ASTM D7731-17 (2024) 用液相色谱/串联质谱法（LC/MS/MS）测定海水中二丙二醇单丁醚和乙二醇单丁醚的标准试验方法

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Designation: D7731 −17 (Reapproved 2024)
Standard Test Method for
Determination of Dipropylene Glycol Monobutyl Ether and
Ethylene Glycol Monobutyl Ether in Sea Water by Liquid
Chromatography/Tandem Mass Spectrometry (LC/MS/MS)
1
This standard is issued under the ﬁxed designation D7731; 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
1.1 This test method covers the determination of dipropyl-
ene glycol monobutyl ether (DPGBE) and ethylene glycol
monobutyl ether (EGBE) in sea water by direct injection 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 selected reaction monitoring (SRM) mass spectrom-
etry.
1.2 The detection veriﬁcation level (DVL) and reporting
range for DPGBE and EGBE 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 and Fig. 2 display the signal/noise
ratio of the single reaction monitoring (SRM) transition.
1.2.2 The reporting limit is the concentration of the Level 1
calibration standard as shown in Table 4 for DPGBE and
EGBE, taking into account the 20 % sample preparation
dilution factor.
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 appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
D1129 Terminology Relating to Water
D1193 Speciﬁcation for Reagent Water
D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
2.2 Other Standards:
3
EPA Publication SW-846 Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods
3. Terminology
3.1 Deﬁnitions:
3.1.1 For deﬁnitions of terms used in this standard, refer to
Terminology D1129.
3.2 Deﬁnitions of Terms Speciﬁc to This Standard:
3.2.1 detection veriﬁcation level, DVL, n—a concentration
that has a signal/noise ratio greater than 3:1 and is at least 3
times below the reporting limit (RL).
3.2.2 reporting limit, RL, n—the concentration of the
lowest-level calibration standard used for quantiﬁcation.
3.2.2.1 Discussion—In this test method, a 20 mL sample
aliquot is diluted to a 25 mL ﬁnal volume after thoroughly
rinsing the collection vial with acetonitrile for quantitative
transfer. In this case, the lowest calibration level of 100 ppb for
EGBE would allow for a reporting limit of 125 ppb to be
achieved.
3.3 Abbreviations:
3.3.1 mM—millimolar, 1 × 10
–3
moles/L
3.3.2 NA—no addition
3.3.3 ND—non-detect
3.3.4 ppb—parts per billion, µg/L
3.3.5 ppt—parts per trillion, ng/L
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved April 1, 2024. Published May 2024. Originally
approved in 2011. Last previous edition approved in 2017 as D7731 – 17. DOI:
10.1520/D7731-17R24.
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
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
Available from National Technical Information Service (NTIS), 5301 Shawnee
Rd., Alexandria, VA 22312, http://www.ntis.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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.
1

4. Summary of Test Method

4.1 This is a performance-based method, and modiﬁcations

are allowed to improve performance.

4.2 For DPGBE and EGBE analysis, samples are shipped to

the lab between 0 °C and 6 °C and analyzed within 5 days of

collection. The DOW MSDS sheet on DOWANOL*DPNB

glycol ether (DPGBE) (Issue Date: 06/18/2010) lists that the

material is readily biodegradable. The Organisation for Eco-

nomic Co-Operation and Development (OECD) 302B Test lists

96 % biodegradation in 28 days.

4.3 In the lab, the entire collected 20 mL sample is spiked

with surrogate and brought to a volume of 25 mL with

acetonitrile. This prepared sample is then ﬁltered using a

syringe driven ﬁlter unit, and analyzed by LC/MS/MS. If

visible oil is present, the prepared sample is allowed to settle

resulting in an oil layer at the top of the 25 mL solution. A

portion of the aqueous (bottom) layer is ﬁltered, leaving the oil

layer behind, through a syringe driven ﬁlter assembly and

analyzed by LC/MS/MS.

4.4 DPGBE, EGBE, and surrogate are identiﬁed by reten-

tion time and one SRM transition. The target analytes and

surrogate are quantitated using the SRM transitions utilizing an

external calibration. The ﬁnal report issued for each sample

lists the concentration of DPGBE, EGBE, and the surrogate

recovery.

5. Signiﬁcance and Use

5.1 DPGBE and EGBE have a variety of residential and

industrial applications such as cleaning formulations, surface

coatings, inks, and cosmetics. These analytes may be released

into the environment at levels that may be harmful to aquatic

life.

5.2 This test method has been investigated for use with

reagent and sea water.

6. Interferences

6.1 Method interferences may be caused by contaminants in

solvents, reagents, glassware, and other apparatus producing

discrete artifacts or elevated baselines. All of these materials

are demonstrated to be free from interferences by analyzing

laboratory reagent blanks under the same conditions as

samples.

6.2 All glassware is washed in hot water with detergent and

rinsed in hot water followed by distilled water. Detergents

containing DPGBE or EGBE must not be used. The glassware

is then dried and heated in an oven at 250 °C for 15 min to

30 min. All glassware is subsequently cleaned with acetone

followed by methanol.

6.3 All reagents and solvents should be pesticide residue

purity or higher to minimize interference problems.

6.4 Matrix interferences may be caused by contaminants in

the sample. The extent of matrix interferences can vary

considerably from sample source depending on variations of

the sample matrix.

7. Apparatus

7.1 LC/MS/MS System:

7.1.1 Liquid Chromatography System—A complete LC sys-

tem is needed in order to analyze samples.

Any system that is

capable of performing at the ﬂows, pressures, controlled

temperatures, sample volumes, and requirements of the stan-

dard may be used.

7.1.2 Analytical Column—Waters XBridge,

2.1 × 150 mm,

3.5 µm particle size was used to develop this test method. Any

column that achieves baseline resolution of these analytes may

be used. Baseline resolution simpliﬁes data analysis and can

reduce the chance of ion suppression, leading to higher limits

of detection. The retention times and order of elution may

change depending on the column used and need to be moni-

tored.

7.1.3 Tandem Mass Spectrometer System—A MS/MS sys-

tem capable of SRM analysis.

Any system that is capable of

performing at the requirements in this procedure may be used.

7.2 Filtration Device:

7.2.1 Hypodermic Syringe—A lock-tip glass syringe ca-

pable of holding a Millex HV Syringe Driven Filter Unit PVDF

0.22 µm,

7,8

or similar, may be used.

7.2.1.1 A 25 mL lock-tip glass syringe size was used in this

test method.

7.2.2 Filter—Millex HV Syringe Driven Filter Unit PVDF

0.22 µm, or similar, may be used.

8. Reagents and Materials

8.1 Purity of Reagents—High Performance Liquid Chroma-

tography (HPLC) pesticide residue analysis and spectropho-

tometry grade chemicals shall be used in all tests. Unless

indicated otherwise, it is intended that all reagents shall

conform to the Committee on Analytical Reagents of the

American Chemical Society.

Other reagent grades may be

A Waters Alliance High Performance Liquid Chromatography (HPLC) System,

a trademark of the Waters Corporation, Milford, MA, was used to develop this test

method. All parameters in this test method are based on this system and may vary

depending on your instrument.

The Waters XBridge is a trademark of the Waters Corporation, Milford, MA.

A Waters Quattro micro API tandem quadrupole mass spectrometer, a trade-

mark of the Waters Corporation, Milford, MA, was used to develop this test method.

All parameters in this test method are based on this system and may vary depending

on your instrument.

The sole source of supply of the Millex HV Syringe Driven Filter Unit PVDF

0.45 µm known to the committee at this time is Millipore Corporation, Catalog #

SLHV033NS. If you are aware of alternative suppliers, please provide this

information to ASTM International Headquarters. Your comments will receive

careful consideration at a meeting of the responsible technical committee,

which

you may attend.

Millex is a trademark of Merck KGAA, Darmstadt, Germany.

ACS Reagent Chemicals, Speciﬁcations and Procedures for Reagents and

Standard-Grade Reference Materials, American Chemical Society, Washington,

DC. For suggestions on the testing of reagents not listed by the American Chemical

Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,

U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-

copeial Convention, Inc. (USPC), Rockville, MD.

TABLE 1 Detection Veriﬁcation Level (DVL) and Reporting Range

Analyte DVL

(µg/L)

Reporting Range

(µg/L)

DPGBE 0.2 1–10

EGBE 25 125–1250

D7731 − 17 (2024)

FIG. 1 Detection Veriﬁcation Level Signal/Noise Ratio

FIG. 2 Reporting Level (Calibration Standard) Signal/Noise Ratio

D7731 − 17 (2024)

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标签： #液相色谱 #串联质谱法 #LC/MS/MS

摘要：

ASTM D7731-17 2024 Standard Test Method for Determination of Dipropylene Glycol Monobutyl Ether and Ethylene Glycol Monobutyl Ether in Sea Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) 用液相色谱/串联质谱法（LC/MS/MS）测定海水中二丙二醇单丁醚和乙二醇单丁醚的标准试验方法

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ASTM D7731-17 (2024) 用液相色谱/串联质谱法（LC/MS/MS）测定海水中二丙二醇单丁醚和乙二醇单丁醚的标准试验方法

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