ASTM E649-17a
(Test Method)Standard Test Method for Bromine in Chlorine
Standard Test Method for Bromine in Chlorine
SIGNIFICANCE AND USE
4.1 Low levels of bromine contaminant in chlorine cause problems in some industrial uses. This test method may be used to determine bromine in liquid or gaseous chlorine at levels as low as 4 ug/kg.
SCOPE
1.1 This test method covers the determination of bromine in liquid chlorine and in gaseous chlorine with a lower limit of detection of 4 ug/kg by weight.
1.2 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first-aid procedures, handling, and safety precautions.
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
1.4 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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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: E649 − 17a
Standard Test Method for
1
Bromine in Chlorine
This standard is issued under the fixed designation E649; 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* 3. Summary of Test Method
1.1 This test method covers the determination of bromine in 3.1 Chlorine gas is sampled by absorption in aqueous
liquid chlorine and in gaseous chlorine with a lower limit of sodium hydroxide (NaOH). Liquid chlorine is first vaporized,
detection of 4 ug/kg by weight. and the vapor is absorbed in aqueous sodium hydroxide. An
aliquot of the sample solution is reduced with an excess of
1.2 Review the current Safety Data Sheets (SDS) for de-
sulfite ion, acidified, and excess sulfur dioxide (SO ) boiled
2
tailed information concerning toxicity, first-aid procedures,
out. In a carefully buffered solution, bromide is oxidized to
handling, and safety precautions.
bromate by hypochlorite. Excess hypochlorite is reduced to
1.3 This standard does not purport to address all of the
chloride by formate. In the presence of molybdate catalyst,
safety concerns, if any, associated with its use. It is the
bromate is reduced to bromide by iodide, and the liberated
responsibility of the user of this standard to establish appro-
iodine is titrated with standard sodium thiosulfate solution.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4. Significance and Use
Specific hazard statements are given in Section 7.
4.1 Low levels of bromine contaminant in chlorine cause
1.4 This international standard was developed in accor-
problems in some industrial uses. This test method may be
dance with internationally recognized principles on standard-
used to determine bromine in liquid or gaseous chlorine at
ization established in the Decision on Principles for the
levels as low as 4 ug/kg.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5. Apparatus
Barriers to Trade (TBT) Committee.
5.1 The construction of the chlorine gas sampling apparatus
and of the assembled sampling equipment is shown in Figs. 1
2. Referenced Documents
and 2. Modification of the equipment to deal with special
2
2.1 ASTM Standards:
sampling circumstances may be necessary. In Fig. 2, the
D1193 Specification for Reagent Water
control valve is shown with an adaptor for connection to a
D6809 Guide for Quality Control and Quality Assurance
chlorine cylinder valve. Other adaptors will be required when
Procedures for Aromatic Hydrocarbons and Related Ma-
sampling liquid chlorine in liquefaction plant streams or from
terials
large shipping or storage containers.
E180 Practice for Determining the Precision of ASTM
5.2 A 10-mL buret calibrated in 0.05-mL divisions is used
Methods for Analysis and Testing of Industrial and Spe-
when titrating with 0.01 N standard sodium thiosulfate solu-
3
cialty Chemicals (Withdrawn 2009)
tion.
E200 Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for ChemicalAnalysis
6. Reagents
6.1 Purity of Reagents—Unless otherwise indicated, it is
intended that all reagents should conform to the specifications
1
This test method is under the jurisdiction of ASTM Committee D16 on
of the Committee on Analytical Reagents of the American
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
4
Chemical Society, where such specifications are available.
bility of Subcommittee D16.13 on Chlorine.
Other grades may be used, provided it is first ascertained that
Current edition approved July 1, 2017. Published July 2017. Originally approved
in 1978. Last previous edition approved in 2017 as E649 – 17. DOI: 10.1520/
E0649-17a.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications, American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
3
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, In
...
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: E649 − 17 E649 − 17a
Standard Test Method for
1
Bromine in Chlorine
This standard is issued under the fixed designation E649; 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 bromine in liquid chlorine and in gaseous chlorine with a lower limit of
detection of 4 ug/kg by weight.
1.2 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first-aid procedures, handling,
and safety precautions.
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard statements are given in Section 7.
1.3 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first-aid procedures, handling,
and safety precautions.
1.4 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:
D1193 Specification for Reagent Water
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
3. Summary of Test Method
3.1 Chlorine gas is sampled by absorption in aqueous sodium hydroxide (NaOH). Liquid chlorine is first vaporized, and the
vapor is absorbed in aqueous sodium hydroxide. An aliquot of the sample solution is reduced with an excess of sulfite ion, acidified,
and excess sulfur dioxide (SO ) boiled out. In a carefully buffered solution, bromide is oxidized to bromate by hypochlorite. Excess
2
hypochlorite is reduced to chloride by formate. In the presence of molybdate catalyst, bromate is reduced to bromide by iodide,
and the liberated iodine is titrated with standard sodium thiosulfate solution.
4. Significance and Use
4.1 Low levels of bromine contaminant in chlorine cause problems in some industrial uses. This test method may be used to
determine bromine in liquid or gaseous chlorine at levels as low as 4 ug/kg.
5. Apparatus
5.1 The construction of the chlorine gas sampling apparatus and of the assembled sampling equipment is shown in Figs. 1 and
2. Modification of the equipment to deal with special sampling circumstances may be necessary. In Fig. 2, the control valve is
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 D16.16 on Industrial and Specialty Product Standards.
Current edition approved March 1, 2017July 1, 2017. Published March 2017July 2017. Originally approved in 1978. Last previous edition approved in 20112017 as
E649 – 00 (2011).E649 – 17. DOI: 10.1520/E0649-17.10.1520/E0649-17a.
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
The last approved version of this historical standard is referenced on www.astm.org.
*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
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E649 − 17a
FIG. 1 Chlorine Gas Sampling Apparatus
1. Inverted liquid chlorine cylinder
2. Chlorine cylinder valve
1
3. Control valve ( ⁄4-in. 316 stainless steel needle valve)
1
4. ⁄4-in. PTFE instrument air tubing
5. Small pail or 2-L beaker filled with water
6. Evaporating coil (two loops held with tape at indicated points)
7. Gas sampling apparatus of Fig. 1
FIG. 2 Liquid Chlorin
...
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