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ASTM D7365-07

(Practice)

Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide

Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide

SIGNIFICANCE AND USE
Cyanide is routinely analyzed in water samples, often to demonstrate regulatory compliance; however, improper sample collection or pretreatment can result in significant positive or negative bias potentially resulting in unnecessary permit violations or undetected cyanide releases into the environment.
SCOPE
1.1 This practice is applicable for the collection and preservation of water samples for the analysis of cyanide. This practice also addresses the mitigation of known interferences prior to the analysis of cyanide.
1.2 The sampling, preservation and mitigation of interference procedures described in this practice are recommended for the analysis of total cyanide, available cyanide, weak acid dissociable cyanide, and free cyanide by Test Methods D 2036, D 4282, D 4374, D 6888, D 6994, and D 7237. This practice can also be applied to other cyanide methods, for example, US EPA Method 335.4 and Standard Methods 4500-CN- C.
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
31-Jul-2007
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 D7365-09 - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
Effective Date
15-Feb-2009
Referred By
ASTM D4193-08(2020)e1 - Standard Test Method for Thiocyanate in Water
Effective Date
01-Aug-2007
Referred By
ASTM D6888-16 - Standard Test Method for Available Cyanides with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
Effective Date
01-Aug-2007
Referred By
ASTM D7572-15(2022) - Standard Guide for Recovery of Aqueous Cyanides by Extraction from Mine Rock and Soil
Effective Date
01-Aug-2007
Referred By
ASTM D7284-20 - Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection
Effective Date
01-Aug-2007
Referred By
ASTM D7295-18 - Standard Practice for Sampling Combustion Effluents and Other Stationary Sources for the Subsequent Determination of Hydrogen Cyanide
Effective Date
01-Aug-2007
Referred By
ASTM E800-20 - Standard Guide for Measurement of Gases Present or Generated During Fires
Effective Date
01-Aug-2007
Referred By
ASTM D7237-18 - Standard Test Method for Free Cyanide and Aquatic Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection
Effective Date
01-Aug-2007
Referred By
ASTM D7728-18 - Standard Guide for Selection of ASTM Analytical Methods for Implementation of International Cyanide Management Code Guidance
Effective Date
01-Aug-2007
Referred By
ASTM D7511-12(2017)e1 - Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection
Effective Date
01-Aug-2007
Referred By
ASTM D8273-20 - Standard Practice for Determination of Total and Available Cyanide in Solid Waste and Soil after Alkaline Extraction
Effective Date
01-Aug-2007
Referred By
ASTM D2036-09(2022) - Standard Test Methods for Cyanides in Water
Effective Date
01-Aug-2007

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ASTM D7365-07 - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of CyanideASTM D7365-07 - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
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ASTM D7365-07 - Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide
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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:D7365–07
Standard Practice for
Sampling, Preservation and Mitigating Interferences in
1
Water Samples for Analysis of Cyanide
This standard is issued under the fixed designation D 7365; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 4282 Test Method for Determination of Free Cyanide in
Water and Wastewater by Microdiffusion
1.1 This practice is applicable for the collection and pres-
D 4374 Test Methods for Cyanides in Water—Automated
ervation of water samples for the analysis of cyanide. This
Methods for Total Cyanide, Weak Acid Dissociable Cya-
practice also addresses the mitigation of known interferences
nide, and Thiocyanate
prior to the analysis of cyanide.
D 4411 Guide for Sampling Fluvial Sediment in Motion
1.2 The sampling, preservation and mitigation of interfer-
D 4840 Guide for Sample Chain-of-Custody Procedures
ence procedures described in this practice are recommended
D 4841 Practice for Estimation of Holding Time for Water
for the analysis of total cyanide, available cyanide, weak acid
Samples Containing Organic and Inorganic Constituents
dissociable cyanide, and free cyanide byTest Methods D 2036,
D 6888 Test Method for Available Cyanide with Ligand
D 4282, D 4374, D 6888, D 6994, and D 7237. This practice
Displacement and Flow InjectionAnalysis (FIA) Utilizing
can also be applied to other cyanide methods, for example, US
-
Gas Diffusion Separation and Amperometric Detection
EPA Method 335.4 and Standard Methods 4500-CN C.
D 6994 Test Method for Determination of Metal Cyanide
1.3 The values stated in SI units are to be regarded as
Complexes in Wastewater, Surface Water, Groundwater
standard. No other units of measurement are included in this
and Drinking Water UsingAnion Exchange Chromatogra-
standard.
phy with UV Detection
1.4 This standard does not purport to address all of the
D 6696 Guide for Understanding Cyanide Species
safety concerns, if any, associated with its use. It is the
D 7237 Test Method for Aquatic Free Cyanide with Flow
responsibility of the user of this standard to establish appro-
Injection Analysis (FIA) Utilizing Gas Diffusion Separa-
priate safety and health practices and determine the applica-
tion and Amperometric Detection
bility of regulatory limitations prior to use.
3
2.2 U.S. EPA Methods:
2. Referenced Documents
EPA OIA-1677
2
EPA Method 335.2
2.1 ASTM Standards:
EPA Method 335.4
D 1129 Terminology Relating to Water
4
2.3 APHA Standard:
D 1193 Specification for Reagent Water
Standard Methods 4500-CN Methods C, D, E, F, G, and I
D 1293 Test Methods for pH of Water
5
2.4 USGS Methods:
D 2036 Test Methods for Cyanides in Water
USGS I-3300-85
D 3370 Practices for SamplingWater from Closed Conduits
USGS I-4302-85
D 3694 Practices for Preparation of Sample Containers and
for Preservation of Organic Constituents
3. Terminology
D 3856 Guide for Good Laboratory Practices in Laborato-
3.1 Definitions:
ries Engaged in Sampling and Analysis of Water
1 3
This practice is under the jurisdiction of ASTM Committee D19 on Water and Available from United States Environmental Protection Association (EPA),
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, www.ep-
Organic Substances in Water. a.gov.
4
Current edition approved Aug. 1, 2007. Published August 2007. Standard Methods for the Examination of Water and Wastewater, 21st edition
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or (2005),AmericanPublicHealthAssociation(APHA),800IStreet,NWWashington,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM DC 20001, www.apha.org.
5
Standards volume information, refer to the standard’s Document Summary page on Available from United States Geological Survey, 12201 Sunrise Valley Drive,
the ASTM website. Reston, VA, 20192, www.usgs.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D7365–07
For definitions of terms used in this practice, refer to dilute to volume. Warning—This is an exothermic reaction
Terminology D 1129 and Guide D 6696. and the solution will become very hot while being prepared. It
3.2 In this practice, refrigeration shall designate storing the is recommended to place the solution in a water bath to cool.
sample between its freezing point and 6°C. 6.9 Hydrated Lime—Ca(OH) powder.
2
6.10 Cadmium chloride, CdCl .
2
4. Summary of Practice
6.11 Ethylenediamine (EDA)
4.1 Sam
...

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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 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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5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
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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

SIGNIFICANCE AND USE
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  
5.2 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency and will biodegrade. BPA has been reported to have adverse effects in aquatic organisms and may be released into environmental waters directly at trace levels through landfill leachate and POTW effluents. This method has been investigated for use with surface water and secondary and tertiary POTW effluent samples therefore, it is applicable to these matrices only. It has not been investigated for use with salt water or solid sample matrices.
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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.  
1.3 The method detection limit (MDL) and reporting limit (RL) for BPA are listed in Table 1.  
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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).
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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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ASTM
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

SIGNIFICANCE AND USE
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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