D19.06 - Methods for Analysis for Organic Substances in Water

SIGNIFICANCE AND USE
5.1 The incidental conversion of organic material to trihalomethanes and other volatile organohalides during chlorination of water is a possible health hazard and is the object of much research. This test method can be used as a rapid, simple means for determining many volatile organohalides in raw and processed water.
SCOPE
1.1 This test method covers the analysis of drinking water. It is also applicable to many environmental and waste waters when adequate validation is included.  
1.2 This test method covers the determination of halomethanes, haloethanes, and some related extractable organohalides amenable to gas chromatographic measurement. The applicable concentration range for trihalomethanes is from 1 μg/L to 200 μg/L. Detection limits depend on the compound, matrix, and on the characteristics of the gas chromatographic system.  
1.3 For compounds not specifically included in the precision and bias section the analyst should validate the test method by collecting precision and bias data on actual samples.  
1.4 Confirmation of component identities is obtained by observing retention times using gas chromatographic columns of different polarities. When concentrations are sufficiently high (>50 μg/L) confirmation with halogen specific detectors or gas chromatography/mass spectrometry (GC/MS) may be used. Confirmation of purgeable compounds at levels down to 1 μg/L can be obtained using Test Method D3871 with GC/MS detection.  
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. Specific precautionary statements are given in Section 8.  
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.

SIGNIFICANCE AND USE
5.1 This test method is used for determination of the carbon content of water from a variety of natural, domestic, and industrial sources. In its most common form, this test method is used to measure organic carbon as a means of monitoring organic pollutants in high purity and drinking water. These measurements are also used in monitoring waste treatment processes.  
5.2 The relationship of TOC to other water quality parameters such as chemical oxygen demand (COD) and total oxygen demand (TOD) is described in the literature (6).
SCOPE
1.1 This test method covers the determination of total carbon (TC), inorganic carbon (IC), and total organic carbon (TOC) in water in the range from 0.5 mg/L to 30 mg/L of carbon. Higher levels may be determined by sample dilution. The test method utilizes ultraviolet-persulfate oxidation of organic carbon, coupled with a CO2 selective membrane to recover the CO2 into deionized water. The change in conductivity of the deionized water is measured and related to carbon concentration in the oxidized sample. Inorganic carbon is determined in a similar manner without the requirement for oxidation. In both cases, the sample is acidified to facilitate CO2 recovery through the membrane. The relationship between the conductivity measurement and carbon concentration is described by a set of chemometric equations for the chemical equilibrium of CO2, HCO3−, H+, and the relationship between the ionic concentrations and the conductivity. The chemometric model includes the temperature dependence of the equilibrium constants and the specific conductances.  
1.2 This test method has the advantage of a very high sensitivity detector that allows very low detection levels on relatively small volumes of sample. Also, use of two measurement channels allows determination of CO2 in the sample independently of organic carbon. Isolation of the conductivity detector from the sample by the CO2 selective membrane results in a very stable calibration, with minimal interferences.  
1.3 This test method was used successfully with reagent water spiked with sodium bicarbonate and various organic materials. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.  
1.4 This test method is applicable only to carbonaceous matter in the sample that can be introduced into the reaction zone. The injector opening size generally limits the maximum size of particles that can be introduced.  
1.5 In addition to laboratory analyses, this test method may be applied to on line monitoring.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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.  
1.8 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.

SIGNIFICANCE AND USE
5.1 This practice is useful in identifying the major organic constituents in wastewater for support of effective in-plant or pollution control programs. Currently, the most practical means for tentatively identifying and measuring a range of volatile organic compounds is gas-liquid chromatography. Positive identification requires supplemental testing (for example, multiple columns, speciality detectors, spectroscopy, or a combination of these techniques).
SCOPE
1.1 This practice covers general guidance applicable to certain test methods for the qualitative and quantitative determination of specific organic compounds, or classes of compounds, in water by direct aqueous injection gas chromatography (1, 2, 3, 4).2  
1.2 Volatile organic compounds at aqueous concentrations greater than about 1 mg/L can generally be determined by direct aqueous injection gas chromatography.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

SIGNIFICANCE AND USE
5.1 This test method is useful for characterization and rapid quantification of PAH mixtures including petroleum oils, fuels, creosotes, and industrial organic mixtures, either waterborne or obtained from tanks.  
5.2 The unknown PAH mixture is first characterized by its fluorescence emission and synchronous scanning spectra. Then a suitable site-specific calibration standard with similar spectral characteristics is selected as described in Annex A1. This calibration standard may also be well-characterized by other independent methods such as gas chromatography (GC), GC-mass spectrometry (GC-MS), or high performance liquid chromatography (HPLC). Some suggested independent analytical methods are included in References (1-7)4 and Test Method D4657. Other analytical methods can be substituted by an experienced analyst depending on the intended data quality objectives. Peak maxima intensities of appropriate fluorescence emission spectra are then used to set up suitable calibration curves as a function of concentration. Further discussion of fluorescence techniques as applied to the characterization and quantification of PAHs and petroleum oils can be found in References (8-18).  
5.3 For the purpose of the present test method polynuclear aromatic hydrocarbons are defined to include substituted polycyclic aromatic hydrocarbons with functional groups such as carboxyl acid, hydroxy, carbonyl and amino groups, and heterocycles giving similar fluorescence responses to PAHs of similar molecular weight ranges. If PAHs in the more classic definition, that is, unsubstituted PAHs, are desired, chemical reactions, extractions, or chromatographic procedures may be required to eliminate these other components. Fortunately, for the most commonly expected PAH mixtures, such substituted PAHs and heterocycles are not major components of the mixtures and do not cause serious errors.
SCOPE
1.1 This test method covers a means for quantifying or characterizing total polycyclic aromatic hydrocarbons (PAHs) by fluorescence spectroscopy (Fl) for waterborne samples. The characterization step is for the purpose of finding an appropriate calibration standard with similar emission and synchronous fluorescence spectra.  
1.2 This test method is applicable to PAHs resulting from petroleum oils, fuel oils, creosotes, or industrial organic mixtures. Samples can be weathered or unweathered, but either the same material or appropriately characterized site-specific PAH or petroleum oil calibration standards with similar fluorescence spectra should be chosen. The degree of spectral similarity needed will depend on the desired level of quantification and on the required data quality objectives.  
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.

SIGNIFICANCE AND USE
4.1 Identification of a recovered oil is determined by comparison with known oils selected because of their possible relationship to the particular recovered oil, for example, suspected or questioned sources. Thus, samples of such known oils must be collected and submitted along with the unknown for analysis. It is unlikely that identification of the sources of an unknown oil by itself can be made without direct matching, that is, solely with a library of analyses.
SCOPE
1.1 This practice covers the preparation for analysis of waterborne oils recovered from water. The identification is based upon the comparison of physical and chemical characteristics of the waterborne oils with oils from suspect sources. These oils may be of petroleum or vegetable/animal origin, or both. Seven procedures are given as follows:    
Sections  
Procedure A (for samples of more than 50 mL volume containing significant quantities of hydrocarbons with boiling points above 280 °C)  
8 to 12  
Procedure B (for samples containing significant quantities of hydrocarbons with boiling points above 280 °C)  
13 to 17  
Procedure C (for waterborne oils containing significant amounts of components boiling below 280 °C and to mixtures of these and higher boiling components)  
18 to 22  
Procedure D (for samples containing both petroleum and vegetable/animal derived oils)  
23 to 27  
Procedure E (for samples of light crudes and medium distillate fuels)  
28 to 34  
Procedure F (for thin films of oil-on-water)  
35 to 39  
Procedure G (for oil-soaked samples)  
40 to 44  
1.2 Procedures for the analytical examination of the waterborne oil samples are described in Practice D3415 and Test Methods D3328, D3414, and D3650. Refer to the individual oil identification test methods for the sample preparation method of choice. The deasphalting effects of the sample preparation method should be considered in selecting the best methods.  
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. Specific caution statements are given in Sections 6 and 32.  
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.

SIGNIFICANCE AND USE
5.1 This test method is used for determination of the carbon content of water from a variety of natural, domestic, and industrial sources. In its most common form, this test method is used to measure organic carbon as a means of monitoring organic pollutants in industrial wastewater. These measurements are also used in monitoring waste treatment processes.  
5.2 The relationship of TOC to other water quality parameters such as chemical oxygen demand (COD) and total oxygen demand (TOD) is described in the literature.4
SCOPE
1.1 This test method covers the determination of total carbon (TC), inorganic carbon (IC), and total organic carbon (TOC) in water, wastewater, and seawater in the range from 0.1 mg/L to 4000 mg/L of carbon.  
1.2 This test method was used successfully with reagent water spiked with sodium carbonate, acetic acid, and pyridine. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.  
1.3 This test method is applicable only to carbonaceous matter in the sample that can be introduced into the reaction zone. The syringe needle or injector opening size generally limit the maximum size of particles that can be so introduced.  
1.4 In addition to laboratory analyses, this test method may be applied to stream monitoring.  
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.

SIGNIFICANCE AND USE
5.1 Matrix spiking of samples is commonly used to determine the bias under specific analytical conditions, or the applicability of a test method to a particular sample matrix, by determining the extent to which the added spike is recovered from the sample matrix under these conditions. Reactions or interactions of the analyte or component of interest with the sample matrix may cause a significant positive or negative effect on recovery and may render the chosen analytical, or monitoring, process ineffectual for that sample matrix.  
5.2 Matrix spiking of samples can also be used to monitor the performance of a laboratory, individual instrument, or analyst as part of a regular quality assurance program. Changes in spike recoveries from the same or similar matrices over time may indicate variations in the quality of analyses and analytical results.  
5.3 Spiking of samples may be performed in the field or in the laboratory, depending on what part of the analytical process is to be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample and may be considered a measure of the stability of the analytes in the matrix. Laboratory spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will be reflective of only that portion of the process subsequent to the addition of the spike.  
5.4 Special precautions shall be observed when nonlaboratory personnel perform spiking in the field. It is recommended that all spike preparation work be performed in a laboratory by experienced analysts so that the field operation consists solely of adding a prepared spiking solution to the sample matrix. Training of field personnel and validation of their spiking techniques are necessary to ensure that spikes are added accurately and reproducibly. Consistent and acceptable recoveries from duplicate field spikes can be used to document the reproducibility of sampling and the spiking technique....
SCOPE
1.1 This guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials cited here are compatible with the analytes of interest.  
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered.  
1.3 This guide is intended for use in conjunction with the individual analytical test method that provides procedures for analysis of the analyte or component of interest. The test method is used to determine an analyte or component's background level and, again after spiking, its now elevated level. Each test method typically provides procedures not only for samples, but also for calibration standards or analytical control solutions, or both. These procedures include preparation, handling, storage, preservation, and analysis techniques. These procedures are applicable by extension, using the analyst's judgement on a case-by-case basis, to spiking solutions, ...

SIGNIFICANCE AND USE
4.1 This practice provides a general procedure for the solvent extraction of volatile and semi-volatile organic compounds from a water matrix. Solvent extraction is used as the initial step in the solvent extraction of organic constituents for the purpose of quantifying extractable organic compounds.  
4.2 Typical detection limits that can be achieved using micro-extraction techniques with gas chromatography (GC) with flame ionization detector (FID), electron capture detector (ECD), or with a mass spectrometer (GC/MS) range from milligrams per litre (mg/L) to nanograms per litre (ng/L). The detection limit, linear concentration range, and sensitivity of the test method for a specific organic compound will depend upon the sample clean-up, injection volume, solvent to sample ratio, solvent concentration methods used, and the determinative technique employed.  
4.3 Micro-extraction has the advantage of speed, simple extraction devices, and the use of small amounts of sample and solvents.  
4.3.1 Selectivity can be improved by the choice of solvent (usually hexane or pentane) or mixed solvents, extraction time and temperature, and ionic strength of the solution.  
4.3.2 Extraction devices can vary from the sample container itself to commercial devices specifically designed for micro-extraction. See 7.1 and 7.2.  
4.3.3 A list of chlorinated organic compounds that can be determined by this practice includes both high and low boiling compounds or chemicals (see Table 1). (A) Based on the injection of chlorinated compounds in pentane solution, taking into consideration the 100:1 concentration of a water sample by the microextraction technique.
SCOPE
1.1 This practice covers standard procedures for extraction of volatile and semi-volatile organic compounds from water using small volumes of solvents.  
1.2 The compounds of interest must have a greater solubility in the organic solvent than the water phase.  
1.3 Not all of the solvents that can be used in micro extraction are addressed in this practice. The applicability of a solvent to extract the compound(s) of interest must be demonstrated before use.  
1.4 This practice provides sample extracts suitable for any technique amenable to solvent injection such as gas chromatography or high performance liquid chromatography (HPLC).  
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. For specific hazard statements, see Section 9.  
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.

SIGNIFICANCE AND USE
4.1 Identification of the source of a spilled oil is established by comparison with known oils selected because of their possible relationship to the spill, that is, potential sources. Generally, the suspected source oils are from pipelines, tanks, etc., and therefore pose little problems in sampling compared to the spilled oil. This practice addresses the sampling of spilled oils in particular, but could be applied to appropriate source situations, for example, a ship's bilge.
SCOPE
1.1 These practices describe the procedures to be used in collecting samples of waterborne oils (see Practice D3415), oil found on adjoining shorelines, or oil-soaked debris, for comparison of oils by spectroscopic and chromatographic techniques, and for elemental analyses.  
1.2 Two practices are described. Practice A involves “grab sampling” macro oil samples. Practice B can be used to sample most types of waterborne oils and is particularly applicable in sampling thin oil films or slicks. Practice selection will be dictated by the physical characteristics and the location of the spilled oil. These two practices are:    
Sections  
Practice A (for grab sampling thick layers of oil, viscous oils or oil soaked debris, oil globules, tar balls, or stranded oil)  
9 to 13  
Practice B (for TFE–fluorocarbon polymer strip samplers)  
14 to 17  
1.3 Each of the two practices is designed to collect oil samples with a minimum of water, thereby reducing the possibility of chemical, physical, or biological alteration by prolonged contact with water between the time of collection and analysis.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 hazards statements, see Section 7.  
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.

SIGNIFICANCE AND USE
5.1 The extensive and widespread use of organochlorine pesticides and PCBs has resulted in their presence in all parts of the environment. These compounds are persistent and may have adverse effects on the environment. Thus, there is a need to identify and quantitate these compounds in water samples.
SCOPE
1.1 This test method (1-3)2 is applicable to the determination of the following analytes in finished drinking water, drinking water during intermediate stages of treatment, and the raw source water:    
Analyte  
Chemical Abstract Service
Registry Number A  
Alachlor  
5972-60-8  
Aldrin  
309-00-2  
Chlordane  
57-74-9  
Dieldrin  
60-57-1  
Endrin  
72-20-8  
Heptachlor  
76-44-8  
Heptachlor Epoxide  
1024-57-3  
Hexachlorobenzene  
118-74-1  
Lindane  
58-89-9  
Methoxychlor  
72-43-5  
Toxaphene  
8001-35-2  
Aroclor B 1016  
12674-11-2  
Aroclor B 1221  
11104-28-2  
Aroclor B 1232  
11141-16-5  
Aroclor B 1242  
53469-21-9  
Aroclor B 1248  
12672-29-6  
Aroclor B 1254  
11097-69-1  
Aroclor B 1260  
11096-82-5  
1.2 Detection limits for most test method analytes are less than 1 μg/L. Actual detection limits are highly dependent on the characteristics of the sample matrix and the gas chromatography system. Table 1 contains the applicable concentration range for the precision and bias statements. Only Aroclor 1016 and 1254 were included in the interlaboratory test used to derive the precision and bias statements. Data for other PCB products are likely to be similar.  
1.3 Chlordane, toxaphene, and Aroclor products (polychlorinated biphenyls) are multicomponent materials. Precision and bias statements reflect recovery of these materials dosed into water samples. The precision and bias statements may not apply to environmentally altered materials or to samples containing complex mixtures of polychlorinated biphenyls (PCBs) and organochlorine pesticides.  
1.4 For compounds other than those listed in 1.1 or for other sample sources, the analyst must demonstrate the applicability of this test method by collecting precision and bias data on spiked samples (groundwater, tap water) (4) and provide qualitative confirmation of results by gas chromatography/mass spectrometry (GC/MS) (5) or by GC analysis using dissimilar columns.  
1.5 This test method is restricted to use by or under the supervision of analysts experienced in the use of GC and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results using the procedure described in Section 13.  
1.6 Analytes that are not separated chromatographically, (analytes that have very similar retention times) cannot be individually identified and measured in the same calibration mixture or water sample unless an alternative technique for identification and quantitation exists (see 13.4).  
1.7 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in 1.1, analyte identifications and concentrations should be confirmed by at least one additional technique.  
1.8 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.  
1.9 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 9.  
1.10 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for th...

SIGNIFICANCE AND USE
4.1 There are four basic steps necessary to obtain meaningful analytical data: preparation of the sample container, sampling, sample preservation, and analysis. In fact these four basic steps comprise the analytical method and for this reason no step should be overlooked. Although the significance of preservation is dependent upon the time between sampling and the analysis, unless the analysis is accomplished within 2 h after sampling, preservation is preferred and usually required.
SCOPE
1.1 These practices cover the various means of (1) preparing sample containers used for collection of waters to be analyzed for organic constituents and (2) preservation of such samples from the time of sample collection until the time of analysis.  
1.2 The sample preservation practice is dependent upon the specific analysis to be conducted. See Section 9 for preservation practices listed with the corresponding applicable general and specific constituent test method. The preservation method for waterborne oils is given in Practice D3325. Use of the information given herein will make it possible to choose the minimum number of sample preservation practices necessary to ensure the integrity of a sample designated for multiple analysis. For further considerations of sample preservation, see the Manual on Water.2  
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. For specific hazard statements, see 6.7, 6.24, and 8.1.3.  
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.

SIGNIFICANCE AND USE
5.1 This test method is useful for the analysis of drinking water and groundwaters. Other waters may be analyzed by this test method, see 1.2.  
5.2 EDB and DBCP have been widely used as soil fumigants. EDB is also used as a lead scavenger in leaded gasolines. These compounds are very water soluble and are often found in groundwater and drinking water. Since they are highly toxic and are suspected carcinogens, there is concern about the potential health impact of even extremely low concentrations in potable water.
SCOPE
1.1 This test method covers the determination of 1,2-dibromoethane (commonly referred to as ethylene dibromide or EDB) and 1,2-dibromo-3-chloropropane (commonly referred to as DBCP) in water at a minimum detection level of 0.010 μg/L by liquid-liquid extraction combined with gas-liquid chromatography. This test method is applicable to the analysis of drinking waters and groundwaters. It is not recommended for wastewaters, due to the potential for interferences from high concentrations of other extractable organics. Similar information can be found in EPA Method 504.  
1.2 This test method was used successfully with reagent water and groundwater. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.  
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. For specific hazard statements, see Sections 6 and 9.  
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.

SIGNIFICANCE AND USE
5.1 N-methylcarbamates and n-methylcarbomoyloximes are used in agriculture as insecticides and herbicides. They are sometimes found in both surface and ground waters and can be toxic to animals and plants at moderate to high concentrations. The manufacturing precursors and degradation products may be equally as hazardous to the environment.
SCOPE
1.1 This is a high-performance liquid chromatographic (HPLC) test method applicable to the determination of certain n-methylcarbamoyloximes and n-methylcarbamates in ground water and finished drinking water (1).2 This test method is applicable to any carbamate analyte that can be hydrolyzed to a primary amine. The following compounds have been validated using this test method:    
Analyte  
Chemical Abstract Services
Registry Number A  
Aldicarb  
116-06-3    
Aldicarb sulfone  
1646-88-4    
Aldicarb sulfoxide  
1646-87-3    
Baygon  
114-26-1    
Carbaryl  
63-25-2    
Carbofuran  
1563-66-2    
3-Hydroxycarbofuran  
16655-82-6    
Methiocarb  
2032-65-7    
Methomyl  
16752-77-5    
Oxamyl  
23135-22-0    
1.2 This test method has been validated in a collaborative round-robin study (2) and estimated detection limits (EDLs) have been determined for the analytes listed in 1.1 (Table 1). Observed detection limits may vary between ground waters, depending on the nature of interferences in the sample matrix and the specific instrumentation used.  
1.3 This test method is restricted to use by, or under the supervision of, analysts experienced in both the use of liquid chromatography and the interpretation of liquid chromatograms. Each analyst should demonstrate an ability to generate acceptable results with this test method using the procedure described in 12.3.  
1.4 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in 1.1, analyte identifications should be confirmed by at least one additional qualitative technique.  
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. Additional guidance on laboratory safety is available and suitable references for the information are provided  (3-5).  
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.

SIGNIFICANCE AND USE
5.1 Purgeable organic compounds, including organohalides, have been identified as contaminants in raw and drinking water. These contaminants may be harmful to the environment and man. Dynamic headspace sampling is a generally applicable method for concentrating these components prior to gas chromatographic analysis (1-5).3 This test method can be used to quantitatively determine purgeable organic compounds in raw source water, drinking water, and treated effluent water.
SCOPE
1.1 This test method covers the determination of most purgeable organic compounds that boil below 200 °C and are less than 2 % soluble in water. It covers the low μg/L to low mg/L concentration range (see Section 15 and Appendix X1).  
1.2 This test method was developed for the analysis of drinking water. It is also applicable to many environmental and waste waters when validation, consisting of recovering known concentrations of compounds of interest added to representative matrices, is included.  
1.3 Volatile organic compounds in water at concentrations above 1000 μg/L may be determined by direct aqueous injection in accordance with Practice D2908.  
1.4 It is the user's responsibility to assure the validity of the test method for untested matrices.  
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. Specific precautionary statements are given in 8.5.5.1.  
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.

SIGNIFICANCE AND USE
4.1 Oil from one crude oil field is readily distinguishable from another, and differences in the makeup of oils from the same crude oil field can often be observed as well. Refined oils are fractions from crude oil stocks, usually derived from distillation processes. Two refined oils of the same type differ because of dissimilarities in the characteristics of their crude oil feed stocks as well as variations in refinery processes and any subsequent contact with other oils mixed in during transfer operations from residues in tanks, ships, pipes, hoses, and so forth. Thus, all petroleum oils, to some extent, have chemical compositions different from each other.  
4.2 Identification of a recovered oil is determined by comparison with known oils selected because of their possible relationship to the particular recovered oil, for example, suspected sources. Thus, samples of such known oils must be collected and submitted along with the unknown for analysis. Identification of the source of an unknown oil by itself cannot be made without comparison to a known oil. The principles of oil spill identification are discussed in Ref (1).4  
4.3 Many similarities (within uncertainties of sampling, analysis and weathering) will be needed to establish the identity beyond a reasonable doubt. The analyses described will distinguish many, but not all samples. Examples of weathering of various classes of oils are included in Ref (2).  
4.4 This practice is a guide to the use of ASTM test methods for the analysis of oil samples for oil spill identification purposes. The evaluation of results from analytical methods and preparation of an Oil Spill Identification Report are discussed in this practice. Other analytical methods are described in Ref (3).  
4.5 A quality assurance program for oil spill identification is specified.
SCOPE
1.1 This practice covers the broad concepts of sampling and analyzing waterborne oils for identification and comparison with suspected source oils. Detailed procedures are referenced in this practice. A general approach is given to aid the investigator in planning a program to solve the problem of chemical characterization and to determine the source of a waterborne oil sample.  
1.2 This practice is applicable to all waterborne oils taken from water bodies, either natural or man-made, such as open oceans, estuaries or bays, lakes, rivers, smaller streams, canals; or from beaches, marshes, or banks lining or edging these water systems. Generally, the waterborne oils float on the surface of the waters or collect on the land surfaces adjoining the waters, but occasionally these oils, or portions, are emulsified or dissolved in the waters, or are incorporated into the sediments underlying the waters, or into the organisms living in the water or sediments.  
1.3 This practice as presently written proposes the use of specific analytical techniques described in the referenced ASTM standards. As additional techniques for characterizing waterborne oils are developed and written up as test methods, this practice will be revised.  
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.

SIGNIFICANCE AND USE
5.1 Preliminary studies have identified polymeric organic compounds as contaminants in treated drinking water, wastewater, surface water, ground water, and marine waters. These polymers may be harmful to the environment and adversely affect human health, and in these circumstances, mass estimation is commonly required. A universal, analytical method will help to normalize data from around the world and better understand which polymers are most frequently found in various climatic and geological locations (5-7). Pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) has many advantages in that both polymer identification and mass quantification can be easily accomplished by chromatographic separation in combination with mass spectral analysis.
SCOPE
1.1 In this pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) test method, an analytical protocol validated specifically for the analysis of water with high to low suspended solids is described. This test method will standardize the identification and simultaneous quantitation of organic polymer particles and fibers in water. It has been designed for and applies to all microplastic particles and fibers, and is intended for use with treated drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters. This test method is not limited to these particular water matrices; however, the applicability of this test method to other aqueous matrices shall be demonstrated.  
1.2 Microgram quantities of a sample containing microplastics are pyrolyzed (Py) at 600 °C. The pyrolyzates are separated on an analytical column (GC) and detected using a 70-eV electron impact mass spectrometer (MS). Polymers often have similar pyrograms, making it difficult to differentiate the pyrolyzates for a given polymer from those of the composite sample. In this test method, ion ratios at predetermined retention times to facilitate the identification of each polymer present in a sample containing microplastics are compared.  
1.3 This test method is to be used in conjunction with Practices D8332, D8333, and D8402. These ASTM International standards enable the collection and preparation of water samples with high, medium, or low suspended solids for the identification and quantification of microplastic particles and fibers without compromising the integrity of the microplastics. This test method is applicable to microplastic fibers and particles, including sizes defined as a nanoparticle; this is a natural extension of this test method because Py-GC/MS technology responds to the total mass of the sample independent of individual particle sizes. The uniformity of particle size influences the reproducibility of the pyrogram and samples with microplastics should be reduced to a fine powder with the final particle size diameter on the order of less than 0.2 mm.  
1.4 It is the responsibility of the user to ensure the validity of this test method for untested matrices.  
1.5 Units—The values stated in SI units are to be regarded as the 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.

SIGNIFICANCE AND USE
5.1 Pesticides and PCBs are Environmental Protection Agency (EPA)-regulated contaminants in treated drinking water, wastewater, and ground water. Liquid-liquid and solid-phase extraction (SPE) are generally applicable procedures for extracting these target analytes before GC/MS/MS analysis.  
5.2 This test method is applicable to pesticides that are extracted from aqueous solution using methylene chloride and can be chromatographed and detected using tandem mass spectrometry procedures. Table 1 lists pesticides and Table 2 lists PCBs validated by this test method. This test method is not limited to the compounds listed in Table 1 or Table 2; however, the applicability of the test method to other compounds shall be demonstrated. Refer to Guide E2857 for guidance in validating the method for additional parameters.    
5.3 Analyte concentrations up to approximately 250 ng/L may be determined. Analytes that are inefficiently extracted from water will not be detected when present at low concentrations, but they can be measured with acceptable accuracy and precision when present in sufficient amounts.  
5.4 Analytes that are not separated chromatographically but that have different transitions can be identified and quantitatively measured.  
5.5 This test method may be used to determine the concentrations of Aroclor6 mixtures or PCB congeners, or both, present in the sample. See Appendix X1 and Appendix X2 for suggested transitions and collisional energies for all 209 congeners. Separation of all 209 congeners may not be possible and may require additional GC columns and operating conditions. Analysis of all congeners is not expected to be achieved by this test method.  
5.6 Method detection limits (MDL) and minimum reporting level (MRL) for analytes in Tables 1 and 2 are given in Table 3. These limits must be met if the method is used for National Pollutant Discharge Elimination System (NPDES) reporting. (A) Priority Pollutant listed in Table 1 of EPA Method 608.3.(...
SCOPE
1.1 This test method covers the identification and simultaneous measurement of extractable chlorinated pesticides and polychlorinated biphenyls (PCBs) by gas chromatography/mass spectrometry/mass spectrometry (GC/MS/MS).  
1.2 This test method has been validated for wastewater influents, effluents, industrial discharges, surface water, and ground water.  
1.3 This test method is not limited to these particular aqueous matrices; however, the applicability of this test method to other aqueous matrices shall be demonstrated.  
1.4 This test method is restricted to use by or under the supervision of analysts experienced in the use of a gas chromatograph with tandem mass spectrometry. Each laboratory that uses this test method shall demonstrate the ability to generate results that meet or exceed the performance criteria of this test method.  
1.5 If sensitivity permits, compound tentative identification of unknowns may be made by analyzing the extract in full-scan mode or, if the system allows simultaneous timed single-reaction monitoring (SRM)/full-scan acquisition. Identify unknown peaks according to Guide D4128.  
1.6 This test method is performance-based. Minor modifications, as allowed by CFR 40 Part 136.6, may be made to improve the method performance, but changes may not be made to the extraction, the extraction solvent, sample-to-solvent ratio, or the MS/MS detection technique.  
1.7 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.  
1.8 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.  
1.9 This international standard was developed in accordance with internationally recognized princ...

SIGNIFICANCE AND USE
5.1 Cyanide and hydrogen cyanide are highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastes and surface waters.3  
5.2 This test method is applicable for natural water, saline waters, metallurgical process solutions, and wastewater effluent.  
5.3 The method may be used for process control in wastewater treatment facilities.
SCOPE
1.1 This test method is used to determine the concentration of available inorganic cyanide in an aqueous wastewater or effluent. The method detects the cyanides that are free (HCN and CN-) and metal-cyanide complexes that are easily dissociated into free cyanide ions. The method does not detect the less toxic strong metal-cyanide complexes, cyanides that are not “amenable to chlorination.”  
1.2 Total cyanide can be determined for samples that have been distilled as described in Test Methods D2036, Test Method A, Total Cyanides after Distillation. The cyanide complexes are dissociated and absorbed into the sodium hydroxide capture solution, which can be analyzed with this test method; therefore, ligand exchange reagents from 8.12 and 8.13 would not be required when determining total cyanide after distillation.  
1.3 This procedure is applicable over a range of approximately 2 μg/L to 400 μg/L (parts per billion) available cyanides. Higher concentrations can be analyzed by dilution or lower injection volume.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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. Specific hazard statements are given in 8.6 and Section 9.  
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.

SIGNIFICANCE AND USE
4.1 This guide provides standard terminology for use in identifying and describing the different chemical forms of cyanide. The complex nature of cyanide chemistry, existence of numerous distinct chemical forms as well as the various regulatory distinctions that may be made can lead to confusion in technical discussions on cyanide and in the selection of appropriate methods for its analysis. This guide is intended to provide clarification and a common framework of terms and definitions to facilitate discussions and referencing different cyanide chemical species and groups of cyanide compounds.  
4.2 The use of such common terminology is particularly important from an environmental perspective because certain forms of cyanide are considered to be toxic. Therefore, their release into the environment is regulated by federal and state agencies. Thus a general understanding of cyanide chemistry and species definitions is needed for proper wastewater management and testing.
SCOPE
1.1 This guide defines guidance based on a consensus of viewpoints for interpretation of test results to identify various chemical forms of cyanide. It is intended to provide a general understanding of the chemical nature of distinct cyanide species as related to chemical analysis and environmental fate and transport.  
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 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.

SIGNIFICANCE AND USE
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  
5.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected carbamates: aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox.
SCOPE
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.  
1.3 Units—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.

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.
SCOPE
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.  
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.

SIGNIFICANCE AND USE
5.1 TTPC may be used in various industrial and commercial products for use as a biocide. Products containing TTPC have been approved for controlling algal, bacterial, and fungal slimes in industrial water systems.2 TTPC should not be persistent in water but may be deposited in sediments at concentrations of concern. Hence, there is a need for quick, easy and robust method to determine TTPC concentration at trace levels in water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been used to determine TTPC in reagent water and a river water (Table 8). (A) Solution A: Level 8 stock solution prepared according to Section 12 and at Table 4 concentrations.(B) Solution B: 75 % Acetone, 25 % Water.    
Note 1: This test method has been used to characterize TTPC in real world water samples with success and similar recoveries as shown in Table 8.
SCOPE
1.1 This test method covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in water by dilution with acetone, filtration and analysis by liquid chromatography/tandem mass spectrometry. This test method is not amenable for the analysis of isomeric mixtures of Tributyl-tetradecylphosphonium chloride. TTPC is a biocide that strongly adsorbs to soils.2 The water samples are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 100 ng/L to 4000 ng/L. This analyte is qualitatively and quantitatively determined by this method. This test 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 test method 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 The Method Detection Limit3 (MDL) and Reporting Range4 for the target analyte are listed in Table 1.      
1.3.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 4 for TTPC after taking into account a 2.5 mL water sample volume and a final diluted sample volume of 10 mL (75 % acetone/25 % water). The final solution volume is 10 mL because a 7.5 mL volume of acetone is added to each 2.5 mL water sample which is shaken and filtered.  
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 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.  
1.6 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.

SIGNIFICANCE AND USE
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.

SIGNIFICANCE AND USE
5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 Bromadiolone, brodifacoum, diphacinone and warfarin are rodenticides for controlling mice, rats, and other rodents that pose a threat to public health, critical habitats, native plants and animals, crops, food and water supplies. These rodenticides also present human and environmental safety concerns. Warfarin and diphacinone are first-generation anticoagulants, while bromadiolone and brodifacoum are second-generation. The anticoagulants interfere with blood clotting, and death can result from excessive bleeding. The second-generation anticoagulants are especially hazardous for several reasons. They are highly toxic and persist a long time in body tissues. The second-generation anticoagulants are designed to be toxic in a single feeding, but time-to-death occurs in several days. This allows rodents to feed multiple times before death, leading to carcasses containing residues that may be many times the lethal dose.4  
5.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected rodenticides.
SCOPE
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.  
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 rodenticides.  
1.2.2 The reporting limit was calculated from the concentration of the Level 1 calibration standard, as shown in Table 4, accounting for the dilution of a 40 mL water sample up to a final volume of 50 mL with methanol to ensure analyte solubility.  
1.3 Units—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.

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.

SIGNIFICANCE AND USE
5.1 The presence and concentration of oil and grease in domestic and industrial wastewater is of concern to the public because of its deleterious aesthetic effect and its impact on aquatic life.  
5.2 Regulations and standards have been established that require monitoring of TOG and TPH in produced water and wastewater.
SCOPE
1.1 This test method covers the determination of total oil and grease, and total petroleum hydrocarbons in produced water and wastewater by an infrared (IR) determination of n-hexane extractable substances from the sample. Included in this estimation of total oil and grease are any other compounds soluble in the n-hexane.  
1.2 This test method defines total oil and grease in produced water and wastewater as that which is extractable in the test method and measured by IR absorption from 3.34 µm to 3.54 µm (2825 cm-1 to 2994 cm-1). Similarly, this test method defines total petroleum hydrocarbons in produced water and wastewater as that oil and grease which is not adsorbed by silica gel in the test method, and is measured by IR absorption from 3.34 µm to 3.54 µm (2825 cm-1 to 2994 cm-1). Alternative methods for total oil and grease or total petroleum hydrocarbons, or both, can produce differing results.  
1.3 This method covers the range of 5 mg/L to 175 mg/L for total oil and grease and the range of 5 mg/L to 50 mg/L for total petroleum hydrocarbons. The range may be extended to a lower or higher level by extraction of a larger or smaller sample volume collected separately.  
1.4 This test method uses horizontal attenuated total reflectance (HATR) with a cubic zirconia crystal.  
1.5 This test method is intended as a field test only and should be treated as such. This method is not intended to replace laboratory-based regulatory methods currently in use.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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. See Guide D3856 for more information.  
1.8 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.

SIGNIFICANCE AND USE
5.1 These procedures can be used to generate microplastic particles as a simulation of microplastic particles found in the natural environment. Suitable uses may include evaluation of microplastic detection and imaging methods. Use of reference samples will support estimation of ambient and flux concentrations in drinking water, wastewater and natural environments, investigations of microplastic particle degradation, and ingestion of microplastics by animals in the contexts of food safety and human health risk assessment.
SCOPE
1.1 This practice describes manufacturing methods to create microplastic particles from pellets of common polymers and the preparation of microplastic reference samples for calibration and proficiency evaluation of microplastic collection practices, preparation practices, and identification methods.  
1.2 This practice does not describe methods for controlling or characterizing the shapes of particles. The procedures have been observed to yield irregularly shaped particles, the use of which in many cases will serve to remove the analytical bias inherent with using distinctive manufactured spherical beads. Other procedures should be used if spheres or elongated fibers are desired.  
1.3 This practice does not describe handling procedures for waste generated when executing the procedures described herein. It is the responsibility of the user of this practice to follow applicable laws and regulations when manufacturing and disposing of microplastic particles, and to establish appropriate procedures to minimize the amount of waste generated.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.  
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.

SIGNIFICANCE AND USE
5.1 Many microplastic particles enter the environment, including ambient waters and drinking water supplies, via wastewater sources resulting from both industrial processes and consumer products. The presence of high percentages of organic particles, including cellulose material originating from toilet paper and chitin-based materials originating from insect exoskeletons, makes visual identification and subsequent quantification of microplastic particles in wastewater difficult.  
5.2 This test method, associated sampling Practice D8332, and preparation Practice D8333 provide a standardized approach for the preparation of water and, particularly, wastewater samples. The isolation of microplastic particles from interfering contaminants by Practice D8333 enables positive identification and, therefore, quantification of microplastic particles.  
5.3 Using this test method, microplastic particles are characterized in terms of size, shape, and quantity, allowing for the enumeration of subsequent particle count for a given volume of sample. The method does not provide qualitative identification of plastic composition.
SCOPE
1.1 This test method covers the determination of microplastic particle size distribution, shape characterization, and number concentration (particle counts) in sample extracts containing particles between 5 µm and 100 µm. Light is transmitted through a flow cell containing particles in liquid medium. The particles create shadows as they pass through the field of vision of a camera, producing a multitude of images. The images are then used to measure size, shape, and concentration.  
1.2 This test method is used as a complementary technique for microplastic particle and fiber polymer identification methods infrared microscopy and gas chromatography/mass spectroscopy pyrolysis.  
1.3 This test method requires that samples are collected according to Practice D8332 and prepared according to Practice D8333 prior to use.  
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 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.  
1.6 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.

SIGNIFICANCE AND USE
5.1 This test method is used for determination of the total or dissolved nitrogen content of water from a variety of natural, domestic, and industrial sources. In its most common form, this test method is used to measure nitrogen as a means of monitoring nutrient pollutant in industrial wastewater, domestic wastewater, and ambient water. These measurements may also be used in monitoring waste treatment processes.  
5.2 This test method measures oxidized ammonia and organic nitrogen (as nitrate) and soluble nitrate simultaneously, subtracting the nitrate + nitrite value from a non-digested sample gives total Kjeldhal nitrogen (TKN).
When using this test method:
     where:  
  TN  =  total nitrogen, and    TKN  =  total Kjeldahl nitrogen.
SCOPE
1.1 This test method covers the determination of total nitrogen (TN) and total dissolved nitrogen (TDN) in surface water, seawater, groundwater, wastewater, and wastewater effluents in the range from 0.2 mg/L N to 10 mg/L N. Concentrations from 10 mg/L to 500 mg/L are possible when used in conjunction with manual or automatic dilution, or automatic injection of less sample volume. The EPA 40 CFR Part 136 Appendix B Method Detection Limit (MDL) is 0.05 mg/L N. Higher concentrations may be determined by sample dilution. Lower concentrations may be possible by injecting larger sample volumes. Follow the manufacturer’s instructions.  
1.2 The sample is injected onto a platinum catalyst heated at ≥720 °C. The sample converts into a gaseous phase and is forced through a layer of catalyst ensuring conversion of all nitrogen containing compounds to nitrogen oxide (NO). Reaction with ozone converts the NO to an exited NO2. As the excited NO2 returns to the ground state, it emits radiation that is measured photo-electrically.  
1.3 Total and dissolved organic carbon analysis by Test Method D7573 can be analyzed at the same time on the same sample simultaneously using a properly equipped analyzer. (See Appendix X1 for an example of simultaneous TOC data.)  
1.4 This test method quantitatively recovers nitrogen from a large range of organic and inorganic nitrogen compounds (see Table 1 and Table 2). The test method does not measure nitrogen gas (N2). It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.    
1.5 This test method is applicable only to nitrogenous matter in the sample that can be introduced into the reaction zone. The syringe needle or injector opening size generally limits the maximum size of particles that can be so introduced. Optional automatic sample homogenization may be used.  
1.6 This test method is performance based. You may make modifications that improve the test method’s performance but do not change the oxidation or detection technique.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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.  
1.9 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.

SIGNIFICANCE AND USE
5.1 The presence and concentration of total oil and grease as well as total petroleum hydrocoarbons, in domestic and industrial wastewater is of concern to the public because of its deleterious aesthetic effect and its impact on aquatic life.  
5.2 Regulations and standards have been established that require monitoring of total oil and grease as well as total petroleum hydrocarbons in water and wastewater.
SCOPE
1.1 This test method covers the determination of total oil and grease (TOG) and total petroleum hydrocarbons (TPH) in water and waste water that are extractable by this test method from an acidified sample with a cyclic aliphatic hydrocarbon (for example cyclohexane, cyclopentane) and measured by IR absorption in the region from 1370 cm–1 to 1380 cm–1 (7.25 μm to 7.30 μm) using a mid-IR laser spectrometer. Polar substances are removed by clean-up with Florisil.2  
1.2 This test method also considers the volatile fraction of petroleum hydrocarbons, which is lost by gravimetric methods that require solvent evaporation prior to weighing, as well as by solvent-less IR methods that require drying of the employed solid phase material prior to measurement. Similarly, a more complete fraction of extracted petroleum hydrocarbons are accessible by this test method as compared to GC methods that use a time window for quantification, as petroleum hydrocarbons eluting outside these windows are quantified too.  
1.3 This test method covers the range of 0.1 mg/L to 1000 mg/L and may be extended to a lower or higher level by extraction of a larger or smaller sample volume collected separately.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.  
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.

SIGNIFICANCE AND USE
5.1 This guide is intended as a means for obtaining an extract from mine rock and soil samples to measure cyanide content in the aqueous portion of the sample on a dry weight basis. Cyanide is analyzed in mine rock and soil extracts for measurement of cyanide concentration; however, improper sample collection and extraction can result in significant positive or negative bias.  
5.2 This guide is designed to mobilize aqueous cyanides present in the solids, so that the resulting extract can be used to assess leachate that could potentially be produced from mine rock or soil.  
5.3 This guide is not intended to simulate actual site leaching conditions.  
5.4 This guide produces extracts that are amenable to the determination of trace cyanides. When trace cyanides are being determined, it is especially important that precautions be taken in sample preservation, storage, and handling to avoid possible contamination of the extracts.  
5.5 This guide uses a comparative test method and is intended for use as a routine method for monitoring mine rock and soils. It is assumed that all who use this guide will be trained analysts capable of performing it skillfully and safely. It is expected that work will be performed in a properly equipped laboratory applying appropriate quality control practices such as those described in Guide D3856.  
5.6 This guide identifies proper methods for obtaining mine rock and soil samples for the specific purpose of measuring cyanide concentrations.
SCOPE
1.1 This guide is applicable for the collection, extraction, and preservation of extracts from mine rock and soil samples for the analysis of cyanide in the extracts. Responsibilities of field sampling personnel and the laboratory are indicated.  
1.2 The sampling, preservation, and extraction procedures described in this guide are recommended for the analysis of total cyanide, available cyanide, weak acid dissociable cyanide, and free cyanide by Test Methods D2036, D4282, D4374, D6888, D6994, D7237, and D7284. The information supplied in this guide can also be applied to other analytical methods for cyanide, for example, US EPA Method 335.4.  
1.3 The procedure options methods appear in the following order:    
Procedure Option  
Sections  
Option A
Laboratory Processing of Field
Preserved Samples  
11 and 12  
Option B
Laboratory Processing of Moist
Field Samples  
13 and 14  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.  
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.

SIGNIFICANCE AND USE
5.1 Source water protection calls for a rapid and reliable optical method to identify and quantify the oil spill contamination, such as water-soluble fraction of aromatic compounds from the BTEX family (benzene, toluene, ethylbenzene, and xylenes) and naphthalene from the polycyclic aromatic hydrocarbon (PAH) group.  
5.2 This test method identifies the presence of contamination and quantifies the target contamination component(s) to provide a threshold-based alert signal.  
5.3 This test method can be used by drinking water treatment plant operators and decision makers as a first line of defense for both initially detecting petroleum product spills, as well as tracking attenuation over time, in source water to prevent contaminant uptake into the processed water and treatment infrastructure.
SCOPE
1.1 This test method covers the (1) detection of trace level (µg/L range) of oil and petroleum (water-soluble fraction) pollutants in surface and ground drinking water sources, (2) identification of the compounds, and (3) alerting analysts with a contaminant concentration prediction. This test method facilitates identification and quantification from 20 to 1000 µg/L of target contaminants, including: water-soluble fraction of aromatic compounds from the BTEX family (benzene, toluene, ethylbenzene, and xylenes) and naphthalene from the polycyclic aromatic hydrocarbon (PAH) group, referred to as BTEXN in this test method, in water samples with up to 15 mg/L of dissolved organic carbon (DOC). The main approach involves analyzing and characterizing key water intake locations before the treatment and developing the contaminant library. The water-soluble (BTEXN) contaminants are associated with, but not limited to petroleum oils and fuels including commercial diesel fuel, gasoline, kerosene, heavy oil, fuel oil and lubricate oil, etc.  
1.2 The data sets are analyzed using multivariate methods to test contaminant identification and quantification. The multivariate methods include classification and regression algorithms to analyze fluorescence EEM data acquired in the laboratory. The common goal of these algorithms is to reduce multidimensionality and eliminate noise of fluorescence and background signals. Automated identification-quantification methods linked directly to the instrument acquisition-analysis software are commercially available.  
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.

SIGNIFICANCE AND USE
5.1 This test method is useful in distinguishing between the potentially available free cyanide (total cyanide) and the free cyanide actually present.  
5.2 This test method provides a convenient technique for making on-site free cyanide determinations.
SCOPE
1.1 This test method covers the determination of free cyanides in waters and wastewaters. Free cyanide is here defined as the cyanide which diffuses as cyanide (HCN), at room temperature, from a solution at pH 6.2  
1.2 This test method does not include complexes that resist dissociation, such as hexacyanoferrates and gold cyanide, nor does it include thiocyanate and cyanohydrin.  
1.3 This test method may be applied to water and wastewater samples containing free cyanide from 10 to 150 μg/L. Greater concentrations may be determined by appropriate dilution.  
1.4 This test method has been fully validated by collaborative testing as specified by Practice D2777.  
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. For specific hazard statements, see 8.6, 8.9, Section 9, and 12.2.1.  
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.

SIGNIFICANCE AND USE
5.1 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 addresses the mitigation of known interferences prior to the analysis of cyanide. Responsibilities of field sampling personnel and the laboratory are indicated.  
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 D2036, D4282, D4374, D6888, D6994, D7237, D7284, and D7511. The information supplied in this practice can also be applied to other analytical methods for cyanide, for example, EPA Method 335.4.  
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.

SIGNIFICANCE AND USE
5.1 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. PFAS have been detected in soils, sludges, surface, and drinking waters. This is a quick, easy, and robust method to quantitatively determine these compounds at trace levels in water matrices.  
5.2 This test method has been validated using reagent water and waters from sites that include landfill leachate, metal finisher, POTW Effluent, Hospital, POTW Influent, Bus washing station, Power Plant and Pulp and paper mill effluent for selected PFAS, refer to the Precision and Bias (Section 17).
SCOPE
1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFASs) in aqueous matrices using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are co-solvated by a 1+1 ratio of sample and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM).  
1.2 The method detection limit (MDL) (see Note 1) and reporting range (see Note 2) for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method is an integer value that is calculated from the concentration from the lowest standard from the final volume of the prepared sample. This value may be lower than the calculated MDL due to sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation. All samples should be taken at a minimal as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable.
Note 1: The MDL is determined following the Code of Federal Regulations (CFR), 40 CFR Part 136, Appendix B utilizing dilution and filtration. A detailed process determining the MDL is explained in the reference and is beyond the scope of this test method.
Note 2: Injection volume variations, and sensitivity of the instrument used will change the reporting limit and ranges.  
1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography and other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this test method at the lower concentrations are met.  
1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening the chromatographic run simply to save time are not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to re-validate the modified test.  
1.2.3 Analyte detections between the method detection limit and the reporting limit are estimated concentrations. The reporting limit is based upon the concentration of the Level 1 calibration standard as shown in Table 5.  
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 P...

SIGNIFICANCE AND USE
5.1 Cyanide is highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastes and in surface waters (Appendix X1).  
5.2 Test Method D is applicable for natural water and clean metal finishing or heat treatment effluents. It may be used for process control in wastewater treatment facilities providing its applicability has been validated by Test Method B or C.  
5.3 The spot test outlined in Annex A1 can be used to detect cyanide and thiocyanate in water or wastewater, and to approximate its concentration.
SCOPE
1.1 These test methods cover the determination of cyanides in water. The following test methods are included:    
Sections  
Test Method A
Total Cyanides after Distillation  
12 – 18  
Test Method B
Cyanides Amenable to Chlorination2
by Difference  
19 – 25  
Test Method C
Weak Acid Dissociable Cyanides  
26 – 32  
Test Method D
Cyanides Amenable to Chlorination without
Distillation (Short-Cut Method)  
33 – 39  
1.2 Cyanogen halides may be determined separately.  
Note 1: Cyanogen chloride is the most common of the cyanogen halide complexes as it is a reaction product and is usually present when chlorinating cyanide-containing industrial waste water. For the presence or absence of CNCl, the spot test method given in Annex A1 can be used.  
1.3 These test methods do not distinguish between cyanide ions and metallocyanide compounds and complexes. Furthermore, they do not detect the cyanates. Cyanates can be determined using ion chromatography without digestion.
Note 2: The cyanate complexes are decomposed when the sample is acidified in the distillation procedure.  
1.4 The cyanide in cyanocomplexes of gold, platinum, cobalt and some other transition metals is not completely recovered by these test methods. Refer to Test Method D6994 for the determination of cyanometal complexes.  
1.5 Cyanide from only a few organic cyanides are recovered, and those only to a minor extent.  
1.6 Part or all of these test methods have been used successfully with reagent water and various waste waters. It is the user's responsibility to assure the validity of the test method for the water matrix being tested.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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. Specific hazard statements are given in 5.1, 8.8, 8.18, Section 9, 11.3, and 16.1.9.  
1.9 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.

SIGNIFICANCE AND USE
5.1 Nitrosamines are a class of nitrogen-containing compounds with a known occurrence in wastewater. They may also be created in deionization and are a potential contaminant in water for reuse. The World Health Organization has issued a guideline for NDMA in drinking water at 0.1 µg/L. NDMA may occur in chlorinated effluents and other wastewaters. Other methods for nitrosamines employ solid phase extraction, which may not be applicable to wastewaters that contain particulate matter or a high organic load. This method analyses nitrosamines directly using LC-MS/MS.
SCOPE
1.1 This test method covers the liquid chromatography tandem mass spectrometry (LC-MS/MS) detection and quantitation of N-nitrosamines after direct injection. It has been validated for groundwater, surface water, wastewater influents, and wastewater effluents. This test method is not limited to these aqueous matrices; however, the applicability of this test method to other aqueous matrices must be demonstrated.  
1.2 This test method is applicable to nitrosamines that can be chromatographed and detected using a mass spectrometry procedure. Table 1 lists the compounds that have been validated for this test method. This test method is not limited to the compounds listed in Table 1; however, the applicability of the test method to other compounds must be demonstrated.  
1.3 Analyte concentrations from 0.05 µg/L up to approximately 5 µg/L may be determined without dilution of the sample. Analytes with insufficient sensitivity will not be detected, but they can be measured with acceptable accuracy and precision when present in sufficient amounts. In addition, newer instruments, or instruments of improved sensitivity may be used to lower detection limits.  
1.4 Analytes that are not separated chromatographically, but that have different mass spectra and noninterfering quantitation ions, can be identified and measured in the same calibration mixture or water sample. Analytes that have very similar product ions cannot be individually identified and measured in the same calibration mixture or water sample unless they have different retention times.  
1.5 It is the responsibility of the user to ensure the validity of this test method for untested matrices.  
1.6 This test method is restricted to use by or under the supervision of analysts experienced in the use of a liquid chromatograph with tandem mass spectrometry (LC-MS/MS).  
1.7 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting method quality acceptance criteria. Shortening the chromatographic run simply to save time is not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to re-validate the modified test.  
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.9 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.  
1.10 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.

SIGNIFICANCE AND USE
5.1 This method directly determines the concentrations of dissolved PAH concentrations in environmental sediment pore water samples. The method is important from an environmental regulatory perspective because it can achieve the analytical sensitivities to meet the goals of the USEPA narcosis model for protecting benthic organisms in PAH contaminated sediments. Regulatory methods using solvent extraction have not achieved the wide calibration ranges from nanograms to milligrams per litre and the required levels of detection in the nanogram-per-litre range. In addition, conventional solvent extraction methods require large aliquot volumes (litre or larger), use of large volumes of organic solvents, and filtration to generate the pore water. This approach entails the storage and processing of large volumes of sediment samples and loss of low molecular weight PAHs in the filtration and solvent evaporation steps.  
5.2 This method can be used to determine nanogram to milligram per litre PAH concentrations in pore water. Small volumes of pore water are required for SPME extraction, only 1.5 mL per determination and virtually no solvent extraction waste is generated.
SCOPE
1.1 The U.S. Environmental Protection Agency (USEPA) narcosis model for benthic organisms in sediments contaminated with polycyclic aromatic hydrocarbons (PAHs) is based on the concentrations of dissolved PAHs in the interstitial water or “pore water” in sediment. This test method covers the separation of pore water from PAH-impacted sediment samples, the removal of colloids, and the subsequent measurement of dissolved concentrations of the required 10 parent PAHs and 14 groups of alkylated daughter PAHs in the pore water samples. The “24 PAHs” are determined using solid-phase microextraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS) analysis in selected ion monitoring (SIM) mode. Isotopically labeled analogs of the target compounds are introduced prior to the extraction, and are used as quantification references.  
1.2 Lower molecular weight PAHs are more water soluble than higher molecular weight PAHs. Therefore, USEPA-regulated PAH concentrations in pore water samples vary widely due to differing saturation water solubilities that range from 0.2 µg/L for indeno[1,2,3-cd]pyrene to 31 000 µg/L for naphthalene. This method can accommodate the measurement of microgram per litre concentrations for low molecular weight PAHs and nanogram per litre concentrations for high molecular weight PAHs.  
1.3 The USEPA narcosis model predicts toxicity to benthic organisms if the sum of the toxic units (ΣTUc) calculated for all “34 PAHs” measured in a pore water sample is greater than or equal to 1. For this reason, the performance limit required for the individual PAH measurements was defined as the concentration of an individual PAH that would yield 1/34 of a toxic unit (TU). However, the focus of this method is the 10 parent PAHs and 14 groups of alkylated PAHs (Table 1) that contribute 95 % of the toxic units based on the analysis of 120 background and impacted sediment pore water samples.3 The primary reasons for eliminating the rest of the 5-6 ring parent PAHs are: (1) these PAHs contribute insignificantly to the pore water TU, and (2) these PAHs exhibit extremely low saturation solubilities that will make the detection of these compounds difficult in pore water. This method can achieve the required detection limits, which range from approximately 0.01 µg/L, for high molecular weight PAHs, to approximately 3 µg/L for low molecular weight PAHs.  
1.4 The test method may also be applied to the determination of additional PAH compounds (for example, 5- and 6-ring PAHs as described in Hawthorne et al.).4 However, it is the responsibility of the user of this standard to establish the validity of the test method for the determination of PAHs other than those referenced in 1.1 and Table 1.  
1.5 The values stated in ...

SIGNIFICANCE AND USE
5.1 The major organic constituents in industrial waste water need to be identified for support of effective in-plant or pollution control programs. Currently, the most practical means for tentatively identifying and measuring a range of volatile organic compounds is gas-liquid chromatography.
SCOPE
1.1 This test method covers a wide range of alcohols with various structures and boiling points that can be separated and detected quantitatively in water and waste water at a minimum detection limit of approximately 1 mg/L by aqueous-injection gas-liquid chromatography.2 This test method can also be used to detect other volatile organic compounds qualitatively. Organic acids, amines, and high boiling, highly polar compounds are not readily detectable under this set of conditions. For analysis of organics with similar functionalities, refer to other test methods in Volumes 11.01 and 11.02 of the Annual Book of ASTM Standards.  
1.2 This test method utilizes the procedures and precautions as described in Practice D2908. Utilize the procedures and precautions as described therein.  
1.3 This test method has been used successfully with reagent grade Type II and natural chlorinated tap waters. It is the user's responsibility to assure the validity of this test method for any untested matrices.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.  
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.

SIGNIFICANCE AND USE
5.1 This practice is useful for detecting and identifying (or determining the absence of) 90 chemicals with relatively high fluorescence yields (see Table 1). Most commonly, this practice will be useful for distinguishing single fluorescent chemicals in solution, simple mixtures or single fluorescing chemicals in the presence of other nonfluorescing chemicals. Chemicals with high fluorescence yields tend to have aromatic rings, some heterocyclic rings or extended conjugated double-bond systems. Typical chemicals included on this list include aromatics, substituted aromatics such as phenols, polycyclic aromatic hydrocarbons (PAH’s), some pesticides such as DDT, polychlorinated biphenyls (PCB’s), some heterocyclics, and some esters, organic acids, and ketones.    
5.2 With appropriate separatory techniques (HPLC, TLC, and column chromatography) and in some cases, special detection techniques (OMA’s and diode arrays), this practice can be used to determine these 90 chemicals even in complex mixtures containing a number of other fluorescing chemicals. With the use of appropriate excitation and emission wavelengths and prior generation of calibration curves, this practice could be used for quantitation of these chemicals over a broad linear range.  
5.3 Fluorescence is appropriately a trace technique and at higher concentrations (greater than 10 to 100 ppm) spectral distortions usually due to self-absorption, or inner-filter effects but sometimes ascribed to fluorescence quenching, may be observed. These effects can usually be eliminated by diluting the solution. Detection limits can be lowered following identification by using broader slit widths, but this may result in spectral broadening and distortion.  
5.4 This practice assumes the use of a corrected spectrofluorometer (that is, one capable of producing corrected fluorescence spectra). On an uncorrected instrument, peak shifts and spectral distortions and changes in peak ratios may be noted. An uncorrected spect...
SCOPE
1.1 This practice allows for the identification of 90 chemicals that may be found in water or in surface layers on water. This practice is based on the use of room-temperature fluorescence spectra taken from lists developed by the U.S. Environmental Protection Agency and the U.S. Coast Guard (1). Ref (1) is the primary source for these spectra. This practice is also based on the assumption that such chemicals are either present in aqueous solution or are extracted from water into an appropriate solvent.2  
1.2 Although many organic chemicals containing aromatic rings, heterocyclic rings, or extended conjugated double-bond systems have appreciable quantum yields of fluorescence, this practice is designed only for the specific compounds listed. If present in complex mixtures, preseparation by high-performance liquid chromatography (HPLC), column chromatography, or thin-layer chromatography (TLC) would probably be required.  
1.3 If used with HPLC, this practice could be used for the identification of fluorescence spectra generated by optical multichannel analyzers (OMA) or diode-array detectors.  
1.4 For simple mixtures, or in the presence of other nonfluorescing chemicals, separatory techniques might not be required. The excitation and emission maximum wavelengths listed in this practice could be used with standard fluorescence techniques (see Refs (2-6)) to quantitate these ninety chemicals once identification had been established. For such uses, generation of a calibration curve, to determine the linear range for use of fluorescence quantitation would be required for each chemical. Examination of solvent blanks to subtract or eliminate any fluorescence background would probably be required.  
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 practi...

SIGNIFICANCE AND USE
5.1 PFASs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFASs have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.6 PFASs have been detected in soils, sludges, surface, and drinking waters. Hence, there is a need for quick, easy, and robust method to determine these compounds at trace levels in water matrices for understanding of the sources and pathways of exposure.  
5.2 This test method has been investigated for use with reagent, surface, sludge and wastewaters for selected PFASs. This test method has not been evaluated on drinking water matrices.
SCOPE
1.1 This procedure covers the determination of selected per- and polyfluoroalkyl substances (PFASs) in a water matrix using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to a technique known as selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM). This is not a drinking water method; performance of this test method has not been evaluated on drinking water matrices.  
1.2 The method detection limit (MDL)2 and reporting range3 for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method was 10 ng/L for most of the target analytes at the time of development.    
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit may be lowered providing your lab meets the minimum performance requirements of this test method at the lower concentrations, this test method is performance based and modifications are allowed to improve performance. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is the concentration of the Level 1 calibration standard as shown in Table 4 for the PFASs after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration concentration for FHEA and FOEA, these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.  
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.

SIGNIFICANCE AND USE
5.1 Chlorinated phenoxyacid herbicides, and other organic acids are used extensively for weed control. Esters and salts of 2,4-D and silvex have been used as aquatic herbicides in lakes, streams, and irrigation canals. Phenoxy acid herbicides can be toxic even at low concentrations. For example, the 96 h, TLm for silvex is 2.4 mg/L for bluegills (1).8 These reasons make apparent the need for a standard test method for such compounds in water.
SCOPE
1.1 This test method covers a gas chromatographic procedure for the quantitative determination of selected chlorinated acids and other acidic herbicides in water. Similar chemicals may also be determined by this test method, but it is the user’s responsibility to verify the applicability of this test method to any compounds not listed in this scope. The acid form of the following compounds were interlaboratory tested using this test method, and the results were found acceptable:2    
Analyte  
Chemical Abstract Services
Registry Number  
Bentazon  
25057-89-0  
2,4-D  
94-75-7  
2,4-DB  
94-82-6  
DCPA acid metabolites 2  
Dicamba  
1918-00-9  
3,5-Dichlorobenzoic acid  
51-36-5  
Dichlorprop  
120-36-5  
5-Hydroxydicamba  
7600-50-2  
Pentachlorophenol (PCP)  
87-86-5  
Picloram  
1918-02-1  
2,4,5-T  
93-76-5  
2,4,5-TP (Silvex)  
93-72-1  
1.2 This test method may be applicable to the determination of salts and esters of analyte compounds. The form of each acid is not distinguished by this test method. Results are calculated and reported for each listed analyte as the total free acid.  
1.3 This test method has been validated in an interlaboratory test for reagent water and finished tap water. The analyst should recognize that precision and bias reported in Section 18 may not be applicable to other waters.  
1.4 This test method is restricted to use by or under the supervision of analysts experienced in the use of gas chromatography (GC) and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this test method using the procedure described in 19.3. It is the user’s responsibility to ensure the validity of this test method for waters of untested matrices.  
1.5 Analytes that are not separated chromatographically, that is, which have very similar retention times, cannot be individually identified and measured in the same calibration mixture or water sample unless an alternate technique for identification and quantitation exists (16.6, 16.7, and 16.8).  
1.6 When this test method is used to analyze unfamiliar samples for any or all of the analytes given in 1.1, analyte identifications must be confirmed by at least one additional qualitative technique.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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 warning statements, see Sections 6, 8, 9, and 10.  
1.9 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.

SIGNIFICANCE AND USE
5.1 Cyanide and hydrogen cyanide are highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastes and surface waters.3  
5.2 This test method is applicable for natural waters, industrial wastewaters and effluents.
SCOPE
1.1 This test method is used to determine the concentration of total cyanide in an aqueous wastewater or effluent. This test method detects the cyanides that are free (HCN and CN–) and strong-metal-cyanide complexes that dissociate and release free cyanide when refluxed under strongly acidic conditions.  
1.2 This test method may not be applicable to process solutions from precious metals mining operations.  
1.3 This procedure is applicable over a range of approximately 2 to 500 μg/L (parts per billion) total cyanide. Higher concentrations can be measured with sample dilution or lower injection volume.  
1.4 The determinative step of this test method utilizes flow injection with amperometric detection based on Test Method D6888. Prior to analysis, samples must be distilled with a micro-distillation apparatus described in this test method or with a suitable cyanide distillation apparatus specified in Test Methods D2036.  
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. Specific hazard statements are given in 8.6 and Section 9.  
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.

SIGNIFICANCE AND USE
5.1 When significant quantities of inorganic or organic material are present in water samples (high suspended solids), microplastic particles/fibers can be masked and the ability to conduct reliable identification and quantification analyses of the plastic particles/fibers can be impeded.  
5.2 In order to quantify the occurrence of microplastic particles/fibers in wastewater influent (high suspended solids), the sampling procedure must be able to reliably collect samples at a constant flow over the desired 24-hour interval to reflect changes in diurnal flow. For wastewater influent the capture flow rate should be no less than 1 GPM over the 24-hour interval (approximately 1440 gal or 5450 L total) to minimize the problem with heterogeneity of the suspended solids and to reduce the standard error (the larger the sample size, the smaller the standard error).  
5.3 In order to quantify the occurrence of microplastic particles/fibers in all other water samples with a lower content of inorganic or organic material present addressed by this practice (low to medium suspended solids), a minimum volume of 1500 L (approximately 400 gal) should be filtered through the appropriate filters or sieves to minimize potential issues with heterogeneity of suspended solids and to reduce the standard error (the larger the sample size, the smaller the standard error).  
5.4 Microplastic particles/fibers retained on the sieves are suitable for characterization in terms of size, shape, quantity, and composition (polymer type), dependent upon the chosen analytical method.
SCOPE
1.1 This practice provides for the collection of water samples with high, medium, or low suspended solids to determine the presence, count, polymer type, and physical characteristics of microplastic particles and fibers. This collection practice has been validated for the collection of samples from drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters. This practice is not limited to these particular water matrices; however, the applicability of this practice to other aqueous matrices must be demonstrated.  
1.2 Water samples are passed through filters or sieves of adequate mesh size to enable capture of the smallest desired particle size. For waters with high or medium suspended solids content, a series of sieves with increasingly smaller mesh size should be used to prevent clogging and allow for the collection of desired particle size fractions.  
1.3 Subsequent sample preparation followed by analysis utilizing either Pyrolysis gas chromatography/mass spectrometry (Py-GC/MS), IR spectroscopy, or Raman spectroscopy may be used to identify the quantity (mass or number count) and composition (polymer type) of microplastic particles/fibers. The spectroscopic methods can provide a count of the number of particles and fibers present in a sample, and Py-GC/MS can provide the mass present in a sample. When desired, microplastic particle/fiber size, shape and surface characteristics can be ascertained with appropriate instruments such as a scanning electron microscope (SEM).  
1.4 Units—The values stated in SI units are to be regarded as the standard except where standard U.S. equipment is specified in imperial units, for example, inches and gallons. No other units of measurement are included in this standard.  
1.5 Standard Practice—This practice offers a set of instructions for performing one or more specific operations. This practice cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this practice may be applicable in all circumstances. This practice is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this practice be applied without consideration of a project’s many unique aspects.  
1.6 This standard does not purport to addre...

SIGNIFICANCE AND USE
5.1 Large volumes of water are required to be sieved for accurate quantification of microplastics. Water with high to medium content of suspended solids can lead to an excess of inorganic and organic background material which can interfere with the ability to conduct reliable analyses. The presence of this background material can often impede the ability to accurately discern, distinguish and identify the number of microplastic particles in solution.  
5.2 The digestion described in this procedure allows for significant reduction of interfering substances and contaminants, rendering a sample suitable for particle and fiber characterization and identification using either Raman and IR spectroscopic analysis or for polymeric quantification and identification by Pyrolysis-GC/MS.  
5.3 For water samples with medium to low suspended solids, the oxidation and digestion steps necessary will be dependent upon the type and nature of interfering substances and contaminants and may be determined through simple trial efforts.
SCOPE
1.1 This practice provides for the sample preparation of collected water samples with high, medium, or low suspended solids to determine the presence, count, polymer type, and physical characteristics of microplastic particles and fibers. It has been designed for the preparation of samples collected from drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters using collection practice (Practice D8332). This practice is not limited to these particular water matrices; however, the applicability of this practice to other aqueous matrices must be demonstrated.  
1.2 This practice consists of a wet peroxide oxidation followed by progressive enzymatic digestion to the extent necessary to remove interfering organic constituents such as cellulose, lipids and chitin that are typically found in abundance in water matrices of samples with high to medium suspended solids such as wastewater influent. For water samples with low suspended solids, such as but not limited to drinking water and tertiary treated wastewater, the oxidation and digestion steps may not be necessary.  
1.3 Water samples prepared using this practice are suitable for analysis utilizing either Pyrolysis-GC/MS methods for qualitative identification and mass quantitation, or IR spectroscopy or Raman spectroscopy for identifying the quantity (number count) and composition (polymer type) of microplastic particles. If desired, microplastic particle size and shape may be ascertained with appropriate instruments such as a scanning electron microscope (SEM) and microscopy techniques.  
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 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.  
1.6 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.

SIGNIFICANCE AND USE
5.1 This test method is useful for the determination of total chemically bound nitrogen in wastewaters and other waters.
SCOPE
1.1 This test method covers the determination of the total nitrogen content of water in concentrations from 0.5 to 1000 mg/L. Higher nitrogen concentrations may be determined by making the proper dilutions.  
1.2 This test method does not determine molecular nitrogen (N2).  
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.

SIGNIFICANCE AND USE
5.1 This test method is necessary because of the need for rapid reliable tests for carbonaceous material in waters and sediments.  
5.2 It is used for determining the concentration of organic carbon in water that comes from a variety of natural, domestic, and industrial sources. Typically, these measurements are used to monitor organic pollutants in domestic and industrial waste water.  
5.3 When a sample is homogenized so that particulate, immiscible phases, and dissolved carbon from both organic and inorganic sources is determined, the measurement is called total carbon (TC). When inorganic carbon response is eliminated by removing the dissolved CO2 prior to the analysis or the dissolved CO2 concentration subtracted from the total carbon concentration, the measurement is called total organic carbon (TOC). When particulates and immiscible phases are removed prior to analysis the measurement is called dissolved carbon (DC), or dissolved organic carbon (DOC) if inorganic carbon response has been eliminated.  
5.4 Homogenizing or sparging of a sample, or both, may cause loss of volatile organics, thus yielding a negative error. The extent and significance of such losses must be evaluated on an individual basis. If significant quantities of volatile carbonaceous materials are present or may be present in samples organic carbon should be determined by the difference between the total carbon and the inorganic carbon concentrations. When organic carbon determined both by difference and by sparging agree it is acceptable to determine organic carbon by sparging for similar samples.  
5.5 The relationship of TOC to other water quality parameters such as COD and BOD is described in the literature.5
SCOPE
1.1 This test method covers the determination of total and organic carbon in water and waste water, including brackish waters and brines in the range from 2 to 20 000 mg/L. This test method has the advantages of a wide range of concentration which may be determined without sample dilution and the provision for boat or capillary introduction of samples containing sediments and particulate matter where syringe injection is inappropriate.  
1.2 This procedure is applicable only to that carbonaceous matter in the sample that can be introduced into the reaction zone. When syringe injection is used to introduce samples into the combustion zone, the syringe needle opening size limits the maximum size of particles that can be present in samples. Sludge and sediment samples must be homogenized prior to sampling with a micropipetor or other appropriate sampler and ladle introduction into the combustion zone is required.  
1.3 The precision and bias information reported in this test method was obtained in collaborative testing that included waters of the following types: distilled, deionized, potable, natural, brine, municipal and industrial waste, and water derived from oil shale retorting. Since the precision and bias information reported may not apply to waters of all matrices, it is the user’s responsibility to ensure the validity of this test method on samples of other matrices.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 precautionary statements, see 9.1 and 10.2.1.  
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.

ABSTRACT
This practice establishes the standard method of preserving waterborne oil samples from the time of collection to the time of analysis. Information is provided to ensure sample integrity and to avoid contamination and to minimize microbial degradation. This practice is for controlled field or laboratory conditions and specifies thorough preparation of equipment and precise operation. If, however, these details must be compromised in a field emergency, nonstandard simplifications that will minimize or eliminate consequent errors are recommended. This procedure requires the use of the following apparatuses: sample containers, preferably borosilicate glass (plastic and metal are not acceptable ); closures; an explosion-proof refrigerator; and shipping containers (sturdy cartons or wooden boxes). Samples may be of several types, such as tar balls, collected oil, oil-water mixtures, emulsions, and oil and water on collecting devices such as silanized glass cloth, TFE-fluorocarbon polymer, or other materials. Instructions are given for the care of samples to minimize changes due to autoxidation and microbial attack between the time of sampling and the time of testing. Services available for transportation of samples are described as well.
SCOPE
1.1 This practice covers the preservation of waterborne oil samples from the time of collection to the time of analysis. Information is provided to ensure sample integrity and to avoid contamination and to minimize microbial degradation.  
1.2 The practice is for controlled field or laboratory conditions and specifies thorough preparation of equipment and precise operation. Where these details must be compromised in a field emergency, nonstandard simplifications are recommended that will minimize or eliminate consequent errors.  
Note 1: Procedures for the analysis of oil spill samples are Practices D3326, D3415, and D4489, and Test Methods D3650, D3327, D3328, and D3414. A guide to the use of ASTM test methods for the analysis of oil spill samples is found in Practice D3415.  
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.

SIGNIFICANCE AND USE
5.1 Phenolic compounds are sometimes found in surface waters from natural and industrial sources. Their presence in streams and other waterways frequently will cause off flavor in fish tissue and other aquatic food.  
5.2 Chlorination of waters containing phenols may produce chlorophenols that are odoriferous and objectionable tasting.
SCOPE
1.1 These test methods cover the preparation of the sample and the determination of the concentration of phenolic compounds in water. They are based on the color reaction of phenol (C6H5OH) with 4-aminoantipyrine and any color produced by the reaction of other phenolic compounds is reported as phenol. The concentration of phenol measured represents the minimum concentration of phenolic compounds present in the sample.  
1.2 Phenolic compounds with a substituent in the para position may not quantitatively produce color with 4-aminoantipyrine. However, para substituents of phenol such as carboxyl, halogen, hydroxyl, methoxyl, or sulfonic acid groups do produce color with 4-aminoantipyrine.  
1.3 These test methods address specific applications as follows:    
Range  
Sections  
Test Method A—Chloroform Extraction  
0 to 100 μg/L  
11 to 17  
Test Method B—Direct Photometric  
>0.1 mg/L
(100 μg/L)  
18 to 24  
1.4 It is the users’ responsibility to assure the validity of the standard test method for use in their particular matrix of interest.  
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. For specific hazard statements see 6.3.2 and 8.6.  
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.

SIGNIFICANCE AND USE
5.1 The widespread use and discharge of detergents into surface waters can result in a lowering of its aesthetic quality by foam formation and by causing toxicity to aquatic wildlife. This test method is capable of detecting small concentrations of detergents as MBAS so that they can be controlled to prevent such problems.  
5.2 Biodegradable linear alkyl benzene sulfonates (LAS) have replaced the branched-chain alkyl benzene sulfonates (ABS) in detergent formulations, which were more resistant to biodegradation. Differentiation between linear and branched-chain alkyl benzene sulfonates, as well as differentiation of the various positional isomers of either type, is not possible by this test method. While the methylene blue method may be employed to monitor studies designed to measure biodegradability, it cannot be used to predict this quality.
SCOPE
1.1 This test method covers the determination of compounds that react with methylene blue under the conditions specified in the test procedure. They are referred to as methylene blue active substances (MBAS), and are calculated and reported in terms of the reference material, linear alkyl benzene sulfonate, LAS.  
1.2 This test method is applicable for determining MBAS in water and wastewater. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.  
1.3 This test method is a simple, rapid, control procedure suitable for monitoring the effectiveness of a biodegradation or other linear alkyl benzene sulfonate (LAS) removal process. For greater specificity and interference removal, the pretreatment procedure in Annex A1 should be used. Data derived without the pretreatment procedure should be interpreted with care. This test method is applicable in the range from 0.03 to 1.5 mg/L for a 100-mL sample.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 a specific hazard statement, see 8.3.  
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.