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ASTM D7781-23

(Test Method)

Standard Test Method for Nitrite-Nitrate in Water by Nitrate Reductase

Standard Test Method for Nitrite-Nitrate in Water by Nitrate Reductase

SIGNIFICANCE AND USE
5.1 This test method replaces Methods D1254 (Nitrite) and D992 (Nitrate). The nitrite test method (Method D1254) used a reagent that is considered to be a potential carcinogen. The nitrate test method (Method D992) has been shown to have relatively large errors when used in wastewaters and also has greater manipulative difficulties than the test method described herein.  
5.2 This test method can be used in place of Test Methods D3867 (Nitrite-Nitrate). Test Methods D3867 uses cadmium for the reduction of nitrate to nitrite. Cadmium is considered a toxic metal. Also, the heterogeneous cadmium reductant creates greater difficulty than the reduction described in this test method.
SCOPE
1.1 This test method is applicable to the determination of nitrate plus nitrite (as nitrogen) in drinking water, surface, saline, wastewater, and ground waters. The applicable range of this test method is from 0.05 to 5 mg/L of nitrogen. The range may be extended upward by dilution of an appropriate aliquot. The 40 CFR Part 136 Method Detection Limit (MDL) is 0.02 mg/L.  
1.2 It is the user's responsibility to ensure the validity of this test method for waters of untested matrices. The quality control criteria in Section 17 for method blanks, laboratory control samples, matrix spikes and matrix duplicates must be met.  
1.3 The values stated in SI units are 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.

General Information

Status
Published
Publication Date
31-Mar-2023
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.05 - Inorganic Constituents in Water
Current Stage
Ref Project

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ASTM D7781-23 - Standard Test Method for Nitrite-Nitrate in Water by Nitrate ReductaseASTM D7781-23 - Standard Test Method for Nitrite-Nitrate in Water by Nitrate Reductase
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ASTM D7781-23 - Standard Test Method for Nitrite-Nitrate in Water by Nitrate Reductase
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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.
Designation: D7781 − 23
Standard Test Method for
1
Nitrite-Nitrate in Water by Nitrate Reductase
This standard is issued under the fixed designation D7781; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D1193 Specification for Reagent Water
D1254 Method of Test for Nitrite Ion in Water (Withdrawn
1.1 This test method is applicable to the determination of
3
1980)
nitrate plus nitrite (as nitrogen) in drinking water, surface,
D3867 Test Methods for Nitrite-Nitrate in Water
saline, wastewater, and ground waters. The applicable range of
D5810 Guide for Spiking into Aqueous Samples
this test method is from 0.05 to 5 mg/L of nitrogen. The range
D6146 Guide for Monitoring Aqueous Nutrients in Water-
may be extended upward by dilution of an appropriate aliquot.
sheds
The 40 CFR Part 136 Method Detection Limit (MDL) is 0.02
mg/L.
3. Terminology
1.2 It is the user’s responsibility to ensure the validity of this
3.1 Definitions—For definitions of terms used in these test
test method for waters of untested matrices. The quality control
methods, refer to Terminology D1129.
criteria in Section 17 for method blanks, laboratory control
3.2 Definitions of Terms Specific to This Standard:
samples, matrix spikes and matrix duplicates must be met.
3.2.1 bispecific NaR, n—nitrate reductase that can use either
1.3 The values stated in SI units are regarded as standard.
NADH or NADPH as its electron donor (cofactor).
No other units of measurement are included in this standard.
3.2.2 discrete analyzer, n—a programmable, computer-
1.4 This standard does not purport to address all of the
controlled instrument that automates wet-chemical analysis by
safety concerns, if any, associated with its use. It is the
using one or more robotic arms interfaced to high-precision
responsibility of the user of this standard to establish appro-
volumetric dispensers to aspirate and dispense samples,
priate safety, health, and environmental practices and deter-
standards, diluents, and reagents.
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
3.2.3 Greiss reaction, n—chemical formation of an azo dye
dance with internationally recognized principles on standard-
by diazotization of nitrite ion with sulfanilamide and subse-
ization established in the Decision on Principles for the
quent coupling with N-(1-naphthyl)ethylenediamine hydro-
Development of International Standards, Guides and Recom-
chloride.
mendations issued by the World Trade Organization Technical
3.2.4 NADH, n—nicotinamide adenine dinucleotide, re-
Barriers to Trade (TBT) Committee.
duced form is a coenzyme found in all living cells.
2. Referenced Documents
3.2.5 NADPH, n—nicotinamide adenine dinucleotide
2
2.1 ASTM Standards: phosphate, reduced form is a coenzyme found in all living
D0992 Method of Test for Nitrate Ion in Water (Withdrawn cells; NADP+ is the oxidizing form and NADPH is the
3
1983) reducing form.
D1129 Terminology Relating to Water
3.2.6 nitrate reductase (NaR), n—NADH:NaR (EC1.7.1.1
D1141 Practice for Preparation of Substitute Ocean Water
and CAS 9013-03-0) or bispecific NaR (EC 1.7.1.2 and CAS
9029-27-0) with 1 unit of enzyme activity defined as 1
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
micromol nitrite produced per minute at 30 °C, at pH 7 with
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
NADH (refer to 3.2.4 and 10.2) as an electron donor.
in Water.
Current edition approved April 1, 2023. Published April 2023. Originally
approved in 2014. Last previous edition was approved in 2014 as D7781 – 14 which 4. Summary of Test Method
was withdrawn January 2023 and reinstated in April 2023. DOI: 10.1520/D7781-23.
2
4.1 Nitrite-Nitrate Nitrogen—The sample is mixed with a
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
buffered solution containing NAD(P)H: nitrate reductase (EC
Standards volume information, refer to the standard’s Document Summary page on
1.7.1-3) and NADH or NADPH to reduce nitrate ion to nitrite
the ASTM website.
3
ion. The combined nitrite-nitrate (expressed as mg/L
The last approved version of this historical standard is referenced on
www.astm.org. NO +NO -N) is determined by diazotizing the total nitrite ion
3 2
Copyright © ASTM International, 100 Barr
...

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5.1 A rapid and routine procedure for determining biomass of the living microorganisms in cultures, waters, wastewaters, and in plankton and periphyton samples taken from surface waters is frequently of vital importance. However, classical techniques such as direct microscope counts, turbidity, organic chemical analyses, cell tagging, and plate counts are expensive, time-consuming, or tend to underestimate total numbers. In addition, some of these methods do not distinguish between living and nonliving cells.  
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5.1 This test method is useful for the analysis of total uranium in water following wet-ashing, as required, due to impurities or suspended materials in the water.
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1.1 This test method covers the determination of total uranium, by mass concentration, in water within the calibrated range of the instrument, 0.1 μg/L or greater. Samples with uranium mass concentrations above the laser phosphorimeter dynamic range are diluted to bring the concentration to a measurable level.  
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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.  
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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.  
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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  
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5.1 Pesticides may be used in various agricultural and household products. These products may enter waterways at low levels through run-off or misuse near water resources. Hence, there is a need for quick, easy and robust method to determine pesticide concentration in water matrices for understanding the sources and concentration levels in affected areas.  
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1.1 This test method covers the determination of bisphenol A (BPA) extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). BPA is qualitatively and quantitatively determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
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Standard Test Method for Determination of Aldicarb, Aldicarb Sulfone, Aldicarb Sulfoxide, Carbofuran, Methomyl, Oxamyl, and Thiofanox in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

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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.

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ASTM
ASTM D8478-23(Test Method)
Standard Test Method for N-Hexane Recoverable Total Oil and Grease and Total Petroleum Hydrocarbons in Water by ATR-Infrared Determination

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.

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