ASTM D5257-17

Standard Test Method for Dissolved Hexavalent Chromium in Water by Ion Chromatography

SIGNIFICANCE AND USE
5.1 Hexavalent chromium salts are used extensively in the metal finishing and plating industries, in the leather industry as a tanning agent, and in the manufacture of paints, dyes, explosives, and ceramics. Trivalent chromium salts are used as mordants in textile dying, in the ceramic and glass industry, and in photography. Chromium, in either oxidation state, may be present in wastewater from these industries and may also be discharged from chromate-treated cooling waters.  
5.2 Hexavalent chromium is toxic to humans, animals, and aquatic life. It can produce lung tumors when inhaled and readily induces skin sensitization. It is not known whether cancer will result from ingestion of chromium in any of its valence states.  
5.3 Ion chromatography provides a means of separating the hexavalent chromium from other species present in the sample, many of which interfere with other detection methods. The combination of this separation with a sensitive colorimetric detection method provides a selective and sensitive analytical method for hexavalent chromium with minimal sample preparation.
SCOPE
1.1 This test method covers procedures for the determination of dissolved hexavalent chromium in wastewater, surface water, and drinking water.  
1.2 The precision and bias of this test method has been tested in reagent water and industrial wastewater and has been found suitable over the range of approximately 1 to 1000 μg/L. Higher levels can be determined by appropriate dilution.  
1.3 Samples containing very high levels of anionic species (that is, chloride, sulfate, etc.) may cause column overload. Samples containing high levels of reducing species (that is, sulfides, sulfites, etc.) may cause reduction of Cr(VI) to Cr(III). This can be minimized by buffering the sample to a pH of 9 to 9.5, filtering it, storing it at  
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered 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.  
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: 30-Nov-2017
• ICS: 71.060.50 - Salts
• Technical Committee: D19 - Water
• Drafting Committee: D19.05 - Inorganic Constituents in Water

Relations

• Refers: ASTM D1066-18 - Standard Practice for Sampling Steam
• Effective Date: 01-Aug-2018
• Refers: ASTM D1066-18e1 - Standard Practice for Sampling Steam
• Effective Date: 01-Aug-2018
• Referred By: ASTM D1687-17 - Standard Test Methods for Chromium in Water
• Effective Date: 01-Dec-2017

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: D5257 − 17
Standard Test Method for
Dissolved Hexavalent Chromium in Water by Ion
1
Chromatography
This standard is issued under the fixed designation D5257; 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
2.1 ASTM Standards:
1.1 This test method covers procedures for the determina-
D1066 Practice for Sampling Steam
tion of dissolved hexavalent chromium in wastewater, surface
D1129 Terminology Relating to Water
water, and drinking water.
D1193 Specification for Reagent Water
1.2 The precision and bias of this test method has been
D2777 Practice for Determination of Precision and Bias of
tested in reagent water and industrial wastewater and has been
Applicable Test Methods of Committee D19 on Water
found suitable over the range of approximately 1 to 1000 µg/L.
D3370 Practices for Sampling Water from Closed Conduits
Higher levels can be determined by appropriate dilution.
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications
1.3 Samples containing very high levels of anionic species
for Standard Test Methods for Water Analysis
(that is, chloride, sulfate, etc.) may cause column overload.
3
2.2 U.S. EPA Standards:
Samples containing high levels of reducing species (that is,
U.S. EPA 40 CFR 136 Guidelines Establishing Test Proce-
sulfides,sulfites,etc.)maycausereductionofCr(VI)toCr(III).
dures for the Analysis of Pollutants
This can be minimized by buffering the sample to a pH of 9 to
U.S. EPA Method 218.6 Determination of Dissolved
9.5, filtering it, storing it at <6°C. A holding time of 28 days
Hexavalent Chromium in Drinking Water, Groundwater
may be used if the user can demonstrate that such holding time
and Industrial Wastewater Effluents by Ion Chromatogra-
does not affect sample integrity in accordance with U.S. EPA
phy
40 CFR 136, Part II.
1.4 The values stated in SI units are to be regarded as 3. Terminology
standard. The values given in parentheses are mathematical
3.1 Definitions:
conversions to inch-pound units that are provided for informa-
3.1.1 For definitions of terms used in this standard, refer to
tion only and are not considered standard.
Terminology D1129.
1.5 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 continuing calibration blank, n—a solution containing
responsibility of the user of this standard to establish appro-
no analytes (of interest) which is used to verify blank response
priate safety, health, and environmental practices and deter-
and freedom from carryover.
mine the applicability of regulatory limitations prior to use.
3.2.2 continuing calibration verification, n—a solution (or
1.6 This international standard was developed in accor-
setofsolutions)ofknownconcentrationusedtoverifyfreedom
dance with internationally recognized principles on standard-
from excessive instrumental drift; the concentration is to cover
ization established in the Decision on Principles for the
the range of calibration curve.
Development of International Standards, Guides and Recom-
3.2.3 eluent, n—the ionic mobile phase used to transport the
mendations issued by the World Trade Organization Technical
sample through the ion-exchange column.
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 D19 on Water contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents Standards volume information, refer to the standard’s Document Summary page on
in Water. the ASTM website.
3
Current edition approved Dec. 1, 2017. Published December 2017. Originally Available from U.S. Government Printing Office, Superintendent of
approved in 1992. Last previous edition approved in 2011 as D5257 – 11. DOI: Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
10.1520/D5257-17. 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 ----------------------
D5257 − 17
3.2.4 resolution, n—the ability of a column to separate 6.5 Trace amounts of Cr a
...

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: D5257 − 11 D5257 − 17
Standard Test Method for
Dissolved Hexavalent Chromium in Water by Ion
1
Chromatography
This standard is issued under the fixed designation D5257; 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 procedures for the determination of dissolved hexavalent chromium in wastewater, surface water,
and drinking water.
1.2 The precision and bias of this test method has been tested in reagent water and industrial wastewater and has been found
suitable over the range of approximately 1 to 1000 μg/L. See Table 1 for details. Higher levels can be determined by appropriate
dilution.
1.3 Samples containing very high levels of anionic species (that is, chloride, sulfate, etc.) may cause column overload. Samples
containing high levels of reducing species (that is, sulfides, sulfites, etc.) may cause reduction of Cr(VI) to Cr(III). This can be
minimized by buffering the sample to a pH of 9 to 9.5, filtering it, storing it at <6°C. aAA holding time of 28 days may be used
if the user can demonstrate that such holding time does not affect sample integrity per US in accordance with U.S. EPA 40 CFR
136, Part II.
1.4 The values stated in either SI or inch-pound units are to be regarded as the standard. The values given in parentheses are
for information only.mathematical conversions to inch-pound units that are provided for information only and are not considered
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.
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:
D1066 Practice for Sampling Steam
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3
2.2 U.S. EPA StandardStandards:
U.S. EPA 40 CFR 136 Guidelines Establishing Test Procedures for the Analysis of Pollutants
U.S. EPA Method 218.6 Determination of Dissolved Hexavalent Chromium in Drinking Water, Groundwater and Industrial
Wastewater Effluents by Ion Chromatography
US EPA 40 CFR 136
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.
Current edition approved March 15, 2011Dec. 1, 2017. Published April 2011December 2017. Originally approved in 1992. Last previous edition approved in 20092011
as D5257 – 09.D5257 – 11. DOI: 10.1520/D5257-11.10.1520/D5257-17.
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.
3
Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.Superintendent of Documents, 732 N. Capitol St., NW,
Washington, DC 20401-0001, 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 ----------------------
D5257 − 17
TABLE 1 Determination of Precision and Bias for Hexavalent
Chromium
Amount Amount
Water Bias,
A
Added, Found, S S
t o
Matrix %
μg/L μg/L
Reagent 1.2 1.40 0.16 0.15 + 16.6
1.6 1.87 0.65 . + 16.9
6.0 6.68 1.03 0.53 + 11.3
8.0 8.64 1.10 . + 8.0
16.0 17.4 2.25 0.77 + 8.8
20.0 21.4 2.31 . + 7.0
100 101 1.91 3.76 + 1.0
140 143 5.52 . + 2.1
800 819 24.3 12.
...