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ASTM D4165-00

(Test Method)

Standard Test Method for Cyanogen Chloride in Water

Standard Test Method for Cyanogen Chloride in Water

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 Notes 1 and 2 and Section 9.

General Information

Status
Historical
Publication Date
09-Jun-2000
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

Replaced By
ASTM D4165-06 - Standard Test Method for Cyanogen Chloride in Water
Effective Date
01-Jul-2006
Referred By
ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
Effective Date
10-Jun-2000

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ASTM D4165-00 - Standard Test Method for Cyanogen Chloride in Water
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
Designation:D 4165–00
Standard Test Method for
Cyanogen Chloride in Water
This standard is issued under the fixed designation D 4165; 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 (e) indicates an editorial change since the last revision or reapproval.
1. 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
solublegaseouscompound.Watersamplesmaycontaincyano-
gen chloride after the chlorination of waste waters containing
cyanide or thiocyanate compounds.
1.2 Cyanogen chloride is unstable.Aquick 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
whetherthetestmethodisapplicabletothewatermatrixbeing
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 appro-
priate safety and health practices and determine the applica-
bility 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
2. Referenced Documents
2.1 ASTM Standards:
D 5789 Practice for Writing Quality Control Specifications
D 1129 Terminology Relating to Water
for Standard Test Methods for Organic Constituents
D 1193 Specification for Reagent Water
D 5847 Practice for Writing Quality Control Specifications
D 2036 Test Methods for Cyanides in Water
for Standard Test Methods for Water Analysis
D 3370 Practices for Sampling Water from Closed Con-
E 60 Practice for Photometric and Spectrophotometric
duits
Methods for Chemical Analysis of Metals
D 3856 Guide for Good Laboratory Practices in Laborato-
E 275 Practice for Describing and Measuring Performance
ries Engaged in Sampling and Analysis of Water
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
D 4210 Practice for Interlaboratory Quality Control Proce-
eters
dures and a Discussion on Reporting Low-Level Data
3. Terminology
3.1 Definitions—For definitions of terms used in this test
This test method is under the jurisdiction ofASTM Committee D-19 on Water
method, refer to Terminology D1129.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
Current edition approved June 10, 2000. Published July 2000. Originally
published as D4165–82. Last previous edition D4165–95.
2 4
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 03.05.
3 5
Annual Book of ASTM Standards, Vol 11.02. Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4165–00
−
4. Summary of Test Method 8.5.1 Cyanide Solution I, Standard (1 mL=25 µg CN )—
Dilute a calculated volume (approximately 100 mL) of KCN
4.1 The water sample is mixed with a pyridine-barbituric
stock solution to 1 L with NaOH solution (1.6 g/L).
acid solution and the color produced is measured with a
−
8.5.2 Cyanide Solution II, Standard(1mL=2.5µgCN )—
spectrophotometer.
Diluteexactly100mLofcyanideSolutionIto1LwithNaOH
solution (1.6 g/L).
5. Significance and Use
8.5.3 Cyanide Solution III, Standard (1 mL = 0.25 µg
5.1 The presence of cyanogen chloride in chlorinated sani-
−
CN )—Dilute exactly 100 mL of cyanide Solution II to 1 L
taryandindustrialeffluentsandthereforereceivingwatersisof
with NaOH solution (1.6 g/L). Prepare fresh solution daily and
concern because of its toxicity to aquatic life.
protect from light.
5.2 This test method provides an analytical procedure for
8.6 Phosphate Buffer— Dissolve 138 g of sodium dihydro-
measuring cyanogen chloride in water.
gen phosphate (NaH PO ·H O) in water and dilute to 1 L.
2 4 2
5.3 This test method is applicable for clean metal finishing
Refrigerate this solution.
and chlorinated sanitary and industrial effluents, and also can
8.7 Pyridine.
be used to establish process control of cyanide destruction by
chlorination in waste water treatment facilities. NOTE 2—Warning:Pyridine may cause irritation to the skin and
respiratory tract. Do not pipet by mouth (see Section 9).
6. Interferences
8.8 Pyridine-Barbituric Acid Reagent—Place 15 g of bar-
bituric acid in a 250-mL volumetric flask and add just enough
6.1 Color and turbidity can interfere.
water to wash the sides of the flask and wet the barbituric acid.
Add 75 mL of pyridine and mix. Add 15 mL of hydrochloric
7. Apparatus
acid (sp gr 1.19), mix, and cool to room temperature. Dilute to
7.1 Spectrophotometer or Filter Photometer, suitable for
volume with water and mix until all of the barbituric acid is
measurementintheregionof578nm,using1.0-cmabsorption
dissolved. This solution is usable for about 6 months if stored
cells. Filter photometers and photometric practices used in this
in a cold, dark place.
test method shall conform to Practice E60. Spectrophotom-
8.9 Sodium Hydroxide Solution (40 g/L)—Dissolve 40 g of
eters shall conform to Practice E275.
sodium hydroxide in water and dilute to 1 L with water.
8.10 Sodium Hydroxide Solution (1.6 g/L)—Dilute 40 mL
8. Reagents
of NaOH (40 g/L) solution to 1 L with water.
8.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
9. Hazards
all reagents shall conform to the specifications of the Commit-
9.1 Warning: Because of the toxicity of cyanogen chloride
teeonAnalyticalReagentsoftheAmericanChem-icalSociety,
and cyanide, great care must be exercised in its handling.
where such specifications are available. Other grades may be
Acidification of cyanide solutions produces toxic hydrocyanic
used, provided it is first ascertained that the reagent is of
acid (HCN). All manipulations should be done in a well-
sufficiently high purity to permit its use without lessening the
ventilatedhoodsothatanyHCNgasthatmightescapeissafely
accuracy of the determination.
vented.
8.2 Purity of Water— Unless otherwise indicated, refer-
9.2 Warning:Manyofthereagentsusedinthistestmethod
ences to water shall be understood to mean reagent water
are highly toxic. These reagents and their solutions must be
conforming to Type II grade of Specification D1193.
disposedofproperly(suchaspotassiumcyanideandpyridine).
8.3 Barbituric Acid.
8.4 Chloramine-T Solution (10 g/L)—Dissolve 1.0 g of the
10. Sampling and Sample Preservation
white colored, water-soluble grade powder chloramine-T in
10.1 Collect the sample in accordance with Practices
100 mL of water. Store in an amber bottle under refrigeration.
D3370.
Prepare fresh weekly.
10.2 Collect a separate sample in a closed container. DO
−
8.5 Cyanide Solution, Stock (1 mL = 250 µg CN )—
NOTADD NaOH, as cyanogen chloride will b
...

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4.1 Most waters rarely contain more than trace concentrations of cobalt from natural sources. Although trace amounts of cobalt seem to be essential to the nutrition of some animals, large amounts have pronounced toxic effects on both plant and animal life.
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1.1 These test methods cover the determination of dissolved and total recoverable cobalt in water and wastewater 2 by atomic absorption spectrophotometry. Three test methods are included as follows:    
Concentration Range  
Sections  
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0.1 mg/L to 10 mg/L  
7 to 16  
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10 μg/L to 1000 μg/L  
17 to 26  
Test Method C—Atomic Absorption, Graphite Furnace  
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27 to 36  
1.2 Test Method A has been used successfully with reagent water, potable water, river water, and wastewater. Test Method B has been used successfully with reagent water, potable water, river water, sea water and brine. Test Method C was successfully evaluated in reagent water, artificial seawater, river water, tap water, and a synthetic brine. It is the analyst's responsibility to ensure the validity of these test methods for other matrices.  
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ASTM D3859-15(2023)(Test Method)
Standard Test Methods for Selenium in Water

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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.
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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  
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7 – 16  
Test Method B—Graphite Furnace AAS  
17 – 26  
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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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ASTM
ASTM D4190-15(2023)(Test Method)
Standard Test Method for Elements in Water by Direct-Current Plasma Atomic Emission Spectroscopy

SIGNIFICANCE AND USE
5.1 This test method is useful for the determination of element concentrations in many natural waters. It has the capability for the simultaneous determination of up to 15 separate elements. High analysis sensitivity can be achieved for some elements, such as boron and vanadium.
SCOPE
1.1 This test method covers the determination of dissolved and total recoverable elements in water, which includes drinking water, lake water, river water, sea water, snow, and Type II reagent water by direct current plasma atomic emission spectroscopy (DCP).  
1.2 The information on precision and bias may not apply to other waters.  
1.3 This test method is applicable to the 15 elements listed in Annex A1 (Table A1.1) and covers the ranges in Table 1.  
1.4 This test method is not applicable to brines unless the sample matrix can be matched or the sample can be diluted by a factor of 200 up to 500 and still maintain the analyte concentration above the detection limit.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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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