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ASTM D4928-00e1

(Test Method)

Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer Titration

Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer Titration

SCOPE
1.1 This test method covers the determination of water in the range from 0.02 to 5 mass or volume % in crude oils. Mercaptan (RSH) and sulfide (S- or H2S) as sulfur are known to interfere with this test method, but at levels of less than 500 μg/g (ppm), the interference from these compounds is insignificant (see Section 5).
1.2 This test method can be used to determine water in the 0.005 to 0.02 mass % range, but the effects of the mercaptan and sulfide interference at these levels has not been determined.
1.3 This test method is intended for use with standard commercially available coulometric Karl Fischer reagent.
1.4 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 hazard statements, see Section 7.

General Information

Status
Historical
Publication Date
09-Sep-2000
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

Replaces
ASTM D4928-00 - Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer Titration
Effective Date
10-Sep-2000
Replaced By
ASTM D4928-00(2005) - Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer Titration
Effective Date
01-Jun-2005
Referred By
ASTM D482-19 - Standard Test Method for Ash from Petroleum Products
Effective Date
10-Sep-2000
Referred By
ASTM E203-23 - Standard Test Method for Water Using Volumetric Karl Fischer Titration
Effective Date
10-Sep-2000
Referred By
ASTM D4177-22e1 - Standard Practice for Automatic Sampling of Petroleum and Petroleum Products
Effective Date
10-Sep-2000
Referred By
ASTM D7829-13(2018) - Standard Guide for Sediment and Water Determination in Crude Oil
Effective Date
10-Sep-2000
Referred By
ASTM D6470-99(2020) - Standard Test Method for Salt in Crude Oils (Potentiometric Method)
Effective Date
10-Sep-2000
Referred By
ASTM D7720-21 - Standard Guide for Statistically Evaluating Measurand Alarm Limits when Using Oil Analysis to Monitor Equipment and Oil for Fitness and Contamination
Effective Date
10-Sep-2000
Referred By
ASTM D7059-21 - Standard Test Method for Determination of Methanol in Crude Oils by Multidimensional Gas Chromatography
Effective Date
10-Sep-2000
Referred By
ASTM D3230-19 - Standard Test Method for Salts in Crude Oil (Electrometric Method)
Effective Date
10-Sep-2000

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ASTM D4928-00e1 - Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer TitrationASTM D4928-00e1 - Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer Titration
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ASTM D4928-00e1 - Standard Test Methods for Water in Crude Oils by Coulometric Karl Fischer Titration
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Standards Content (Sample)

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
An American National Standard
e1
Designation:D4928–00
Designation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.9
Designation: 386/99
Standard Test Methods for
1
Water in Crude Oils by Coulometric Karl Fischer Titration
This standard is issued under the fixed designation D4928; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1
e NOTE—Footnote 1 and the Referenced Documents were corrected editorially to comply with theASTM-API joint standard
contract in October 2002.
1. Scope D5854 Practice for Mixing and Handling Liquid Samples
ofPetroleumandPetroleumProducts(API MPMSChapter
1.1 This test method covers the determination of water in
4
8.3)
the range from 0.02 to 5 mass or volume % in crude oils.
5
−
E203 Test Method for Water Using Karl Fischer Titration
Mercaptan (RSH) and sulfide (S or H S) as sulfur are known
2
6
2.2 API Standards:
to interfere with this test method, but at levels of less than 500
MPMS Chapter 8.1 Manual Sampling of Petroleum and
µg/g (ppm), the interference from these compounds is insig-
Petroleum Products (ASTM Practice D4057)
nificant (see Section 5).
MPMS Chapter 8.2 Automatic Sampling of Petroleum and
1.2 This test method can be used to determine water in the
Petroleum Products (ASTM Practice D4177)
0.005 to 0.02 mass % range, but the effects of the mercaptan
MPMSChapter8.3 MixingandHandlingLiquidSamplesof
and sulfide interference at these levels has not been deter-
Petroleum and Petroleum Products (ASTM Practice
mined.
D5854)
1.3 This test method is intended for use with standard
commercially available coulometric Karl Fischer reagent.
3. Summary of Test Method
1.4 This standard does not purport to address all of the
3.1 After homogenizing the crude oil with a mixer, an
safety concerns, if any, associated with its use. It is the
aliquot is injected into the titration vessel of a Karl Fischer
responsibility of the user of this standard to establish appro-
apparatus in which iodine for the Karl Fischer reaction is
priate safety and health practices and determine the applica-
generatedcoulometricallyattheanode.Whenallthewaterhas
bility of regulatory limitations prior to use. For specific hazard
been titrated, excess iodine is detected by an electrometric
statements, see Section 7.
end-point detector and the titration is terminated. Based on the
2. Referenced Documents stoichiometry of the reaction, one mole of iodine reacts with
one mole of water, thus the quantity of water is proportional to
2.1 ASTM Standards:
2
the total integrated current according to Faraday’s Law.
D1193 Specification for Reagent Water
3.2 The precision of this test method is critically dependent
D4057 Practice for Manual Sampling of Petroleum and
3
ontheeffectivenessofthehomogenizationstep.Theefficiency
Petroleum Products (API MPMS Chapter 8.1)
of the mixer used to achieve a homogeneous sample is
D4177 Practice for Automatic Sampling of Petroleum and
3
determined by the procedure given in Practice D5854 (API
Petroleum Products (API MPMS Chapter 8.2)
MPMS Chapter 8.3).
3.3 Two procedures are provided for the determination of
water in crude oils. In one procedure, a weighed aliquot of
1
This test method is under the jurisdiction of ASTM Committee D02 on
sample is injected into the titration vessel and the mass % of
Petroleum Products and Lubricants and theAPI Committee on Petroleum Measure-
ment, and is the direct responsibility of Subcommittee D02.02 /COMQ, the joint
ASTM-API Committee on Static Petroleum Measurement.
4
Current edition approved Sept. 10, 2000. Published October 2000. Originally Annual Book of ASTM Standards, Vol 05.03.
5
published as D4928–89. Last previous edition D4928–96. Annual Book of ASTM Standards, Vol 15.05.
2 6
Annual Book of ASTM Standards, Vol 11.01. Published as Manual of Petroleum Standards. Available from the American
3
Annual Book of ASTM Standards, Vol 05.02. Petroleum Institute (API), 1220 L St., NW, Washington, DC 20005.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
e1
D4928–00
water is determined. The other procedure provides for the 6.3.1.2 Syringes, 250 µL, 500 µL, and 1000 µL (1 mL), for
direct determination of the volume % of water in the crude oil crudeoilsamples.Forthevolumetricdeterminationprocedure,
bymeasuringthevolumeofcrudeoilinjectedintothetitration thesyringesshouldbeaccurateto5µL,10µL,and20µL(0.02
vessel. mL), respectively.
7. Reagents and
...

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Note 1: Defined as having a Reid vapor pressure less than 82.7 kPa (12 psi).  
1.2 This test method details procedures for the production of a liquefied gas, distillate fractions, and residuum of standardized quality on which analytical data can be obtained, and the determination of yields of the above fractions by both mass and volume. From the preceding information, a graph of temperature versus mass % distilled can be produced. This distillation curve corresponds to a laboratory technique, which is defined at 15/5 (15 theoretical plate column, 5:1 reflux ratio) or TBP (true boiling point).  
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4.1 Theoretically, all of the sediment and water determination methods are valid for crude oils containing from 0 % to 100 % by volume sediment and water; the range of application is specified within the scope of each method. The round robins for all methods were conducted on relatively dry oil. All precision and bias statements included in the methods are based upon the round robin data. Analysis becomes more challenging with crude oils containing higher water contents due to the difficulty in obtaining a representative sample, and maintaining the sample quality until analysis begins.  
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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.  
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Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry

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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.
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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.  
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1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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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 D4929-22(Test Method)
Standard Test Method for Determination of Organic Chloride Content in Crude Oil

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits at  
5.1.2.1 To ensure Eq 3).  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on the refining operations as the organic chlorides.  
5.3 Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly when transfer of custody is involved.
SCOPE
1.1 The procedures in this test method cover the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using either distillation and sodium biphenyl reduction, distillation and microcoulometry, or distillation and X-ray fluorescence (XRF) spectrometry.  
1.2 The procedures in this test method involve the distillation of crude oil test specimens to obtain a naphtha fraction prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 6 regarding potential interferences.  
1.3 Procedure A covers the determination of organic chloride in the washed naphtha fraction of crude oil by sodium biphenyl reduction followed by potentiometric titration.  
1.4 Procedure B covers the determination of organic chloride in the washed naphtha fraction of crude oil by oxidative combustion followed by microcoulometric titration.  
1.5 Procedure C covers the determination of organic chloride in the washed naphtha fraction of crude oil by X-ray fluorescence spectrometry.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are micrograms of chloride per gram of sample, though milligrams of chloride per kilogram of sample is commonly used for Procedure C.  
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.  
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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