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ASTM D7994-17

(Test Method)

Standard Test Method for Total Fluorine, Chlorine, and Sulfur in Liquid Petroleum Gas (LPG) by Oxidative Pyrohydrolytic Combustion Followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)

Standard Test Method for Total Fluorine, Chlorine, and Sulfur in Liquid Petroleum Gas (LPG) by Oxidative Pyrohydrolytic Combustion Followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)

SIGNIFICANCE AND USE
5.1 The total fluorine, chlorine, and sulfur contained in LPG, similar low molecular weight hydrocarbons, and DME can be harmful to many catalytic chemical processes, lead to corrosion, and contribute to pollutant emissions. While LPG specifications limit sulfur, some specifications also contain precautionary statements about fluorine. Chlorine has been known to contaminate LPG with detrimental consequences. This test method can be used to determine total fluorine (as fluoride), chlorine (as chloride), and sulfur (as sulfate ion) in process streams, intermediate and finished LPG products, similar low molecular weight hydrocarbons, and DME (1.1).
SCOPE
1.1 This test method covers the individual determination of total fluorine, chlorine, and sulfur in liquid petroleum gas (LPG), low molecular weight hydrocarbons, their mixtures, and dimethyl ether (DME) in the range of 1 mg/kg to 300 mg/kg fluorine and sulfur and 5 mg/kg to 300 mg/kg for chlorine. This test method is applicable to products described in Specifications D1835 and D7901 and it can be applicable to process streams with similar properties to LPG and other materials such as butylene, propylene, and olefins.  
1.2 This test method can also be applied to the measurement of the bromine and iodine in samples covered by the scope of this test method, but the precision and bias statement of this test method is not applicable to these halides.  
1.3 This test method can be applied to sample concentrations outside the scope of this test method through adjustments of sample injection volume or number of injections combusted (or both), adjustment of injection volume to the ion chromatograph, and adjustment of the final dilution volume of the absorbing solution prior to injection to the ion chromatograph. The precision and scope of this test method is not applicable to samples that are outside the scope of the method.  
1.4 The values stated in SI units are to be regarded as standard.  
1.4.1 Exception—Values given in parentheses are for information only.  
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 and health practices and determine the applicability of regulatory limitations prior to use. See Section 9.  
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.

General Information

Status
Published
Publication Date
31-Dec-2016
ICS
75.160.30 - Gaseous fuels
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.H0 - Liquefied Petroleum Gas
Current Stage
Ref Project

Relations

Refers
ASTM E288-10(2017) - Standard Specification for Laboratory Glass Volumetric Flasks
Effective Date
01-Nov-2017
Refers
ASTM E969-02(2019) - Standard Specification for Glass Volumetric (Transfer) Pipets
Effective Date
01-Jul-2019
Refers
ASTM D7901-14b - Standard Specification for Dimethyl Ether for Fuel Purposes
Effective Date
15-Oct-2014
Referred By
ASTM D1835-22 - Standard Specification for Liquefied Petroleum (LP) Gases
Effective Date
01-Jan-2017
Referred By
ASTM D5273-18 - Standard Guide for Analysis of Propylene Concentrates
Effective Date
01-Jan-2017
Referred By
ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
Effective Date
01-Jan-2017

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ASTM D7994-17 - Standard Test Method for Total Fluorine, Chlorine, and Sulfur in Liquid Petroleum Gas (LPG) by Oxidative Pyrohydrolytic Combustion Followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)ASTM D7994-17 - Standard Test Method for Total Fluorine, Chlorine, and Sulfur in Liquid Petroleum Gas (LPG) by Oxidative Pyrohydrolytic Combustion Followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)
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ASTM D7994-17 - Standard Test Method for Total Fluorine, Chlorine, and Sulfur in Liquid Petroleum Gas (LPG) by Oxidative Pyrohydrolytic Combustion Followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)
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Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D7994 − 17
Standard Test Method for
Total Fluorine, Chlorine, and Sulfur in Liquid Petroleum Gas
(LPG) by Oxidative Pyrohydrolytic Combustion Followed by
Ion Chromatography Detection (Combustion Ion
1
Chromatography-CIC)
This standard is issued under the fixed designation D7994; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 This test method covers the individual determination of
mendations issued by the World Trade Organization Technical
total fluorine, chlorine, and sulfur in liquid petroleum gas
Barriers to Trade (TBT) Committee.
(LPG), low molecular weight hydrocarbons, their mixtures,
and dimethyl ether (DME) in the range of 1mg⁄kg to
2. Referenced Documents
300mg⁄kg fluorine and sulfur and 5mg⁄kg to 300mg⁄kg for
2
chlorine. This test method is applicable to products described
2.1 ASTM Standards:
in Specifications D1835 and D7901 and it can be applicable to
D1193Specification for Reagent Water
process streams with similar properties to LPG and other
D1265Practice for Sampling Liquefied Petroleum (LP)
materials such as butylene, propylene, and olefins.
Gases, Manual Method
D1835Specification for Liquefied Petroleum (LP) Gases
1.2 Thistestmethodcanalsobeappliedtothemeasurement
D3700Practice for Obtaining LPG Samples Using a Float-
of the bromine and iodine in samples covered by the scope of
ing Piston Cylinder
this test method, but the precision and bias statement of this
D6849Practice for Storage and Use of Liquefied Petroleum
test method is not applicable to these halides.
Gases (LPG) in Sample Cylinders for LPG Test Methods
1.3 This test method can be applied to sample concentra-
D7901Specification for Dimethyl Ether for Fuel Purposes
tionsoutsidethescopeofthistestmethodthroughadjustments
E29Practice for Using Significant Digits in Test Data to
of sample injection volume or number of injections combusted
Determine Conformance with Specifications
(or both), adjustment of injection volume to the ion
E288Specification for Laboratory Glass Volumetric Flasks
chromatograph, and adjustment of the final dilution volume of
E969Specification for Glass Volumetric (Transfer) Pipets
the absorbing solution prior to injection to the ion chromato-
3
2.2 OSHA Standards:
graph. The precision and scope of this test method is not
29 CFR Part 1910.1000Air Contaminants
applicable to samples that are outside the scope of the method.
29 CFR Part 1910.1200Hazard Communication
1.4 The values stated in SI units are to be regarded as
standard.
3. Terminology
1.4.1 Exception—Values given in parentheses are for infor-
3.1 Definitions:
mation only.
3.1.1 combustion ion chromatography (CIC), n—ananalyti-
1.5 This standard does not purport to address all of the
cal system consisting of oxidative pyrohydrolytic combustion
safety concerns, if any, associated with its use. It is the
followed by ion chromatographic detection.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.1.2 halogen (X), n—a generic term which includes the
bility of regulatory limitations prior to use. See Section 9.
elements fluorine, chlorine, bromine, and iodine.
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D02 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Standards volume information, refer to the standard’s Document Summary page on
Subcommittee D02.H0 on Liquefied Petroleum Gas. the ASTM website.
3
Current edition approved Jan. 1, 2017. Published April 2017. DOI: 10.1520/ Available from Occupational Safety and Health Administration (OSHA), 200
D7994-17. Constitution Ave., NW, Washington, DC 20210, http://www.osha.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7994 − 17
3.1.3 hydrogen halide (HX), n—inorganic compounds with 3.3.3 CRM—certified reference material
the formula HX where X is one of the halogens: fluoride,
3.3.4 DME—dimethyl ether
chloride,
...

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ASTM D2163-23e1(Test Method)
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5.1 The hydrocarbon component distribution of liquefied petroleum gases and propene mixtures is often required for end-use sale of this material. Applications such as chemical feed stocks or fuel require precise compositional data to ensure uniform quality. Trace amounts of some hydrocarbon impurities in these materials can have adverse effects on their use and processing.  
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1.1 This test method covers the quantitative determination of individual hydrocarbons in liquefied petroleum (LP) gases and mixtures of propane and propene, excluding high-purity propene in the range of C1 to C5. Component concentrations are determined in the range of 0.01 % to 100 % by volume.  
1.2 This test method does not fully determine hydrocarbons heavier than C5 and non-hydrocarbon materials, and additional tests may be necessary to fully characterize an LPG sample.  
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Standard Test Method for Determination of Ethyl Mercaptan in LP-Gas Vapor

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5.1 LP-gas is colorless and odorless, and not detectable by normal human senses. To provide an olfactory warning in the event of a leak, LP-gas intended for domestic or commercial fuel use is intentionally odorized so as to be readily detectable well below flammable or suffocating concentration levels of LP-gas in air. (See Appendix X1 for important explanations.) The most common odorant for LP-gas is ethyl mercaptan. The field use of this test method will rapidly determine the presence and concentration of ethyl mercaptan in LP-gas vapor without the necessity for complex laboratory equipment.
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1.1 This test method describes a rapid and simple procedure using length-of-stain tubes for field measurement of ethyl mercaptan in the vapor phase of LP-gas systems. Although length-of-stain tubes are available to detect ethyl mercaptan concentrations in the range of 0.5 to 120 parts per million by volume, this test method is specifically applicable to systems containing 5 ppm by volume or more of ethyl mercaptan in LP-gas vapors.  
Note 1: A chromatographic technique can be used for more precise, quantitative determination of ethyl mercaptan in LP-gas.  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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ASTM D2384-23(Test Method)
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SIGNIFICANCE AND USE
4.1 These test methods are used to determine trace amounts of volatile chlorides in butane-butene mixtures. Such information is valuable in cases where chloride is deleterious in the use of this product; also, chloride contributes to corrosion problems in processing units in instances where further processing of this material is involved.
SCOPE
1.1 These test methods cover the determination of the total volatile organic chlorides in concentrations from 10 mg/kg to 100 mg/kg in butane-butene mixtures. The amperometric finish is not directly applicable in the presence of other substances that combine with silver ion or oxidize chloride ion in dilute acid solution. Bromides, sulfides, ammonia, tobacco smoke, and more than 25 μg of hydrogen peroxide in the test solution interfere in the spectrophotometric procedure.  
1.2 Dissolved sodium chloride is not quantitatively determined using these test methods.  
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.   Specific warning statements are given in Sections 5, 8, 11, 14, 19, and Annex A1.  
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ASTM D2420-23(Test Method)
Standard Test Method for Hydrogen Sulfide in Liquefied Petroleum (LP) Gases (Lead Acetate Method)

SIGNIFICANCE AND USE
5.1 Liquefied petroleum gases and their products of combustion must not be unduly corrosive to the materials with which they come in contact. The potential personnel exposure hazards of H2S also make the detection and measurement of hydrogen sulfide important, even in low concentrations. In addition, in some cases the odor of the gases shall not be objectionable. (See Specification D1835 and GPA 2140.)
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ASTM D1267-23(Test Method)
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SIGNIFICANCE AND USE
5.1 Information on the vapor pressures of liquefied petroleum gas products under temperature conditions from 37.8 °C to 70 °C (100 °F to 158 °F) is pertinent to selection of properly designed storage vessels, shipping containers, and customer utilization equipment to ensure safe handling of these products.  
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SCOPE
1.1 This test method covers the determination of the gauge vapor pressures of liquefied petroleum gas products at temperatures of 37.8 °C (100 °F) up to and including a test temperature of 70 °C (158 °F). (Warning—Extremely flammable gas. May be harmful when inhaled.)
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This specification covers liquefied petroleum gases consisting of propane, propene (propylene), butane, and mixtures of these materials. The products are intended for use as domestic, commercial and industrial heating, and engine fuels. Care must be taken to in sampling of the liquefied gases for test results to be significant. All four types of liquefied petroleum gases covered by this specification should conform to the specified requirements for vapor pressure, volatile residue, residue matter, relative density, and corrosion.
SCOPE
1.1 This specification covers those products commonly referred to as liquefied petroleum gases, consisting of propane, propene (propylene), butane, and mixtures of these materials. Four basic types of liquefied petroleum gases are provided to cover the common use applications.  
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ASTM D2158-21(Test Method)
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SIGNIFICANCE AND USE
5.1 Control over the residue content (required by Specification D1835) is of considerable importance in end-use applications of LPG. In liquid feed systems, residues can lead to troublesome deposits and, in vapor withdrawal systems, residues that are carried over can foul regulating equipment. Residues that remain in vapor-withdrawal systems will accumulate, can be corrosive, and will contaminate subsequent product. Water, particularly if alkaline, can cause failure of regulating equipment and corrosion of metals.  
5.2 See Appendix X2 for information on the effect of temperature on the measurement of residue in LPG.
SCOPE
1.1 This test method covers the determination of extraneous materials weathering above 38 °C that are present in liquefied petroleum gases. The extraneous materials will generally be dissolved in the LPG, but may have phase-separated in some instances.  
1.2 Liquefied petroleum gases that contain certain anti-icing additives can give erroneous results by this test method.  
1.3 Although this test method has been used to verify cleanliness and lack of heavy contaminants in propane for many years, it might not be sensitive enough to protect some equipment from operational problems or increased maintenance. A more sensitive test, able to detect lower levels of dissolved contaminants, could be required for some applications.  
1.4 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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ASTM D2598-21(Practice)
Standard Practice for Calculation of Certain Physical Properties of Liquefied Petroleum (LP) Gases from Compositional Analysis

SIGNIFICANCE AND USE
4.1 Vapor pressure is an important specification property of commercial propane, special duty propane, propane/butane mixtures, and commercial butane that assures adequate vaporization, safety, and compatibility with commercial appliances. Relative density, while not a specification criterion, is necessary for determination of filling densities and custody transfer. The motor octane number (MON) is useful in determining the products' suitability as a fuel for internal combustion engines.
SCOPE
1.1 This practice covers, by compositional analysis, the approximate determination of the following physical characteristics of commercial propane, special-duty propane, commercial propane/butane mixtures, and commercial butane (covered by Specification D1835): vapor pressure, relative density, and motor octane number (MON).  
1.1.1 This practice is not applicable to any product exceeding specifications for nonvolatile residues. (See Test Method D2158.)  
1.1.2 For calculating motor octane number, this practice is applicable only to mixtures containing 20 % or less of propene.  
1.1.3 For calculated motor octane number, this practice is based on mixtures containing only components shown in Table 1.  
1.2 The values stated in SI units are to be regarded as standard.  
1.2.1 Exceptions:  
1.2.1.1 Non-SI units in parentheses are given for information only.
1.2.1.2 Motor octane number and relative density are given in MON numbers and dimensionless units, respectively.  
1.3 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 D6667-21(Test Method)
Standard Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence

SIGNIFICANCE AND USE
4.1 The sulfur content of LPG, used for fuel purposes, contributes to SOx emissions and can lead to corrosion in engine and exhaust systems. Some process catalysts used in petroleum and chemical refining can be poisoned by sulfur bearing materials in the feed stocks. This test method can be used to determine sulfur in process feeds, to measure sulfur in finished products, and can also be used for compliance determinations when acceptable to a regulatory authority.
SCOPE
1.1 This test method covers the determination of total volatile sulfur in gaseous hydrocarbons and liquefied petroleum (LP) gases. It is applicable to analysis of natural, processed, and final product materials. Precision has been determined for sulfur in gaseous hydrocarbons in the range of 1 mg/kg to 100 mg/kg and for sulfur in LP gases in the range of 1 mg/kg to 196 mg/kg (Note 1).
Note 1: An estimate of pooled limit of quantification (PLOQ), information regarding sample stability and other general information derived from the interlaboratory studies on precision can be referenced in the ASTM research reports.2,3  
1.2 This test method may not detect sulfur compounds that do not vaporize under the conditions of the test.  
1.3 This test method is applicable for total volatile sulfur determination in LP gases containing less than 0.35 % (mass/mass) halogen(s).  
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. See 3.1 and Sections 6 and 7 for specific warning statements.  
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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