ASTM D7536-16

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 from 0.66 mg/kg to 10.07 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 was determined to be 0.18 mg/kg.  
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. For specific hazard information, see Section 9.

General Information

• Status: Historical
• Publication Date: 31-May-2016
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

Relations

• Replaced By: ASTM D7536-20 - Standard Test Method for Chlorine in Aromatics by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry
• Effective Date: 15-Aug-2020

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
Designation: D7536 − 16
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 D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
1.1 Thistestmethodcoversthedeterminationofchlorineby
terials
monochromatic, wavelength-dispersive X-ray fluorescence
E29 Practice for Using Significant Digits in Test Data to
(MWDXRF) spectrometry in aromatic hydrocarbons, their
Determine Conformance with Specifications
derivatives, and related chemicals.
E691 Practice for Conducting an Interlaboratory Study to
1.2 This test method is applicable to samples with chlorine
Determine the Precision of a Test Method
concentrations from 0.66 mg/kg to 10.07 mg/kg. Higher
3
2.2 Other Documents:
chlorine concentrations can be determined by quantitatively
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
diluting the sample with a suitable solvent. In an interlabora-
1910.1200
tory study, the limit of detection was determined to be 0.18
mg/kg.
3. Terminology
1.3 In determining the conformance of the test results using
3.1 See Terminology D4790 for definitions of terms used in
this method to applicable specifications, results shall be
this test method.
rounded off in accordance with the rounding-off method of
Practice E29.
4. Summary of Test Method
1.4 The values stated in SI units are to be regarded as
4.1 A monochromatic X-ray beam with a wavelength suit-
standard. No other units of measurement are included in this
able to excite the K-shell electrons of chlorine is focused onto
standard.
a test specimen contained in a sample cell (see Fig. 1). The
fluorescent Kα radiation at 0.473 nm (4.73Å) emitted by
1.5 This standard does not purport to address all of the
chlorine is collected by a fixed monochromator (analyzer).The
safety concerns, if any, associated with its use. It is the
intensity (counts per second) of the chlorine X-rays is mea-
responsibility of the user of this standard to establish appro-
sured using a suitable detector and converted to the concen-
priate safety and health practices and determine the applica-
tration of chlorine (mg/kg) in a test specimen using a calibra-
bility of regulatory limitations prior to use. For specific hazard
tion equation. Excitation by monochromatic X-rays reduces
information, see Section 9.
background, simplifies matrix correction and increases the
signal/background ratio compared to polychromatic excitation
2. Referenced Documents
4
2 used in conventional WDXRF techniques.
2.1 ASTM Standards:
D3437 Practice for Sampling and Handling Liquid Cyclic
5. Significance and Use
Products
5.1 This test method provides for the precise measurement
D4790 Terminology ofAromatic Hydrocarbons and Related
of the chlorine content of aromatics with minimal sample
Chemicals
preparation and analyst involvement.The typical time for each
analysis is five or ten minutes.
1
This test method is under the jurisdiction of ASTM Committee D16 on
5.2 Knowledge of the chlorine content of aromatics is
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
important for process control as well as the prediction and
Subcommittee D16.04 on Instrumental Analysis.
CurrenteditionapprovedJune1,2016.PublishedJuly2016.Originallyapproved
in 2009. Last previous edition approved in 2009 as D7356 – 09. DOI: 10.1520/
3
D7536-16. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM www.access.gpo.gov.
4
Standards volume information, refer to the standard’s Document Summary page on Bertin, E. P., Principles and Practices of X-ray Spectrometric Analysis, Plenum
the ASTM website. Press, New York, 1975, pp. 115-118.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7536 − 16
FIG. 1 Schematic of the MWDXRF Analyzer
control of operational problems such as unit corrosion and 7.1.1 X-ray Source, capable of producing X-rays to excite
catalyst poisoning, and in the blending of products to com- chlorine. X-ray tubes capable of producing Rh Lα,PdLα,Ag
modity specifications. Lα,TiKα,ScKα, and Cr Kα radiation are recommended for
this purpose.
5.3
...

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 − 09 D7536 − 16
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
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 from 0.50.66 mg/kg to 1510.07 mg/kg. Higher
chlorine concentrations can be determined by quantitatively diluting the sample with a suitable solvent. In a preliminary robustness
an interlaboratory study, the limit of detection was estimateddetermined to be 0.060.18 mg/kg.
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.For specific hazard information, see Section 9.
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. For specific hazard information, see Section 9.
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
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 using a calibration equation. Excitation by
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 Sept. 1, 2009June 1, 2016. Published September 2009July 2016. Originally approved in 2009. Last previous edition approved in 2009 as D7356
– 09. DOI: 10.1520/D7536-09.10.1520/D7536-16.
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‘sstandard’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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7536 − 16
FIG. 1 Schematic of the MWDXRF Analyzer
monochromatic X-rays reduces background, simplifies matrix correction and increases the signal/background ratio compared to
4
polychromatic excitation used in conventional WDXRF techniques.
5. Significance and Use
5.1 This test method provides for the p
...