Standard Test Methods for Cyanides in Water

SIGNIFICANCE AND USE
Cyanide is highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastes and in surface waters (Appendix X1).
Test Method D is applicable for natural water and clean metal finishing or heat treatment effluents. It may be used for process control in wastewater treatment facilities providing its applicability has been validated by Test Method B or C.
The spot test outlined in Annex A1 can be used to detect cyanide and thiocyanate in water or wastewater, and to approximate its concentration.
SCOPE
1.1 These test methods cover the determination of cyanides in water. The following test methods are included:
  Sections Test Method A—Total Cyanides after Distillation12 to 18 Test Method B—Cyanides Amenable to Chlorination by Difference19 to 25 Test Method C—Weak Acid Dissociable Cyanides26 to 32 Test Method D—Cyanides Amenable to Chlorination without Distillation (Short-Cut Method)33 to 39
1.2 Cyanogen halides may be determined separately.
Note 1—Cyanogen chloride is the most common of the cyanogen halide complexes as it is a reaction product and is usually present when chlorinating cyanide-containing industrial waste water. For the presence or absence of CNCl, the spot test method given in Annex A1 can be used.  
1.3 These test methods do not distinguish between cyanide ions and metallocyanide compounds and complexes. Furthermore, they do not detect the cyanates. Cyanates can be determined using ion chromatography without digestion.
Note 2—The cyanate complexes are decomposed when the sample is acidified in the distillation procedure.  
1.4 The cyanide in cyanocomplexes of gold, platinum, cobalt and some other transition metals is not completely recovered by these test methods. Refer to Test Method D6994 for the determination of cyanometal complexes.
1.5 Cyanide from only a few organic cyanides are recovered, and those only to a minor extent.
1.6 Part or all of these test methods have been used successfully with reagent water and various waste waters. It is the user's responsibility to assure the validity of the test method for the water matrix being tested.
1.7 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 sections 5.1, 8.8, 8.18, 9, 11.3, and 16.1.9.  
12.1 This test method covers the determination of cyanides in water, including the iron cyanide complexes (total cyanide).
12.2 The cyanide in some cyano complexes of transition metals, for example, cobalt, gold, platinum, etc., is not determined.
12.3 The cyanide concentration can be determined with titration, IC-PAD, colorimetric, selective ion electrode procedure, or flow injection analysis with gas diffusion separation and amperometric detection as described in Test Method D6888.
12.4 This test method has been used successfully on reagent and surface water and coke plant, refinery, and sanitary waste waters. It is the user's responsibility to assure the validity of the test method for the water matrix being tested.
12.5 Because of the sample preservation, certain suspended and/or colloidal forms of metal cyanide complexes such as those from iron and copper will dissolve prior to the distillation step. The recovery of this cyanide may depend on solution parameters such as the cyanide concentration in suspended solids, ionic strength of the sample, sample temperature, acid digestion times, and so forth.  
19.1 This test method covers the determination of cyanides amenable to chlorination in water.
19.2 Iron cyanides are the most commonly encountered compounds not amenable to chlorination.
19.3 This test method has been used on reagent, surface, and industrial waste waters. It is the ...

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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: D2036 − 09
StandardTest Methods for
1
Cyanides in Water
This standard is issued under the fixed designation D2036; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover the determination of cyanides
responsibility of the user of this standard to establish appro-
in water. The following test methods are included:
priate safety and health practices and determine the applica-
Sections
bility of regulatory limitations prior to use. Specific hazard
Test Method A—Total Cyanides after 12 to 18
Distillation statements are given in sections 5.1, 8.8, 8.18, 9, 11.3, and
Test Method B—Cyanides Amenable 19 to 25
16.1.9.
2
to Chlorination by Difference
Test Method C—Weak Acid 26 to 32
2. Referenced Documents
Dissociable Cyanides
Test Method D—Cyanides Amenable 33 to 39 3
2.1 ASTM Standards:
to Chlorination without Distillation
D1129Terminology Relating to Water
(Short-Cut Method)
D1193Specification for Reagent Water
1.2 Cyanogen halides may be determined separately.
D2777Practice for Determination of Precision and Bias of
NOTE 1—Cyanogen chloride is the most common of the cyanogen
Applicable Test Methods of Committee D19 on Water
halide complexes as it is a reaction product and is usually present when
D3370Practices for Sampling Water from Closed Conduits
chlorinating cyanide-containing industrial waste water. For the presence
D5788Guide for Spiking Organics into Aqueous Samples
or absence of CNCl, the spot test method given in AnnexA1 can be used.
D5847Practice for Writing Quality Control Specifications
1.3 These test methods do not distinguish between cyanide
for Standard Test Methods for Water Analysis
ions and metallocyanide compounds and complexes.
D6696Guide for Understanding Cyanide Species
Furthermore, they do not detect the cyanates. Cyanates can be
D6888Test Method for Available Cyanide with Ligand
determined using ion chromatography without digestion.
DisplacementandFlowInjectionAnalysis(FIA)Utilizing
NOTE 2—The cyanate complexes are decomposed when the sample is
Gas Diffusion Separation and Amperometric Detection
acidified in the distillation procedure.
D6994Test Method for Determination of Metal Cyanide
1.4 The cyanide in cyanocomplexes of gold, platinum, Complexes in Wastewater, Surface Water, Groundwater
cobalt and some other transition metals is not completely
and Drinking Water Using Anion Exchange Chromatog-
recovered by these test methods. Refer to Test Method D6994 raphy with UV Detection
for the determination of cyanometal complexes.
D7284Test Method for Total Cyanide in Water by Micro
Distillation followed by Flow InjectionAnalysis with Gas
1.5 Cyanide from only a few organic cyanides are
Diffusion Separation and Amperometric Detection
recovered, and those only to a minor extent.
D7365Practice for Sampling, Preservation and Mitigating
1.6 Part or all of these test methods have been used
Interferences in Water Samples for Analysis of Cyanide
successfully with reagent water and various waste waters. It is
D7511Test Method for Total Cyanide by Segmented Flow
the user’s responsibility to assure the validity of the test
InjectionAnalysis, In-Line Ultraviolet Digestion andAm-
method for the water matrix being tested.
perometric Detection
E60Practice for Analysis of Metals, Ores, and Related
1
These test methods are under the jurisdiction of ASTM Committee D19 on
Materials by Spectrophotometry
Water and are the direct responsibility of Subcommittee D19.06 on Methods for
E275PracticeforDescribingandMeasuringPerformanceof
Analysis for Organic Substances in Water.
Ultraviolet and Visible Spectrophotometers
Current edition approved Oct. 1, 2009. Published October 2009. Originally
approved in 1964. Last previous edition approved in 2006 as D2036–06. DOI:
10.1520/D2036-09.
2 3
For an explanation of the term cyanides amenable to alkaline chlorination, see For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Lancy, L. E. and Zabban, W., “Analytical Methods and Instrumentation for contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Determining Cyanogen Compounds,” Papers on Industrial Water and Industrial Standards volume information, refer to the standard’s Document Summary page on
Waste Water, ASTM STP 337, 1962, pp. 32–45. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D2036–06 Designation:D2036–09
Standard Test Methods for
1
Cyanides in Water
This standard is issued under the fixed designation D2036; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
1.1 These test methods cover the determination of cyanides in water. The following test methods are included:
Sections
Test Method A—Total Cyanides after 12 to 18
Distillation
Test Method B—Cyanides Amenable 19 to 25
2
to Chlorination by Difference
Test Method C—Weak Acid Disso- 26 to 32
ciable Cyanides
Test Method D—Cyanides Amenable 33 to 39
to Chlorination without Distillation
(Short-Cut Method)
1.2 Cyanogen halides may be determined separately.
NOTE 1—Cyanogenchlorideisthemostcommonofthecyanogenhalidecomplexesasitisareactionproductandisusuallypresentwhenchlorinating
cyanide-containing industrial waste water. For the presence or absence of CNCl, the spot test method given in Annex A1 can be used.
1.3 These test methods do not distinguish between cyanide ions and metallocyanide compounds and complexes. Furthermore,
they do not detect the cyanates. Cyanates can be determined using ion chromatography without digestion.
NOTE 2—The cyanate complexes are decomposed when the sample is acidified in the distillation procedure.
1.4The cyanide in cyanocomplexes of gold, platinum, cobalt and some other transition metals is not completely recovered by
these test methods.
1.4 The cyanide in cyanocomplexes of gold, platinum, cobalt and some other transition metals is not completely recovered by
these test methods. Refer to Test Method D6994 for the determination of cyanometal complexes.
1.5 Cyanide from only a few organic cyanides are recovered, and those only to a minor extent.
1.6Part1.6 Part or all of these test methods have been used successfully with reagent water and various waste waters. It is the
user’s responsibility to assure the validity of the test method for the water matrix being tested.
1.7 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 sections 5.1, 8.8, 8.18, 9, 11.211.3, and 16.1.9.
2. Referenced Documents
3
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water D3370
D3370 Practices for Sampling Water from Closed Conduits
D5788 Guide for Spiking Organics into Aqueous Samples
1
These test methods are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.06 on Methods for Analysis
for Organic Substances in Water.
Current edition approved Feb. 15, 2006. Published February 2006. Originally approved in 1964. Last previous edition approved in 1998 as D2036–98. DOI:
10.1520/D2036-06.
Current edition approved Oct. 1, 2009. Published October 2009. Originally approved in 1964. Last previous edition approved in 2006 as D2036–06. DOI:
10.1520/D2036-09.
2
For an explanation of the term cyanides amenable to alkaline chlorination, see Lancy, L. E. and Zabban, W., “Analytical Methods and Instrumentation for Determining
Cyanogen Compounds,” Papers on Industrial Water and Industrial Waste Water, ASTM STP 337, 1962, pp. 32–45.
3
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book ofASTM 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

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D2036–09
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
D6994 Test Method for Determination of Metal Cyanide Complexe
...

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