Standard Test Method for Free Cyanide and Aquatic Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection

SIGNIFICANCE AND USE
5.1 Cyanide and hydrogen cyanide are highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastes and surface waters.4  
5.2 It is useful to determine the aquatic free cyanide to establish an index of toxicity when a wastewater is introduced into the natural environment at a given pH and temperature.  
5.3 This test method is applicable for natural water, saline waters, and wastewater effluent.  
5.4 Free cyanide measured using this test method is applicable for implementation of the International Cyanide Code Guidance in accordance with Guide D7728.
SCOPE
1.1 This test method is used to establish the concentration of free cyanide in an aqueous wastewater, effluent and in-stream free cyanide concentrations after mixing treated water with receiving water. The test conditions of this test method are used to measure free cyanide (HCN and CN–) and cyanide bound in the metal-cyanide complexes that are easily dissociated into free cyanide ions at the pH of 6. Free cyanide is determined at pH 6 at room temperature. The aquatic free cyanide can be determined by matching the pH to the water in the receiving environment in the range of pH 6 to 8. The extent of HCN formation is less dependent on temperature than the pH; however, the temperature can be regulated if deemed necessary for aquatic free cyanide to further simulate the actual aquatic environment.  
1.2 The free cyanide test method is based on the same instrumentation and technology that is described in Test Method D6888, but employs milder conditions (pH 6–8 buffer versus HCl or H2SO4 in the reagent stream), and does not utilize ligand displacement reagents.  
1.3 The aquatic free cyanide measured by this procedure should be similar to actual levels of HCN in the original aquatic environment. This in turn may give a reliable index of toxicity to aquatic organisms.  
1.4 This procedure is applicable over a range of approximately 5 to 500 μg/L (parts per billion) free cyanide. Sample dilution may increase cyanide recoveries depending on the cyanide speciation; therefore, it is not recommended to dilute samples. Higher concentrations can be analyzed by increasing the range of calibration standards or with a lower injection volume. In accordance with Guide E1763 and Practice D6512 the lower scope limit was determined to be 9 μg/L for chlorinated gold leaching barren effluent water and the IQE10 % is 12 µg/L in the gold processing detoxified reverse osmosis permeate waste water sample matrix.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This test method is not recommended for samples that contain reduced sulfur compounds such as sulfides.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in 8.6 and Section 9.  
1.8 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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ASTM D7237-18 - Standard Test Method for Free Cyanide and Aquatic Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
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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: D7237 − 18
Standard Test Method for
Free Cyanide and Aquatic Free Cyanide with Flow Injection
Analysis (FIA) Utilizing Gas Diffusion Separation and
1
Amperometric Detection
This standard is issued under the fixed designation D7237; 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* is 12 µg/L in the gold processing detoxified reverse osmosis
permeate waste water sample matrix.
1.1 Thistestmethodisusedtoestablishtheconcentrationof
free cyanide in an aqueous wastewater, effluent and in-stream 1.5 The values stated in SI units are to be regarded as
free cyanide concentrations after mixing treated water with standard. No other units of measurement are included in this
receivingwater.Thetestconditionsofthistestmethodareused standard.

to measure free cyanide (HCN and CN ) and cyanide bound in
1.6 This test method is not recommended for samples that
the metal-cyanide complexes that are easily dissociated into
contain reduced sulfur compounds such as sulfides.
free cyanide ions at the pH of 6. Free cyanide is determined at
1.7 This standard does not purport to address all of the
pH 6 at room temperature. The aquatic free cyanide can be
safety concerns, if any, associated with its use. It is the
determined by matching the pH to the water in the receiving
responsibility of the user of this standard to establish appro-
environment in the range of pH 6 to 8. The extent of HCN
priate safety, health, and environmental practices and deter-
formation is less dependent on temperature than the pH;
mine the applicability of regulatory limitations prior to use.
however,thetemperaturecanberegulatedifdeemednecessary
Specific hazard statements are given in 8.6 and Section 9.
for aquatic free cyanide to further simulate the actual aquatic
1.8 This international standard was developed in accor-
environment.
dance with internationally recognized principles on standard-
1.2 The free cyanide test method is based on the same
ization established in the Decision on Principles for the
instrumentation and technology that is described in Test
Development of International Standards, Guides and Recom-
Method D6888, but employs milder conditions (pH 6–8 buffer
mendations issued by the World Trade Organization Technical
versus HCl or H SO in the reagent stream), and does not
2 4 Barriers to Trade (TBT) Committee.
utilize ligand displacement reagents.
2. Referenced Documents
1.3 The aquatic free cyanide measured by this procedure
2
should be similar to actual levels of HCN in the original
2.1 ASTM Standards:
aquatic environment. This in turn may give a reliable index of
D1129 Terminology Relating to Water
toxicity to aquatic organisms.
D1193 Specification for Reagent Water
D1293 Test Methods for pH of Water
1.4 This procedure is applicable over a range of approxi-
D2036 Test Methods for Cyanides in Water
mately 5 to 500 µg/L (parts per billion) free cyanide. Sample
D2777 Practice for Determination of Precision and Bias of
dilution may increase cyanide recoveries depending on the
Applicable Test Methods of Committee D19 on Water
cyanide speciation; therefore, it is not recommended to dilute
D3856 Guide for Management Systems in Laboratories
samples. Higher concentrations can be analyzed by increasing
Engaged in Analysis of Water
the range of calibration standards or with a lower injection
D4658 Test Method for Sulfide Ion in Water
volume. In accordance with Guide E1763 and Practice D6512
D4841 Practice for Estimation of Holding Time for Water
the lower scope limit was determined to be 9 µg/L for
Samples Containing Organic and Inorganic Constituents
chlorinatedgoldleachingbarreneffluentwaterandtheIQE
10 %
D5847 Practice for Writing Quality Control Specifications
for Standard Test Methods for Water Analysis
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
2
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2018. Published January 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2006. Last previous edition approved in 2015 as D7237 – 15a. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7237-18. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM
...

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: D7237 − 15a D7237 − 18
Standard Test Method for
Free Cyanide and Aquatic Free Cyanide with Flow Injection
Analysis (FIA) Utilizing Gas Diffusion Separation and
1
Amperometric Detection
This standard is issued under the fixed designation D7237; 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 is used to establish the concentration of free cyanide in an aqueous wastewater, effluent and in-stream free
cyanide concentrations after mixing treated water with receiving water. The test conditions of this test method are used to measure
-–
free cyanide (HCN and CN ) and cyanide bound in the metal-cyanide complexes that are easily dissociated into free cyanide ions
at the pH of 6. Free cyanide is determined at pH 6 at room temperature. The aquatic free cyanide can be determined by matching
the pH to the water in the receiving environment in the range of pH 6 to 8. The extent of HCN formation is less dependent on
temperature than the pH; however, the temperature can be regulated if deemed necessary for aquatic free cyanide to further
simulate the actual aquatic environment.
1.2 The free cyanide test method is based on the same instrumentation and technology that is described in Test Method D6888,
but employs milder conditions (pH 6–8 buffer versus HCl or H SO in the reagent stream), and does not utilize ligand displacement
2 4
reagents.
1.3 The aquatic free cyanide measured by this procedure should be similar to actual levels of HCN in the original aquatic
environment. This in turn may give a reliable index of toxicity to aquatic organisms.
1.4 This procedure is applicable over a range of approximately 5 to 500 μg/L (parts per billion) free cyanide. Sample dilution
may increase cyanide recoveries depending on the cyanide speciation; therefore, it is not recommended to dilute samples. Higher
concentrations can be analyzed by increasing the range of calibration standards or with a lower injection volume. In accordance
with Guide E1763 and Practice D6512 the lower scope limit was determined to be 9 μg/L for chlorinated gold leaching barren
effluent water and the IQE is 12 μg/L in the gold processing detoxified reverse osmosis permeate waste water sample matrix.
10 %
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This test method is not recommended for samples that contain reduced sulfur compounds such as sulfides.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific hazard statements are given in 8.6 and Section 9.
1.8 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:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D1293 Test Methods for pH of Water
D2036 Test Methods for Cyanides in Water
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved June 1, 2015Dec. 1, 2018. Published June 2015January 2019. Originally approved in 2006. Last previous edition approved in 2015 as
D7237 – 15.D7237 – 15a. DOI: 10.1520/D7237-15A.10.1520/D7237-18.
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’sstandard’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
1

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D7237 − 18
D2777 Practice for Determina
...

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