ASTM D4282-02

Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion

SIGNIFICANCE AND USE
This test method is useful in distinguishing between the potentially available free cyanide (total cyanide) and the free cyanide actually present.
This test method provides a convenient technique for making on-site free cyanide determinations.
SCOPE
1.1 This test method covers the determination of free cyanides in waters and wastewaters. Free cyanide is here defined as the cyanide which diffuses as cyanide (HCN), at room temperature, from a solution at pH 6.
1.2 This test method does not include complexes that resist dissociation, such as hexacyanoferrates and gold cyanide, nor does it include thiocyanate and cyanohydrin.
1.3 This test method may be applied to water and wastewater samples containing free cyanide from 10 to 150 μg/L. Greater concentrations may be determined by appropriate dilution.
1.4 This test method has been fully validated by collaborative testing as specified by Practice D 2777.
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. For specific hazard statements, see 8.6, 8.9, Section 9, and 12.2.1.

General Information

• Status: Historical
• Publication Date: 09-Jul-2002
• 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

Relations

• Replaces: ASTM D4282-95(2001) - Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion
• Effective Date: 10-Jul-2002
• Replaced By: ASTM D4282-02(2010) - Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion
• Effective Date: 15-Jun-2010
• Referred By: ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 10-Jul-2002
• Referred By: ASTM D7728-18 - Standard Guide for Selection of ASTM Analytical Methods for Implementation of International Cyanide Management Code Guidance
• Effective Date: 10-Jul-2002
• Referred By: ASTM D7365-09a(2022) - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
• Effective Date: 10-Jul-2002
• Referred By: ASTM D7572-15(2022) - Standard Guide for Recovery of Aqueous Cyanides by Extraction from Mine Rock and Soil
• Effective Date: 10-Jul-2002

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: D4282 – 02
Standard Test Method for
Determination of Free Cyanide in Water and Wastewater by
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Microdiffusion
This standard is issued under the fixed designation D4282; 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 D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.1 This test method covers the determination of free
D3370 Practices for Sampling Water from Closed Conduits
cyanides in waters and wastewaters. Free cyanide is here
D3856 Guide for Good Laboratory Practices in Laborato-
defined as the cyanide which diffuses as cyanide (HCN), at
2
ries Engaged in Sampling and Analysis of Water
room temperature, from a solution at pH 6.
D4210 Practice for Intralaboratory Quality Control Proce-
1.2 This test method does not include complexes that resist
4
dures and a Discussion on Reporting Low-Level Data
dissociation, such as hexacyanoferrates and gold cyanide, nor
D5788 Guide for Spiking Organics into Aqueous Samples
does it include thiocyanate and cyanohydrin.
D5789 Practice for Writing Quality Control Specifications
1.3 This test method may be applied to water and wastewa-
4
for Standard Test Methods for Organic Constituents
ter samples containing free cyanide from 10 to 150 µg/L.
D5847 Practice for Writing Quality Control Specifications
Greater concentrations may be determined by appropriate
for Standard Test Methods for Water Analysis
dilution.
E275 Practice for Describing and Measuring Performance
1.4 This test method has been fully validated by collabora-
of Ultraviolet and Visible Spectrophotometers
tive testing as specified by Practice D2777.
1.5 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 For a definition of terms used in this test method refer
priate safety and health practices and determine the applica-
to Terminology D1129.
bility of regulatory limitations prior to use. For specific hazard
3.2 Definitions of Terms Specific to This Standard:
statements, see 8.6, 8.9, Section 9, and 12.2.1.
3.2.1 free cyanide—refers to those simple cyanides or
2. Referenced Documents looselyheldcomplexesofcyanidethatdiffuseatpH6,atroom
3
temperature.
2.1 ASTM Standards:
D1129 Terminology Relating to Water
4. Summary of Test Method
D1192 GuideforEquipmentforSamplingWaterandSteam
4 4.1 The reactions are carried out in a microdiffusion cell.
in Closed Conduits
4.2 The sample is treated with cadmium ion to precipitate
D1193 Specification for Reagent Water
the hexacyanoferrates.
4.3 The sample is buffered at pH 6 and allowed to stand for
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
4h.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
4.4 The HCN diffuses into sodium hydroxide solution.
Organic Substances in Water.
4.5 An aliquot of the sodium hydroxide solution is treated
Current edition approved July 10, 2002. Published August 2002. Originally
published as D4282–83. Last previous edition D4282–95(2001). DOI: 10.1520/ with chloramine-T, and the cyanogen chloride formed is
D4282-02.
reacted with barbituric acid in pyridine. The absorbance of the
2
The paper by J. M. Kruse and L. E. Thibault “Determination of Free Cyanide
color formed is measured using a spectrophotometer at a
in Ferro- and Ferricyanides,”Analytical Chemistry, 45(13): 2260–2261; 1973 Nov.,
wavelength of 580 nm.
recommendsadiffusionatpH7.TheANSImodification(ANSIPH4.41-1978)uses
pH 6. Using the conditions of the ANSI method, diffusion is completed within 4
hoursatpH6.LongerdiffusiontimewasrequiredatpH7onthesamplesanalyzed. 5. Significance and Use
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.1 This test method is useful in distinguishing between the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
potentially available free cyanide (total cyanide) and the free
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
cyanide actually present.
4
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4282 – 02
5.2 This test method provides a convenient technique for 8.6 Cyanide Solution Stock—Dissolve 2.51 g of potassium
making on-site free cyanide determination
...