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ASTM D8193-18

(Test Method)

Standard Test Method for Total Oil and Grease (TOG) and Total Petroleum Hydrocarbon (TPH) in Water and Wastewater with Solvent Extraction Using Non-Dispersive Mid-IR Transmission Spectroscopy

Standard Test Method for Total Oil and Grease (TOG) and Total Petroleum Hydrocarbon (TPH) in Water and Wastewater with Solvent Extraction Using Non-Dispersive Mid-IR Transmission Spectroscopy

SIGNIFICANCE AND USE
5.1 The presence and concentration of total petroleum hydrocarbons, as well as total 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 total petroleum hydrocarbons as well as total oil and grease in water and wastewater.
SCOPE
1.1 This test method covers the determination of total oil and grease (TOG) that can be extracted from water or wastewater samples by cyclohexane and measured by non-dispersive IR spectroscopy from 1370–1380 cm-1. Treating the extract with Florisil2 to remove polar substances prior to the IR measurement enables determination of the total petroleum (TPH).  
1.2 This 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 solventless IR methods that require drying of the employed solid phase material prior to measurement. Similarly, a more complete fraction of extracted petroleum hydrocarbon is accessible by this method as compared to GC methods that use a time window for quantification, as petroleum hydrocarbons eluting outside these windows are also quantified.  
1.3 This method defines total oil and grease in water as material that can be extracted with cyclohexane and measured by IR absorption in the region of 1370–1380 cm-1 (7.25–7.3 µm). Similarly, total petroleum hydrocarbon in water is defined as material that can be extracted with cyclohexane, remains in the extract after filtration over Florisil and is measured by IR absorption in the region of 1370–1380 cm-1 (7.25–7.3 µm). The concentration of total grease is defined as the difference between the total oil and grease and total petroleum hydrocarbon concentrations.  
1.4 This method covers the range of 0.5 to 1000 mg/L for total oil and grease as well as for total petroleum hydrocarbons and has a method detection limit (MDL) of 0.5 mg/L. The range and method detection limit may be extended to higher or lower concentrations by adjusting the water or solvent volume used in the liquid-liquid extraction.  
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.

General Information

Status
Published
Publication Date
14-Dec-2018
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

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ASTM D8193-18 - Standard Test Method for Total Oil and Grease (TOG) and Total Petroleum Hydrocarbon (TPH) in Water and Wastewater with Solvent Extraction Using Non-Dispersive Mid-IR Transmission SpectroscopyASTM D8193-18 - Standard Test Method for Total Oil and Grease (TOG) and Total Petroleum Hydrocarbon (TPH) in Water and Wastewater with Solvent Extraction Using Non-Dispersive Mid-IR Transmission Spectroscopy
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ASTM D8193-18 - Standard Test Method for Total Oil and Grease (TOG) and Total Petroleum Hydrocarbon (TPH) in Water and Wastewater with Solvent Extraction Using Non-Dispersive Mid-IR Transmission Spectroscopy
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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: D8193 − 18
Standard Test Method for
Total Oil and Grease (TOG) and Total Petroleum
Hydrocarbon (TPH) in Water and Wastewater with Solvent
Extraction Using Non-Dispersive Mid-IR Transmission
1
Spectroscopy
This standard is issued under the fixed designation D8193; 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 lower concentrations by adjusting the water or solvent volume
used in the liquid-liquid extraction.
1.1 This test method covers the determination of total oil
1.5 The values stated in SI units are to be regarded as
and grease (TOG) that can be extracted from water or waste-
standard. No other units of measurement are included in this
watersamplesbycyclohexaneandmeasuredbynon-dispersive
-1
standard.
IR spectroscopy from 1370–1380 cm . Treating the extract
2
with Florisil to remove polar substances prior to the IR
1.6 This standard does not purport to address all of the
measurement enables determination of the total petroleum
safety concerns, if any, associated with its use. It is the
(TPH).
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.2 This method also considers the volatile fraction of
mine the applicability of regulatory limitations prior to use.
petroleum hydrocarbons which is lost by gravimetric methods
1.7 This international standard was developed in accor-
that require solvent evaporation prior to weighing, as well as
dance with internationally recognized principles on standard-
by solventless IR methods that require drying of the employed
ization established in the Decision on Principles for the
solid phase material prior to measurement. Similarly, a more
Development of International Standards, Guides and Recom-
complete fraction of extracted petroleum hydrocarbon is ac-
mendations issued by the World Trade Organization Technical
cessible by this method as compared to GC methods that use a
Barriers to Trade (TBT) Committee.
time window for quantification, as petroleum hydrocarbons
eluting outside these windows are also quantified.
2. Referenced Documents
1.3 This method defines total oil and grease in water as
3
2.1 ASTM Standards:
material that can be extracted with cyclohexane and measured
D1129 Terminology Relating to Water
-1
by IR absorption in the region of 1370–1380 cm (7.25–7.3
D1141 Practice for the Preparation of Substitute Ocean
µm). Similarly, total petroleum hydrocarbon in water is defined
Water
as material that can be extracted with cyclohexane, remains in
D1193 Specification for Reagent Water
the extract after filtration over Florisil and is measured by IR
D2777 Practice for Determination of Precision and Bias of
-1
absorptionintheregionof1370–1380cm (7.25–7.3µm).The
Applicable Test Methods of Committee D19 on Water
concentration of total grease is defined as the difference
D3370 Practices for Sampling Water from Closed Conduits
between the total oil and grease and total petroleum hydrocar-
D5847 Practice for Writing Quality Control Specifications
bon concentrations.
for Standard Test Methods for Water Analysis
1.4 This method covers the range of 0.5 to 1000 mg/L for D7678 Test Method for Total Oil and Grease (TOG) and
total oil and grease as well as for total petroleum hydrocarbons TotalPetroleumHydrocarbons(TPH)inWaterandWaste-
and has a method detection limit (MDL) of 0.5 mg/L. The water with Solvent Extraction using Mid-IR Laser Spec-
range and method detection limit may be extended to higher or troscopy
E168 Practices for General Techniques of Infrared Quanti-
tative Analysis
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
3
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 15, 2018. Published January 2019. DOI: 10.1520/ contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
D8193-18. Standards volume information, refer to the standard’s Document Summary page on
2
Florisil is a trademark by U.S. Silica Company, Frederick, MD. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8193 − 18
4
2.2 ISO Standards: This test method contains procedures that can assist the analyst
ISO 9377
...

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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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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.  
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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.  
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1.1 This test method covers the determination of bromadiolone, brodifacoum, diphacinone and warfarin (referred to collectively as rodenticides in this test method) in water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
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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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1.1 This test method covers the determination of hardness in water by titration with potentiometric detection via optical sensor. This test method is applicable to waters that are free of chemicals that will complex calcium or magnesium. The lower detection limit of this test method is approximately 2 mg/L to 5 mg/L as CaCO3; the upper limit can be extended to all concentrations by sample dilution. It is possible to differentiate between hardness due to calcium ions and that due to magnesium ions by this test method.  
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5.1 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.4 BPA has become an important high volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings and many other products.5  
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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.  
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Standard Test Method for Determination of Select Pesticides in Water by Multiple Reaction Monitoring Liquid Chromatography Tandem Mass Spectrometry

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5.1 Pesticides may be used in various agricultural and household products. These products may enter waterways at low levels through run-off or misuse near water resources. Hence, there is a need for quick, easy and robust method to determine pesticide concentration in water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been single-laboratory validated in reagent water and surface waters (Tables 12-14).
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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.  
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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.  
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Standard Test Method for Determination of Nonylphenol, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

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5.1 NP and OP have been shown to have toxic effects in aquatic organisms. The source of NP and OP is prominently from the use of common commercial surfactants. The most widely used surfactant is nonylphenol ethoxylate (NPEO) which has an average ethoxylate chain length of nine. The ethoxylate chain is readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This method has been investigated and is applicable for environmental waters, including seawater.
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1.1 This test method covers the determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.    
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM D7645-23(Test Method)
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)

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.

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