ASTM D6888-09
(Test Method)Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
SIGNIFICANCE AND USE
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.
This test method is applicable for natural water, saline waters, and wastewater effluent.
The method may be used for process control in wastewater treatment facilities.
SCOPE
1.1 This method is used to determine the concentration of available inorganic cyanide in an aqueous wastewater or effluent. The method detects the cyanides that are free (HCN and CN-) and metal-cyanide complexes that are easily dissociated into free cyanide ions. The method does not detect the less toxic strong metal-cyanide complexes, cyanides that are not “amenable to chlorination.”
1.2 Total cyanide can be determined for samples that have been distilled as described in Test Methods D 2036, Test Method A, Total Cyanides after Distillation. The cyanide complexes are dissociated and absorbed into the sodium hydroxide capture solution, which can be analyzed with this test method; therefore, ligand exchange reagents from Sections 8.12 and 8.13 would not be required when determining total cyanide after distillation.
1.3 This procedure is applicable over a range of approximately 2 to 400 μg/L (parts per billion) available cyanide. Higher concentrations can be analyzed by dilution or lower injection volume.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
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Designation: D6888 − 09
StandardTest Method for
Available Cyanide with Ligand Displacement and Flow
Injection Analysis (FIA) Utilizing Gas Diffusion Separation
1
and Amperometric Detection
This standard is issued under the fixed designation D6888; 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 2. Referenced Documents
2
1.1 This method is used to determine the concentration of
2.1 ASTM Standards:
available inorganic cyanide in an aqueous wastewater or
D1129 Terminology Relating to Water
effluent. The method detects the cyanides that are free (HCN
D1193 Specification for Reagent Water
-
and CN ) and metal-cyanide complexes that are easily disso-
D2036 Test Methods for Cyanides in Water
ciated into free cyanide ions. The method does not detect the
D2777 Practice for Determination of Precision and Bias of
less toxic strong metal-cyanide complexes, cyanides that are
Applicable Test Methods of Committee D19 on Water
not “amenable to chlorination.”
D3856 Guide for Management Systems in Laboratories
Engaged in Analysis of Water
1.2 Total cyanide can be determined for samples that have
D4375 Practice for Basic Statistics in Committee D19 on
been distilled as described in Test Methods D2036, Test
Water
Method A, Total Cyanides after Distillation. The cyanide
D5847 Practice for Writing Quality Control Specifications
complexes are dissociated and absorbed into the sodium
for Standard Test Methods for Water Analysis
hydroxide capture solution, which can be analyzed with this
D6696 Guide for Understanding Cyanide Species
test method; therefore, ligand exchange reagents from Sections
D7365 Practice for Sampling, Preservation and Mitigating
8.12 and 8.13 would not be required when determining total
Interferences in Water Samples for Analysis of Cyanide
cyanide after distillation.
E60 Practice for Analysis of Metals, Ores, and Related
1.3 This procedure is applicable over a range of approxi-
Materials by Spectrophotometry
mately 2 to 400 µg/L (parts per billion) available cyanide.
E275 PracticeforDescribingandMeasuringPerformanceof
Higher concentrations can be analyzed by dilution or lower
Ultraviolet and Visible Spectrophotometers
injection volume.
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions:
standard.
3.1.1 For definitions of terms used in this test method, refer
1.5 This standard does not purport to address all of the
to Terminology D1129 and Guide D6696.
safety concerns, if any, associated with its use. It is the
3.1.2 available cyanide, n—Inorganic cyanides that are free
responsibility of the user of this standard to establish appro-
-
(HCN and CN ) and metal-cyanide complexes that are easily
priate safety and health practices and determine the applica-
dissociated into free cyanide ions. Available cyanide does not
bility of regulatory limitations prior to use. Specific hazard
include the less toxic strong metal-cyanide complexes, cya-
statements are given in Note 2 and Section 9.
nides that are not “amenable to chlorination.”
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
2
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2009. Published October 2009. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2003. Last previous addition approved in 2004 as D6888 – 04. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D6888-09. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6888 − 09
FIG. 1 Flow Injection Analysis Apparatus 1
4. Summary of Test Method ricdetectorthatresultinaslightmaskingeffect(15 %negative
biaswith20ppbcyanidein1500ppmcarbonate).Referto11.2
4.1 Complex cyanides bound with nickel or mercury are
for sample pretreatment.
released by ligand displacement by the addition of a ligand
displacement agent prior to analysis.
6.2 Sulfide above 50 mg/L will diffuse through the gas
diffusion membrane and can be detected in the amperometric
4.2 Other weak and dissociable cyanide species do not
flowcell. Oxidized products of sulfide can also rapidly convert
require ligand displacement.
- -
CN to SCN at a high pH. Refer to Practice D7365 for sulfide
4.3 The treated sample is introduced into a flow i
...
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:D6888–04 Designation:D6888–09
Standard Test Method for
Available Cyanide with Ligand Displacement and Flow
Injection Analysis (FIA) Utilizing Gas Diffusion Separation
1
and Amperometric Detection
This standard is issued under the fixed designation D 6888; 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
1.1 Thismethodisusedtodeterminetheconcentrationofavailableinorganiccyanideinanaqueouswastewateroreffluent.The
-
methoddetectsthecyanidesthatarefree(HCNandCN )andmetal-cyanidecomplexesthatareeasilydissociatedintofreecyanide
ions. The method does not detect the less toxic strong metal-cyanide complexes, cyanides that are not “amenable to chlorination.”
1.2 Total cyanide can be determined for samples that have been distilled as described in Test Methods D 2036, Test MethodA,
Total Cyanides after Distillation.The cyanide complexes are dissociated and absorbed into the sodium hydroxide capture solution,
which can be analyzed with this test method; therefore, ligand exchange reagents from sections Sections 8.12 and 8.13 would not
be required when determining total cyanide after distillation.
1.3 This procedure is applicable over a range of approximately 2 to 400 µg/L (parts per billion) available cyanide. Higher
concentrations can be analyzed by dilution or lower injection volume.
1.4
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1129 Terminology Relating to Water
D 1193 Specification for Reagent Water
D 2036 Test Methods for Cyanides in Water
D 2777 Practice for Determination of Precision and Bias of Applicable Methods of Committee D19 on Water
D3370Practices for Sampling Water from Closed Conduits Practice for Determination of Precision and Bias ofApplicable Test
Methods of Committee D19 on Water
D 3856 Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water D4210Practice for
Intralaboratory
Quality Control
Procedures and
a Discussion on
Reporting Low-
Level Data
D 4375 Practice for Basic Statistics in Committee D19 on Water
D 5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D 6696 Guide for Understanding Cyanide Species
D 7365 Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
E60 Practice for Analysis of Metals, Ores, and Related Materials by Molecular Absorption Spectrometry
E 275 Practice for Describing and Measuring Performance of Ultraviolet, Visible, and Near Infrared Spectrophotometers
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 JuneOct. 1, 2004.2009. Published June 2004.October 2009. Originally approved in 2003. Last previous addition approved in 20032004 as
D6888—03.D 6888 – 04.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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 ----------------------
D6888–09
E1601Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method Practice for
Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D 1129 and Guide D 6696.
-
3.2 available cyanideavailable cyanide, n—Inorganic cyanides that are free (HCN and CN ) and metal-cyanide complexes that
are easily dissociated into free cyanide ions. Available cyanide does not include the
...
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