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ASTM D4193-02

(Test Method)

Standard Test Method for Thiocyanate in Water

Standard Test Method for Thiocyanate in Water

SIGNIFICANCE AND USE
Many natural waters contain thiocyanate from organic decomposition products and waste water discharges. Some industrial wastes, such as those from the 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.
5.1.1 For information on the impact of cyanogen compounds, see Appendix X1 of Test Method D 2036.
SCOPE
1.1 This 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.
1.2 This 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.
1.3 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 9.

General Information

Status
Historical
Publication Date
09-Jul-2002
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 D4193-95 - Standard Test Method for Thiocyanate in Water
Effective Date
10-Jul-2002
Replaced By
ASTM D4193-08 - Standard Test Method for Thiocyanate in Water
Effective Date
01-May-2008
Referred By
ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
Effective Date
10-Jul-2002

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ASTM D4193-02 - Standard Test Method for Thiocyanate 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D 4193–02
Standard Test Method for
1
Thiocyanate in Water
This standard is issued under the fixed designation D 4193; 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 E60 Practice for Molecular Absorption Spectrometric
Methods for Chemical Analysis of Metals, Ores, and
1.1 This test method covers the determination of dissolved
4
Related Materials
thiocyanateinwater,wastewater,andsalinewaterintherange
E 275 Practice for Describing and Measuring Performance
from0.1to2.0mg/L.Forhigherconcentrations,useanaliquot
of Ultraviolet, Visible, and Near-Infrared Spectrophotom-
from the diluted sample.
5
eters
1.2 This test method has been used successfully with
reagentgrade,natural,andtreatedsanitaryeffluentwaters.Itis
3. Terminology
the user’s responsibility to assure the validity of the test
3.1 Definitions—For definitions of terms used in this test
method on any untested matrices.
method, refer to Terminology D1129.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Thiocyanate reacts with ferric ions at a pH of<2to
priate safety and health practices and determine the applica-
form a colored complex which is determined colorimetrically
bility of regulatory limitations prior to use. For specific
at 460 nm and adheres to Beer’s Law.
hazards, see Section 9.
4.2 Industrial wastes may be highly colored and contain
2. Referenced Documents variousinterferingorganiccompoundswhichmustberemoved
6
by adsorption on macroreticular resin prior to analysis.
2.1 ASTM Standards:
2
D 1129 Terminology Relating to Water
5. Significance and Use
D 1192 Guide for Equipment for Sampling Water and
2 5.1 Many natural waters contain thiocyanate from organic
Steam in Closed Conduits
decomposition products and waste water discharges. Some
2
D 1193 Specification for Reagent Water
3 industrial wastes, such as those from the steel industry,
D 2036 Test Methods for Cyanides in Water
petroleum refining, and coal gasification, may contain signifi-
D 3370 Practices for Sampling Water from Closed Con-
2 cant concentrations of thiocyanate. Thiocyanate per se is not
duits
recognized as a toxic chemical compound. However, when
D 3856 Guide for Good Laboratory Practices in Laborato-
2 chlorinated, thiocyanate is converted to the highly toxic and
ries Engaged in Sampling and Analysis of Water
volatile cyanogen chloride.
D 4210 Practice for Interlaboratory Quality Control Proce-
2 5.1.1 For information on the impact of cyanogen com-
dures and a Discussion on Reporting Low-Level Data
pounds, see Appendix X1 of Test Method D2036.
3
D 5788 Guide for Spiking Organics intoAqueous Samples
D 5789 Practice for Writing Quality Control Specifications
6. Interferences
3
for Standard Test Methods for Organic Constituents
6.1 Hexavalent chromium interference is removed by ad-
D 5847 Practice for Writing Quality Control Specifications
3 justing the pH to 2 with concentrated nitric acid and adding
for Standard Test Methods for Water Analysis
ferroussulfate.RaisingthepHto8.5-9withsodiumhydroxide
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
4
Organic Substances in Water. Annual Book of ASTM Standards, Vol 03.05.
5
Current edition approved July 10, 2002. Published August 2002. Originally Annual Book of ASTM Standards, Vol 03.06.
6
published as D4193–82. Last previous edition D4193–95. Spencer, R. R., Leenheer, J., and Marti, V. C., “Automated Colorimetric
2
Annual Book of ASTM Standards, Vol 11.01. Determination of Thiocyanate, Thiosulfate, and Tetrathionate in Water,’’ AOAC
3
Annual Book of ASTM Standards, Vol 11.02. 94th Annual Meeting, Washington, DC, 1980.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 4193–02
precipitates Fe (III) and Cr (III) as the hydroxides, which are 8.10 NitricAcid (0.1 M)—Mix6.4mLofconcentratednitric
removed by filtration. acid in about 800 mL of water. Dilute to 1 L with water and
6.2 Reducing agents that reduce Fe (III) to Fe (II), thus mix.
−
preventing formation of the ferric thiocyanate complex, are 8.11 Thiocyanate Solution, Stock (1 mL = 1.0 mg SCN )—
destroyed by a few drops of hydrogen peroxide. Dissolve 1.673 g of potassium thiocyanate (KSCN) in water
6.3 High concentrations of cyanide in proportion to the and dilute to 1 L.
concentrati
...

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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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ASTM D1291-17(2023)(Practice)
Standard Practice for Estimation of Chlorine Demand of Water

SIGNIFICANCE AND USE
5.1 Chlorine is added to potable water, waste water, and industrial water for a variety of purposes. Some of these purposes are:  
5.1.1 To eliminate or reduce the growth of microorganisms in water,  
5.1.2 To destroy or modify decomposable organic substances so as to reduce the biochemical oxygen demand of the water,  
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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.
SCOPE
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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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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5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
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5.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected rodenticides.
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1.1 This test method covers the determination of bromadiolone, brodifacoum, diphacinone and warfarin (referred to collectively as rodenticides in this test method) in water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The Detection Verification Level (DVL) and Reporting Range for the rodenticides are listed in Table 1.  
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Standard Test Method for Determination of Aldicarb, Aldicarb Sulfone, Aldicarb Sulfoxide, Carbofuran, Methomyl, Oxamyl, and Thiofanox in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

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5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 The N-methyl carbamate (NMC) pesticides: aldicarb, carbofuran, methomyl, oxamyl, and thiofanox have been identified by EPA as working through a common mechanism. These affect the nervous system by reducing the ability of enzymes. Enzyme inhibition was the primary toxicological effect of regulatory concern to EPA in assessing the NMC’s food, drinking water, and residential risks. In most of the country, NMC residues in drinking water sources are at levels that are not likely to contribute substantially to the multi-pathway cumulative exposure. Shallow private wells extending through highly permeable soils into shallow, acidic ground water represent what the EPA believes to be the most vulnerable drinking water. Aldicarb sulfone and aldicarb sulfoxide are breakdown products of aldicarb and should also be monitored due to their toxicological effects.4  
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1.1 This test method covers the determination of aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox (referred to collectively as carbamates in this test method) in water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.    
1.2.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios of the primary single reaction monitoring (SRM) transitions, and Fig. 2 displays the confirmatory SRM transitions at the DVLs for the carbamates.  
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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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Standard Test Method for Hardness in Colored and Colorless Water

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5.1 Hardness salts in water, notably calcium and magnesium, are the primary cause of tube and pipe scaling, which frequently causes failures and loss of process efficiency due to clogging or loss of heat transfer, or both.  
5.2 Hardness is caused by any polyvalent cations, but those other than Ca+2 and Mg+2 are seldom present in more than trace amounts. The term hardness was originally applied to water in which it was hard to wash; it referred to the soap-wasting properties of water. With most normal alkaline water, these soap-wasting properties are directly related to the calcium and magnesium content.
SCOPE
1.1 This test method covers the determination of hardness in water by titration with potentiometric detection via optical sensor. This test method is applicable to waters that are free of chemicals that will complex calcium or magnesium. The lower detection limit of this test method is approximately 2 mg/L to 5 mg/L as CaCO3; the upper limit can be extended to all concentrations by sample dilution. It is possible to differentiate between hardness due to calcium ions and that due to magnesium ions by this test method.  
1.2 This test method is applicable to both colorless and colored water samples including groundwater, surface water, wastewater, and drinking water.  
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.  
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ASTM D7485-23(Test Method)
Standard Test Method for Determination of Nonylphenol, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

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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.
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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.  
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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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Standard Test Method for Determination of Select Pesticides in Water by Multiple Reaction Monitoring Liquid Chromatography Tandem Mass Spectrometry

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5.1 Pesticides may be used in various agricultural and household products. These products may enter waterways at low levels through run-off or misuse near water resources. Hence, there is a need for quick, easy and robust method to determine pesticide concentration in water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been single-laboratory validated in reagent water and surface waters (Tables 12-14).
SCOPE
1.1 This test method covers a method for analysis of selected pesticides in a water matrix by filtration followed with liquid chromatography/electrospray ionization tandem mass spectrometry analysis. The samples are prepared in 20 % methanol, filtered, and analyzed by liquid chromatography/tandem mass spectrometry. This method was developed for an agricultural run-off study, not for low level analysis of pesticides in drinking water. This method may be modified for lower level analysis. The analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This standard contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community.  
1.3 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is adapted to report much lower or near the MDL then a MDL study would be warranted.  
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.  
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8 mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).  
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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