ASTM D4193-08

Standard Test Method for Thiocyanate in Water

SIGNIFICANCE AND USE
This test method is useful for analysis of many natural waters that contain thiocyanate from organic decomposition products and waste water discharges. Some industrial wastes, such as those from the metallurgical processing of gold ores, steel industry, petroleum refining, and coal gasification, may contain significant concentrations of thiocyanate. Thiocyanate per se is not recognized as a toxic chemical compound. However, when chlorinated, thiocyanate is converted to the highly toxic and volatile cyanogen chloride at high pH. Oxidation of thiocyanate may also release toxic hydrogen cyanide. The user of the method is advised to perform holding time studies in accordance with Practice D 4841 whenever oxidants are present in the samples.
For information on the impact of cyanogens and cyanide compounds, see Appendix X1 of Test Method D 2036.
SCOPE
1.1 This test method covers the quantitative colorimetric laboratory measurement of dissolved thiocyanate in water, waste water, and saline water in the range from 0.1 to 2.0 mg/L. For higher concentrations, use an aliquot from the diluted sample.
1.1.1 Validation—This test method was validated over the range of 0.07 to 1.42 mg/L. This test method was validated at nine laboratories at four levels. This test method may be valid for reporting results down to lower levels as validated in individual user laboratories.
1.1.2 Application—This test method has been validated in reagent water, Type II, in multiple laboratories and 7 natural waters, 1 laboratory effluent, 1 steel mill effluent, and 2 dechlorinated and treated sanitary effluents in single laboratories. It is the user's responsibility to assure the validity of the test method on any untested matrices.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 Section 9.

General Information

• Status: Historical
• Publication Date: 30-Apr-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

Relations

• Replaces: ASTM D4193-02 - Standard Test Method for Thiocyanate in Water
• Effective Date: 01-May-2008
• Replaced By: ASTM D4193-08(2013)e1 - Standard Test Method for Thiocyanate in Water
• Effective Date: 01-Jun-2013
• Referred By: ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 01-May-2008

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: D4193 − 08
StandardTest Method for
1
Thiocyanate in Water
This standard is issued under the fixed designation D4193; 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* D1192Guide for Equipment for Sampling Water and Steam
3
in Closed Conduits (Withdrawn 2003)
1.1 This test method covers the quantitative colorimetric
D1193Specification for Reagent Water
laboratory measurement of dissolved thiocyanate in water,
D2036Test Methods for Cyanides in Water
wastewater,andsalinewaterintherangefrom0.1to2.0mg/L.
D2777Practice for Determination of Precision and Bias of
For higher concentrations, use an aliquot from the diluted
Applicable Test Methods of Committee D19 on Water
sample.
D3370Practices for Sampling Water from Closed Conduits
1.1.1 Validation—This test method was validated over the
D3856Guide for Management Systems in Laboratories
range of 0.07 to 1.42 mg/L. This test method was validated at
Engaged in Analysis of Water
nine laboratories at four levels. This test method may be valid
D4210Practice for Intralaboratory Quality Control Proce-
for reporting results down to lower levels as validated in
dures and a Discussion on Reporting Low-Level Data
individual user laboratories.
3
(Withdrawn 2002)
1.1.2 Application—This test method has been validated in
D4841Practice for Estimation of Holding Time for Water
reagent water, Type II, in multiple laboratories and 7 natural
Samples Containing Organic and Inorganic Constituents
waters, 1 laboratory effluent, 1 steel mill effluent, and 2
D5788Guide for Spiking Organics into Aqueous Samples
dechlorinated and treated sanitary effluents in single laborato-
D5789Practice for Writing Quality Control Specifications
ries. It is the user’s responsibility to assure the validity of the
for Standard Test Methods for Organic Constituents
test method on any untested matrices.
3
(Withdrawn 2002)
1.2 The values stated in SI units are to be regarded as
D5847Practice for Writing Quality Control Specifications
standard. No other units of measurement are included in this
for Standard Test Methods for Water Analysis
standard.
D7237Test Method for Free Cyanide with Flow Injection
1.3 This standard does not purport to address all of the
Analysis (FIA) Utilizing Gas Diffusion Separation and
safety concerns, if any, associated with its use. It is the Amperometric Detection
responsibility of the user of this standard to establish appro-
D7365Practice for Sampling, Preservation and Mitigating
priate safety and health practices and determine the applica- Interferences in Water Samples for Analysis of Cyanide
bility of regulatory limitations prior to use.Forspecifichazard
E60Practice for Analysis of Metals, Ores, and Related
statements, see Section 9. Materials by Spectrophotometry
E275PracticeforDescribingandMeasuringPerformanceof
2. Referenced Documents
Ultraviolet and Visible Spectrophotometers
2
2.1 ASTM Standards:
3. Terminology
D1129Terminology Relating to Water
3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology D1129.
1
4. Summary of Test Method
This test method is under the jurisdiction ofASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
4.1 This test method consists of thiocyanate reacting with
Organic Substances in Water.
ferric ions at a pH of<2to form a colored complex which is
Current edition approved May 1, 2008. Published June 2008. Originally
approved in 1982. Last previous edition approved in 2002 as D4193–02. DOI:
determined colorimetrically at 460 nm and adheres to Beer’s
10.1520/D4193-08.
Law.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on
The last approved version of this historical standard is referenced on
the ASTM website.
www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4193 − 08
4.2 Industrial wastes may be highly colored and contain 7. Apparatus
variousinterferingorganiccompoundswhichmustberemoved
7.1 Spectrophotometer or Filter Photometer, suitable for
4
by adsorption on macroreticular resin prior to analysis.
absorbance measurements at 460 nm and using a 5-cm cell.
Filter photometers and photometric practices used in this test
5. Significance and Use
method shall conform to Pract
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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:D 4193–02 Designation:D4193–08
Standard Test Method for
1
Thiocyanate in Water
This standard is issued under the fixed designation D4193; 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
1.1This test method covers the determination of dissolved thiocyanate in water, waste water, and saline water in the range from
0.1 to 2.0 mg/L. For higher concentrations, use an aliquot from the diluted sample.
1.2This test method has been used successfully with reagent grade, natural, and treated sanitary effluent waters. It is the user’s
responsibility to assure the validity of the test method on any untested matrices. *
1.1 Thistestmethodcoversthequantitativecolorimetriclaboratorymeasurementofdissolvedthiocyanateinwater,wastewater,
and saline water in the range from 0.1 to 2.0 mg/L. For higher concentrations, use an aliquot from the diluted sample.
1.1.1 Validation—This test method was validated over the range of 0.07 to 1.42 mg/L. This test method was validated at nine
laboratories at four levels.This test method may be valid for reporting results down to lower levels as validated in individual user
laboratories.
1.1.2 Application—This test method has been validated in reagent water,Type II, in multiple laboratories and 7 natural waters,
1 laboratory effluent, 1 steel mill effluent, and 2 dechlorinated and treated sanitary effluents in single laboratories. It is the user’s
responsibility to assure the validity of the test method on any untested matrices.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 hazards, see Section For specific hazard statements, see Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits
D1193 Specification for Reagent Water
D2036 Test Methods for Cyanides in Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D3856 Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
2
D4210Practice for Interlaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data 4210 Practice
for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
D5788 Guide for Spiking Organics into Aqueous Samples
D5789 Practice for Writing Quality Control Specifications for Standard Test Methods for Organic Constituents
3
D5847Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis 5847 Practice for
Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D7237 Test Method for Aquatic Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and
Amperometric Detection
D7365 Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
E60Practice for Molecular Absorption Spectrometric Methods for Chemical Analysis of Metals, Ores, and Related Materials
60 Practice for Analysis of Metals, Ores, and Related Materials by Molecular Absorption Spectrometry
E275 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 July 10, 2002. Published August 2002. Originally published as D4193–82. Last previous edition D4193–95.
Current edition approved May 1, 2008. Published June 2008. Originally approved in 1982. Last previous edition approved in 2002 as D4193–02.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatser
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