ASTM D7359-13
(Test Method)Standard Test Method for Total Fluorine, Chlorine and Sulfur in Aromatic Hydrocarbons and Their Mixtures by Oxidative Pyrohydrolytic Combustion followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)
Standard Test Method for Total Fluorine, Chlorine and Sulfur in Aromatic Hydrocarbons and Their Mixtures by Oxidative Pyrohydrolytic Combustion followed by Ion Chromatography Detection (Combustion Ion Chromatography-CIC)
SIGNIFICANCE AND USE
4.1 The total fluorine, chlorine and sulfur contained in aromatic hydrocarbon matrices can contribute to emissions, be harmful to many catalytic chemical processes, and lead to corrosion. This test method can be used to determine total sulfur and halogens aromatic hydrocarbon matrices, in finished products and can be used for compliance determinations when acceptable to a regulatory authority using performance based criteria.
SCOPE
1.1 This test method covers the individual determination of total fluorine, chlorine and sulfur in aromatic hydrocarbons and their mixtures. Samples containing 0.10 to 50 mg/kg of each element can be analyzed.
1.2 This method can be applied to sample types outside the range of the scope by dilution of the sample in an appropriate solvent to bring the total concentrations of fluorine, chlorine and sulfur within the range covered by the test method. However, it is the responsibility of the analyst to verify the solubility of the sample in the solvent and that the diluted sample results conform to the precision and accuracy of the method.
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
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 and health practices and determine the applicability of regulatory limitations prior to use. See Section 8.
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Designation: D7359 − 13
StandardTest Method for
Total Fluorine, Chlorine and Sulfur in Aromatic
Hydrocarbons and Their Mixtures by Oxidative
Pyrohydrolytic Combustion followed by Ion
Chromatography Detection (Combustion Ion
1
Chromatography-CIC)
This standard is issued under the fixed designation D7359; 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. Scope* 2. Referenced Documents
2
1.1 This test method covers the individual determination of 2.1 ASTM Standards:
totalfluorine,chlorineandsulfurinaromatichydrocarbonsand D1193 Specification for Reagent Water
their mixtures. Samples containing 0.10 to 50 mg/kg of each D6809 Guide for Quality Control and Quality Assurance
element can be analyzed. Procedures for Aromatic Hydrocarbons and Related Ma-
terials
1.2 This method can be applied to sample types outside the
E29 Practice for Using Significant Digits in Test Data to
range of the scope by dilution of the sample in an appropriate
Determine Conformance with Specifications
solvent to bring the total concentrations of fluorine, chlorine
2.2 Other Documents:
and sulfur within the range covered by the test method.
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
However, it is the responsibility of the analyst to verify the
3
1910.1200
solubility of the sample in the solvent and that the diluted
sample results conform to the precision and accuracy of the
3. Summary of Test Method
method.
3.1 A sample of known weight or volume is placed into a
1.3 In determining the conformance of the test results using
sample boat and introduced at a controlled rate into a high
this method to applicable specifications, results shall be
temperature combustion tube. There the sample is combusted
rounded off in accordance with the rounding-off method of
in an oxygen rich pyrohydrolytic environment. The gaseous
Practice E29.
by-products of the combusted sample are trapped in an
absorption medium where the hydrogen halides (HX) formed
1.4 The values stated in SI units are to be regarded as
-
during combustion disassociate into their respective ions, X
standard. No other units of measurement are included in this
while the sulfur oxides (SO ) formed are further oxidized to
standard.
X
2-
SO in the presence of an oxidizing agent. An aliquot of
4
1.5 This standard does not purport to address all of the
known volume of the adsorbing solution is then automatically
safety concerns, if any, associated with its use. It is the
injected into an ion chromatograph (IC) by means of a sample
responsibility of the user of this standard to establish appro-
injectionvalve.Thehalideandsulfateanionsareseparatedinto
priate safety and health practices and determine the applica-
individualelutionbandsontheseparatorcolumnoftheIC.The
bility of regulatory limitations prior to use. See Section 8.
conductivity of the eluent is reduced with an anion suppression
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D16 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Standards volume information, refer to the standard’s Document Summary page on
Subcommittee D16.04 on Instrumental Analysis. the ASTM website.
3
Current edition approved July 15, 2013. Published September 2013. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 2008. Last previous edition approved in 2008 as D7359 – 08. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D7359-13. www.access.gpo.gov.
*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 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7359 − 13
device prior to the ion chromatograph’s thermal conductivity 6.7 Gas Adsorption Unit, having an adsorption tube of
detector, where the anions of interest are measured. Quantifi- either 10 or 20 mL which is automatically filled with a known
cation of the fluorine, chlorine and sulfur in the original volume of absorption solution by a built-in burette or other
combusted sample is achieved by first calibrating the system similardevice.TheGasAdsorptionUnitisinterfacedtotheIon
with a series of standards containing known amounts of Chromatograph and injects an aliquot of the adsorption solu-
fluorine, chlorine and sulfur and then analyzing unknown tion into the Ion Chromatograph after the sample is combus
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7359 − 08 D7359 − 13
Standard Test Method for
Total Fluorine, Chlorine and Sulfur in Aromatic
Hydrocarbons and Their Mixtures by Oxidative
Pyrohydrolytic Combustion followed by Ion
Chromatography Detection (Combustion Ion
1
Chromatography-CIC)
This standard is issued under the fixed designation D7359; 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. Scope Scope*
1.1 This test method covers the individual determination of total fluorine, chlorine and sulfur in aromatic hydrocarbons and their
mixtures. Samples containing 0.10.10 to 50 mg/kg of each element can be analyzed.
1.2 This method can be applied to sample types outside the range of the scope by dilution of the sample in an appropriate solvent
to bring the total concentrations of fluorine, chlorine and sulfur within the range covered by the test method. However, it is the
responsibility of the analyst to verify the solubility of the sample in the solvent and that the diluted sample results conform to the
precision and accuracy of the method.
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded
off in accordance with the rounding-off method of Practice E29.
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 and health practices and determine the applicability of regulatory
limitations prior to use. See Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
2.2 Other Documents:
3
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 A sample of known weight or volume is placed into a sample boat and introduced at a controlled rate into a high temperature
combustion tube. There the sample is combusted in an oxygen rich pyrohydrolytic environment. The gaseous by-products of the
combusted sample are trapped in an absorption medium where the hydrogen halides (HX) formed during combustion disassociate
- 2-
into their respective ions, X while the sulfur oxides (SO ) formed are further oxidized to SO in the presence of an oxidizing
X 4
agent. An aliquot of known volume of the adsorbing solution is then automatically injected into an ion chromatograph (IC) by
means of a sample injection valve. The halide and sulfate anions are separated into individual elution bands on the separator
column of the IC. The conductivity of the eluent is reduced with an anion suppression device prior to the ion chromatograph’s
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.04 on Instrumental Analysis.
Current edition approved Oct. 15, 2008July 15, 2013. Published November 2008September 2013. Originally approved in 2008. Last previous edition approved in 2008
as D7359 – 08. DOI: 10.1520/D7359-08.10.1520/D7359-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
*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 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7359 − 13
thermal conductivity detector, where the anions of interest are measured. Quantification of the fluorine, chlorine and sulfur in the
original combusted sample is achieved by first calibrating the system with a series of standards containing known amounts of
fluorine, chlorine and sulfur and the
...
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