ASTM E649-17
(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 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.
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Designation: E649 − 17
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* bromate is reduced to bromide by iodide, and the liberated
iodine is titrated with standard sodium thiosulfate solution.
1.1 This test method covers the determination of bromine in
liquid chlorine and in gaseous chlorine with a lower limit of
4. Significance and Use
detection of 4 ug/kg by weight.
4.1 Low levels of bromine contaminant in chlorine cause
1.2 This standard does not purport to address all of the
problems in some industrial uses. This test method may be
safety concerns, if any, associated with its use. It is the
used to determine bromine in liquid or gaseous chlorine at
responsibility of the user of this standard to establish appro-
levels as low as 4 ug/kg.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
5. Apparatus
statements are given in Section 7.
1.3 Review the current Safety Data Sheets (SDS) for de-
5.1 The construction of the chlorine gas sampling apparatus
tailed information concerning toxicity, first-aid procedures,
and of the assembled sampling equipment is shown in Figs. 1
handling, and safety precautions.
and 2. Modification of the equipment to deal with special
sampling circumstances may be necessary. In Fig. 2, the
2. Referenced Documents
control valve is shown with an adaptor for connection to a
2
chlorine cylinder valve. Other adaptors will be required when
2.1 ASTM Standards:
sampling liquid chlorine in liquefaction plant streams or from
D1193 Specification for Reagent Water
large shipping or storage containers.
E180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
5.2 A 10-mL buret calibrated in 0.05-mL divisions is used
3
cialty Chemicals (Withdrawn 2009)
when titrating with 0.01 N standard sodium thiosulfate solu-
E200 Practice for Preparation, Standardization, and Storage
tion.
of Standard and Reagent Solutions for ChemicalAnalysis
6. Reagents
3. Summary of Test Method
6.1 Purity of Reagents—Unless otherwise indicated, it is
3.1 Chlorine gas is sampled by absorption in aqueous
intended that all reagents should conform to the specifications
sodium hydroxide (NaOH). Liquid chlorine is first vaporized,
of the Committee on Analytical Reagents of the American
and the vapor is absorbed in aqueous sodium hydroxide. An
4
Chemical Society, where such specifications are available.
aliquot of the sample solution is reduced with an excess of
Other grades may be used, provided it is first ascertained that
sulfite ion, acidified, and excess sulfur dioxide (SO ) boiled
2
the reagent is of sufficiently high purity to permit its use
out. In a carefully buffered solution, bromide is oxidized to
without lessening the accuracy of the determination.
bromate by hypochlorite. Excess hypochlorite is reduced to
6.2 Purity of Water—Unless otherwise indicated, references
chloride by formate. In the presence of molybdate catalyst,
to water shall be understood to mean Type II or Type III
reagent water conforming to Specification D1193.
1
This test method is under the jurisdiction of ASTM Committee D16 on
6.3 Chloride Solution—Dissolve 200 g of sodium chloride
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
(NaCl) in 940 mL of water.
Subcommittee D16.16 on Industrial and Specialty Product Standards.
Current edition approved March 1, 2017. Published March 2017. Originally
approved in 1978. Last previous edition approved in 2011 as E649 – 00 (2011).
DOI: 10.1520/E0649-17.
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, Inc. (USPC), Rockville,
www.astm.org. MD.
*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
-
...
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 − 00 (Reapproved 2011) E649 − 17
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 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 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 Materials Safety Data Sheets (MSDS)(SDS) for detailed information concerning toxicity, first-aid
procedures, handling, and safety precautions.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
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
shown with an adaptor for connection to a chlorine cylinder valve. Other adaptors will be required when sampling liquid chlorine
in liquefaction plant streams or from large shipping or storage containers.
5.2 A 10-mL buret calibrated in 0.05-mL divisions is used when titrating with 0.01 N standard sodium thiosulfate solution.
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
D16.16 on Industrial and Specialty Product Standards.
Current edition approved Aug. 1, 2011March 1, 2017. Published November 2011March 2017. Originally approved in 1978. Last previous edition approved in 20052011
ε1
as E649 – 00 (2005)(2011). . DOI: 10.1520/E0649-00R11.10.1520/E0649-17.
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 − 17
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 Chlorine Sampling Equipment
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E649 − 17
6. Reagents
6.1 Purity of Reagents—Unless otherwise indicated, it is intended that all reagents should conform to the specifications of the
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Committee on
...
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