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ASTM D7284-08e1

(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 400 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 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 2 and Section 9.

General Information

Status
Historical
Publication Date
31-Mar-2008
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Replaces
ASTM D7284-08 - Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection
Effective Date
01-Apr-2008
Replaced By
ASTM D7284-13 - Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection
Effective Date
15-Jun-2013
Referred By
ASTM D7572-15(2022) - Standard Guide for Recovery of Aqueous Cyanides by Extraction from Mine Rock and Soil
Effective Date
01-Apr-2008
Referred By
ASTM D7365-09a(2022) - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
Effective Date
01-Apr-2008
Referred By
ASTM D8273-20 - Standard Practice for Determination of Total and Available Cyanide in Solid Waste and Soil after Alkaline Extraction
Effective Date
01-Apr-2008
Referred By
ASTM D7728-18 - Standard Guide for Selection of ASTM Analytical Methods for Implementation of International Cyanide Management Code Guidance
Effective Date
01-Apr-2008
Referred By
ASTM D2036-09(2022) - Standard Test Methods for Cyanides in Water
Effective Date
01-Apr-2008

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ASTM D7284-08e1 - Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric DetectionASTM D7284-08e1 - Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection
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ASTM D7284-08e1 - Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with 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
´1
Designation: D7284 − 08
StandardTest 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
´ NOTE—This Test Method was editorially corrected in September 2012.
1. Scope D2036 Test Methods for Cyanides in Water
D2777 Practice for Determination of Precision and Bias of
1.1 This test method is used to determine the concentration
Applicable Test Methods of Committee D19 on Water
of total cyanide in an aqueous wastewater or effluent. The
-
D3856 Guide for Management Systems in Laboratories
method detects the cyanides that are free (HCN and CN ) and
Engaged in Analysis of Water
strong-metal-cyanide complexes that dissociate and release
D5847 Practice for Writing Quality Control Specifications
free cyanide when refluxed under strongly acidic conditions.
for Standard Test Methods for Water Analysis
1.2 This method may not be applicable to process solutions
D6696 Guide for Understanding Cyanide Species
from precious metals mining operations.
D6888 Test Method for Available Cyanide with Ligand
1.3 This procedure is applicable over a range of approxi-
Displacement and Flow InjectionAnalysis (FIA) Utilizing
mately 2 to 400 µg/L (parts per billion) total cyanide. Higher
Gas Diffusion Separation and Amperometric Detection
concentrations can be measured with sample dilution or lower
D7365 Practice for Sampling, Preservation and Mitigating
injection volume.
Interferences in Water Samples for Analysis of Cyanide
1.4 The determinative step of this method utilizes flow
3. Terminology
injection with amperometric detection based on Test Method
D6888. Prior to analysis, samples must be distilled with a
3.1 Definitions:
micro-distillation apparatus described in this test method or
3.1.1 For definitions of terms used in this test method, refer
with a suitable cyanide distillation apparatus specified in Test
to Terminology D1129 and Guide D6696.
Methods D2036.
3.1.2 total cyanide—Total cyanide is an analytically defined
1.5 This standard does not purport to address all of the
term that refers to the sum total of all of the inorganic chemical
safety concerns, if any, associated with its use. It is the
forms of cyanide that dissociate and release free cyanide when
responsibility of the user of this standard to establish appro-
refluxed under strongly acidic conditions. Total cyanide is
priate safety and health practices and determine the applica-
determined analytically through strong acid distillation or UV
bility of regulatory limitations prior to use. Specific hazard
radiation followed by analysis of liberated free cyanide on
statements are given in Note 2 and Section 9.
aqueous samples preserved with NaOH (pH~12). In water,
total cyanide includes the following dissolved species: free
2. Referenced Documents
cyanide, weak acid dissociable metal cyanide complexes and
2
2.1 ASTM Standards:
strong metal cyanide complexes. Also, some of the strong
D1129 Terminology Relating to Water
metal cyanide complexes, such as those of gold, cobalt and
D1193 Specification for Reagent Water
platinum, might not be fully recovered during the total cyanide
analytical procedure. Additionally, total cyanide may also
include some organic forms of cyanide such as nitriles that
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
release free cyanide under the conditions of the analysis.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
Current edition approved April 1, 2008. Published April 2008. DOI: 10.1520/
4. Summary of Test Method
D7284-08E01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 The samples are distilled with a strong acid in the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
presence of magnesium chloride catalyst and captured in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sodium hydroxide absorber solution.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
´1
D7284 − 08
4.2 The absorber solution is introduced into a flow injection resulting in positive interference regardless of the determina-
analysis (FIA) system where it is acidified to form hydrogen tive step (amperometry, colorimetry, etc.). During acidic
cyanide (HCN). The
...

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Standard Practice for Estimation of Chlorine Demand of Water

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5.1 Chlorine is added to potable water, waste water, and industrial water for a variety of purposes. Some of these purposes are:  
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5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
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5.2 This method has been single-laboratory validated in reagent water and surface waters (Tables 12-14).
SCOPE
1.1 This test method covers a method for analysis of selected pesticides in a water matrix by filtration followed with liquid chromatography/electrospray ionization tandem mass spectrometry analysis. The samples are prepared in 20 % methanol, filtered, and analyzed by liquid chromatography/tandem mass spectrometry. This method was developed for an agricultural run-off study, not for low level analysis of pesticides in drinking water. This method may be modified for lower level analysis. The analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This standard contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community.  
1.3 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is adapted to report much lower or near the MDL then a MDL study would be warranted.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The Reporting Range for the target analytes are listed in Table 1.  
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8 mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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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