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ASTM D4007-81(1995)e1

(Test Method)

Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)

Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)

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1.1 This test method describes the laboratory determination of water and sediment in crude oils by means of the centrifuge procedure. This centrifuge method for determining water and sediment in crude oils is not entirely satisfactory. The amount of water detected is almost always lower than the actual water content. When a highly accurate value is required, the revised procedures for water by distillation (Test Method D4006 (Note 1)) and sediment by extraction (Test Method D473) must be used.  Note 1-Test Method D4006 has been determined to be the preferred and most accurate method for the determination of water.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see 6.1 and 7.

General Information

Status
Historical
Publication Date
31-Dec-1994
ICS
75.040 - Crude petroleum
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.02 - Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API)
Current Stage
Ref Project

Relations

Replaced By
ASTM D4007-02 - Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)
Effective Date
10-Dec-2002

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ASTM D4007-81(1995)e1 - Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)ASTM D4007-81(1995)e1 - Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)
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ASTM D4007-81(1995)e1 - Standard Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact
ASTM International (www.astm.org) for the latest information.
e1
Designation: D 4007 – 81 (Reapproved 1995) An American National Standard
Designation: Manual of Petroleum Measurement Standards Chapter 10.3 (MPMS)
Designation: IP 359/82
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Water and Sediment in Crude Oil by the Centrifuge Method
(Laboratory Procedure)
This standard is issued under the fixed designation D 4007; 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 (e) indicates an editorial change since the last revision or reapproval.
This test method has been approved by the sponsoring committees and accepted by the Cooperating Societies in accordance with
established procedures. This method was issued as a joint ASTM-API-IP standard in 1981.
e NOTE—Editorial changes were made throughout in September 1995.
1. Scope D 362 Specification for Industrial Grade Toluene
D 473 Test Method for Sediment in Crude Oils and Fuel
1.1 This test method describes the laboratory determination
Oils by the Extraction Method
of water and sediment in crude oils by means of the centrifuge
D 665 Test Method for Rust-Preventing Characteristics of
procedure. This centrifuge method for determining water and
Inhibited Mineral Oil in the Presence of Water
sediment in crude oils is not entirely satisfactory. The amount
D 1796 Test Method for Water and Sediment in Fuel Oils by
of water detected is almost always lower than the actual water
the Centrifuge Method (Laboratory Procedure)
content. When a highly accurate value is required, the revised
D 4006 Test Method for Water in Crude Oil by Distillation
procedures for water by distillation (Test Method D 4006 (Note
D 4057 Practice for Manual Sampling of Petroleum and
1)) and sediment by extraction (Test Method D 473) must be
Petroleum Products
used.
D 4177 Practice for Automatic Sampling of Petroleum and
NOTE 1—Test Method D 4006 has been determined to be the preferred
Petroleum Products
and most accurate method for the determination of water.
2.2 API Standards:
1.2 The values stated in SI units are to be regarded as the
MPMS8 “Sampling Petroleum and Petroleum Products”
standard. The values given in parentheses are for information
2.3 IP Standard:
only.
Specification for Toluole
1.3 This standard does not purport to address all of the
3. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1 Equal volumes of crude oil and water saturated toluene
priate safety and health practices and determine the applica-
are placed into a cone-shaped centrifuge tube. After centrifu-
bility of regulatory limitations prior to use. For specific
gation, the volume of the higher gravity water and sediment
precautionary statements, see 6.1 and 7.
layer at the bottom of the tube is read.
2. Referenced Documents
4. Significance and Use
2.1 ASTM Standards:
4.1 The water and sediment content of crude oil is signifi-
D 95 Test Method for Water in Petroleum Products and
cant because it can cause corrosion of equipment and problems
Bituminous Materials by Distillation
in processing. A determination of water and sediment content is
D 96 Test Methods for Water and Sediment in Crude Oil by
Centrifuge Method (Field Procedure)
Annual Book of ASTM Standards, Vol 06.03.
1 4
This test method is under the jurisdiction of ASTM Committee D-2 on Annual Book of ASTM Standards, Vol 05.02.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Available from the American Petroleum Institute, 1220 L St., N.W., Washing-
D 02.02 on Static Petroleum Measurement. ton, DC 20005.
Current edition approved March 27, 1981. Published May 1981. Available from the Institute of Petroleum, 61 New Cavendish St., London, W.I.,
Annual Book of ASTM Standards, Vol 05.01. England.
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4007
required to measure accurately net volumes of actual oil in
sales, taxation, exchanges, and custody transfers.
5. Apparatus
5.1 Centrifuge:
5.1.1 A centrifuge capable of spinning two or more filled
cone-shaped, 203-mm (8-in.) centrifuge tubes at a speed that
can be controlled to give a relative centrifugal force (rcf) of a
minimum of 600 at the tip of the tubes shall be used.
5.1.2 The revolving head, trunnion rings, and trunnion cups,
including the cushions, shall be soundly constructed to with-
stand the maximum centrifugal force capable of being deliv-
ered by the power source. The trunnion cups and cushions shall
firmly support the tubes when the centrifuge is in motion. The
centrifuge shall be enclosed by a metal shield or case strong
enough to eliminate danger if any breakage occurs.
5.1.3 The centrifuge shall be heated and should be con-
trolled thermostatically to avoid unsafe conditions. It should be
capable of maintaining the sample temperature during the
entire run at 60 6 3°C (140 6 5°F).
5.1.4 Electric powered and heated centrifuges must meet all
safety requirements for use in hazardous areas.
5.1.5 Calculate the speed of the rotating head in revolutions
per minute (r/min) as follows:
r/min 5 1335 =rcf/d (1)
where:
rcf 5 relative centrifugal force and
d 5 diameter of swing measured between tips of opposite
tubes when in rotating position, mm, or
FIG. 1 Eight-Inch (203-mm) Centrifuge Tube
rpm 5 265 =rcf/d (2)
TABLE 1 Centrifuge Tube Calibration Tolerances for 8-in. (203-
mm) Tube
where:
rcf 5 relative centrifugal force and
Range, mm Subdivision, mm Volume Tolerance, mm
d 5 diameter of swing measured between tips of opposite
0 to 0.1 0.05 60.02
tubes when in rotating position, in. Above 0.1 to 0.3 0.05 60.03
Above 0.3 to 0.5 0.05 60.05
5.2 Centrifuge Tubes—Each centrifuge tube shall be a
Above 0.5 to 1.0 0.10 60.05
203-mm (8-in.) cone-shaped tube, conforming to dimensions
Above 1.0 to 2.0 0.10 60.10
given in Fig. 1 and made of thoroughly annealed glass. The Above 2.0 to 3.0 0.20 60.10
Above 3.0 to 5.0 0.5 60.20
graduations, numbered as shown in Fig. 1, shall be clear and
Above 5.0 to 10 1.0 60.50
distinct, and the mouth shall be constricted in shape for closure
Above 10 to 25 5.0 61.00
Above 25 to 100 25.0 61.00
with a cork. Scale error tolerances and the smallest graduations
between various calibration marks are given in Table 1 and
apply to calibrations made with air-free water at 20°C (68°F),
Molecular weight 92.14
when reading the bottom of the shaded meniscus.
Color (APHA) 10
A
5.3 Bath—The bath shall be either a solid metal block bath Boiling range (initial to dry point) 2.0°C (36°F)
Residue after evaporation 0.001 %
or a liquid bath of sufficient depth for immersing the centrifuge
Substances darkened by H SO passes ACS test
2 4
tube in the vertical position to the 100-mL mark. Means shall
Sulfur compounds (as S) 0.003 %
be provided for maintaining the temperature at 60 6 3°C (140 _______
A
6 5°F).
Recorded boiling point 110.6°C
6.1.2 The solvent shall be water-saturated at 60 6 3°C (140
NOTE 2—By contractual agreement 49 6 3°C (120 6 5°F) may be
6 5°F) (see Note 2) but shall be free of suspended water. See
used.
Annex A1 for the solvent-water saturation procedure.
6. Solvent 6.2 Demulsifier—A demulsifier should be used to promote
the separation of water from the sample and to prevent its
6.1 Toluene (Warning—See Note 3.) conforming to
clinging to the walls of the centrifuge tube. The recommended
Specification D 362 or to the IP Specification for Toluole.
stock solution is 25 % demulsifier to 75 % toluene. For some
NOTE 3—Warning: Flammable.
crude oils a different ratio of demulsifier to toluene may be
6.1.1 Typical characteristics for this material are required. Demulsifiers used in the concentration and quantity
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4007
recommended will not add to the water and sediment volume 8.6 Repeat this operation until the combined volume of
determined. The solution must be stored in a dark bottle that is water and sediment remains constant for two consecutive
tightly closed. readings. In general, not more than two spinnings are required.
8.7 The temperature of the sample during the entire
7. Sampling
centrifuging procedure should be maintained at 60 6 3°C (140
7.1 Sampling is defined as all steps required to obtain an
6 5°F) (see Note 2).
aliquot of the contents of any pipe, tank, or other system and to 8.8 To avoid the danger of tubes breaking in the cups, care
place the sample into the laboratory test container.
must be taken that the tubes are bedded onto the bottom
7.2 Only representative samples obtained as specified in the cushion so that no part of the tube is in contact with the rim of
API MPMS, Chapter 8 (or Practice D 4057 and Practice
the cup.
D 4177), shall be used for this test method.
9. Calculation
8. Procedure 9.1 Record the final volume of water and sediment in each
tube. If the difference between the two readings is greater than
8.1 Fill each of two centrifuge tubes (5.2) to the 50-mL
one subdivision on the centrifuge tube (see Table 1) or 0.025
mark with sample directly from the sample container. Then,
mL for readings of 0.10 mL and below, the readings are
with a pipet, add 50 mL of toluene, which has been water
inadmissible and the determination shall be repeated.
saturated at 60°C (140°F) or 49°C (120°F) (see Note 2). Read
9.2 Express the sum of the two admissible readings as the
the top of the meniscus at both the 50 and 100-mL marks. Add
percent by volume of water and sediment; report the results as
0.2 mL of demulsifier solution (6.2) to each tube, using a
shown in Table 2.
0.2-mL pipet. An automatic pipettor may be used. Stopper the
tube tightly and invert the tubes ten times to ensure that the oil
10. Precision
and solvent are uniformly mixed.
10.1 The precision of this method, as obtained by statistical
8.2 In the case where the crude oil is very viscous and
examination of interlaboratory test results in the range from
mixing of the solvent with the oil would be difficult, the solvent
0.01 to 1.0 %, is described in 10.1.1 and 10.1.2.
may be added to the centrifuge tube first to facilitate mixing.
10.1.1 Repeatability—The difference between successive
Care must be taken in order not to fill the centrifuge tube past
test results, obtained by the same operator with the same
the 100-mL mark with the sample.
apparatus under constant operating conditions on identical test
8.3 Loosen the stoppers slightly and immerse the tubes to
material, would, in the long run, in the normal and correct
the 100-mL mark for at least 15 min in the bath maintained at
operation of the test method, exceed the following value in
60 6 3°C (140 6 5°F) (see Note 2). Secure the stoppers and
only one case in twenty:
again invert the tubes ten times to ensure uniform mixing of oil
From 0.0 % to 0.3 % water, see Fig. 3.
and solvent. The vapor pressure at 60°C (140°F) is
From 0.3 % to 1.0 % water, repeatability is constant at 0.12.
approximately double that at 40°C (104°F).
10.1.2 Reproducibility—The difference between two single
8.4 Place the tubes in the trunnion cups on opposite sides of
and independent test results obtained by different operators
the centrifuge to establish a balanced condition. Retighten the
working in different laboratories on identical test material,
corks and spin for 10 min at a minimum relative centrifugal
would, in the long run, in the normal and correct operation of
force of 600 calculated from the equation given in 5.1.5.
the test method, exceed the following value in only one case in
8.5 Immediately after the centrifuge comes to rest following
twenty:
the spin, read and record the combined volume of water and
From 0.0 % to 0.3 % water, see Fig. 3.
sediment at the bottom of each tube to the nearest 0.05 mL
From 0.3 % to 1.0 % water, reproducibility is constant at 0.28.
from 0.1 to 1-mL graduations and to the nearest 0.1-mL above
11. Keywords
1-mL graduations. Below 0.1 mL, estimate to the nearest 0.025
mL (refer to Fig. 2). Return the tubes without agitation to the 11.1 centrifuge; centrifuge tube; crude oil; laboratory
centrifuge and spin for another 10 min at the same rate. procedure; sampling; sediment and water; solvent
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4007
FIG. 2 Procedure for Reading Water and Sediment When Using an ASTM 100-mm Cone-Shaped Centrifuge Tube
A
TABLE 2 Expression of Results, mm
Total Percent Water and
Tube 1 Tube 2
Sediment
No visible water and No visible water and —
sediment sediment
No visible water and 0.025 0.025
sediment
0.025 0.025 0.05
0.025 0.05 0.075
0.05 0.05 0.10
0.05 0.075 0.125
0.075 0.075 0.15
0.075 0.10 0.175
0.10 0.10 0.20
0.10 0.15 0.25
A
For volumetric tolerances, see Table 1.
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4007
FIG. 3 Basic Sediment and Water Precision
ANNEXES
(Mandatory Information)
A1. PROCEDURE TO WATER-SATURATE TOLUENE
A1.1 Scope significant extent. The percent of water that will dissolve
increases as the temperature is increased from about 0.03 % at
A1.1.1 This method is satisfactory for the water saturation
21°C (70°F) to about 0.17 % at 70°C (158°F). Toluene, as
of toluene to be used for determination of water and sediment
normally supplied, is relatively dry and if used in an as-
in crude oils by the centrifuge method.
received condition, will dissolve a portion of or even all of any
A1.2 Significance
water present in a crude oil sample. This would reduce the
A1.2.1 Fig. A1.1 shows that water is soluble in toluene to a
FIG. A1.1 Solubility of Water in Toluene
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4007
apparent sediment and water level in the crude sample. To A1.5.3 Loosen the cap and place the bottle in the bath for 30
determin
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ASTM
ASTM D7691-23(Test Method)
Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

SIGNIFICANCE AND USE
5.1 Most often determined trace elements in crude oils are nickel and vanadium, which are usually the most abundant; however, as many as 45 elements in crude oils have been reported. Knowledge of trace elements in crude oil is important because they can have an adverse effect on petroleum refining and product quality. These effects can include catalyst poisoning in the refinery and excessive atmospheric emission in combustion of fuels. Trace element concentrations are also useful in correlating production from different wells and horizons in a field. Elements such as iron, arsenic, and lead are catalyst poisons. Vanadium compounds can cause refractory damage in furnaces, and sodium compounds have been found to cause superficial fusion on fire brick. Some organometallic compounds are volatile which can lead to the contamination of distillate fractions, and a reduction in their stability or malfunctions of equipment when they are combusted.  
5.2 The value of crude oil can be determined, in part, by the concentrations of nickel, vanadium, and iron.  
5.3 Inductively coupled plasma-atomic emission spectrometry (ICP-AES) is a widely used technique in the oil industry. Its advantages over traditional atomic absorption spectrometry (AAS) include greater sensitivity, freedom from molecular interferences, wide dynamic range, and multi-element capability. See Practice D7260.
SCOPE
1.1 This test method covers the determination of several elements (including iron, nickel, sulfur, and vanadium) occurring in crude oils.  
1.2 For analysis of any element using wavelengths below 190 nm, a vacuum or inert gas optical path is required.  
1.3 Analysis for elements such as arsenic, selenium, or sulfur in whole crude oil may be difficult by this test method due to the presence of their volatile compounds of these elements in crude oil; but this test method should work for resid samples.  
1.4 Because of the particulates present in crude oil samples, if they do not dissolve in the organic solvents used or if they do not get aspirated in the nebulizer, low elemental values may result, particularly for iron and sodium. This can also occur if the elements are associated with water which can drop out of the solution when diluted with solvent.  
1.4.1 An alternative in such cases is using Test Method D5708, Procedure B, which involves wet decomposition of the oil sample and measurement by ICP-AES for nickel, vanadium, and iron, or Test Method D5863, Procedure A, which also uses wet acid decomposition and determines vanadium, nickel, iron, and sodium using atomic absorption spectrometry.  
1.4.2 From ASTM Interlaboratory Crosscheck Programs (ILCP) on crude oils data available so far, it is not clear that organic solvent dilution techniques would necessarily give lower results than those obtained using acid decomposition techniques.2  
1.4.3 It is also possible that, particularly in the case of silicon, low results may be obtained irrespective of whether organic dilution or acid decomposition is utilized. Silicones are present as oil field additives and can be lost in ashing. Silicates should be retained but unless hydrofluoric acid or alkali fusion is used for sample dissolution, they may not be accounted for.  
1.5 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent and low results may be obtained for particles larger than a few micrometers.  
1.6 The precision in Section 18 defines the concentration ranges covered in the interlaboratory study. However, lower and particularly higher concentrations can be determined by this test method. The low concentration limits are dependent on the sensitivity of the ICP instrument and the dilution factor used. The high concentration limits are determined by the product of the maximum concentration defined by the calibration curve and the sample di...

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ASTM
ASTM D7157-23(Test Method)
Standard Test Method for Determination of Intrinsic Stability of Asphaltene-Containing Residues, Heavy Fuel Oils, and Crude Oils (n-Heptane Phase Separation; Optical Detection)

SIGNIFICANCE AND USE
5.1 This test method describes a sensitive method for estimating the intrinsic stability of an oil. The intrinsic stability is expressed as S-value. An oil with a low S-value is likely to undergo flocculation of asphaltenes when stressed (for example, extended heated storage) or blended with a range of other oils. Two oils each with a high S-value are likely to maintain asphaltenes in a peptized state and not lead to asphaltene flocculation when blended together.  
5.2 This test method can be used by petroleum refiners to control and optimize the refinery processes and by blenders and marketers to assess the intrinsic stability of blended asphaltene-containing heavy fuel oils.
SCOPE
1.1 This test method covers procedures for quantifying the intrinsic stability of the asphaltenes in an oil by automatic instruments using optical detection.  
1.2 This test method is applicable to residual products from thermal and hydrocracking processes, to products typical of Specifications D396 Grades No. 5L, 5H, and 6, and D2880 Grades No. 3-GT and 4-GT, and to crude oils, providing these products contain 0.5 % by mass or greater concentration of asphaltenes (see Test Method D6560).  
1.3 This test method quantifies asphaltene stability in terms of state of peptization of the asphaltenes (S-value), intrinsic stability of the oily medium (So) and the solvency requirements of the peptized asphaltenes (Sa).  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

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ASTM
ASTM D8045-17(2023)(Test Method)
Standard Test Method for Acid Number of Crude Oils and Petroleum Products by Catalytic Thermometric Titration

SIGNIFICANCE AND USE
5.1 Crude oils and oil sands bitumen contain naturally occurring acidic species. Acidity of crude oil has been implicated in corrosion of distribution and process systems. The relative amount of these materials can be determined by titrating with bases. The acid number is a measure of this amount of acidic substance in the oil under the conditions of the test.  
5.2 Acid number of crude and distilled petroleum fractions has been measured by Test Method D664. Test Method D664 was developed for the analysis of lubricants and biodiesel. The titration solvent used in Test Method D664 does not properly address dissolving difficult samples such as crude oil, bitumen, and high wax samples addressed in this test method. Refer to Appendix X1.  
5.3 Test Method D974 is also not applicable to measuring acidity of crudes and highly colored samples because the indicator is not visible or it is difficult to discern a color change to detect the end point of the titration.
SCOPE
1.1 This test method covers the determination of acidic components in crude oil and petroleum products including waxes, bitumen, base stocks, and asphalts that are soluble in mixtures of xylenes and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. The values obtained by this test method may not be numerically equivalent to other acid value measurements. The range of KOH acid numbers included in the precision statement is 0.1 mg/g to 16 mg/g.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Some specific hazards statements are given in Section 7 on Safety Precautions.  
1.4 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.

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ASTM
ASTM D5863-22(Test Method)
Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry

SIGNIFICANCE AND USE
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 catalysts during processing. These test methods provide a means of quantitatively determining the concentrations of vanadium, nickel, iron, and sodium. Thus, these test methods can be used to aid in determining the quality and value of the crude oil and residual oil.
SCOPE
1.1 These test methods cover the determination of nickel, vanadium, iron, and sodium in crude oils and residual fuels by flame atomic absorption spectrometry (AAS). Two different test methods are presented.  
1.2 Procedure A, Sections 8–14—Flame AAS is used to analyze a sample that is decomposed with acid for the determination of total Ni, V, and Fe.  
1.3 Procedure B, Sections 15–20—Flame AAS is used to analyze a sample diluted with an organic solvent for the determination of Ni, V, and Na. This test method uses oil-soluble metals for calibration to determine dissolved metals and does not purport to quantitatively determine nor detect insoluble particulates. Hence, this test method may underestimate the metal content, especially sodium, present as inorganic sodium salts.  
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in Note 1.  
1.5 For each element, each test method has its own unique precision. The user can select the appropriate test method based on the precision required for the specific analysis.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard, unless specifically stated. Other units that appear in this standard are included for information purposes only or because they are in embedded pictures that cannot be edited.  
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 8.1, 9.2, 9.5, 11.2, 11.4, and 16.1.  
1.8 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.

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ASTM
ASTM D4310-22a(Test Method)
Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils

SIGNIFICANCE AND USE
5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.  
5.2 Significant formation of oil insolubles or metal corrosion products, or both, during this test may indicate that the oil will form insolubles or corrode metals, or both, during field service. However, no correlation with field service has been established.
SCOPE
1.1 This test method covers and is used to evaluate the tendency of inhibited mineral oil based steam turbine lubricants and mineral oil based anti-wear hydraulic oils to corrode copper catalyst metal and to form sludge during oxidation in the presence of oxygen, water, and copper and iron metals at an elevated temperature. The test method is also used for testing circulating oils having a specific gravity less than that of water and containing rust and oxidation inhibitors.  
Note 1: During round robin testing copper and iron in the oil, water and sludge phases were measured. However, the values for the total iron were found to be so low (that is, below 0.8 mg), that statistical analysis was inappropriate. The results of the cooperative test program are available (see Section 16).  
1.2 This test method is a modification of Test Method D943 where the oxidation stability of the same kinds of oils is determined by following the acid number of oil. The number of test hours required for the oil to reach an acid number of 2.0 mg KOH/g is the oxidation lifetime.  
1.3 Procedure A of this test method requires the determination and report of the weight of the sludge and the total amount of copper in the oil, water, and sludge phases. Procedure B requires the sludge determination only. The acid number determination is optional for both procedures.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Section 7 and X1.1.5.  
1.7 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.

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ASTM
ASTM D8003-22(Test Method)
Standard Test Method for Determination of Light Hydrocarbons and Cut Point Intervals in Live Crude Oils and Condensates by Gas Chromatography

SIGNIFICANCE AND USE
5.1 This test method determines methane (nC1) to hexane (nC6), cut point carbon fraction intervals to nC24 and recovery (nC24+) of live crude oils and condensates without depressurizing, thereby avoiding the loss of highly volatile components and maintaining sample integrity. This test method provides a highly resolved light end profile which can aid in determining and improving appropriate safety measures and product custody transport procedures. Decisions in regards to marketing, scheduling, and processing of crude oils may rely on light end compositional results.  
5.2 Equation of state calculations can be applied to variables provided by this method to allow for additional sample characterization.
SCOPE
1.1 This test method covers the determination of light hydrocarbons and cut point intervals by gas chromatography in live crude oils and condensates with VPCR4 (see Note 1) up to 500 kPa at 37.8 °C.
Note 1: As described in Test Method D6377.  
1.2 Methane (C1) to hexane (nC6) and benzene are speciated and quantitated. Samples containing mass fractions of up to 0.5 % methane, 2.0 % ethane, 10 % propane, or 15 % isobutane may be analyzed. A mass fraction with a lower limit of 0.001 % exists for these compounds.  
1.3 This test method may be used for the determination of cut point carbon fraction intervals (see 3.2.1) of live crude oils and condensates from initial boiling point (IBP) to 391 °C (nC24). The nC24 plus fraction is reported.  
1.4 Dead oils or condensates sampled in accordance with 12.1 may also be analyzed.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5.1 Exception—Where there is no direct SI equivalent such as tubing size.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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.

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