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 5to 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 E1763E1763 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 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 8.6 and Section 9.

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ASTM D7237-15 - 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)

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: D7237 − 15
StandardTest 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 standard does not purport to address all of the
the metal-cyanide complexes that are easily dissociated into
safety concerns, if any, associated with its use. It is the
free cyanide ions at the pH of 6. Free cyanide is determined at
responsibility of the user of this standard to establish appro-
pH 6 at room temperature. The aquatic free cyanide can be
priate safety and health practices and determine the applica-
determined by matching the pH to the water in the receiving
bility of regulatory limitations prior to use. Specific hazard
environment in the range of pH 6 to 8. The extent of HCN
statements are given in 8.6 and Section 9.
formation is less dependent on temperature than the pH;
however,thetemperaturecanberegulatedifdeemednecessary 2. Referenced Documents
for aquatic free cyanide to further simulate the actual aquatic 2
2.1 ASTM Standards:
environment.
D1129 Terminology Relating to Water
1.2 The free cyanide test method is based on the same D1193 Specification for Reagent Water
instrumentation and technology that is described in Test D1293 Test Methods for pH of Water
Method D6888, but employs milder conditions (pH 6-8 buffer D2036 Test Methods for Cyanides in Water
versus HCl or H SO in the reagent stream), and does not D2777 Practice for Determination of Precision and Bias of
2 4
utilize ligand displacement reagents. Applicable Test Methods of Committee D19 on Water
D3856 Guide for Management Systems in Laboratories
1.3 The aquatic free cyanide measured by this procedure
Engaged in Analysis of Water
should be similar to actual levels of HCN in the original
D4841 Practice for Estimation of Holding Time for Water
aquatic environment. This in turn may give a reliable index of
Samples Containing Organic and Inorganic Constituents
toxicity to aquatic organisms.
D5847 Practice for Writing Quality Control Specifications
1.4 This procedure is applicable over a range of approxi-
for Standard Test Methods for Water Analysis
mately 5 to 500 µg/L (parts per billion) free cyanide. Sample
D6512 Practice for Interlaboratory Quantitation Estimate
dilution may increase cyanide recoveries depending on the
D6696 Guide for Understanding Cyanide Species
cyanide speciation; therefore, it is not recommended to dilute
D6888 Test Method for Available Cyanide with Ligand
samples. Higher concentrations can be analyzed by increasing
Displacement and Flow InjectionAnalysis (FIA) Utilizing
the range of calibration standards or with a lower injection
Gas Diffusion Separation and Amperometric Detection
volume. In accordance with Guide E1763 and Practice D6512
D7365 Practice for Sampling, Preservation and Mitigating
the lower scope limit was determined to be 9 µg/L for
Interferences in Water Samples for Analysis of Cyanide
chlorinatedgoldleachingbarreneffluentwaterandtheIQE
10 %
D7728 GuideforSelectionofASTMAnalyticalMethodsfor
Implementation of International Cyanide Management
Code Guidance
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 Feb. 1, 2015. Published March 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2006. Last previous edition approved in 2010 as D7237 – 10. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7237-15. 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

---------------------- Page: 1 ----------------------
D7237
...

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 − 10 D7237 − 15
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 or effluent. 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 standard test method
Test Method D6888, but employs milder conditions (pH 6-8 buffer versus HCl or H SO in the reagent stream), and does not utilize
2 4
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 25 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.water and the IQE is 12 μg/L in the gold processing detoxified reverse osmosis permeate waste water sample
10 %
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 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 8.6 and Section 9.
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
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
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 and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved May 1, 2010Feb. 1, 2015. Published June 2010March 2015. Originally approved in 2006. Last previous edition approved in 20062010 as
D7237 – 06.D7237 – 10. DOI: 10.1520/D7237-10.10.1520/D7237-15.
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.
*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 ----------------------
D7237 − 15
D6512 Practice for Interlaboratory Quantitation
...

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