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ASTM D4165-06(2012)

(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 Fig. 1 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 D2036 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.
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 1 and Note 2 and Section 9.
FIG. 1 Cyanogen Chloride Stability

General Information

Status
Historical
Publication Date
14-Jun-2012
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 D4165-06 - Standard Test Method for Cyanogen Chloride in Water
Effective Date
15-Jun-2012
Replaced By
ASTM D4165-06(2020)e1 - Standard Test Method for Cyanogen Chloride in Water 
Effective Date
01-Jan-2020
Referred By
ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
Effective Date
15-Jun-2012

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ASTM D4165-06(2012) - Standard Test Method for Cyanogen Chloride in Water ASTM D4165-06(2012) - Standard Test Method for Cyanogen Chloride in Water 
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ASTM D4165-06(2012) - 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 (Reapproved 2012)
Standard Test Method for
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
(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.
(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
2.1 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
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
Current edition approved June 15, 2012. Published August 2012. Originally
approved in 1982. Last previous edition approved in 2006 as D4165–06 DOI: 7.1 Spectrophotometer or Filter Photometer, suitable for
10.1520/D4165-06R12.
measurementintheregionof578nm,using1.0-cmabsorption
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
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
D4165 − 06 (2012)
−
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. Do not pipet by mouth (see Section 9).
−
8.5.1 Cyanide Solution I, Standard (1 mL=25 µg CN )
—Diluteacalculatedvolume(approximately100mL)ofKCN
stock solution to 1 L with NaOH solution (1.6 g/L).
−
8.5.2 Cyanide Solution II, Standard(1mL=2.5µgCN )—
Diluteexactly100mLofcyanideSolutionIto1LwithNaOH
solution (1.6 g/L).
−
8.5.3 Cyanide Solution III, Standard (1 mL=0.25 µg CN
)—Dilute exactly 100 mL of cyanide Solution II to 1 L with
NaOH solution (1.6 g/L). Prepare fresh solution daily and
protect from light.
8.6 Phosphate Buffer—Dissolve 138 g of sodium dihydro-
gen phosphate (NaH PO ·H O) in water and dilute to 1 L.
2 4 2
Refrigerate this solution.
8.7 Pyridine.
NOTE 2—Warning: Pyridine may cause irritation to the skin and
respiratory tract. Do not pipet by mouth (see Section 9).
8.8 Pyridine-Barbituric Acid Reagent—Place 15 g of barbi-
FIG. 1 Cyanogen Chloride Stability
turic acid in a 250-mL volumetric flask and add just enough
watertowashthesidesoftheflaskandwetthebarbituricacid.
Add 75 mL of pyridine and mix. Add 15 mL of hydrochloric
cells. Filter photometers and photometric practices used in this
acid (sp gr 1.19), mix, and cool to room temperature. Dilute to
testmethodshallconformtoPracticeE60.Spectrophotometers
volume with water and mix until all of the barbituric acid is
shall conform to Practice E275.
dissolved. This solution is usable for about 6 months if stored
in a cold, dark place.
8. Reagents
8.9 Sodium Hydroxide Solution (40 g/L)—Dissolve 40 g of
8.1 Purity of Reagents—Reagent grade chemicals shall be
sodium hydroxide in water and dilute to 1 L with water.
used in all tests. Unless otherwise indicated, it is intended that
8.10 Sodium Hydroxide Solution(1.6g/L)—Dilute40mLof
all reagents shall conform to the specifications of the Commit-
NaOH (40 g/L) solution to 1 L with water.
teeonAnalyticalReagentsoftheAmericanChem-icalSociety,
where such specifications are available. Other grades may be
9. Hazards
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the 9.1 Warning: Because of the toxicity of cyanogen chloride
accuracy of the determination. and cyanide, great care must be exercised in its handling.
Acidification of cyanide solutions produces toxic hydrocyanic
8.2 Purity of Water—Unless otherwise indicated, references
acid (HCN). All manipulations should be done in a well-
to water shall be understood to mean reagent water that meets
ventilatedhoodsothatanyHCNgasthatmightescapeissafely
thepurityspecificationsofTypeIorTypeIIwaterpresentedin
vented.
Specification D1193.
9.2 Warning:Manyofthereagentsusedinthistestmethod
8.3 Barbituric Acid.
are highly toxic. These reagents and their solutions must be
8.4 Chloramine-T Solution (10 g/L)—Dissolve 1.0 g of the
disposedofproperly(suchaspotassiumcyanideandpyridine).
white colored, water-soluble grade powder chloramine-T in
100 mL of water. Stor
...

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10 μg/L to 50 μg/L  
18 to 26  
1.2 The analyst should direct attention to the precision and bias statements for each test method. It is the user's responsibility to ensure the validity of these test methods for waters of untested matrices.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered 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. For specific hazard statements, see Section 12 and 24.4.  
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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ASTM
ASTM D3859-15(2023)(Test Method)
Standard Test Methods for Selenium in Water

SIGNIFICANCE AND USE
4.1 In most natural waters selenium concentrations seldom exceed 10 μg/L. However, the runoff from certain types of seleniferous soils at various times of the year can produce concentrations as high as several hundred micrograms per litre. Additionally, industrial contamination can be a significant source of selenium in rivers and streams.  
4.2 High concentrations of selenium in drinking water have been suspected of being toxic to animal life. Selenium is a priority pollutant and all public water agencies are required to monitor its concentration.  
4.3 These test methods determine the dominant species of selenium reportedly found in most natural and wastewaters, including selenities, selenates, and organo-selenium compounds.
SCOPE
1.1 These test methods cover the determination of dissolved and total recoverable selenium in most waters and wastewaters. Both test methods utilize atomic absorption procedures, as follows:    
Sections  
Test Method A—Gaseous Hydride AAS2, 3  
7 – 16  
Test Method B—Graphite Furnace AAS  
17 – 26  
1.2 These test methods are applicable to both inorganic and organic forms of dissolved selenium. They are applicable also to particulate forms of the element, provided that they are solubilized in the appropriate acid digestion step. However, certain selenium-containing heavy metallic sediments may not undergo digestion.  
1.3 These test methods are most applicable within the following ranges:    
Test Method A—Gaseous Hydride AAS2, 3  
1 μg/L to 20 μg/L  
Test Method B—Graphite Furnace AAS  
2 μg/L to 100 μg/L
These ranges may be extended (with a corresponding loss in precision) by decreasing the sample size or diluting the original sample, but concentrations much greater than the upper limits are more conveniently determined by flame atomic absorption spectrometry.  
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see 11.12 and 13.14.  
1.6 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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