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ASTM D4310-06a

(Test Method)

Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils

Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils

SCOPE
1.1 This test method 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.
1.2 This test method is a modification of Test Method D 943 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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 warning statements, see Section 7 and X1.1.5.

General Information

Status
Historical
Publication Date
30-Jun-2006
ICS
75.040 - Crude petroleum
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.09.0C - Oxidation of Turbine Oils
Current Stage
Ref Project

Relations

Replaces
ASTM D4310-06 - Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils
Effective Date
01-Jul-2006
Replaced By
ASTM D4310-06b - Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils
Effective Date
01-Dec-2006
Referred By
ASTM D8324-21 - Standard Guide for Selection of Environmentally Acceptable Lubricants for the U.S. Environmental Protection Agency (EPA) Vessel General Permit
Effective Date
01-Jul-2006
Referred By
ASTM D8029-18 - Standard Specification for Biodegradable, Low Aquatic Toxicity Hydraulic Fluids
Effective Date
01-Jul-2006
Referred By
ASTM D7873-22a - 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)
Effective Date
01-Jul-2006
Referred By
ASTM D7155-20 - Standard Practice for Evaluating Compatibility of Mixtures of Turbine Lubricating Oils
Effective Date
01-Jul-2006
Referred By
ASTM D943-20 - Standard Test Method for Oxidation Characteristics of Inhibited Mineral Oils
Effective Date
01-Jul-2006
Referred By
ASTM D8506-23 - Standard Guide for Microbial Contamination and Biodeterioration in Turbine Oils and Turbine Oil Systems
Effective Date
01-Jul-2006
Referred By
ASTM D4304-22 - Standard Specification for Mineral and Synthetic Lubricating Oil Used in Steam or Gas Turbines
Effective Date
01-Jul-2006
Referred By
ASTM D6158-18 - Standard Specification for Mineral Hydraulic Oils
Effective Date
01-Jul-2006

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ASTM D4310-06a - Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral OilsASTM D4310-06a - Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils
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ASTM D4310-06a - Standard Test Method for Determination of Sludging and Corrosion Tendencies of Inhibited Mineral Oils
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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
Designation:D4310–06a
Standard Test Method for
Determination of Sludging and Corrosion Tendencies of
1
Inhibited Mineral Oils
This standard is issued under the fixed designation D 4310; 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.
1. Scope* Rods and Coarse Round Wire, Carbon Steel
B1 Specification for Hard-Drawn Copper Wire
1.1 This test method is used to evaluate the tendency of
D 664 Test Method forAcid Number of Petroleum Products
inhibited mineral oil based steam turbine lubricants and min-
by Potentiometric Titration
eral oil based anti-wear hydraulic oils to corrode copper
D 874 Test Method for Sulfated Ash from Lubricating Oils
catalyst metal and to form sludge during oxidation in the
and Additives
presence of oxygen, water, and copper and iron metals at an
D 943 Test Method for Oxidation Characteristics of Inhib-
elevated temperature. The test method is also used for testing
ited Mineral Oils
circulating oils having a specific gravity less than that of water
D 1193 Specification for Reagent Water
and containing rust and oxidation inhibitors.
D 3339 Test Method for Acid Number of Petroleum Prod-
NOTE 1—During round robin testing copper and iron in the oil, water
ucts by Semi-Micro Color Indicator Titration
and sludge phases were measured. However, the values for the total iron
D 4057 Practice for Manual Sampling of Petroleum and
were found to be so low (that is, below 0.8 mg), that statistical analysis
Petroleum Products
was inappropriate. The results of the cooperative test program are
2
E1 Specification forASTM Liquid-in-Glass Thermometers
available.
4
2.2 IP Standard:
1.2 ThistestmethodisamodificationofTestMethodD 943
Specification for IP Standard Thermometers
where the oxidation stability of the same kinds of oils is
5
2.3 British Standard:
determinedbyfollowingtheacidnumberofoil.Thenumberof
BS 1829 Reference Tables for Iron v. Constantan Thermo-
test hours required for the oil to reach an acid number of 2.0
couples
mg KOH/g is the oxidation lifetime.
1.3 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions:
standard.
3.1.1 sludge—a precipitate or sediment from oxidized min-
1.4 This standard does not purport to address all of the
eral oil and water.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 An oil sample is contacted with oxygen in the presence
bility of regulatory limitations prior to use. For specific
of water and an iron-copper catalyst at 95°C for 1000 h. The
warning statements, see Section 7 and X1.1.5.
weight of insoluble material is determined gravimetrically by
filtration of the oxidation tube contents through 5-µm pore size
2. Referenced Documents
filter disks. The total amount of copper in the oil, water, and
3
2.1 ASTM Standards:
sludge phases is also determined.
A 510 Specification for General Requirements for Wire
NOTE 2—Optionally, some operators may choose to: (1) assess the
change in weight of the catalyst coil, or (2) determine the acid number at
1000 h, or both. The acid number may serve as a criterion to determine if
1
This test method is under the jurisdiction of ASTM Committee D02 on
measurement of insoluble material is warranted. Normally, further testing
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
is not recommended on a highly oxidized oil (that is an oil which has
D02.09 on Oxidation.
attained an acid number >2.0 mg KOH/g). Instructions for these optional
Current edition approved July 1, 2006. Published July 2006. Originally approved
tests are not included in this test method.
in 1983. Last previous edition approved in 2006 as D 4310–06.
2
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: D02-1291.
3 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from Energy Institute, 61 New Cavendish St., London WIM, 8AR,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM England.
5
Standards volume information, refer to the standard’s Document Summary page on Available from British Standards Institute (BSI), 389 Chiswick High Rd.,
the ASTM website. London W4 4AL, U.K.
*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
...

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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.  
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5.1 This test method is one of a number of tests conducted on a crude oil to determine its value. It provides an estimate of the yields of fractions of various boiling ranges and is therefore valuable in technical discussions of a commercial nature.  
5.2 This test method corresponds to the standard laboratory distillation efficiency referred to as 15/5. The fractions produced can be analyzed as produced or combined to produce samples for analytical studies, engineering, and product quality evaluations. The preparation and evaluation of such blends is not part of this test method.  
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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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1.6 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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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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Standard Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

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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.  
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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.  
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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.
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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.  
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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.  
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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.
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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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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.  
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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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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 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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