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ASTM D7578-10e1

(Guide)

Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants

Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants

SIGNIFICANCE AND USE
Crude oil, petroleum, petroleum products, additives, biofuels, and lubricants are routinely analyzed for their elemental content such as chlorine, nitrogen, hydrogen, phosphorus, sulfur, and various metals using a variety of analytical techniques. Some of these methods require little to no method calibration; some others require only simple one step calibration; while others require elaborate calibration routine before the product is analyzed for its elemental content.  
Fairly often it can be shown that the round robin results by a co-operator are all biased with respect to those from other laboratories. Presumably, the failure to follow good laboratory practices and instructions in the test methods can be a causal factor of such errors. A further consequence is an unnecessarily large reproducibility estimate or the data being dropped from the study as an outlier.
Another cause of such discrepancies could be different or inadequate calibration practice used in the laboratory. Most test methods spell out the calibration requirements but often do not quote the frequency required letting the laboratories use good laboratory practices for this task. Thus, uniform practice for instrument calibration would be beneficial in standardizing the test procedures and obtaining consistent results across the laboratories.
Committee D02 has already issued standard practices for uniform sample preparation (D7455), standard operating procedures for ICP-AES (D7260) and XRF (D7343) as well as standard quality assurance protocol (D6792). This guide should be considered as a continuing effort on behalf of this subcommittee to achieve standardized practices in all parts of an analytical sequence.
SCOPE
1.1 This guide covers different ways by which the test methods used for elemental analysis of petroleum product and lubricant samples are calibrated before the sample analysis.
1.2 Uniform practice for test method calibration is beneficial in standardizing the procedures, and obtaining consistent results across different laboratories.
1.3 This guide includes only the basic steps for generally encountered instrument types. Anything out of the ordinary may require special procedures. See individual test methods for instructions to handle such situations.
1.4 This guide is not a substitute for a thorough understanding of the actual test method to be used, caveats it contains, and additional instrument preparation that may be required.
1.5 The user should not expand the scope of the test methods to materials or concentrations outside the scope of the test methods being used.  
1.6 This guide should also be applicable to sample preparation of non-petroleum based bio-fuels for elemental analysis. Work is underway on these aspects in Subcommittee D02.03. As more information becomes available, it will be added to this standard.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 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.

General Information

Status
Historical
Publication Date
14-Feb-2010
ICS
75.080 - Petroleum products in general
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D7578-10 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
15-Feb-2010
Replaced By
ASTM D7578-15 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-Jun-2015
Referred By
ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
15-Feb-2010
Referred By
ASTM D8188-23 - Standard Test Method for Determination of Density and Relative Density of Asphalt, Semi-Solid Bituminous Materials, and Soft-Tar Pitch by Use of a Digital Density Meter (U-Tube)
Effective Date
15-Feb-2010
Referred By
ASTM D7961-22 - Standard Practice for Calibrating U-tube Density Cells over Large Ranges of Temperature and Pressure
Effective Date
15-Feb-2010

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ASTM D7578-10e1 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and LubricantsASTM D7578-10e1 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
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ASTM D7578-10e1 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
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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
´1
Designation: D7578 − 10
StandardGuide for
Calibration Requirements for Elemental Analysis of
1
Petroleum Products and Lubricants
This standard is issued under the fixed designation D7578; 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
´ NOTE—Updated Table 8 to correct Referenced Document editorially in August 2011.
1. Scope 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This guide covers different ways by which the test
D129 Test Method for Sulfur in Petroleum Products (Gen-
methods used for elemental analysis of petroleum product and
eral High Pressure Decomposition Device Method)
lubricant samples are calibrated before the sample analysis.
D445 Test Method for Kinematic Viscosity of Transparent
1.2 Uniform practice for test method calibration is benefi-
and Opaque Liquids (and Calculation of Dynamic Viscos-
cial in standardizing the procedures, and obtaining consistent
ity)
results across different laboratories.
D482 Test Method for Ash from Petroleum Products
D808 Test Method for Chlorine in New and Used Petroleum
1.3 This guide includes only the basic steps for generally
Products (High Pressure Decomposition Device Method)
encountered instrument types. Anything out of the ordinary
D874 Test Method for Sulfated Ash from Lubricating Oils
mayrequirespecialprocedures.Seeindividualtestmethodsfor
and Additives
instructions to handle such situations.
D892 Test Method for Foaming Characteristics of Lubricat-
1.4 This guide is not a substitute for a thorough understand- ing Oils
ingoftheactualtestmethodtobeused,caveatsitcontains,and D1018 Test Method for Hydrogen In Petroleum Fractions
D1091 Test Methods for Phosphorus in Lubricating Oils and
additional instrument preparation that may be required.
Additives
1.5 The user should not expand the scope of the test
D1266 Test Method for Sulfur in Petroleum Products (Lamp
methods to materials or concentrations outside the scope of the
Method)
test methods being used.
D1318 Test Method for Sodium in Residual Fuel Oil (Flame
Photometric Method)
1.6 This guide should also be applicable to sample prepa-
1
D1548 Test Method for Vanadium in Heavy Fuel Oil
ration of non-petroleum based bio-fuels for elemental analysis.
3
(Withdrawn 1997)
Work is underway on these aspects in Subcommittee D02.03.
D1552 Test Method for Sulfur in Petroleum Products (High-
Asmoreinformationbecomesavailable,itwillbeaddedtothis
Temperature Method)
standard.
D1839 Test Method for Amyl Nitrate in Diesel Fuels
1.7 The values stated in SI units are to be regarded as
D2622 Test Method for Sulfur in Petroleum Products by
standard. No other units of measurement are included in this
Wavelength Dispersive X-ray Fluorescence Spectrometry
standard.
D2784 Test Method for Sulfur in Liquefied Petroleum Gases
(Oxy-Hydrogen Burner or Lamp)
1.8 This standard does not purport to address all of the
D3120 Test Method for Trace Quantities of Sulfur in Light
safety concerns, if any, associated with its use. It is the
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
responsibility of the user of this standard to establish appro-
lometry
priate safety and health practices and determine the applica-
D3228 Test Method for Total Nitrogen in Lubricating Oils
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on Standards volume information, refer to the standard’s Document Summary page on
Elemental Analysis. the ASTM website.
3
Current edition approved Feb. 15, 2010. Published March 2010. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D7578-10. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
´1
D7578 − 10
and Fuel Oils by Modified Kjeldahl Method D5291 Test Methods for Instrumental Determination of
D3230 Test Method for Salts in Crude Oil (Electrometric Carbon, Hydrogen, and Nitrogen in Petroleum Products
Method) and Lubricants
D5384 Test Methods for Chlorine in Used Petroleum Prod-
D3231 Test Method for Phosphorus in Gasoline
ucts (Field Test Kit Method)
D3237 TestMethodforLeadinGasolinebyAtomicAbsorp-
D5453 Test Method for Determination of Total Sulfur in
tion Spectroscopy
Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel
D3246 Tes
...

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SIGNIFICANCE AND USE
5.1 The bromine number is useful as a measure of aliphatic unsaturation in petroleum samples. When used in conjunction with the calculation procedure described in Annex A2, it can be used to estimate the percentage of olefins in petroleum distillates boiling up to approximately 315 °C (600 °F).  
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Note 1: These limits are imposed since the precision of this test method has been determined only up to or within the range of these bromine numbers.  
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1.3 For petroleum hydrocarbon mixtures of bromine number less than 1.0, a more precise measure for bromine-reactive constituents can be obtained by using Test Method D2710. If the bromine number is less than 0.5, then Test Method D2710 or the comparable bromine index methods for industrial aromatic hydrocarbons, Test Methods D1492 or D5776 must be used in accordance with their respective scopes. The practice of using a factor of 1000 to convert bromine number to bromine index is not applicable for these lower values of bromine number.  
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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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4.1 A petroleum products, liquid fuels, and lubricants testing laboratory plays a crucial role in product quality management and customer satisfaction. It is essential for a laboratory to provide quality data. This document provides guidance for establishing and maintaining a quality management system in a laboratory.  
4.1.1 The word ‘customer’ can refer to both customers internal and external to the laboratory or organization.
SCOPE
1.1 This practice covers the establishment and maintenance of the essentials of a quality management system in laboratories engaged in the analysis of petroleum products, liquid fuels, and lubricants. It is designed to be used in conjunction with Practice D6299.
Note 1: This practice is based on the quality management concepts and principles advocated in ANSI/ISO/ASQ Q9000 standards, ISO/IEC 17025, ASQ Manual,2 and ASTM standards such as D3244, D4182, D4621, D6299, D6300, D7372, E29, E177, E456, E548, E882, E994, E1301, E1323, STP 15D,3 and STP 1209.4  
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5.1 The solvent extractables in a wax may have significant effects on several of its properties such as strength, hardness, flexibility, scuff resistance, coefficient of friction, coefficient of expansion, melting point, and staining characteristics. Whether these effects are desirable or undesirable depends on the intended use of the wax.
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1.1 This test method covers the determination of solvent extractables in petroleum waxes.  
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ASTM D7873-22a(Test Method)
Standard Test Method for Determination of Oxidation Stability and Insolubles Formation of Inhibited Turbine Oils at 120 °C Without the Inclusion of Water (Dry TOST Method)

SIGNIFICANCE AND USE
5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.  
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1.3 The values stated in SI units are to be regarded as standard.  
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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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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.  
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5.1 New and used petroleum products can contain basic or acidic constituents that are present as additives or as degradation products formed during service, such as oxidation products. The relative amount of these materials can be determined by titrating with acids or bases. This number, whether expressed as acid number or base number, is a measure of this amount of acidic or basic substances, respectively, in the oil—always under the conditions of the test. This number is used as a guide in the quality control of lubricating oil formulations. It is also sometimes used as a measure of lubricant degradation in service; however, any condemning limits must be empirically established.  
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5.1 The results obtained by this test are a useful guideline in determining the ability of water-miscible metalworking fluids to prevent or minimize rust under specific conditions. There is usually a relationship between the results of this test and a similar ability of the subject coolant to prevent rust on nested parts or in drilled holes containing chips, etc. It must be understood, however, that conditions, metal types, etc. found in practice will not correlate quantitatively with these controlled laboratory conditions. The procedure may not be able to differentiate between two products with poor rust control due to the wide spacing between test dilutions.
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1.1 This test method covers evaluation of the ferrous corrosion control characteristics of water–miscible metalworking fluids.  
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ASTM D4177-22e1(Practice)
Standard Practice for Automatic Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
4.1 Representative samples of petroleum and petroleum products are required for the determination of chemical and physical properties, which are used to establish standard volumes, prices, and compliance with commercial terms and regulatory requirements. This practice does not cover sampling of electrical insulating oils and hydraulic fluids. This practice does not address how to sample crude at temperatures below the freezing point of water.
PART I—General
This part is applicable to all petroleum liquid sampling whether it be crude oil or refined products. Review this section before designing or installing any automatic sampling system.
SCOPE
1.1 This practice describes general procedures and equipment for automatically obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container. This practice also provides additional specific information about sample container selection, preparation, and sample handling. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3). This practice does not cover sampling of electrical insulating oils and hydraulic fluids.  
1.2 Table of Contents:    
Section  
INTRODUCTION  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Significance and Use  
4  
PART I–GENERAL  
Representative Sampling Components  
5  
Design Criteria  
6  
Automatic Sampling Systems  
7  
Sampling Location  
8  
Mixing of the Flowing Stream  
9  
Proportionality  
10  
Sample Extractor Grab Volume  
11  
Containers  
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Sample Handling and Mixing  
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Control Systems  
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Sample System Security  
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System Proving (Performance Acceptance Tests)  
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Performance Monitoring  
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PART II–CRUDE OIL  
Crude Oil  
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PART III–REFINED PRODUCTS  
Refined Products  
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KEYWORDS  
Keywords  
20  
ANNEXES  
Calculations of the Margin of Error based on Number of Sample Grabs  
Annex A1  
Theoretical Calculations for Selecting the Sampler Probe Location  
Annex A2  
Portable Sampling Units  
Annex A3  
Profile Performance Test  
Annex A4  
Sampler Acceptance Test Data  
Annex A5  
APPENDIXES  
Design Data Sheet for Automatic Sampling System  
Appendix X1  
Comparisons of Percent Sediment and Water versus Unloading Time Period  
Appendix X2  
Sampling Frequency and Sampling System Monitoring Spreadsheet  
Appendix X3  
Sampling System Monitoring—Additional Diagnostics  
Appendix X4  
1.3 Units—The values stated in either SI units or US Customary (USC) units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard. Except where there is no direct SI equivalent, such as for National Pipe Threads/diameters, or tubing.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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 D4057-22(Practice)
Standard Practice for Manual Sampling of Petroleum and Petroleum Products

SIGNIFICANCE AND USE
4.1 Samples of petroleum and petroleum products are obtained for many reasons, including the determination of chemical and physical properties. These properties may be used for: calculating standard volumes; establishing product value; and often safety and regulatory reporting.  
4.2 There are inherent limitations when performing any type of sampling, any one of which may affect the representative nature of the sample. As examples, a spot sample provides a sample from only one particular point in the tank, vessel compartment, or pipeline. In the case of running or all-level samples, the sample only represents the column of material from which it was taken.  
4.3 Based on the product, and testing to be performed, this practice provides guidance on sampling equipment, container preparation, and manual sampling procedures for petroleum and petroleum products of a liquid, semi-liquid, or solid state, from the storage tanks, flowlines, pipelines, marine vessels, process vessels, drums, cans, tubes, bags, kettles, and open discharge streams into the primary sample container.
SCOPE
1.1 This practice covers procedures and equipment for manually obtaining samples of liquid petroleum and petroleum products, crude oils, and intermediate products from the sample point into the primary container are described. Procedures are also included for the sampling of free water and other heavy components associated with petroleum and petroleum products.  
1.2 This practice also addresses the sampling of semi-liquid or solid-state petroleum products. For the sampling of green petroleum coke, see Practice D8145. For the sampling of calcined petroleum coke, see Practice D6970.  
1.3 This practice provides additional specific information about sample container selection, preparation, and sample handling.  
1.4 This practice does not cover sampling of electrical insulating oils and hydraulic fluids. If sampling is for the precise determination of volatility, use Practice D5842 (API MPMS Chapter 8.4) in conjunction with this practice. For sample mixing and handling, refer to Practice D5854 (API MPMS Chapter 8.3).  
1.5 The procedures described in this practice may also be applicable in sampling most non-corrosive liquid industrial chemicals provided that all safety precautions specific to these chemicals are followed. Also, refer to Practice E300. The procedures described in this practice are also applicable to sampling liquefied petroleum gases and chemicals. Also refer to Practices D1265 and D3700. The procedure for sampling bituminous materials is described in Practice D140. Practice D4306 provides guidance on sample containers and preparation for sampling aviation fuel.  
1.6 Units—The values stated in SI units are to be regarded as the standard. USC units are reflected in parentheses.  
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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ASTM D5291-21(Test Method)
Standard Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants

SIGNIFICANCE AND USE
5.1 This is the first ASTM standard covering the simultaneous determination of carbon, hydrogen, and nitrogen in petroleum products and lubricants.  
5.2 Carbon, hydrogen, and particularly nitrogen analyses are useful in determining the complex nature of sample types covered by this test method. The CHN results can be used to estimate the processing and refining potentials and yields in the petrochemical industry.  
5.3 The concentration of nitrogen is a measure of the presence of nitrogen containing additives. Knowledge of its concentration can be used to predict performance. Some petroleum products also contain naturally occurring nitrogen. Knowledge of hydrogen content in samples is helpful in addressing their performance characteristics. Hydrogen to carbon ratio is useful to assess the performance of upgrading processes.
SCOPE
1.1 These test methods cover the instrumental determination of carbon, hydrogen, and nitrogen in laboratory samples of petroleum products and lubricants. Values obtained represent the total carbon, the total hydrogen, and the total nitrogen.  
1.2 These test methods are applicable to samples such as crude oils, fuel oils, additives, and residues for carbon and hydrogen and nitrogen analysis. These test methods were tested in the concentration range of at least 75 % to 87 % by mass for carbon, at least 9 % to 16 % by mass for hydrogen, and  
1.3 The nitrogen test method is not applicable to light materials or those containing  
1.3.1 However, using Test Method D levels of 0.1 % by mass nitrogen in lubricants could be determined.  
1.4 These test methods are not recommended for the analysis of volatile materials such as gasoline, gasoline-oxygenate blends, or gasoline type aviation turbine fuels.  
1.5 The results of these tests can be expressed as mass % carbon, hydrogen or nitrogen.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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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ASTM
ASTM D6304-20(Test Method)
Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration

SIGNIFICANCE AND USE
5.1 A knowledge of the water content is important in the manufacturing, purchase, sale, or transfer of petroleum products to help in predicting their quality and performance characteristics.  
5.2 The presence of moisture could lead to premature corrosion and wear, an increase in the debris load resulting in diminished lubrication and premature plugging of filters, an impedance in the effect of additives, and undesirable support of deleterious bacterial growth.
SCOPE
1.1 This test method covers the direct determination of entrained water in petroleum products and hydrocarbons using automated instrumentation. This test method also covers the indirect analysis of water thermally removed from samples and swept with dry inert gas into the Karl Fischer titration cell. Mercaptan, sulfide (S– or H2S), sulfur, and other compounds are known to interfere with this test method (see Section 6). The precision statement of this method covers the nominal range of 20 mg/kg to 25 000 mg/kg for Procedure A, 30 mg/kg to 2100 mg/kg for Procedure B, and 20 mg/kg to 360 mg/kg for Procedure C.  
1.2 This test method is intended for use with commercially available coulometric Karl Fischer reagents and for the determination of water in additives, lube oils, base oils, automatic transmission fluids, hydrocarbon solvents, and other petroleum products. By proper choice of the sample size, this test method may be used for the determination of water from mg/kg to percent level concentrations.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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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