard—Using the aqueous standard
solutions, prepare a multi-element standard containing
100 mg ⁄kg each of vanadium, nickel, and iron. Standards
should be prepared to ensure accuracy and stability and should
be stored in clean containers to safeguard against physical
degradation.
10.2 Working Standards—Prepare at least two working
standards to cover the concentration ranges specified in Table
1. For vanadium, add the specified interference suppressant.
Each working standard must contain 5 % (V ⁄V) nitric acid.
Standards should be prepared to ensure accuracy and stability
and should be stored in clean containers to safeguard against
physical degradation.
10.3 Standard Blank, the standard blank contains 5 % (V/V)
NOTE 1—All parts 16 gage (1.5 mm, 0.060 in.) aluminum. All dimen-
sions are in inches.
nitric acid and any interference suppressant specified in Table
1.
Metric Equivalents
10.4 Check Standard—Prepare a calibration check standard
in. mm in. mm
in the same way as the working standards and at analyte
1 25.4 37⁄8 98.4
1 1⁄ 2 38.1 5 127 concentrations that are typical of the specimens being ana-
2 50.8 61⁄2 165.1 lyzed.
31⁄16 77.8 ... ...
11. Preparation of Test Solutions
FIG. 2 Air Bath
11.1 Into a beaker, weigh an amount of sample estimated to
contain between 0.0025 mg and 0.12 mg of each metal to be
determined. A typical mass is 10 g. Add 0.5 mL of H2SO4 for
each gram of sample.
9. Reagents
NOTE 1—If it is desired to extend the lower concentration limits of the
9.1 Aqueous Standard Solutions—Individual aqueous stan- test method, it is recommended that the decomposition be done in 10 g
dards with 1000 mg ⁄kg concentrations of vanadium, nickel, increments up to a maximum of 100 g. It is not necessary to destroy all the
and iron, purchased or prepared in acid matrix to ensure organic matter each time before adding additional amounts of the sample
stability. and acid. When it is desired to determine higher concentrations, reduce the
sample size accordingly.
9.2 Nitric Acid—Concentrated nitric acid, HNO3 .
11.2 At the same time prepare reagent blanks using the same
(Warning—Poison, oxidizer. Causes severe burns. Harmful or
amount of sulfuric acid as used for sample decomposition.
fatal if swallowed or inhaled.)
Reagent blanks should be carried through the same procedure
9.3 Nitric Acid 50 % (V/V)—Carefully add, with stirring, as the samples. (Warning—Reagent blanks are critical when
one volume of concentrated nitric acid to one volume of water. determining concentrations below 1 mg ⁄kg. To simplify the
9.4 Dilute Nitric Acid, 5 % (V/V)—Carefully add, with analysis, use the same volume of acid and the same dilutions as
stirring, one volume of concentrated nitric acid to 19 volumes used for the samples. For example, if 20 g of sample is being
of water. decomposed, use 10 mL of sulfuric acid for the reagent blank.)
9.5 Sulfuric Acid—Concentrated sulfuric acid, H2SO4. 11.3 The use of the air bath apparatus (Fig. 2) is optional.
(Warning—Poison, oxidizer. Causes severe burns. Harmful or Place the beaker in the air bath, which is located in the hood.
fatal if swallowed or inhaled.) The hot plate is off at this time. Heat gently from the top with
the infrared lamp (Fig. 1) while stirring the test solution with a
9.6 Aluminum Nitrate, Al(NO3)3 9HOH. glass rod. As decomposition proceeds (indicated by a frothing
9.7 Potassium Nitrate, KNO3. and foaming), control the heat of the infrared lamp to maintain

3
 D5863 − 22
steady evolution of fumes. Give constant attention to each 13.5 Nebulize the test solutions and measure and record the
sample mixture until all risk of spattering and foaming is past. absorbance. If appropriate, blank correct this absorbance by
Then, gradually increase the temperature of both the hot plate subtracting the reagent blank absorbance.
and lamp until the sample is reduced to a carbonaceous ash. 13.6 After measuring absorbances for a test solution, check
11.4 If the air bath apparatus is not used, heat the sample the blank standard. If this does not read zero, check the system,
and acid on a temperature controlled hot plate. As described in and then repeat steps 13.2 – 13.5.
11.3, monitor the decomposition reaction and adjust the tem- 13.7 Test solutions that give absorbances greater than that
perature of the hot plate accordingly. (Warning—Hot fuming obtained with the most concentrated working standard must be
concentrated sulfuric acid is very corrosive and a strong diluted. The dilution must contain interference suppressant at
oxidizing acid. The analyst should work in a well-ventilated the specified concentrations.
hood and wear rubber gloves and a suitable face shield to
protect against spattering acid.) 14. Quality Assurance/Quality Control (QA/QC)
11.5 Place the sample in the muffle furnace maintained at 14.1 Confirm the performance of the instrument and the test
525 °C 6 25 °C. Optionally, introduce a gentle stream of procedure by analyzing a control QC sample.
oxygen into the furnace to expedite oxidation. Continue to heat 14.1.1 When QA/QC protocols are already established in
until the carbon is completely removed. the testing facility, these may be used to confirm the reliability
of the test result.
11.6 Dissolve the inorganic residue by washing down the
14.1.2 When there is no QA/QC protocol established in the
wall of the beaker with about 10 mL of the 1 + 1 HNO3. Digest
testing facility, Appendix X1 can be used as the QA/QC
on a steam bath for 15 min to 30 min. Transfer to a hot plate
protocol.
and gently evaporate to incipient dryness.
14.2 Users of this test method are advised that in contractual
11.7 Wash down the wall of the beaker with about 10 mL of agreements, one or more of the contracting parties can and may
dilute nitric acid (5 % V/V). Digest on the steam bath until all make Appendix X1 a mandatory practice.
salts are dissolved. Allow to cool. Transfer quantitatively to a
volumetric flask of suitable volume and make up to volume PROCEDURE B—FLAME ATOMIC ABSORPTION
with dilute nitric acid. This is the test solution. WITH AN ORGANIC SOLVENT TEST SOLUTION
11.8 Pipette aliquots of the test solution into two separate 15. Apparatus
volumetric flasks. Retain one flask for the determination of
nickel and iron. To the other flask add aluminum interference 15.1 Refer to Section 8.1.
suppressant for vanadium determination (refer to Table 1) and 15.2 Test Solution Containers—Glass or plastic vials or
dilute up to mark with dilute nitric acid (5 % V/V). Similarly, bottles, with screw caps and a capacity of between 50 mL to
prepare a reagent blank solution for vanadium analysis. 100 mL. Glass bottles of 100 mL capacity are satisfactory.

12. Preparation of Apparatus 16. Reagents

12.1 Consult the manufacturer’s instructions for the opera- 16.1 Dilution Solvent—Mixed xylenes, o-xylene, tetralin
tion of the atomic absorption spectrometer. This test method and mixed paraffin-aromatic solvents are satisfactory.
assumes that good operating procedures are followed. Design (Warning—Combustible. Vapor harmful.) Solvent purity can
differences between spectrometers make it impractical to affect analytical accuracy when the sample contains low
exactly specify required instrument settings. concentrations (typically, a few mg/kg) of the analytes.
12.2 Set up the instrument to determine each analyte se- 16.2 Mineral Oil—A high-purity oil such as U.S.P. white
quentially. oil.
16.3 Organometallic Standards—Pre-prepared multi-
13. Calibration and Analysis element concentrates containing 100 mg ⁄kg concentrations of
each element are satisfactory.4
13.1 For each analyte in turn, perform the following opera-
tion: 17. Preparation of Standards and Test Solutions
13.2 Nebulize the appropriate blank standard and zero the 17.1 Test Solution—Weigh a portion of well-mixed sample
instrument. into a container and add solvent to achieve a sample concen-
13.3 Nebulize the working standards, determine the absor- tration of either 5 % (m/m) or 20 % (m ⁄m). Mix well. If the
bance and construct a calibration curve of absorbance versus concentration of V, Ni, or Na in the sample exceeds 20 mg ⁄kg,
analyte concentration utilizing the instrument’s concentration the analysis for that element is performed on a test solution
mode if available, otherwise plot these values.
4
13.4 Use the check standard to determine if the calibration The sole source of supply of the standards known to the committee at this time
is Conoco, Inc., Conostan Division, P.O. Box 1269, Ponca City, OK 74602. If you
for each analyte is accurate. If the results obtained on the check
are aware of alternative suppliers, please provide this information to ASTM
standard are not within 65 % of the expected concentration for International Headquarters. Your comments will receive careful consideration at a
each analyte, take corrective action and repeat the calibration. meeting of the responsible technical committee,1 which you may attend.

4
 D5863 − 22
TABLE 2 AAS Conditions for the Determination of Vanadium, TABLE 3 Repeatability
Nickel, and Sodium Following Solvent Dilution of the Sample Concentration Range,
Element Procedure Repeatability, mg/kgA
Wavelength, Concentration Interference mg/kg
Element Flame
nm Range, mg/kg Suppressant Vanadium 50–500 A 1.1X0.50
Vanadium 318.4 0.5–15 15 mg/kg AlA N2O-C2H2 B 0.13X0.92
Nickel 232.0 0.5–20 None Air-C2H2 Nickel 10–100 A 0.20X0.65
Sodium 589.0 0.1–5 None Air-C2H2 B 0.005X1.4
A
Iron 3–10 A 0.98
Prepared from an organometallic standard, mineral oil, and dilution solvent. Sodium 1–20 B 0.12X
A
X = mean concentration, mg/kg.

containing 5 % (m/m) sample. For concentrations less than

20 mg ⁄kg, the analysis for that element is performed on a test
solution that contains 20 % (m/m) sample.
17.2 Standards—If the test solution contains 5 % (m/m) F = dilution factor, volume/volume or mass/mass.
sample, then the corresponding working standards and check
standard must contain 5 % (m/m) oil. Similarly, if the test 22. Report
solution contains 20 % (m/m) sample, the standards must 22.1 Report the following information:
contain 20 % (m/m) oil. A consistent dilution factor is neces- 22.1.1 Report concentrations in mg/kg to two significant
sary so that all aspirated samples and standards will have the figures.
same viscosity. This is essential to obtain consistent uptake 22.1.2 Report which sample preparation method was used:
rates. Procedure A or Procedure B.
17.2.1 Working Standards—Prepare a blank (from mineral
oil) and three additional working standards (from the organo- 23. Precision and Bias5
metallic standards) that cover the ranges of concentration 23.1 Precision—The precision of this test method was
specified in Table 2. determined by statistical analysis on interlaboratory test re-
17.2.2 Check Standard—Using the organometallic sults. For Procedures A and B, six cooperators participated in
standards, mineral oil, and dilution solvent, prepare a check the interlaboratory study. Seven samples (four residual oils and
standard to contain analyte concentrations approximately the three crude oils) comprised the test set. One residual oil was
same as expected in the test solutions. NIST SRM 1618.6 One crude oil was NIST SRM 8505.6
23.1.1 Repeatability—The difference between two test
18. Preparation of Apparatus
results, obtained by the same operator with the same apparatus
18.1 Refer to Section 12. under constant operating conditions on identical test materials
would, in the long run, in the normal and correct operation of
19. Calibration and Analysis the test method, exceed the values in Table 3 and Table 4 only
19.1 Refer to Section 13. in one case in twenty.
23.1.2 Reproducibility—The difference between two single
20. Quality Assurance/Quality Control (QA/QC) and independent results, obtained by different operators work-
20.1 Refer to Section 14. ing in different laboratories on identical test materials, would in
the long run, in the normal and correct operation of the test
21. Calculation method, exceed the values in Table 5 and Table 6 only in one
21.1 For Procedure A, calculate the concentration of each case in twenty.
analyte in the sample using the following equation: 23.2 Bias—Bias was evaluated from results obtained on two
analyte concentration, mg/kg 5 ~ C 3 V 3 F ! /W (1) NIST samples. For Procedure A, the means of the reported
values for V and Ni do not differ from the corresponding
where: expected values by more than the repeatability of the test
C = concentration of the analyte in the test solution (cor- method. For Procedure B, the mean of the reported values for
rected for the concentration determined in the reagent V does not differ from the corresponding expected value by
blank), µg/mL, more than the repeatability of the test method, and the mean of
V = volume of the test solution, mL, the reported values for Ni is higher than the expected value by
F = dilution factor, volume/volume or mass/mass, and an amount approximately equal to twice the repeatability of the
W = sample mass, g. test method. Standard reference materials for Fe and Na are not
21.2 For Procedure B, calculate the concentration of each available, so bias was not determined for these elements.
analyte in the sample using the following equation.
analyte concentration, mg/kg 5 C 3 F (2)
5
Supporting data have been filed at ASTM International Headquarters and may
where: be obtained by requesting Research Report RR:D02-1351. Contact ASTM Customer
C = concentration of the analyte in the test solution, mg/kg, Service at service@astm.org.
6
Available from the National Institute of Standards and Technology,
and
Gaithersburg, MD 20899.

5
 D5863 − 22
TABLE 4 Calculated Repeatability (mg/kg) at Selected TABLE 5 Reproducibility
Concentrations (mg/kg) Concentration
Element Procedure Reproducibility, mg/kgA
Concentration Range, mg/kg
Element Procedure
1 10 50 100 500 Vanadium 50–500 A 0.33X0.90
B 1.2X0.80
Vanadium A ... ... 7.8 11.0 25.0
Nickel 10–100 A 1.3X0.53
B ... ... 4.8 9.0 40.0
B 0.06X1.2
Nickel A ... 0.89 2.5 4.0 ...
Iron 3–10 A 1.45X0.45
B ... 0.13 1.2 3.2 ...
Sodium 1–20 B 0.69X
Iron A ... 0.98 ... ... ...
A
Sodium B 0.12 1.2 ... ... ... X = mean concentration, mg/kg.

24. Keywords
24.1 AAS; atomic absorption spectrometry; iron; nickel;
sodium; vanadium

6
 D5863 − 22
TABLE 6 Calculated Reproducibility (mg/kg) at Selected
Concentrations (mg/kg)
Concentration
Element Procedure
1 10 50 100 500
Vanadium A ... ... 11.0 21.0 89.0
B ... ... 27.0 48.0 170.0
Nickel A ... 4.4 10.0 15.0 ...
B ... 0.95 6.6 15.0 ...
Iron A ... 4.1 ... ... ...
Sodium B 0.69 6.9 ... ... ...

APPENDIXES

(Nonmandatory Information)

X1. GENERIC QUALITY CONTROL STATEMENT FOR D02 TEST METHODS

X1.1 Confirm the performance of the instrument or the test criticality of the quality being measured, the demonstrated
procedure by analyzing a QC sample that is, if possible, stability of the testing process, and customer requirements.
representative of the samples typically analyzed. Generally, a QC sample should be analyzed each testing day
with routine samples. The QC frequency should be increased if
X1.2 Prior to monitoring the measurement process, the user
a large number of samples is routinely analyzed. However,
of the test method needs to determine the average value and
control limits of the QC sample (see Test Method D6299 and when it is demonstrated that the testing is under statistical
ASTM MNL77). control, the QC testing frequency may be reduced. The QC
sample precision should be periodically checked against the
X1.3 Record the QC results and analyze by control charts or ASTM method precision to ensure data quality.
other statistically equivalent techniques to ascertain the statis-
tical control status of the total test process (see Test Method X1.5 It is recommended that, if possible, the type of QC
D6299 and MNL7). Any out-of-control data should trigger sample that is regularly tested be representative of the sample
investigation for root cause(s). The results of this investigation routinely analyzed. An ample supply of QC sample material
may not necessarily result in instrument calibration. should be available for the intended period of use, and must be
homogeneous and stable under the anticipated storage condi-
X1.4 In the absence of explicit requirements given in the
test method, the frequency of QC testing is dependent on the tions.

7
X1.6 Refer to relevant documents (see Test Method D6299
ASTM MNL7, Manual on Presentation of Data Control Chart Analysis,
“Control Chart for Individuals,” 6th Ed, Section 3, ASTM International, W. and ASTM MNL7) for further guidance on QC and control
Conshohocken, PA. charting techniques.

X2. AIDS TO THE ANALYST

X2.1 Employ adequate mixing and sampling procedures for X2.6 Calibrate the instrument each time the flame is ignited.
crude and heavy oils. Use paint mixers for mixing of crude oils.
Heat heavy oils sufficiently to obtain good fluidity, and then X2.7 Monitor deposit formation on the burner head and
shake vigorously. nebulizer. Clean when deposits cause unacceptable absorbance
drift.
X2.2 Use the specified analytical wavelengths because they
have been established by experiment to be optimal and free X2.8 Adjust gas flow rates to minimize carbon deposition
from spectral interferences. on the burner head. Carbon deposition can be particularly
troublesome when nebulizing non-aqueous solutions. The
X2.3 Disassemble and clean the burner on a maintenance burner head can be cleaned with a carbon rod.
schedule that is appropriate for the type of samples analyzed.
X2.9 During analysis, continually observe the appearance
X2.4 Inspect the nebulizer tubing daily for kinks, of the flame to note any change in conditions.
restrictions, or cracks. Replace when necessary.
X2.10 Prevent leakage of acetone from the acetylene cylin-
X2.5 Measure the nebulizer uptake rate daily to check for ders by monitoring cylinder pressure and replacing the cylinder
plugging. Clean when the rate is not normal. when the pressure is less than 75 psig.

7
 D5863 − 22
X2.11 Prior to analysis, check the alignment of the hollow X2.17 For sample decompositions (Procedure A), follow
cathode lamp. good laboratory practices.
X2.12 Clean all apparatus to prevent contamination. X2.17.1 Work in a well-ventilated hood and use adequate
protection as prescribed in the appropriate safety practices.
X2.13 Establish the frequency of preparation of standards
by experiment. X2.17.2 Prevent contamination from the muffle furnace by
covering the sample containers.
X2.14 Matrix match standard and sample solutions as
closely as possible. X2.17.3 Prepare reagent blanks by processing reagents used
in the decomposition through the entire procedure.
X2.15 Prepare and analyze reagent blanks. Correct final
results for blank contributions. X2.17.4 Slowly raise the temperature of oils that are known
to contain significant quantities of water. The intent is to avoid
X2.16 Establish and implement a QC protocol that can aid
spraying oil and acid.
in achieving the required data quality.

SUMMARY OF CHANGES

Subcommittee D02.has identified the location of selected changes to this standard since the last issue
(D5863 – 00a (2016)) that may impact the use of this standard. (Approved Dec. 1, 2022.)

(1) Revised subsection 1.6. (4) Replaced Test Method A and Test Method B with Procedure
(2) Added Terminology D4175 to Section 2. A and Procedure B, respectively, throughout.
(3) Added Section 3 on Terminology.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/