ASTM D7284-13
(Test Method)Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection
Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with 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.3
5.2 This test method is applicable for natural waters, industrial wastewaters and effluents.
SCOPE
1.1 This test method is used to determine the concentration of total cyanide in an aqueous wastewater or effluent. The method detects the cyanides that are free (HCN and CN-) and strong-metal-cyanide complexes that dissociate and release free cyanide when refluxed under strongly acidic conditions.
1.2 This method may not be applicable to process solutions from precious metals mining operations.
1.3 This procedure is applicable over a range of approximately 2 to 500 μg/L (parts per billion) total cyanide. Higher concentrations can be measured with sample dilution or lower injection volume.
1.4 The determinative step of this method utilizes flow injection with amperometric detection based on Test Method D6888. Prior to analysis, samples must be distilled with a micro-distillation apparatus described in this test method or with a suitable cyanide distillation apparatus specified in Test Methods D2036.
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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Designation: D7284 − 13
Standard Test Method for
Total Cyanide in Water by Micro Distillation followed by
Flow Injection Analysis with Gas Diffusion Separation and
1
Amperometric Detection
This standard is issued under the fixed designation D7284; 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 D1193 Specification for Reagent Water
D2036 Test Methods for Cyanides in Water
1.1 This test method is used to determine the concentration
D2777 Practice for Determination of Precision and Bias of
of total cyanide in an aqueous wastewater or effluent. The
-
Applicable Test Methods of Committee D19 on Water
method detects the cyanides that are free (HCN and CN ) and
D3856 Guide for Management Systems in Laboratories
strong-metal-cyanide complexes that dissociate and release
Engaged in Analysis of Water
free cyanide when refluxed under strongly acidic conditions.
D5847 Practice for Writing Quality Control Specifications
1.2 This method may not be applicable to process solutions
for Standard Test Methods for Water Analysis
from precious metals mining operations.
D6696 Guide for Understanding Cyanide Species
1.3 This procedure is applicable over a range of approxi-
D6888 Test Method for Available Cyanide with Ligand
mately 2 to 500 µg/L (parts per billion) total cyanide. Higher
Displacement and Flow InjectionAnalysis (FIA) Utilizing
concentrations can be measured with sample dilution or lower
Gas Diffusion Separation and Amperometric Detection
injection volume.
D7365 Practice for Sampling, Preservation and Mitigating
1.4 The determinative step of this method utilizes flow
Interferences in Water Samples for Analysis of Cyanide
injection with amperometric detection based on Test Method
E691 Practice for Conducting an Interlaboratory Study to
D6888. Prior to analysis, samples must be distilled with a
Determine the Precision of a Test Method
micro-distillation apparatus described in this test method or
with a suitable cyanide distillation apparatus specified in Test
3. Terminology
Methods D2036.
3.1 Definitions:
1.5 The values stated in SI units are to be regarded as
3.1.1 For definitions of terms used in this test method, refer
standard. No other units of measurement are included in this
to Terminology D1129 and Guide D6696.
standard.
3.2 Definitions of Terms Specific to This Standard:
1.6 This standard does not purport to address all of the
3.2.1 total cyanide—Total cyanide is an analytically defined
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- term that refers to the sum total of all of the inorganic chemical
priate safety and health practices and determine the applica- forms of cyanide that dissociate and release free cyanide when
bility of regulatory limitations prior to use. Specific hazard
refluxed under strongly acidic conditions. Total cyanide is
statements are given in 8.6 and Section 9.
determined analytically through strong acid distillation or UV
radiation followed by analysis of liberated free cyanide on
2. Referenced Documents
aqueous samples preserved with NaOH (pH~12). In water,
2
2.1 ASTM Standards:
total cyanide includes the following dissolved species: free
D1129 Terminology Relating to Water
cyanide, weak acid dissociable metal cyanide complexes and
strong metal cyanide complexes. Also, some of the strong
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
metal cyanide complexes, such as those of gold, cobalt and
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
platinum, might not be fully recovered during the total cyanide
Current edition approved June 15, 2013. Published July 2013. Originally
analytical procedure. Additionally, total cyanide may also
ε1
approved in 2008. Last previous edition approved in 2008 as D7284 – 08 . DOI:
include some organic forms of cyanide such as nitriles that
10.1520/D7284-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
release free cyanide under the conditions of the analysis.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7284 − 13
4. Summary of Test Method amperometric flowcell as a positive response. Refer to Section
11.2 for sulfide abatement.
4.1 The samples are distilled with a stron
...
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.
´1
Designation: D7284 − 08 D7284 − 13
Standard Test Method for
Total Cyanide in Water by Micro Distillation followed by
Flow Injection Analysis with Gas Diffusion Separation and
1
Amperometric Detection
This standard is issued under the fixed designation D7284; 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
ε NOTE—This Test Method was editorially corrected in September 2012.
1. Scope
1.1 This test method is used to determine the concentration of total cyanide in an aqueous wastewater or effluent. The method
-
detects the cyanides that are free (HCN and CN ) and strong-metal-cyanide complexes that dissociate and release free cyanide
when refluxed under strongly acidic conditions.
1.2 This method may not be applicable to process solutions from precious metals mining operations.
1.3 This procedure is applicable over a range of approximately 2 to 400500 μg/L (parts per billion) total cyanide. Higher
concentrations can be measured with sample dilution or lower injection volume.
1.4 The determinative step of this method utilizes flow injection with amperometric detection based on Test Method D6888.
Prior to analysis, samples must be distilled with a micro-distillation apparatus described in this test method or with a suitable
cyanide distillation apparatus specified in Test Methods D2036.
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 Note 28.6 and Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent 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
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D6696 Guide for Understanding Cyanide Species
D6888 Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion
Separation and Amperometric Detection
D7365 Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D1129 and Guide D6696.
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 April 1, 2008June 15, 2013. Published April 2008July 2013. Originally approved in 2008. Last previous edition approved in 2008 as D7284 –
ε1
08 . DOI: 10.1520/D7284-08E01.10.1520/D7284-13.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7284 − 13
3.2 Definitions:Definitions of Terms Specific to This Standard:
3.1.1 For definitions of terms used in this test method, refer to Terminology D1129 and Guide D6696.
3.2.1 total cyanide—Total cyanide is an analytically defined term that refers to the sum total of all of the inorganic chemical
forms of cyanide that dissociate and release free cyanide when refluxed under strongly acidic conditions. Total cyanide is
determined analytically through strong acid distillation or UV radiation followed by analysis of liberated free cyanide on aqueous
samples preserved with NaOH (pH~12). In water, total cyanide includes the following dissolved species: free cyanide, weak acid
dissociable metal cya
...
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