Norm

ASTM D7742-11

Standard Practice for Determination of Nonylphenol Polyethoxylates (NPnEO, 3 ≤ n ≤ 18) and Octylphenol Polyethoxylates (OPnEO, 2 ≤ n ≤ n ≤ 12 in Water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spe

61,51

Over deze norm

Status Definitief
Aantal pagina's 12
Commissie D19.06
Gepubliceerd op 15-06-2011
Taal Engels

1.1 This procedure covers the determination of nonylphenol polyethoxylates (NPnEO, 3 n 18) and octylphenol polyethoxylates (OPnEO, 2 n 12) in water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spectrometry (LC/MS/MS) using direct injection liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS) detection. This is a screening Practice with qualified quantitative data to check for the presence of longer chain ethoxylates in a water sample.

1.1.1 All data are qualified because neat standards of each alkylphenol ethoxylate (APEO) are not available and the synthesis and characterization of these neat standards would be very expensive. The Igepal® Brand standards, which contain a mixture of various chain lengths of the alkylphenol ethoxylates (APEOs), were used. The mixture was characterized in-house assuming the instrument response at an optimum electrospray ionization cone and collision voltage for each APEO was the same. This assumption, which may not be accurate, is used to determine qualified amounts of each ethoxylate in the standards. The n-Nonylphenol diethoxylate (n- NP2EO) surrogate was available as a neat characterized standard, therefore, this concentration and recovery data was not estimated. APEOs are not regulated by the EPA, but nonylphenol, a breakdown product of NPnEOs, is regulated for fresh and saltwater dischargers. A request by a sewage treatment plant (STP) was made to make this Practice available through ASTM in order to screen for the influent or effluent from sources of APEOs coming into the STP. The interest lies in stopping the source of the longer chain APEOs from entering the STP in order to meet effluent guidelines. Based upon the above, this is a Practice rather than a Standard Method. A comparison between samples is possible using this Practice to determine which has a higher concentration of APEOs.

1.2 UnitsThe values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

1.3 The estimated screening range shown in Table 1 was calculated from the concentration of the Level 1 and 7 calibration standards shown in Table 4. These numbers are qualified, as explained in Section 1, and must be reported as such. Figs. 1-5 show the SRM chromatograms of each analyte at the Level 1 concentration with the signal to noise (S/N) ratio. This is a screening Practice and method detection limits are not given. The S/N ratio for each analyte at the Level 1 concentration must be at least 5:1 for adequate sensitivity. If the instrument can not meet the criteria, the screening limit must be raised to an acceptable level.

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 and health practices and determine the applicability of regulatory limitations prior to use.

TABLE 1 Estimated Screening Range

AnalyteEstimated Screening
Range (μg/L)
Nonylphenol
triethoxylate (NP3EO)
0.73-11.6
Nonylphenol
tetraethoxylate (NP4EO)
1.1-18.3
Nonylphenol
pentaethoxylate (NP5EO)
1.4-22.1
Nonylphenol
hexaethoxylate (NP6EO)
1.8-28.2
Nonylphenol
heptaethoxylate (NP7EO)
1.9-30.1
Nonylphenol
octaethoxylate (NP8EO)
1.8-29.2
Nonylphenol
nonaethoxylate (NP9EO)
1.6-26.3
Nonylphenol
decaethoxylate (NP10EO)
1.5-24.1
Nonylphenol
undecaethoxylate (NP11EO)
1.3-21.3
Nonylphenol
dodecaethoxylate (NP12EO)
1.0-15.7
Nonylphenol
tridecaethoxylate (NP13EO)
0.64-10.3
Nonylphenol
tetradecaethoxylate (NP14EO)
0.41-6.5
Nonylphenol
pendecaethoxylate (NP15EO)
0.21-3.4
Nonylphenol
hexadecaethoxylate (NP16EO)
0.11-1.7
Nonylphenol
heptadecaethoxylate (NP17EO)
0.05-0.80
Nonylphenol
octodecaethoxylate (NP18EO)
0.023-0.4
Total NPnEO16-250
Octylphenol
diethoxylate (OP2EO)
0.14-2.3
Octylphenol
triethoxylate (OP3EO)
1.4-22.2
Octylphenol
tetraethoxylate (OP4EO)
2.2-35.2
Octylphenol
pentaethoxylate (OP5EO)
2.9-45.8
Octylphenol
hexaethoxylate (OP6EO)
2.6-41.9
Octylphenol
heptaethoxylate (OP7EO)
2.5-40.4
Octylphenol
octaethoxylate (OP8EO)
1.8-28.8
Octylphenol
nonaethoxylate (OP9EO)
1.1-17.6
Octylphenol
decaethoxylate (OP10EO)
0.62-9.9
Octylphenol
undecaethoxylate (OP11EO)
0.26-4.2
Octylphenol
dodecaethoxylate (OP12EO)
0.11-1.8
Total OPnEO16-250
n-Nonylphenol
diethoxylate (n-NP2EO)
15.6-250 (Not Estimated)


FIG. 1 SRM Chromatograms NP3EO-NP8EO


FIG. 2 SRM Chromatograms NP9EO-NP14EO


FIG. 3 SRM Chromatograms NP15EO-NP18EO and n-NP2EO


FIG. 4 SRM Chromatograms OP2EO-OP7EO


FIG. 5 SRM Chromatograms OP8EO-OP12EO

Details

ICS-code 71.100.40
Nederlandse titel Standard Practice for Determination of Nonylphenol Polyethoxylates (NPnEO, 3 ≤ n ≤ 18) and Octylphenol Polyethoxylates (OPnEO, 2 ≤ n ≤ n ≤ 12 in Water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spe
Engelse titel Standard Practice for Determination of Nonylphenol Polyethoxylates (NPnEO, 3 ≤ n ≤ 18) and Octylphenol Polyethoxylates (OPnEO, 2 ≤ n ≤ n ≤ 12 in Water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spe

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