ASTM D5257-03

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

SIGNIFICANCE AND USE
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.
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.
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. See 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 4°C and analyzing it within 24 h.
1.4 The values stated in SI units are to be regarded as the 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.

General Information

• Status: Historical
• Publication Date: 09-Jan-2003
• ICS: 71.060.50 - Salts
• Technical Committee: D19 - Water
• Drafting Committee: D19.05 - Inorganic Constituents in Water

Relations

• Replaces: ASTM D5257-97 - Standard Test Method for Dissolved Hexavalent Chromium in Water by Ion Chromatography
• Effective Date: 10-Jan-2003
• Replaced By: ASTM D5257-11 - Standard Test Method for Dissolved Hexavalent Chromium in Water by Ion Chromatography
• Effective Date: 15-Mar-2011
• Referred By: ASTM D1687-17 - Standard Test Methods for Chromium in Water
• Effective Date: 10-Jan-2003

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:D5257–03
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.
TABLE 1 Determination of Precision and Bias for Hexavalent
1. Scope*
Chromium
1.1 This test method covers procedures for the determina-
Amount Amount
Water Bias,
tion of dissolved hexavalent chromium in wastewater, surface
A
Added, Found, S S
t o
Matrix %
water, and drinking water.
µg/L µg/L
1.2 The precision and bias of this test method has been
Reagent 1.2 1.40 0.16 0.15 + 16.6
tested in reagent water and industrial wastewater and has been 1.6 1.87 0.65 . + 16.9
6.0 6.68 1.03 0.53 + 11.3
found suitable over the range of approximately 1 to 1000 µg/L.
8.0 8.64 1.10 . + 8.0
See Table 1 for details. Higher levels can be determined by
16.0 17.4 2.25 0.77 + 8.8
20.0 21.4 2.31 . + 7.0
appropriate dilution.
100 101 1.91 3.76 + 1.0
1.3 Samples containing very high levels of anionic species
140 143 5.52 . + 2.1
(that is, chloride, sulfate, etc.) may cause column overload.
800 819 24.3 12.7 + 2.4
960 966 18.5 . + 7.3
Samples containing high levels of reducing species (that is,
Waste 6.0 5.63 1.17 0.55 −6.2
sulfides,sulfites,etc.)maycausereductionofCr(VI)toCr(III).
8.0 7.31 1.91 . −8.6
This can be minimized by buffering the sample to a pH of 9 to
16.0 15.1 2.70 1.85 −5.6
20.0 19.8 1.01 . −1.0
9.5, filtering it, storing it at 4°C and analyzing it within 24 h.
100 98.9 4.36 3.31 −1.1
1.4 The values stated in SI units are to be regarded as the
140 138 8.39 . −1.4
standard.
800 796 60.6 27.1 −0.5
960 944 72.1 . −1.7
1.5 This standard does not purport to address all of the
A
Each Youden pair was used to calculate one lab data point, S .
safety concerns, if any, associated with its use. It is the
o
responsibility of the user of this standard to establish appro-
2
Applicable Test Methods of Committee D19 on Water
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. D3370 Practices for Sampling Water from Closed Conduits
2
2. Referenced Documents 2
D5810 Guide for Spiking into Aqueous Samples
2
2.1 ASTM Standards: D5847 Practice for Writing Quality Control Specifications
2
D1066 Practice for Sampling Steam for Standard Test Methods for Water Analysis
2
D1129 Terminology Relating to Water 2.2 EPA Standard:
D1192 Guide for Equipment for SamplingWater and Steam EPA Method 218.6 Determination of Dissolved Hexavalent
32
in Closed Conduits Chromium in DrinkingWater, Groundwater and Industrial
2 4
D1193 Specification for Reagent Water Wastewater Effluents by Ion Chromatography
D2777 Practice for Determination of Precision and Bias of
3. Terminology
3.1 Definitions—For definitions of terms used in this test
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
method, refer to Terminology D1129.
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
3.2 Definitions of Terms Specific to This Standard:
in Water.
3.2.1 eluant— the ionic mobile phase used to transport the
Current edition approved Jan. 10, 2003. Published January 2003. Originally
approved in 1992. Last previous edition approved in 1997 as D5257 – 97. DOI: sample through the ion exchange column.
10.1520/D5257-03.
2
Annual Book of ASTM Standards, Vol 11.01.
3 4
Withdrawn. The last approved version of this historical standard is referenced Available from Superintendent of Documents, U.S. Government Printing
on www.astm.org. Office, Washington, DC 20402.
*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

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D5257–03
3.2.2 resolution—the ability of a column to separate con- ware or contact with caustic or acidic reagents with chromium
stituents under specified test conditions. containing stainless steel or pigmented materials.
7. Apparatus
4. Summary of Test Method
7.1 Ion Chromatograph—An ion chromatograph having the
4.1 Afixedvolumeofbufferedandfilteredsample,typically
following components configured as shown in Fig. 1.
100 µL, is injected into the eluant flow path and separated by
7.1.1 Pump, capable of delivering a constant flow in the
anion exchange using an ammonium sulfate based eluant.
range of 1 to 5 mL/min at a pressure of 200 to 2000 psi.
4.2 After separation, the sample is reacted with an acidic
7.1.2 Injection Valve— A high pressure, low dead volume
...