ASTM D6994-15
(Test Method)Standard Test Method for Determination of Metal Cyanide Complexes in Wastewater, Surface Water, Groundwater and Drinking Water Using Anion Exchange Chromatography with UV Detection
Standard Test Method for Determination of Metal Cyanide Complexes in Wastewater, Surface Water, Groundwater and Drinking Water Using Anion Exchange Chromatography with UV Detection
SIGNIFICANCE AND USE
5.1 This method directly determines the concentration of metal cyanide complexes in environmental waters. The method is important from an environmental regulatory perspective because it differentiates metal cyanide complexes of lesser toxicity from metal cyanide complexes of greater toxicity. Previous determinations of strong metal cyanide complexes assumed that the concentration of strong metal cyanide complexes is equivalent to the difference between the total cyanide and the free cyanide. This approach is subject to error because different methods used to determine free cyanide often provide widely varying results, thus impacting the strong metal cyanide complex concentration that is determined by difference. The direct analysis using anion exchange chromatography avoids these method biases and provides for a more accurate and precise determination of metal cyanide complexes.
SCOPE
1.1 This test method covers the determination of the metal cyanide complexes of iron, cobalt, silver, gold, copper and nickel in waters including groundwaters, surface waters, drinking waters and wastewaters by anion exchange chromatography and UV detection. The use of alkaline sample preservation conditions (see 10.3) ensures that all metal cyanide complexes are solubilized and recovered in the analysis (1-3).2
1.2 Metal cyanide complex concentrations between 0.20 to 200 mg/L may be determined by direct injection of the sample. This range will differ depending on the specific metal cyanide complex analyte, with some exhibiting greater or lesser detection sensitivity than others. Approximate concentration ranges are provided in 12.2. Concentrations greater than the specific analyte range may be determined after appropriate dilution. This test method is not applicable for matrices with high ionic strength (conductivity greater than 500 meq/L as Cl) and TDS (greater than 30 000 mg/L), such as ocean water.
1.3 Metal cyanide complex concentrations less than 0.200 mg/L may be determined by on-line sample preconcentration coupled with anion exchange chromatography as described in 11.3. This range will differ depending on the specific metal cyanide complex analyte, with some exhibiting greater or lesser detection sensitivity than others. Approximate concentration ranges are provided in 12.2. The preconcentration method is not applicable for silver and copper cyanide complexes in matrices with high TDS (greater than 1000 mg/L).
1.4 The test method may also be applied to the determination of additional metal cyanide complexes, such as those of platinum and palladium. However, it is the responsibility of the user of this standard to establish the validity of the test method for the determination of cyanide complexes of metals other than those in 1.1.
1.5 The presence of metal complexes within a sample may be converted to Metal CN complexes and as such, are altered with the use of this method. This method is not applicable to samples that contain anionic complexes of metals that are weaker than cyanide complexes of those metals.
1.6 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.
1.7 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 statements, refer to Section 9.
General Information
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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: D6994 − 15
Standard Test Method for
Determination of Metal Cyanide Complexes in Wastewater,
Surface Water, Groundwater and Drinking Water Using
1
Anion Exchange Chromatography with UV Detection
This standard is issued under the fixed designation D6994; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 1.5 The presence of metal complexes within a sample may
be converted to Metal CN complexes and as such, are altered
1.1 This test method covers the determination of the metal
with the use of this method. This method is not applicable to
cyanide complexes of iron, cobalt, silver, gold, copper and
samples that contain anionic complexes of metals that are
nickelinwatersincludinggroundwaters,surfacewaters,drink-
weaker than cyanide complexes of those metals.
ing waters and wastewaters by anion exchange chromatogra-
phyandUVdetection.Theuseofalkalinesamplepreservation
1.6 The values stated in SI units are to be regarded as
conditions (see 10.3) ensures that all metal cyanide complexes
standard. The values given in parentheses are mathematical
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are solubilized and recovered in the analysis (1-3).
conversions to inch-pound units that are provided for informa-
tion only and are not considered standard.
1.2 Metal cyanide complex concentrations between 0.20 to
200mg/Lmaybedeterminedbydirectinjectionofthesample.
1.7 This standard does not purport to address all of the
This range will differ depending on the specific metal cyanide
safety concerns, if any, associated with its use. It is the
complex analyte, with some exhibiting greater or lesser detec-
responsibility of the user of this standard to establish appro-
tion sensitivity than others.Approximate concentration ranges
priate safety, health, and environmental practices and deter-
are provided in 12.2. Concentrations greater than the specific
mine the applicability of regulatory limitations prior to use.
analyte range may be determined after appropriate dilution.
For specific hazard statements, refer to Section 9.
This test method is not applicable for matrices with high ionic
1.8 This international standard was developed in accor-
strength (conductivity greater than 500 meq/L as Cl) and TDS
dance with internationally recognized principles on standard-
(greater than 30000 mg/L), such as ocean water.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.3 Metal cyanide complex concentrations less than 0.200
mendations issued by the World Trade Organization Technical
mg/L may be determined by on-line sample preconcentration
Barriers to Trade (TBT) Committee.
coupled with anion exchange chromatography as described in
11.3. This range will differ depending on the specific metal
2. Referenced Documents
cyanide complex analyte, with some exhibiting greater or
3
lesser detection sensitivity than others. Approximate concen-
2.1 ASTM Standards:
tration ranges are provided in 12.2. The preconcentration
D1129Terminology Relating to Water
method is not applicable for silver and copper cyanide com-
D1193Specification for Reagent Water
plexes in matrices with high TDS (greater than 1000 mg/L).
D2777Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.4 The test method may also be applied to the determina-
D3370Practices for Sampling Water from Closed Conduits
tion of additional metal cyanide complexes, such as those of
D3856Guide for Management Systems in Laboratories
platinumandpalladium.However,itistheresponsibilityofthe
Engaged in Analysis of Water
user of this standard to establish the validity of the test method
D5810Guide for Spiking into Aqueous Samples
for the determination of cyanide complexes of metals other
D5847Practice for Writing Quality Control Specifications
than those in 1.1.
for Standard Test Methods for Water Analysis
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D6696Guide for Understanding Cyanide Species
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 Oct. 1, 2015. Published October 2015. Originally
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approved in 2004. Last previous edition approved in 2010 as D6994–10. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D6994-15. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
Theboldfacenumbersinparenthesesrefe
...
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: D6994 − 10 D6994 − 15
Standard Test Method for
Determination of Metal Cyanide Complexes in Wastewater,
Surface Water, Groundwater and Drinking Water Using
1
Anion Exchange Chromatography with UV Detection
This standard is issued under the fixed designation D6994; 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 the metal cyanide complexes of iron, cobalt, silver, gold, copper and nickel
in waters including groundwaters, surface waters, drinking waters and wastewaters by anion exchange chromatography and UV
detection. The use of alkaline sample preservation conditions (see 10.3) ensures that all metal cyanide complexes are solubilized
2
and recovered in the analysis (1-3).
1.2 Metal cyanide complex concentrations between 0.20 to 200 mg/L may be determined by direct injection of the sample. This
range will differ depending on the specific metal cyanide complex analyte, with some exhibiting greater or lesser detection
sensitivity than others. Approximate concentration ranges are provided in 12.112.2. Concentrations greater than the specific analyte
range may be determined after appropriate dilution. This test method is not applicable for matrices with high ionic strength
(conductivity greater than 500 meq/L as Cl) and TDS (greater than 30 000 mg/L), such as ocean water.
1.3 Metal cyanide complex concentrations less than 0.200 mg/L may be determined by on-line sample preconcentration coupled
with anion exchange chromatography as described in 11.3. This range will differ depending on the specific metal cyanide complex
analyte, with some exhibiting greater or lesser detection sensitivity than others. Approximate concentration ranges are provided
in 12.112.2. The preconcentration method is not applicable for silver and copper cyanide complexes in matrices with high TDS
(greater than 1000 mg/L).
1.4 The test method may also be applied to the determination of additional metal cyanide complexes, such as those of platinum
and palladium. However, it is the responsibility of the user of this standard to establish the validity of the test method for the
determination of cyanide complexes of metals other than those in 1.1.
1.5 The presence of metal complexes within a sample may be converted to Metal CN complexes and as such, are altered with
the use of this method. This method is not applicable to samples that contain anionic complexes of metals that are weaker than
cyanide complexes of those metals.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this The values
given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not
considered standard.
1.7 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 statements, refer to Section 9.
2. Referenced Documents
3
2.1 ASTM Standards:
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
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 Sept. 15, 2010Oct. 1, 2015. Published November 2010October 2015. Originally approved in 2004. Last previous edition approved in 20042010
as D6994 – 04.D6994 – 10. DOI: 10.1520/D6994-10.10.1520/D6994-15.
2
The boldface numbers in parentheses refer to the list of references at the end of this standard.
3
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.
*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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