ASTM D8273-20

Standard Practice for Determination of Total and Available Cyanide in Solid Waste and Soil after Alkaline Extraction

SIGNIFICANCE AND USE
5.1 Cyanide and hydrogen cyanide are highly toxic. Regulations have been established requiring the measurement of cyanide in soil and solid waste samples. This practice is also useful for performing material balances to account for the distribution of cyanides in cyanidation products from metallurgical processes.  
5.2 This practice is applicable to the determination of available or total water soluble, or both, and water insoluble cyanides in soil and solid waste.  
5.3 Water insoluble cyanide complexes, such as Prussian blue, are not completely recovered by distillation methods. This practice extracts all cyanides, including the water insoluble cyanides such as Prussian blue, and then the extract solution can be analyzed for cyanide with Test Methods D6888, D7284, or D7511.
SCOPE
1.1 This practice is used for the determination of total or available cyanide in solid waste, sediment and soil samples after alkaline extraction. Simple cyanide (CN-) salts of group 1 and group 2 (alkali and alkaline earth) metals; soluble alkali and alkaline earth salts of zinc, copper, cadmium, mercury, nickel, silver, and iron cyanide complexes; and insoluble metal-metal cyanide complexes, such as Prussian blue, are quantitatively recovered. Gold, platinum group metals and cobalt cyanide complexes are not recovered during analysis.  
1.2 Free cyanide cannot be determined due to the change of equilibrium conditions during the extraction process.  
1.3 Cyanide complexes are extracted into an alkaline solution as described in this practice. Measure the total cyanide using Test Methods D7511 or D7284. Measure the available cyanide using Test Method D6888. Calculate cyanide content in the soil or waste.  
1.4 The method detection limit (MDL) is dependent on the test method used to measure the cyanide content. Based on the methods cited, it is approximately 1 mg/kg and the minimum level (ML) is 5 mg/kg. The applicable range is also dependent on the test method used to measure cyanide. Based on the methods cited, it is 5 to 100 mg/kg.  
1.5 This practice should be used by analysts experienced with extractions and flow injection analysis (FIA), or working under the close supervision of such qualified persons.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 This practice offers a set of instructions for performing one or more specific operations. This document cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this practice may be applicable in all circumstances. This ASTM standard is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this document be applied without consideration of a project’s many unique aspects. The word “Standard” in the title means only that the document has been approved through the ASTM consensus process.  
1.8 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 Section 9.  
1.9 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.

General Information

• Status: Published
• Publication Date: 31-Dec-2019
• ICS: 13.030.99 - Other standards related to wastes
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Refers: ASTM D6888-16(2023) - Standard Test Method for Available Cyanides with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
• Effective Date: 15-Nov-2023
• Refers: ASTM D6696-16(2023) - Standard Guide for Understanding Cyanide Species
• Effective Date: 15-Nov-2023
• Refers: ASTM D7284-20 - 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-Aug-2020
• Refers: ASTM D1129-13(2020)e2 - Standard Terminology Relating to Water
• Effective Date: 01-May-2020
• Refers: ASTM D7284-13(2017) - 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-Jul-2017
• Refers: ASTM D7511-12(2017)e1 - Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection
• Effective Date: 01-Jul-2017
• Refers: ASTM D6696-16 - Standard Guide for Understanding Cyanide Species
• Effective Date: 01-Apr-2016
• Refers: ASTM D6696-14 - Standard Guide for Understanding Cyanide Species
• Effective Date: 01-Jan-2014
• Refers: 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
• Refers: ASTM D7511-12 - Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection
• Effective Date: 01-Jan-2012
• Refers: ASTM D3856-11 - Standard Guide for Management Systems in Laboratories Engaged in Analysis of Water
• Effective Date: 15-Nov-2011
• Refers: ASTM D6696-10 - Standard Guide for Understanding Cyanide Species
• Effective Date: 01-Jun-2010
• Refers: ASTM D1129-10 - Standard Terminology Relating to Water
• Effective Date: 01-Mar-2010
• Refers: ASTM D7365-09a - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
• Effective Date: 01-Oct-2009
• Refers: ASTM D6888-09 - Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
• Effective Date: 01-Oct-2009

Overview

ASTM D8273-20 is the internationally recognized standard practice for the determination of total and available cyanide in solid waste, sediment, and soil after alkaline extraction. Developed and published by ASTM International, this standard addresses the critical need to accurately quantify cyanide concentrations for regulatory compliance, environmental protection, and process monitoring. Cyanide, including both simple cyanide salts and metal–cyanide complexes, is highly toxic, making precise measurement in environmental samples essential for safeguarding public health and environmental quality.

Key Topics

• Total and Available Cyanide Measurement: The practice outlines analytical procedures to determine both total and available (easily dissociable) cyanide after extraction from solid matrices using an alkaline solution.
• Wide Applicability: The method is suited for a range of samples, including solid waste, soils, and sediments, and is particularly valuable in environmental monitoring and management of contaminated sites.
• Comprehensive Extraction: Unlike traditional distillation-based protocols, ASTM D8273-20 achieves recovery of both water-soluble and water-insoluble cyanide complexes, including Prussian blue, thereby providing more complete cyanide quantification.
• Analytical Methods: Extracted solutions can be analyzed using referenced test methods (ASTM D6888, D7284, and D7511), employing flow injection analysis for robust and sensitive detection.
• Detection Limits and Quality Control: The method detection limit is approximately 1 mg/kg, with an applicable range generally between 5 and 100 mg/kg, depending on the analytical test method used. The document emphasizes the need for quality assurance practices, such as control samples and method blanks, to ensure accuracy and reliability.
• Health and Safety: Due to the high toxicity of cyanide and hydrogen cyanide, stringent safety protocols are emphasized throughout the practice, ensuring safe handling and proper disposal of chemicals.

Applications

• Regulatory Compliance: The standard is essential for laboratories and environmental professionals needing to meet legal requirements for cyanide analysis in soil and solid waste.
• Remediation Projects: Used in site assessments to determine the extent of cyanide contamination and to verify the effectiveness of cleanup activities.
• Metallurgical Process Monitoring: Enables the tracking and management of cyanide in byproducts and residues from mining and extraction processes, supporting industry best practices and material balance calculations.
• Environmental Risk Assessment: Provides reliable data supporting risk analyses for contaminated land and waste management, guiding protection measures for human health and ecosystems.
• Analytical Laboratories: Suitable for experienced analysts utilizing flow injection analysis (FIA) techniques for environmental monitoring and compliance testing.

Related Standards

• ASTM D6888 – Test Method for Available Cyanides with Ligand Displacement and Flow Injection Analysis
• ASTM D7284 – Test Method for Total Cyanide in Water by Micro Distillation and Flow Injection Analysis
• ASTM D7511 – Test Method for Total Cyanide by Segmented Flow Injection Analysis
• ASTM D1129 – Terminology Relating to Water
• ASTM D1193 – Specification for Reagent Water
• ASTM D3856 – Guide for Management Systems in Laboratories Engaged in Water Analysis
• ASTM D6696 – Guide for Understanding Cyanide Species in Mill and Heap Leach Solutions
• ASTM D5847 – Practice for Writing Quality Control Specifications for Water Analysis

Practical Value

ASTM D8273-20 is a cornerstone for laboratories, environmental consultants, and regulatory agencies involved in cyanide analysis. By ensuring reliable detection and quantification of both simple and complex cyanides in varied solid matrices, this standard supports regulatory compliance, environmental stewardship, and industrial safety. Its adoption promotes best practices in sample collection, extraction, analysis, and quality control, ultimately protecting public health and the environment from the dangers of cyanide contamination.

Keywords: ASTM D8273, total cyanide, available cyanide, alkaline extraction, cyanide in soil, cyanide in solid waste, environmental analysis, flow injection analysis, cyanide determination, cyanide standard, regulatory compliance.

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: D8273 − 20
Standard Practice for
Determination of Total and Available Cyanide in Solid Waste
and Soil after Alkaline Extraction
This standard is issued under the fixed designation D8273; 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 the adequacy of a given professional service must be judged,
nor should this document be applied without consideration of
1.1 This practice is used for the determination of total or
a project’s many unique aspects. The word “Standard” in the
available cyanide in solid waste, sediment and soil samples
- title means only that the document has been approved through
after alkaline extraction. Simple cyanide (CN ) salts of group 1
the ASTM consensus process.
and group 2 (alkali and alkaline earth) metals; soluble alkali
1.8 This standard does not purport to address all of the
and alkaline earth salts of zinc, copper, cadmium, mercury,
safety concerns, if any, associated with its use. It is the
nickel, silver, and iron cyanide complexes; and insoluble
responsibility of the user of this standard to establish appro-
metal-metal cyanide complexes, such as Prussian blue, are
priate safety and health practices and determine the applica-
quantitatively recovered. Gold, platinum group metals and
bility of regulatory limitations prior to use. Specific hazard
cobalt cyanide complexes are not recovered during analysis.
statements are given in Section 9.
1.2 Free cyanide cannot be determined due to the change of
1.9 This international standard was developed in accor-
equilibrium conditions during the extraction process.
dance with internationally recognized principles on standard-
1.3 Cyanide complexes are extracted into an alkaline solu-
ization established in the Decision on Principles for the
tion as described in this practice. Measure the total cyanide
Development of International Standards, Guides and Recom-
using Test Methods D7511 or D7284. Measure the available
mendations issued by the World Trade Organization Technical
cyanide using Test Method D6888. Calculate cyanide content
Barriers to Trade (TBT) Committee.
in the soil or waste.
2. Referenced Documents
1.4 The method detection limit (MDL) is dependent on the
test method used to measure the cyanide content. Based on the 2.1 ASTM Standards:
methods cited, it is approximately 1 mg/kg and the minimum D1129 Terminology Relating to Water
level (ML) is 5 mg/kg. The applicable range is also dependent D1193 Specification for Reagent Water
on the test method used to measure cyanide. Based on the D3856 Guide for Management Systems in Laboratories
methods cited, it is 5 to 100 mg/kg. Engaged in Analysis of Water
D4210 Practice for Intralaboratory Quality Control Proce-
1.5 This practice should be used by analysts experienced
dures and a Discussion on Reporting Low-Level Data
with extractions and flow injection analysis (FIA), or working
(Withdrawn 2002)
under the close supervision of such qualified persons.
D5847 Practice for Writing Quality Control Specifications
1.6 The values stated in SI units are to be regarded as
for Standard Test Methods for Water Analysis
standard. No other units of measurement are included in this
D6696 Guide for Understanding Cyanide Species
standard.
D6888 Test Method for Available Cyanides with Ligand
Displacement and Flow InjectionAnalysis (FIA) Utilizing
1.7 This practice offers a set of instructions for performing
one or more specific operations. This document cannot replace Gas Diffusion Separation and Amperometric Detection
D7284 Test Method for Total Cyanide in Water by Micro
educationorexperienceandshouldbeusedinconjunctionwith
professional judgment. Not all aspects of this practice may be Distillation followed by Flow InjectionAnalysis with Gas
Diffusion Separation and Amperometric Detection
applicable in all circumstances. This ASTM standard is not
intended to represent or replace the standard of care by which
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This practice is under the jurisdiction of ASTM Committee D19 on Water and contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Standards volume information, refer to the standard’s Document Summary page on
Organic Substances in Water. the ASTM website.
Current edition approved Jan. 1, 2020. Published February 2020. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D8273-20. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8273 − 20
D7365 Practice for Sampling, Preservation and Mitigating 6. Interference
Interferences in Water Samples for Analysis of Cyanide
6.1 Methodinterferencescanbecausedbycontaminationin
D7511 Test Method for Total Cyanide by Segmented Flow
the reagents, reagent water, glassware, etc., which may bias the
InjectionAnalysis, In-Line Ultraviolet Digestion andAm-
results. Take care to keep all such items from contaminants.
perometric Detection
6.2 Sulfide and sulfide-containing compounds interfere with
direct distillation methods; however, the preliminary extraction
3. Terminology
described in this practice only extracts soluble sulfides and
3.1 Definitions:
does not decompose metal-sulfide minerals. The reagents in
Test Methods D6888, D7284,or D7511 are capable of com-
3.1.1 For definitions of terms used in this standard, refer to
plexing up to 50 mg/L of sulfide.
Terminology D1129 and Guide D6696.
6.3 Many compounds that are known to cause interference
3.2 Definitions of Terms Specific to This Standard:
with distillation procedures do not interfere under the alkaline
3.2.1 available cyanide, n—cyanidesthatarefree(HCNand
-
extraction conditions of this practice.
CN ) and metal-cyanide complexes that are easily dissociated
into free cyanide ions. 6.4 See Test Methods D6888, D7284, and D7511 and
Practice D7365 for a more detailed discussion of interferences
3.2.1.1 Discussion—The method does not detect the less
and interference removal.
toxic strong metal-cyanide complexes, cyanides that are not
“amenable to chlorination.” Available cyanide determines the
7. Apparatus
same cyanide compounds determined as weak acid dissociable
(WAD) and as cyanide amenable to chlorination (CATC). 7.1 Refer to Test Methods D6888, D7284,or D7511 for
description of required apparatus.
3.2.2 total cyanide, n—inorganic cyanide containing com-
pounds in a sample, including free cyanide, available cyanide,
8. Reagents and Materials
strong metal cyanide complexes, and water and acid insoluble
8.1 Purity of Reagents—Reagent grade chemicals shall be
metal-metal cyanide complexes.
used in all tests. Unless otherwise indicated, it is intended that
3.2.2.1 Discussion—Analytically, gold, platinum group
all reagents shall conform to the specifications of theAmerican
metals, and cobalt cyanide complexes are not detected.
Chemical Society, where such specifications are available.
Other grades may be used, provided it is first ascertained that
4. Summary of Practice
the reagent is of sufficiently high purity to permit its use
4.1 A 1.00 6 0.05 g portion of the prepared sample is without lessening the accuracy of the determination.
measured into a 50-mL screw cap vial and extracted with 10
8.2 Purity of Water—Unless otherwise indicated, references
mLof 1 M Sodium Hydroxide Solution and mixed by shaking.
to water shall be understood to mean interference free reagent
Thesampleextractisfilteredanddilutedto200mLwithwater.
water conforming to Type I or Type II grade of Specification
An aliquot of the extract is injected into a flow injection
D1193.
analyzer (FIA) as described inTest Methods D6888, D7284,or
8.3 Sodium Hydroxide Solution (1 M)—Dissolve 40 g of
D7511. The cyanide extracted from the solid sample is calcu-
sodium hydroxide (NaOH) in laboratory water and dilute to 1
lated.
L.
4.2 Calibration and data are processed with the instrument’s
9. Hazards
data acquisition software.
9.1 Warning—Because of the toxicity of cyanide, great
5. Significance and Use
care must be exercised in its handling.Acidification of cyanide
solutions produces toxic hydrocyanic acid (HCN).All manipu-
5.1 Cyanide and hydrogen cyanide are highly toxic. Regu-
lations must be done in the hood so that any HCN gas that
lations have been established requiring the measurement of
might escape is safely vented.
cyanide in soil and solid waste samples. This practice is also
useful for performing material balances to account for the
9.2 Warning—Many of the reagents used in these test
distribution of cyanides in cyanidation products from metal-
methods are highly toxic. These reagents and their solutions
lurgical processes.
must be disposed of properly.
9.3 All reagents and standards should be prepared in vol-
5.2 This practice is applicable to the determination of
umesconsistentwithlaboratoryusetominimizethegeneration
available or t
...