ASTM D7599-09e1
(Test Method)Standard Test Method for Determination of Diethanolamine, Triethanolamine, N-Methyldiethanolamine and N-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Sp
Standard Test Method for Determination of Diethanolamine, Triethanolamine, <span class="italic">N</span>-Methyldiethanolamine and <span class="italic">N</span>-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Sp
SIGNIFICANCE AND USE
N-Ethyldiethanolamine, N-methyldiethanolamine and triethanolamine are Schedule 3 compounds under the Chemical Weapons Convention (CWC). Schedule 3 chemicals include those that have been produced, stockpiled or used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC because they possess such lethal or incapacitating toxicity as well as other properties that might enable it to be used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC by virtue of it’s importance in the production of one or more chemicals listed in Schedules 1 or 2, or it may be produced in large commercial quantities for purposes not prohibited under the CWC. Ethanolamines have a broad spectrum of applications. They are used to produce adhesives, agricultural products, cement grinding aids, concrete additives, detergents, specialty cleaners, personal care products, gas treatments, metalwork, oil well chemicals, packaging and printing inks, photographic chemicals, rubber, textile finishing, urethane coatings, textile lubricants, polishes, pesticides, and pharmaceuticals. Ethanolamines are readily dissolved in water, biodegradable and the bio-concentration potential is low.
This method has been investigated for use with reagent and surface water.
SCOPE
1.1 This procedure covers the determination of diethanolamine, triethanolamine, N-methyldiethanolamine and N-ethyldiethanolamine (referred to collectively as ethanolamines in this test method) in surface 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 method. This method adheres to single reaction monitoring (SRM) mass spectrometry.
1.2 This test method has been developed by US EPA Region 5 Chicago Regional Laboratory (CRL).
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 The Detection Verification Level (DVL) and Reporting Range for the ethanolamines are listed in Table 1.
1.4.1 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 at the DVLs and at higher concentrations for N-methyldiethanolamine.
1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for diethanolamine, triethanolamine, and N-ethyldiethanolamine and Level 2 for N-methyldiethanolamine. The reporting limit for N-methyldiethanolamine is set at 50 μg/L due to poor sensitivity at a 5 μg/L concentration which did not meet the DVL criteria. The DVL for N-methyldiethanolamine is at 10 μg/L, which forces a raised reporting limit (chromatograms are shown in Fig. 1). However, the multi-laboratory validation required a spike of all target analytes at 25 μg/L. The mean recovery for N-methyldiethanolamine at this level was 88 % as shown in Table 3. If your instrument’s sensitivity can meet the requirements in this test method, N-methyldiethanolamine may have a 25 μg/L reporting limit.
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 and health practices and determine the applicability of regulatory limitations prior to use.
TABLE 1 Detection Verification Level and Reporting Range AnalyteDVL (μg/L)Reporting Range (μg/L) Diethanolamine525-500 Triethanolamine525-500 N-Ethyldiethanolamine525-500 N-Methyldiethanolamine1050-500
TABLE 2 Concentrations of Calibration Standards (PPB) Analyte/Surrogate LV 1LV 2LV 3LV 4LV 5LV 6LV 7 Diethanolamine255075150250350500 Triethanolamine255075150250350500 N-Ethyldiethanolamine255075150250350500 N-Methyldiethanolamine255075150250350500 Diethanolamine-D8 (Surrogate)255075150250350500
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Designation:D7599 −09
StandardTest Method for
Determination of Diethanolamine, Triethanolamine,
N-Methyldiethanolamine and N-Ethyldiethanolamine in Water
by Single Reaction Monitoring Liquid Chromatography/
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Tandem Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7599; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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´ NOTE—This Test Method was changed editorially in 2012.
1. Scope required a spike of all target analytes at 25 µg/L. The mean
recoveryfor N-methyldiethanolamineatthislevelwas88%as
1.1 This procedure covers the determination of
shown in Table 3. If your instrument’s sensitivity can meet the
diethanolamine, triethanolamine, N-methyldiethanolamine and
requirementsinthistestmethod, N-methyldiethanolaminemay
N-ethyldiethanolamine (referred to collectively as ethano-
have a 25 µg/L reporting limit.
laminesinthistestmethod)insurfacewaterbydirectinjection
using liquid chromatography (LC) and detected with tandem
1.5 This standard does not purport to address all of the
mass spectrometry (MS/MS). These analytes are qualitatively
safety concerns, if any, associated with its use. It is the
and quantitatively determined by this method. This method
responsibility of the user of this standard to establish appro-
adheres to single reaction monitoring (SRM) mass spectrom-
priate safety and health practices and determine the applica-
etry.
bility of regulatory limitations prior to use.
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
2. Referenced Documents
5 Chicago Regional Laboratory (CRL).
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2.1 ASTM Standards:
1.3 The values stated in SI units are to be regarded as
D1129Terminology Relating to Water
standard. No other units of measurement are included in this
D1193Specification for Reagent Water
standard.
D2777Practice for Determination of Precision and Bias of
1.4 The Detection Verification Level (DVL) and Reporting
Applicable Test Methods of Committee D19 on Water
Range for the ethanolamines are listed in Table 1.
D3856Guide for Management Systems in Laboratories
1.4.1 The DVL is required to be at a concentration at least
Engaged in Analysis of Water
3 times below the Reporting Limit (RL) and have a signal/
D3694Practices for Preparation of Sample Containers and
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
for Preservation of Organic Constituents
ratios at the DVLs and at higher concentrations for
D5847Practice for Writing Quality Control Specifications
N-methyldiethanolamine.
for Standard Test Methods for Water Analysis
1.4.2 The reporting limit is the concentration of the Level 1
E2554Practice for Estimating and Monitoring the Uncer-
calibration standard as shown in Table 2 for diethanolamine,
tainty of Test Results of a Test Method in a Single
triethanolamine, and N-ethyldiethanolamine and Level 2 for
Laboratory Using a Control Sample Program
N-methyldiethanolamine. The reporting limit for
2.2 Other Documents:
N-methyldiethanolamine is set at 50 µg/L due to poor sensi-
EPApublication SW-846Test Methods for Evaluating Solid
tivity at a 5 µg/L concentration which did not meet the DVL
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Waste, Physical/Chemical Methods
criteria. The DVL for N-methyldiethanolamine is at 10 µg/L,
which forces a raised reporting limit (chromatograms are
shown in Fig. 1). However, the multi-laboratory validation
2
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
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This test method is under the jurisdiction ofASTM Committee D19 on Water Standards volume information, refer to the standard’s Document Summary page on
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor the ASTM website.
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Organic Substances in Water. Available from National Technical Information Service (NTIS), U.S. Depart-
CurrenteditionapprovedDec.1,2009.PublishedFebruary2012.DOI:10.1520/ ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
D7599-09E01. www.epa.gov/epawaste/hazard/testmethods/index.htm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D7599−09
TABLE 1 Detection Verification Level and Reporting Range
ing aids, concrete additives, detergents, specialty cleaners,
Analyte DVL (µg/L) Reporting Range personal care products, gas treatments, metalwork, oil well
(µg/L)
chemicals, packaging and printing inks, photographic chemi-
Diethanolamine 5 25-500
cals, rubber, textile finishing, urethane coatings, textile lubri-
Triethanolamine
...
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