ASTM D7536-20

Standard Test Method for Chlorine in Aromatics by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry

SIGNIFICANCE AND USE
5.1 This test method provides for the precise measurement of the chlorine content of aromatics with minimal sample preparation and analyst involvement. The typical time for each analysis is five or ten minutes.  
5.2 Knowledge of the chlorine content of aromatics is important for process control as well as the prediction and control of operational problems such as unit corrosion and catalyst poisoning, and in the blending of products to commodity specifications.  
5.3 Various federal, state, and local agencies regulate the chlorine content of some petroleum products, including aromatics. Unbiased and precise determination of chlorine in aromatics is critical to compliance with regulatory standards.  
5.4 When the elemental composition of the samples differ significantly from the calibration standards used to prepare the calibration curve, the cautions and recommendation in Section 6 should be carefully observed.
SCOPE
1.1 This test method covers the determination of chlorine by monochromatic wavelength-dispersive X-ray fluorescence (MWDXRF) spectrometry in aromatic hydrocarbons, their derivatives, and related chemicals.  
1.2 This test method is applicable to samples with chlorine concentrations to 10 mg/kg. Higher chlorine concentrations can be determined by quantitatively diluting the sample with a suitable solvent. The limit of detection (LOD) is 0.2 mg/kg and the limit of quantitation is 0.7 mg/kg. With careful analytical technique or the measurement of replicates, or both, this method can be used to successfully analyze concentrations below the LOD.
Note 1: The maximum is the highest concentration from the interlaboratory study (ILS) and the LOD and LOQ were calculated from Performance Testing Program (PTP) data. See Table 3.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard information, 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: 14-Aug-2020
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

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: D7536 − 20
Standard Test Method for
Chlorine in Aromatics by Monochromatic Wavelength
1
Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D7536; 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 Thistestmethodcoversthedeterminationofchlorineby 2.1 ASTM Standards:
monochromatic wavelength-dispersive X-ray fluorescence D3437 Practice for Sampling and Handling Liquid Cyclic
(MWDXRF) spectrometry in aromatic hydrocarbons, their Products
derivatives, and related chemicals. D4790 Terminology ofAromatic Hydrocarbons and Related
Chemicals
1.2 This test method is applicable to samples with chlorine
D6809 Guide for Quality Control and Quality Assurance
concentrations to 10 mg/kg. Higher chlorine concentrations
Procedures for Aromatic Hydrocarbons and Related Ma-
can be determined by quantitatively diluting the sample with a
terials
suitablesolvent.Thelimitofdetection(LOD)is0.2mg/kgand
E29 Practice for Using Significant Digits in Test Data to
the limit of quantitation is 0.7 mg/kg. With careful analytical
Determine Conformance with Specifications
technique or the measurement of replicates, or both, this
E691 Practice for Conducting an Interlaboratory Study to
method can be used to successfully analyze concentrations
Determine the Precision of a Test Method
below the LOD.
3
2.2 Other Documents:
NOTE 1—The maximum is the highest concentration from the inter-
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
laboratory study (ILS) and the LOD and LOQ were calculated from
1910.1200
Performance Testing Program (PTP) data. See Table 3.
1.3 In determining the conformance of the test results using
3. Terminology
this method to applicable specifications, results shall be
3.1 See Terminology D4790 for definitions of terms used in
rounded off in accordance with the rounding-off method of
Practice E29. this test method.
1.4 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
standard. 4.1 A monochromatic X-ray beam with a wavelength suit-
able to excite the K-shell electrons of chlorine is focused onto
1.5 This standard does not purport to address all of the
a test specimen contained in a sample cell (see Fig. 1). The
safety concerns, if any, associated with its use. It is the
fluorescent Kα radiation at 0.473 nm (4.73Å) emitted by
responsibility of the user of this standard to establish appro-
chlorine is collected by a fixed monochromator (analyzer).The
priate safety, health, and environmental practices and deter-
intensity (counts per second) of the chlorine X-rays is mea-
mine the applicability of regulatory limitations prior to use.
sured using a suitable detector and converted to the concen-
For specific hazard information, see Section 9.
tration of chlorine (mg/kg) in a test specimen using a calibra-
1.6 This international standard was developed in accor-
tion equation. Excitation by monochromatic X-rays reduces
dance with internationally recognized principles on standard-
background, simplifies matrix correction and increases the
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
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 [e-mail]. For Annual Book of ASTM
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- Standards volume information, refer to the standard’s Document Summary page on
bility of Subcommittee D16.04 on Instrumental Analysis. the ASTM website.
3
Current edition approved Aug. 15, 2020. Published August 2020. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 2009. Last previous edition approved in 2016 as D7356 – 16. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D7536-20. 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 ----------------------
D7536 − 20
FIG. 1 Schematic of the MWDXRF Analy
...

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: D7536 − 16 D7536 − 20
Standard Test Method for
Chlorine in Aromatics by Monochromatic Wavelength
1
Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D7536; 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 determination of chlorine by monochromatic,monochromatic wavelength-dispersive X-ray
fluorescence (MWDXRF) spectrometry in aromatic hydrocarbons, their derivatives, and related chemicals.
1.2 This test method is applicable to samples with chlorine concentrations from 0.66 mg/kg to 10.07to 10 mg/kg. Higher chlorine
concentrations can be determined by quantitatively diluting the sample with a suitable solvent. In an interlaboratory study, The
limit of detection (LOD) is 0.2 mg/kg and the limit of detection was determined to be 0.18 mg/kg.quantitation is 0.7 mg/kg. With
careful analytical technique or the measurement of replicates, or both, this method can be used to successfully analyze
concentrations below the LOD.
NOTE 1—The maximum is the highest concentration from the interlaboratory study (ILS) and the LOD and LOQ were calculated from Performance
Testing Program (PTP) data. See Table 3.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard information, 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the direct
responsibility of Subcommittee D16.04 on Instrumental Analysis.
Current edition approved June 1, 2016Aug. 15, 2020. Published July 2016August 2020. Originally approved in 2009. Last previous edition approved in 20092016 as D7356
– 09.16. DOI: 10.1520/D7536-16.10.1520/D7536-20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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 ----------------------
D7536 − 20
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 See Terminology D4790 for definitions of terms used in this test method.
4. Summary of Test Method
4.1 A monochromatic X-ray beam with a wavelength suitable to excite the K-shell electrons of chlorine is focused onto a test
specimen contained in a sample cell (see Fig. 1). The fluorescent Kα radiation at 0.473 nm (4.73Å) emitted by chlorine is collected
by a fixed monochromator (analyzer). The intensity (counts per second) of the chlorine X-rays is measured using a suitable detector
and converted to the concentration of chlorine (mg/kg) in a test specimen usi
...