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ASTM D4165-06

(Test Method)

Standard Test Method for Cyanogen Chloride in Water

Standard Test Method for Cyanogen Chloride in Water

SIGNIFICANCE AND USE
The presence of cyanogen chloride in chlorinated sanitary and industrial effluents and therefore receiving waters is of concern because of its toxicity to aquatic life.
This test method provides an analytical procedure for measuring cyanogen chloride in water.
This test method is applicable for clean metal finishing and chlorinated sanitary and industrial effluents, and also can be used to establish process control of cyanide destruction by chlorination in waste water treatment facilities.
SCOPE
1.1 This test method covers the determination of cyanogen chloride in water. Cyanogen chloride is normally present only at very low concentrations; it is a very labile and sparsely soluble gaseous compound. Water samples may contain cyanogen chloride after the chlorination of waste waters containing cyanide or thiocyanate compounds.
1.2 Cyanogen chloride is unstable. A quick test using a spot plate or comparator as soon as the sample is collected may be the best test, reducing the loss of cyanogen chloride during the time lapse between sampling and analysis. (See for a typical decay curve for cyanogen chloride in a solution.)
1.3 This test method has been used successfully with reagent water. The analyst is responsible for determining whether the test method is applicable to the water matrix being tested. Reference is made to Test Method D of Test Methods D 2036 which is based on similar chemical reactions and has been evaluated by collaborative testing in this matrix.
1.4 The lower limit of detectability is 0.005 mg CN /L.
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 0 and Note 0 and Section .

General Information

Status
Historical
Publication Date
30-Jun-2006
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
Current Stage
Ref Project

Relations

Replaces
ASTM D4165-00 - Standard Test Method for Cyanogen Chloride in Water
Effective Date
01-Jul-2006
Replaced By
ASTM D4165-06(2012) - Standard Test Method for Cyanogen Chloride in Water 
Effective Date
15-Jun-2012
Referred By
ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
Effective Date
01-Jul-2006

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ASTM D4165-06 - Standard Test Method for Cyanogen Chloride in Water
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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: D4165 − 06
StandardTest Method for
1
Cyanogen Chloride in Water
This standard is issued under the fixed designation D4165; 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 D3856Guide for Management Systems in Laboratories
Engaged in Analysis of Water
1.1 This test method covers the determination of cyanogen
D4210Practice for Intralaboratory Quality Control Proce-
chloride in water. Cyanogen chloride is normally present only
dures and a Discussion on Reporting Low-Level Data
at very low concentrations; it is a very labile and sparsely
3
(Withdrawn 2002)
soluble gaseous compound. Water samples may contain cya-
D5789Practice for Writing Quality Control Specifications
nogen chloride after the chlorination of waste waters contain-
for Standard Test Methods for Organic Constituents
ing cyanide or thiocyanate compounds.
3
(Withdrawn 2002)
1.2 Cyanogen chloride is unstable.Aquick test using a spot
D5847Practice for Writing Quality Control Specifications
plate or comparator as soon as the sample is collected may be
for Standard Test Methods for Water Analysis
the best test, reducing the loss of cyanogen chloride during the
E60Practice for Analysis of Metals, Ores, and Related
time lapse between sampling and analysis. (See Fig. 1 for a
Materials by Spectrophotometry
typical decay curve for cyanogen chloride in a solution.)
E275PracticeforDescribingandMeasuringPerformanceof
Ultraviolet and Visible Spectrophotometers
1.3 This test method has been used successfully with
reagent water. The analyst is responsible for determining
3. Terminology
whetherthetestmethodisapplicabletothewatermatrixbeing
3.1 Definitions—For definitions of terms used in this test
tested. Reference is made to Test Method D of Test Methods
method, refer to Terminology D1129.
D2036 which is based on similar chemical reactions and has
been evaluated by collaborative testing in this matrix.
4. Summary of Test Method
−
1.4 The lower limit of detectability is 0.005 mg CN /L.
4.1 The water sample is mixed with a pyridine-barbituric
1.5 This standard does not purport to address all of the
acid solution and the color produced is measured with a
safety concerns, if any, associated with its use. It is the
spectrophotometer.
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
5.1 The presence of cyanogen chloride in chlorinated sani-
statements are given in Note 1 and Note 2 and Section 9.
taryandindustrialeffluentsandthereforereceivingwatersisof
concern because of its toxicity to aquatic life.
2. Referenced Documents
5.2 This test method provides an analytical procedure for
2
2.1 ASTM Standards:
measuring cyanogen chloride in water.
D1129Terminology Relating to Water
5.3 This test method is applicable for clean metal finishing
D1193Specification for Reagent Water
and chlorinated sanitary and industrial effluents, and also can
D2036Test Methods for Cyanides in Water
be used to establish process control of cyanide destruction by
D3370Practices for Sampling Water from Closed Conduits
chlorination in waste water treatment facilities.
6. Interferences
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
6.1 Color and turbidity can interfere.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
7. Apparatus
CurrenteditionapprovedJuly1,2006.PublishedJuly2006.Originallyapproved
in 1982. Last previous edition approved in 2000 as D4165–00. DOI: 10.1520/ 7.1 Spectrophotometer or Filter Photometer, suitable for
D4165-06.
measurementintheregionof578nm,using1.0-cmabsorption
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4165 − 06
−
8.5 Cyanide Solution, Stock (1 mL = 250 µg CN )—
Dissolve 0.6258 g of potassium cyanide (KCN) in 40 mL of
sodium hydroxide solution (40 g/L). Dilute to 1 L with water.
Mix thoroughly; standardize with standard silver nitrate solu-
tion (see Section 8 of Test Methods D2036).
NOTE 1—Warning: Because KCN is highly toxic, avoid contact or
inhalation.
...

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5.1 Chlorine is added to potable water, waste water, and industrial water for a variety of purposes. Some of these purposes are:  
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5.1 Home reverse osmosis devices are typically used to remove salts and other impurities from drinking water at the point of use. They are usually operated at tap water line pressure, with water containing up to several hundred milligrams per litre of total dissolved solids. This practice permits measurement of the performance of home reverse osmosis devices using a standard set of conditions and is intended for short-term testing (less than 24 h). This practice can be used to determine changes that may have occurred in the operating characteristics of home reverse osmosis devices during use, but it is not intended to be used for system design. This practice does not necessarily determine the device’s performance when solutes other than sodium chloride are present. Use Practice D4516 and Test Methods D4194 to standardize actual field data to a standard set of conditions.  
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5.1 A rapid and routine procedure for determining biomass of the living microorganisms in cultures, waters, wastewaters, and in plankton and periphyton samples taken from surface waters is frequently of vital importance. However, classical techniques such as direct microscope counts, turbidity, organic chemical analyses, cell tagging, and plate counts are expensive, time-consuming, or tend to underestimate total numbers. In addition, some of these methods do not distinguish between living and nonliving cells.  
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1.1 This test method covers a protocol for capturing, extracting and quantifying the cellular adenosine triphosphate (cATP) content associated with microorganisms normally found in laboratory cultures and waters in plankton and periphyton samples from waters.  
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5.1 This test method is useful for the analysis of total uranium in water following wet-ashing, as required, due to impurities or suspended materials in the water.
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1.1 This test method covers the determination of total uranium, by mass concentration, in water within the calibrated range of the instrument, 0.1 μg/L or greater. Samples with uranium mass concentrations above the laser phosphorimeter dynamic range are diluted to bring the concentration to a measurable level.  
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1.2 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.    
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Standard Test Method for Determination of Bisphenol A in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

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5.1 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.4 BPA has become an important high volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings and many other products.5  
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1.1 This test method covers the determination of bisphenol A (BPA) extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). BPA is qualitatively and quantitatively determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The Reporting Range for the target analytes are listed in Table 1.  
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5.1 NP and OP have been shown to have toxic effects in aquatic organisms. The source of NP and OP is prominently from the use of common commercial surfactants. The most widely used surfactant is nonylphenol ethoxylate (NPEO) which has an average ethoxylate chain length of nine. The ethoxylate chain is readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This method has been investigated and is applicable for environmental waters, including seawater.
SCOPE
1.1 This test method covers the determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.    
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

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