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: D8310 − 20
Standard Test Method for
Analysis of Target Phenols (TPs) in Soil by Multiple
Reaction Monitoring Liquid Chromatography/Mass
Spectrometry (LC/MS/MS)1
This standard is issued under the fixed designation D8310; 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 analysis of nonylphenol (NP),
nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxy-
late (NP2EO), octylphenol (OP), and bisphenol A (BPA),
referred to collectively as target phenols (TPs), in soil,
sediments, and biosolids by extraction with acetone, filtration,
dilution with water, and analysis by liquid chromatography/
tandem mass spectrometry. The sample extracts are prepared in
a solution of 75 % acetone and 25 % water because TPs have
an affinity for surfaces and particles that is more pronounced at
lower concentrations. The range of applicability of the test
method is shown in Table 1. The method may be extended
outside of these ranges depending on additional performance
studies not undertaken here.
1.2 Units—The values stated in SI units are to be regarded
as the standard. No other units of measurement are included in
this standard.
1.3 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.
1.4 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
D1193 Specification for Reagent Water
1
This test method is under the jurisdiction of ASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.06 on
Analytical Methods.
Current edition approved Feb. 1, 2020. Published February 2020. DOI: 10.1520/
D8310-20.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7858 Test Method for Determination of Bisphenol A in
Soil, Sludge, and Biosolids by Pressurized Fluid Extrac-
tion and Analyzed by Liquid Chromatography/Tandem
Mass Spectrometry
2.2 Federal Standards:3
29 CFR Part 1910 Occupational Safety and Health Standards
40 CFR Part 136, Appendix B Definition and Procedure for
the Determination of the Method Detection Limit—
Revision 1.11
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 batch quality control, n—all the quality control (QC)
samples and standards included in an analytical procedure.
3.1.2 bisphenol A, BPA—defined in Test Method D7858.
3.1.3 bisphenol A (propane-D6), BPA-D6—defined in Test
Method D7858.
3.1.4 2-bromo-4-(1,1,3,3-tetramethylbutyl)phenol, Br-OP,
n—used in this test method as a surrogate.
3.1.4.1 Discussion—2-bromo-4-(1,1,3,3-tetramethylbutyl)
phenol is not produced commercially and is not expected to be
found in the environment. It was reported that compounds in
highly chlorinated, bromide-rich wastewaters could potentially
interfere with the Br-OP surrogate. If this interference is
encountered, n-nonylphenol is suggested as an alternative
surrogate.
3.1.5 nonylphenol, NP, n—mixture of branched
p-nonylphenol isomers.
3.1.5.1 Discussion—Commercial NP is produced by the
reaction of phenol with commercial nonene. Commercial
nonene is not simply a linear C9H18 alpha olefin; it is a
complex mixture of predominantly nine-carbon olefins, called
propylene trimer, containing no linear isomers. This synthesis
results in a mixture of various branched nonylphenol isomers
rather than a discrete chemical structure. The branched nonyl
group is positioned predominantly in the para position on the
phenol ring.
3
Available from U.S. Government Printing Office, Superintendent of
Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
www.access.gpo.gov.
 D8310 − 20
TABLE 1 Tested Method Parameters of the Standard 3.2.19 MSP—method specific parameter
ESI MDL Reporting 3.2.20 NA—not available
Analyte
Mode (µg/kg)A Range (µg/kg)
Bisphenol A Negative 15.5 100–2500 3.2.21 NP1EO—nonylphenol monoethoxylate
Octylphenol Negative 44.2 200–5000
Nonylphenol Negative 30.4 100–2500 3.2.22 NP2EO—nonylphenol diethoxylate
Nonylphenol Monoethoxylate Positive 931.2 3000–45 000
Nonylphenol Diethoxylate Positive 7.4 100–2500
3.2.23 OP—octylphenol
A
MDL is calculated based upon nine spiked samples. 3.2.24 P&A—precision and accuracy
3.2.25 PPB—parts per billion
3.2.26 PPM—parts per million
3.1.6 nonylphenol diethoxylate, NP2EO, n—branched non- 3.2.27 PPT—parts per trillion
ylphenol diethoxylate. 3.2.28 PTFE—polytetrafluoroethylene
3.1.7 nonylphenol monoethoxylate, NP1EO, n—branched 3.2.29 PVDF—poly-vinylidene dichloride
nonylphenol monoethoxylate. 3.2.30 QA—quality assurance
3.1.8 normal nonylphenol, n-NP, n—normal straight chain 3.2.31 QC—quality control
nonylphenol. 3.2.32 QMP—quality management plan
3.1.8.1 Discussion—n-NP is used in this test method as a
surrogate. It is not produced commercially and is not expected 3.2.33 REC—percent recovery
to be found in the environment. 3.2.34 RL—reporting limit
3.1.9 normal nonylphenol diethoxylate, n-NP2EO, 3.2.35 RLCS—reporting limit check sample
n—normal straight chain nonylphenol diethoxylate. 3.2.36 RSD—relative standard deviation
3.1.9.1 Discussion—n-NP2EO is used in this test method as 3.2.37 RT—retention time
a surrogate. It is not produced commercially and is not
expected to be found in the environment. 3.2.38 RTS—retention time shift
3.1.10 octylphenol, OP, n—produced by the reaction of 3.2.39 SOP—standard operating procedure
phenol and diisobutylene to produce predominantly the 4-(1, 3.2.40 SRM—single reaction monitoring
1,3,3-tetramethylbutyl)phenol isomer. 3.2.41 SS—surrogate standard
3.1.11 reporting limit check sample, RLCS, n—this sample 3.2.42 TC—target compound
verifies that if the analyte was present at the reporting limit, it
3.2.43 TCL—target compound limit
would be confidently identified.
3.2.44 TP—target phenols
3.1.12 target phenols, TPs, n—in this test method, NP,
NP1EO, NP2EO, OP, and BPA, collectively. 3.2.45 UPLC—ultra performance liquid chromatography
3.2 Abbreviations: 3.2.46 VOA—volatile organic analysis
3.2.1 ADOC—analyst demonstration of capability
4. Summary of Test Method
3.2.2 BPA—bisphenol A
4.1 A sample (~2 g) is transferred to a VOA vial and spiked
3.2.3 Br-OP—2-bromo-4-(1,1,3,3-tetramethylbutyl)phenol
with surrogates (all samples) and TPs (laboratory control and
3.2.4 CAS—chemical abstract service matrix spike samples) and then extracted with 7.5 mL of
3.2.5 CCC—continuing calibration check acetone by tumbling on a rotator for 2 h. Any device may be
3.2.6 DL—detection limit used that mixes the sample; a rotator device was chosen in this
case because it inverts the sample, allowing the soil to be in a
3.2.7 EPA—U.S. Environmental Protection Agency
constant fluid motion and not clumped. The samples are
3.2.8 IC—initial calibration centrifuged at 1900 rpm for 10 min and then filtered through an
3.2.9 IDOC—initial demonstration of capability Acrodisc GxF/0.2 µm PVDF membrane syringe-driven filter
3.2.10 LC—liquid chromatography unit. Of Specification D1193 Type 1 water, 2.5 mL is added to
the filtered extract and then analyzed by LC/MS/MS. All
3.2.11 LCS—laboratory control sample
concentrations reported, only to the RL, using this method are
3.2.12 LCSD—laboratory control sample duplicate based upon a dry-weight basis.
3.2.13 LIMS—relational laboratory information manage- 4.2 The TCs are identified by comparing the SRM transition
ment system and RT. BPA has a confirmatory SRM transition also. The
3.2.14 MDL—method detection limit confirmatory SRM transition will be correlated to the known
3.2.15 MI—matrix interference standard SRM transition for identification of BPA (Table 2).
The RT for the analyte of interest shall also agree with the RT
3.2.16 MRM—multiple reaction monitoring
of the mid-level standard by 65 %. The TC is quantitated using
3.2.17 MS—mass spectrometry the SRM transition of the TC using external calibration. As an
3.2.18 MS/MSD—matrix spike/matrix spike duplicate additional QC measure, non-labeled surrogates (listed in 8.2)

2
 D8310 − 20
TABLE 2 Variable Mass Spectrometer Parameters
Retention Time, SRM Mass Transition Cone Voltage, Collision Energy,
Analyte ESI Mode
min (Parent > Product) V eV
BPA negative 5.58 227.1 > 211.9 40 18
BPA confirmatoryA negative 5.58 227.1 > 132.7 40 25
OP negative 8.53 205.1 > 132.7 40 24
NP negative 9.70 219.3 > 133.1 40 28
NP1EO positive 9.71 282.3 > 126.9 20 9
NP2EO positive 9.65 326.3 > 182.9 25 11
BPA-D6 (surrogate) negative 5.57 233.3 > 214.9 40 19
BPA-D6 confirmatoryA (surrogate) negative 5.57 233.3 > 137.8 40 25
Br-OP (surrogate) negative 9.56 283.1 > 78.6 40 25
n-NP (surrogate) negative 10.71 219.3 > 105.6 40 20
n-NP2EO (surrogate) positive 10.69 326.4 > 88.8 25 15
A
Confirmatory transitions are optional but should be included for added qualitative information.

recoveries are monitored; the percent recovery of each should
fall within the control limits of the method. The final report
issued for each sample lists concentration of TPs and
surrogates, if detected, or non-detect at the RL if not detected,
in microgram/kilogram on a dry-weight basis.
5. Significance and Use
5.1 This test method developed for the analysis of TPs in
soil and sediment samples is based upon an LC/MS/MS
analysis. Any type of coupled liquid chromatography/mass
spectrometry system may be used that meets the study objec-
tives of the individual project. These may include, but are not
limited to: trap, single quadrupoles, time-of-flight, high
resolution, and others not mentioned here.
5.2 The MDL and reporting range for TPs are listed in Table
1. This SOP has been tested on Ottawa sand, four ASTM soil
types, biosolid sample, and one commercial soil. The P&A QC
acceptance criteria are listed in Table 3. Tables 4-17 display the
TC and surrogate recoveries in the various soil types. 40 CFR
Part 136, Appendix B was used as a guide to determine the
MDLs. The 40 CFR Part 136 MDL criteria were not met for
NP2EO; this does not affect the method because the SOP only
reports to the RL and is not a regulatory method. All site
sample results are not reported below the RL using this
method. RLCS concentrations may be reported below the RL
because they are spiked at or near the RL.
5.3 The RL for a specific soil sample may differ from that
listed depending on the nature of the interferences in the
sample matrix. Variability in historical LCS spike recovery
may be used to estimate uncertainty. The estimate of minimum
laboratory contribution to measurement uncertainty of this test
method for each analyte is listed in Table 3. These values are
derived from P&A samples from the initial IDOC study for this
test method. The uncertainty will be greater near the RL and
much greater near the DL. Also, uncertainty estimated based on
variability in LCS recovery is conservative because some
sources of variability are not included, such as subsample
variability and matrix analyte recovery. This SOP covers
multiple soil matrices and the uncertainty among the various
matrices is variable.
6. Interferences
6.1 Method interferences may be caused by contaminants in
solvents, reagents, glassware, LC vials/caps, disposable
pipettes, and other apparatus that lead to discrete artifacts or
elevated baselines in the selected ion current profiles. The
presence and magnitude of method interferences are deter-
mined by analysis of solvent and laboratory blanks.
6.2 Matrix interferences may be caused by contaminants
from the sample, sampling devices, or storage containers. The
extent of matrix interferences will vary considerably from
sample source to sample source depending on variations of the
sample matrix. The analysis of matrix spikes is critical for
determining the impact of matrix interferences.
6.3 Warnings:
6.3.1 All reagents and solvents should be of pesticide
residue purity or higher to minimize interference problems,
preferably LC/MS grade.
6.3.2 Contaminants have been found in improperly cleaned
glassware and glass syringes. TPs stick to surfaces if the

TABLE 3 QC Acceptance Criteria and UncertaintyA

Standard Deviation
Average Recovery, Number of Lower Control Limit Upper Control Limit Uncertainty (95 %
Parameter of Percentage
% Replicates, n (LCL), % (UCL), % Confidence Interval)
Recovery
BPA 92.6 4.5 6 70 130 4.7
OP 88.4 6.5 6 60 130 6.9
NP 92.9 3.4 6 70 130 3.6
NP1EO 98.4 7.0 6 70 130 7.3
NP2EO 96.1 4.5 6 70 130 4.7
BPA-D6 (surrogate) 91.1 3.2 8 70 130 2.7
Br-OP (surrogate) 87.9 4.7 8 70 130 3.9
n-NP (surrogate) 87.4 2.6 8 70 130 2.2
n-NP2EO (surrogate) 93.6 6.1 8 70 130 5.1
A
Uncertainty calculation based upon 95 % confidence interval and a two-tailed Student t distribution.
Uncertainty = Student t Value [(standard deviation) / (number of LCS)½].

3
 D8310 − 20
TABLE 4 P&A Study for TPs in Ottawa Sand (Target Spike Recoveries)
P&A Data (625 µg/kg spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and 18 750 µg/kg for NP1EO)
Sample
BPA OP NP NP1EO NP2EO
MB1 <RL <RL <RL <RL <RL
MB2 <RL <RL <RL <RL <RL
P&A1 555.0 1020.0 1120.0 18 500.0 1150.0
P&A2 597.0 1070.0 1190.0 18 600.0 1160.0
P&A3 554.0 1160.0 1110.0 17 400.0 1160.0
P&A4 567.0 1010.0 1150.0 16 600.0 1200.0
P&A5 626.0 1180.0 1220.0 19 400.0 1280.0
P&A6 572.0 1190.0 1180.0 20 200.0 1260.0
Average Recovery, µg/kg 578.5 1105.0 1161.7 18 450.0 1201.7
% Average Recovery 92.6 88.4 92.9 98.4 96.1
Standard Deviation 28.0 81.7 42.6 1305.0 56.0
RSD, % 4.8 7.4 3.7 7.1 4.7

TABLE 5 P&A Study for TPs in Ottawa Sand (Surrogate Recoveries)

P&A Data (625 µg/kg Spike)
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 548 500 557 539
MB2 590 518 555 552
P&A1 538 567 569 564
P&A2 569 567 547 582
P&A3 579 556 515 566
P&A4 556 533 536 597
P&A5 583 581 553 637
P&A6 592 574 540 643
Average Recovery, µg/kg 569.4 549.5 546.5 585.0
% Average Recovery 91.1 87.9 87.4 93.6
Standard Deviation 20.1 29.2 16.4 38.2
RSD, % 3.5 5.3 3.0 6.5

TABLE 6 P&A Study in ASTM CL-1 Soil (Target Compound Recoveries)

P&A for ASTM CL-1 Soil (Lean Clay, Red Bucket) (625 µg/kg Spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and
Sample 18 750 µg/kg for NP1EO)
BPA OP NP NP1EO NP2EO
MB1 <RL <RL <RL <RL <RL
MB2 <RL <RL <RL <RL <RL
P&A1 553.0 1173.7 1231.1 17 936.0 1239.4
P&A2 586.3 1259.1 1300.3 19 901.6 1271.3
P&A3 564.7 1209.6 1188.7 18 313.8 1225.9
P&A4 587.3 1224.9 1226.7 17 870.8 1233.9
P&A5 609.7 1201.5 1239.1 17 757.6 1254.0
P&A6 553.6 1119.0 1179.7 18 965.0 1195.1
Mean Recovery (µg/kg dry weight) 575.8 1198.0 1227.6 18 457.5 1236.6
% Mean Recovery 92.1 95.8 98.2 98.4 98.9
Standard Deviation 22.5 47.8 43.0 833.0 25.9
RSD, % 3.9 4.0 3.5 4.5 2.1

TABLE 7 Surrogate Recoveries for P&A Study in ASTM CL-1 Soil

ASTM CL-1 Soil (Lean Clay, Red Bucket), 625 µg/kg Spike
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 627.5 571.5 602.3 603.2
MB2 599.6 535.9 618.2 592.2
P&A1 549.4 594.1 595.1 637.6
P&A2 628.8 608.5 579.3 669.0
P&A3 600.6 579.6 557.8 633.0
P&A4 605.5 597.4 569.7 645.5
P&A5 601.3 602.6 636.9 660.3
P&A6 589.8 601.7 589.8 622.5
Mean Recovery (µg/kg dry weight) 595.9 597.3 588.1 644.6
% Mean Recovery 95.3 95.6 94.1 103.1
Standard Deviation 26.2 10.0 27.4 17.4
RSD, % 4.4 1.7 4.7 2.7

glassware is not properly cleaned and rinsed with solvent, such trations affecting the analysis may be found. All of these
as acetone, 2-propanol, and acetonitrile, and low µg/L concen-

4
 D8310 − 20
TABLE 8 P&A Study in ASTM CH-1 Soil (Target Compound Recoveries)
P&A Data for ASTM CH-1 Soil (Fat Clay, White Bucket) (625 µg/kg Spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and
Sample 18 750 µg/kg for NP1EO)
BPA OP NP NP1EO NP2EO
MB1 <RL <RL <RL <RL <RL
MB2 <RL <RL <RL <RL <RL
P&A1 622.3 1245.6 1220.7 19 408.3 1272.0
P&A2 639.1 1173.9 1192.9 19 910.7 1267.6
P&A3 666.6 1236.3 1260.1 20 325.8 1301.7
P&A4 604.4 1178.0 1200.8 19 328.7 1232.3
P&A5 644.1 1164.7 1327.7 19 230.7 1325.0
P&A6 664.5 1338.0 1268.8 19 386.1 1350.5
Mean Recovery (µg/kg dry weight) 640.2 1222.7 1245.1 19 598.4 1291.5
% Mean Recovery 102.4 97.8 99.6 104.5 103.3
Standard Deviation 24.1 65.9 50.8 428.0 42.8
RSD, % 3.8 5.4 4.1 2.2 3.3

TABLE 9 Surrogate Recoveries for P&A Study in ASTM CH-1 Soil

ASTM CH-1 Soil (Fat Clay, White Bucket), 625 µg/kg Spike
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 645.2 537.0 603.7 571.1
MB2 635.6 572.0 645.5 591.9
P&A1 634.1 602.6 553.9 660.0
P&A2 609.7 593.7 569.1 644.4
P&A3 632.4 650.5 628.1 686.3
P&A4 623.4 590.2 577.3 631.9
P&A5 661.0 645.6 659.3 660.9
P&A6 672.2 649.6 686.4 702.2
Mean Recovery (µg/kg dry weight) 638.8 622.0 612.3 664.3
% Mean Recovery 102.2 99.5 98.0 106.3
Standard Deviation 23.5 29.4 53.8 26.0
RSD, % 3.7 4.7 8.8 3.9

TABLE 10 P&A Study in ASTM SP-1 Soil (Target Compound Recoveries)

P&A Data (625 µg/kg Spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and 18 750 µg/kg for NP1EO)
Sample
BPA OP NP NP1EO NP2EO
MB1 <RL <RL <RL <RL <RL
MB2 <RL <RL <RL <RL <RL
P&A1 611.5 1231.4 1205.7 17 023.3 1205.9
P&A2 631.0 1234.1 1252.3 18 426.6 1229.1
P&A3 574.3 1067.6 1140.7 17 788.8 1153.3
P&A4 626.9 1262.1 1211.8 18 010.4 1232.4
P&A5 586.7 1213.2 1200.2 17 549.9 1230.1
P&A6 578.4 1230.4 1184.4 16 480.0 1113.1
Mean Recovery (µg/kg dry weight) 601.5 1206.5 1199.2 17 546.5 1194.0
% Mean Recovery 96.2 96.5 95.9 93.6 95.5
Standard Deviation 24.9 69.8 36.5 701.4 49.7
RSD, % 4.1 5.8 3.0 4.0 4.2

TABLE 11 Surrogate Recoveries for P&A Study in ASTM SP-1 Soil

ASTM SP-1 Soil (Sand, Yellow Bucket), 625 µg/kg Spike
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 568.1 518.1 605.1 533.2
MB2 610.1 548.3 545.4 553.0
P&A1 629.8 589.7 567.6 622.4
P&A2 608.8 588.7 596.6 601.7
P&A3 543.8 534.5 513.0 594.4
P&A4 576.1 589.2 593.4 601.3
P&A5 559.4 616.7 590.1 629.7
P&A6 552.5 532.5 548.5 551.9
Mean Recovery (µg/kg dry weight) 578.4 575.2 568.2 600.2
% Mean Recovery 92.5 92.0 90.9 96.0
Standard Deviation 34.1 34.0 32.7 27.3
RSD, % 5.9 5.9 5.8 4.6

materials are routinely demonstrated to be free from interfer- conditions as the samples. If found, measures should be taken
ences by analyzing laboratory reagent blanks under the same to remove the contamination or data should be qualified.

5
 D8310 − 20
TABLE 12 P&A Study in ASTM ML-1 Soil (Target Compound Recoveries)
P&A Data for ASTM ML-1 Soil (Silt, Green Bucket) (625 µg/kg Spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and
Sample 18 750 µg/kg for NP1EO)
BPA OP NP NP1EO NP2EO
MB1 <RL <RL <RL <RL <RL
MB2 <RL <RL <RL <RL <RL
P&A1 559.5 1117.4 1076.1 16 702.3 1124.2
P&A2 547.9 1179.6 1091.9 17 457.8 1106.4
P&A3 573.0 1148.2 1146.7 17 540.1 1152.7
P&A4 550.3 1193.2 1108.3 16 291.8 1111.0
P&A5 549.0 1151.9 1121.4 16 871.6 1131.9
P&A6 568.6 1121.2 1102.0 16 855.4 1139.1
Mean Recovery (µg/kg dry weight) 558.0 1151.9 1107.7 16 953.2 1127.6
% Mean Recovery 89.3 92.2 88.6 90.4 90.2
Standard Deviation 10.8 30.4 24.4 472.4 17.4
RSD, % 1.9 2.6 2.2 2.8 1.5

TABLE 13 Surrogate Recoveries for P&A Study in ASTM ML-1 Soil

ASTM ML-1 Soil (Silt, Green Bucket), 625 µg/kg Spike
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 555.6 479.8 513.4 522.6
MB2 504.3 499.8 492.9 525.8
P&A1 530.0 522.7 512.2 571.7
P&A2 518.3 538.0 516.1 563.2
P&A3 553.1 551.1 512.9 580.9
P&A4 527.9 519.3 532.0 548.6
P&A5 527.2 537.0 554.7 551.0
P&A6 551.5 522.6 524.5 588.0
Mean Recovery (µg/kg dry weight) 534.7 531.8 525.4 567.2
% Mean Recovery 85.5 85.1 84.1 90.8
Standard Deviation 14.2 12.4 16.2 15.9
RSD, % 2.7 2.3 3.1 2.8

TABLE 14 P&A Study in Fairfield Biosolid Samples (Target Compound Recoveries)

P&A Data for Fairfield Biosolid Samples (625 µg/kg Spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and 18 750 µg/kg
Sample for NP1EO)
BPA OPA NPA NP1EO NP2EO
MB1 <RL 388.9 10 677.6 <RL <RL
MB2 <RL 224.7 6843.1 <RL <RL
P&A1 457.7 821.8 1727.7 13 795.6 931.3
P&A2 514.1 889.4 1329.6 15 307.5 996.4
P&A3 496.8 1002.2 2243.0 15 135.0 1007.5
P&A4 496.0 1007.7 2148.3 15 158.7 1005.0
P&A5 471.7 1114.0 6930.9 14 673.7 982.7
P&A6 456.5 1018.1 3984.5 14 310.2 966.2
Mean Recovery (µg/kg dry weight) 482.1 975.5 3060.7 14 730.1 981.5
% Mean Recovery 77.1 78.0 244.9 78.6 78.5
Standard Deviation 23.6 103.7 2102.7 588.8 29.0
RSD, % 4.9 10.6 68.7 4.0 3.0
A
P&A values are after subtraction of average of MB if $RL.

6.3.3 Glass syringes are used with this test method. A
thoroughly cleaned 10 or 20-mL hypodermic glass syringe
with a PVDF filter unit is used to filter samples and has been
shown to perform well.
6.3.4 Nonylphenol was found in polypropylene. The filter
units shall be rinsed with at least 10 mL of acetonitrile and
10 mL of methanol before use to remove nonylphenol.
6.3.5 The procedure described in 7.3.8 should be followed
to make glassware free from interferences. Alkylphenol deter-
gents shall not be used. Detergent may contain TPs, precursor,
or breakdown products and these shall be avoided.
7. Apparatus
7.1 Equipment:
7.1.1 Liquid Chromatograph (LC) System—An ultra-
performance LC (UPLC) with flow-through needle design.
7.1.2 Analytical Column—An analytical column that will
achieve adequate results that meet or exceed this test method.4
7.1.3 Mass Spectrometer (MS) System—A triple quadrupole
mass spectrometer is used. A mass spectrometer capable of
MRM analysis with fast enough cycle time to obtain at least ten
scans over a peak is needed with adequate sensitivity.
7.1.4 Data Backup Device—A data archival unit to archive
data.
4
A Waters Acquity UPLC® BEH C18, 2.1 × 100 mm and 1.7 µm particle size
was used to develop this test method. Any column may be used that meets or
exceeds the performance of this test method.

6
 D8310 − 20
TABLE 15 Surrogate Recoveries for P&A Study in Fairfield Biosolid Samples
Fairfield Biosolid Samples, 625 µg/kg Spike
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 447.1 387.8 176.8 431.0
MB2 466.9 417.6 214.5 449.7
P&A1 413.3 391.4 179.6 450.8
P&A2 432.4 420.8 190.2 486.9
P&A3 456.1 419.7 177.0 496.5
P&A4 460.1 449.1 195.1 507.0
P&A5 433.6 408.5 151.4 468.0
P&A6 436.2 425.1 165.8 492.2
Mean Recovery (µg/kg dry weight) 438.6 419.1 176.5 483.5
% Mean Recovery 70.2 67.1 28.2 77.4
Standard Deviation 17.2 19.1 16.1 20.6
RSD, % 3.9 4.6 9.1 4.3

TABLE 16 P&A Study in Commercial Soil (Milorganite)

P&A Data for Milorganite (625 µg/kg Spike for BPA; 1250 µg/kg for OP, NP, and NP2EO; and 18 750 µg ⁄kg for NP1EO)
Sample
BPAA OPA NPA NP1EOA NP2EOA
MB1 109.7 194.2 3460.9 7875.8 4971.7
MB2 89.3 196.5 3512.1 7637.2 4587.9
P&A1 454.9 801.7 729.7 17 038.9 1832.0
P&A2 432.1 783.8 590.0 15 539.7 1452.2
P&A3 422.7 785.6 555.3 15 936.5 1453.7
P&A4 428.5 836.5 713.5 15 928.4 1550.2
P&A5 402.9 790.4 569.2 16 070.2 1306.2
P&A6 433.1 843.0 756.4 16 216.7 1669.0
Mean Recovery (µg/kg dry weight) 429.0 806.8 652.3 16 121.7 1543.9
% Mean Recovery 68.6 64.5 52.2 86.0 123.5
Standard Deviation 16.9 26.3 90.3 502.6 185.3
RSD, % 3.9 3.3 13.8 3.1 12.0
A
P&A values are after subtraction of average of MB if $RL.

TABLE 17 Surrogate Recoveries for Precision and Accuracy Study in Commercial Soil (Milorganite)
Milorganite, 625 µg/kg Spike
Sample
BPA-D6 Br-OP n-NP n-NP2EO
MB1 402.2 324.1 <RLA 508.3
MB2 425.1 335.5 <RL 512.7
P&A1 431.0 341.7 <RL 557.7
P&A2 363.5 325.9 <RL 548.5
P&A3 405.8 330.3 <RL 550.4
P&A4 354.4 312.1 <RL 545.0
P&A5 371.3 309.4 <RL 550.1
P&A6 404.9 329.1 <RL 564.9
Mean Recovery (µg/kg dry weight) 388.5 324.8 No recovery 552.8
% Mean Recovery 62.2 52.0 NA 88.4
Standard Deviation 29.8 12.1 NA 7.2
RSD, % 7.7 3.7 NA 1.3
A
<RL = below reporting limit.

7.1.5 Data System—Software shall be interfaced to the
LC/MS/MS that allows the continuous acquisition and storage
on machine-readable media of all mass spectra obtained
throughout the duration of the chromatographic program.
Software is used for all data quantitation.
7.2 Calibrated Support Equipment:
7.2.1 Graduated Syringes—Use 10, 25, 50, 100, 250, 500,
and 1000-µL graduated syringes.
7.2.2 Analytical Balance (Certified Annually)—Use an ana-
lytical balance accurate to 60.1 % of sample mass with Class
3 or 4 weights to verify calibration.
7.3 Glassware and Miscellaneous Supplies:
7.3.1 Vials—Use 2-mL autosampler vials with pre-slit
PTFE/silicone septa or equivalent.
7.3.2 Gases—Ultra-pure argon and nitrogen.
7.3.3 Class A volumetric glassware.
7.3.4 VOA Vials—20, 40, or 60 mL.
7.3.5 GxF/0.2 µm PVDF Membrane Syringe-Driven Filter
Unit—The filters are washed with 10 mL acetonitrile followed
by 10 mL methanol before use.
7.3.6 Syringe—Use 10 to 25-mL filter-adaptable glass sy-
ringe with luer lock.
7.3.7 Disposable glass pipettes. (Warning—Syringes shall
be cleaned with copious amounts of warm tap water, distilled
water, and thoroughly rinsed with acetonitrile and methanol
between uses.)
7.3.8 Glassware Cleaning Instructions—All glassware is
washed in hot water (above 50 °C) with detergent, rinsed in hot
water, and rinsed with distilled water. The glassware is then
dried in an oven for up to 1 h (except volumetric glassware,

7
 D8310 − 20
which is air dried). All glassware is subsequently rinsed with
an organic solvent such as acetone, methanol, and acetonitrile.
(Warning—Detergents containing alkylphenolic compounds
shall not be used.)
8. Reagents and Materials
8.1 Purity of Reagents—Reagent-grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society, where
such specifications are available.5 Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
the determination.
8.2 Solvents and Reagents:
8.2.1 Acetonitrile.
8.2.2 Water—HPLC mass spectrometry pesticide quality.
8.2.2.1 Purity of Water—Unless otherwise indicated, refer-
ences to water shall be understood to mean reagent water as
defined by Type I of Specification D1193.
8.2.3 Methanol.
8.2.4 Isopropyl alcohol.
8.2.5 Ammonium acetate.
8.2.6 Acetone.
8.2.7 Nonylphenol monoethoxylate.
8.2.8 Nonylphenol diethoxylate.
8.2.9 Nonylphenol.
8.2.10 Octylphenol.
8.2.11 n-Nonylphenol diethoxylate.
8.2.12 n-Nonylphenol.
8.2.13 2-bromo-4-(1,1,3,3-tetramethylbutyl)phenol.
8.2.14 Bisphenol A.
8.2.15 Bisphenol A (propane-D6).
8.3 Reagents and Standard Preparation:
8.3.1 All calibration standard preparations shall be re-
corded. All calibration solutions are prepared with acetone:wa-
ter (75:25) unless otherwise stated. The concentrated stock
standard concentration can vary when preparing from neat
material, usually between 50 to 100 mg/L of each TP in
methanol.
8.3.2 Expiration time of a prepared standard is six months
from the time prepared. The standards can be used for more
than six months if they fall within 630 % from the calibration
standard that is less than six months old. Presently, there is no
holding time study for this standard and the six months is an
estimate with no laboratory data supporting this time period.
8.3.3 Label all standards and verify the correct grade of
solvents were used. Traceability of standards is established
using the manufacturer’s specifications provided at the time of
purchase.
8.3.4 The specific instructions for the preparation of stock
standards, spiking solutions, and QC batch are listed in 8.3.4.1
5
Reagent Chemicals, American Chemical Society Specifications, 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. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
8
– 8.3.4.4. The calibration levels (prepared from the high-level
calibration stock), laboratory control samples, matrix spike
samples, and duplicates are made for each batch of samples.
They are usually prepared and analyzed immediately. A CCC
standard is also prepared for each batch of samples.
8.3.4.1 TP Surrogate Spiking Solution—A surrogate stan-
dard solution containing Br-OP, n-NP, BPA-D6, and n-NP2EO
is added to each 2-g soil sample. Br-OP and n-NP are used as
the surrogates for NP and OP, BPA-D6 is used as a surrogate for
BPA, and n-NP2EO is used as a surrogate for NP1EO and
NP2EO. A stock surrogate spiking solution is prepared in
methanol at 12.5 mg/L for Br-OP, n-NP, BPA-D6, and
n-NP2EO. The surrogates are added to each sample to achieve
a concentration of 625 µg/L (that is, 100 µL of a 12.5-mg/L
methanol solution containing Br-OP, n-NP, BPA-D6, and
n-NP2EO is added to a 2-g soil sample).
8.3.4.2 MS/MSD and LCS/LCSD Spiking Solution (Target
Spike Solution)—Each ~2-g sample, approximately 2 g and
weighed to the hundredths, MS/MSD or LCS/LCSD sample is
spiked with TPs containing BPA at 12.5 mg/L, NP, OP and
NP2EO at 25 mg/L, and NP1EO at 375 mg/L to achieve a
concentration of 1250 µg/L for OP, NP, and NP2EO, 625 µg/L
for BPA, and 18 750 µg/L for NP1EO (that is, 100 µL of a
methanol solution containing BPA at 12.5 mg/L, NP, OP, and
NP2EO at 25 mg/L and NP1EO at 375 mg/L is added to a 2-g
soil sample).
8.3.4.3 RL Check Spiking Solution—The RLCS is prepared
by spiking the RLCS with the RL check standard near RL. A
50-µL volume of a methanolic RL check standard containing
BPA at 2 mg/L; NP, OP, and NP2EO at 4 mg/L; and NP1EO at
60 mg/L is added to RLCS to achieve a concentration of 50
µg/L for BPA; 100 µg/L for OP, NP, and NP2EO; and 1500
µg/L for NP1EO.
8.3.4.4 Calibration Standards—Calibration stock standard
Solution A is prepared from target spiking solutions containing
BPA at 12.5 mg/L; NP, OP, and NP2EO at 25 mg/L; and
NP1EO at 375 mg/L and surrogate spiking solutions containing
Br-OP, n-NP, BPA-D6; and n-NP2EO at 12.5 mg/L. Add 1000
µL of the target spike solution and surrogate spiking solution to
a 25-mL volumetric flask and diluted to 25 mL volume with
75:25 (acetone:water) (Solution B). Stock standard Solution A
(Level 8, Tables 18 and 19) containing BPA and each surrogate
at 500 µg ⁄L; OP, NP, and NP2EO at 1000 µg/L; and NP1EO at
15 000 µg ⁄L is diluted to prepare Levels 1 through 7 as shown
in Tables 18 and 19. All calibration standards should contain
75:25 acetone to water in 2-mL LC vials. The CCC is a
mid-level calibration standard.
9. Hazards
9.1 Users of this test method should operate a formal safety
program.
9.2 Warnings—Health Hazards—The toxicity and carcino-
genicity of each reagent used in this test method have not been
precisely defined; however, each chemical compound is treated
as a health hazard. From this viewpoint, exposure to these
chemicals should be reduced to the lowest possible level and
appropriate PPE used. Review SDSs for specific physical and
health and hazards, including appropriate PPE to be used.
 D8310 − 20
TABLE 18 Concentrations of Calibration Standards, µg/L
Analyte/Surrogate LV 1 LV 2 LV 3 LV 4 LV 5 LV 6 LV 7 LV 8
BPAA 10 20 50 100 200 300 400 500
OPA 20 40 100 200 400 600 800 1000
NP 20 40 100 200 400 600 800 1000
NP1EOA 300 600 1500 3000 6000 9000 12 000 15 000
NP2EO 20 40 100 200 400 600 800 1000
BPA-D6 (surrogate) 10 20 50 100 200 300 400 500
Br-OP (surrogate) 10 20 50 100 200 300 400 500
n-NP (surrogate) 10 20 50 100 200 300 400 500
n-NP2EO (surrogate) 10 20 50 100 200 300 400 500
A
RL is set at Level 2 concentration; all others at Level 1 because of MDL determination. The Level 1 concentration did display adequate sensitivity for all analytes
(signal/noise ratio > 5).

TABLE 19 Preparation of Calibration Standards

SolutionA LV 1 LV 2 LV 3 LV 4 LV 5 LV 6 LV 7 LV 8
A 20 µL 40 µL 100 µL 200 µL 400 µL 600 µL 800 µL 1000 µL
B 980 µL 960 µL 900 µL 800 µL 600 µL 400 µL 200 µL 0
A
Solution A—Level 8 stock solution prepared according to Section 8 and at Table 18 concentrations.
Solution B—75 % acetone to 25 % water.

9.3 Waste Handling and Pollution Prevention:
9.3.1 A tag identifying the contents of the carboy is placed
on the waste container. Attach the appropriate chemical waste
label with the date of beginning collection before using the
container.
9.3.2 Report all major spills according to your laboratory
chemical hygiene plan.
9.3.3 All used vials shall be placed in the labeled carboy for
disposal.
9.3.4 Analyses performed by this test method will generate
solid and liquid wastes that are potentially hazardous.
10. Sample Handling and Preservation
10.1 Sample Collection Criteria—Grab samples are col-
lected in glass containers with polytetrafluoroethylene (PTFE)
lined caps. Surface binding may bias data. All samples are iced
or refrigerated at ≤6 °C from the time of collection until
extraction.
10.2 Sample Preservation and Storage—All samples are
iced or refrigerated at ≤6 °C from the time of collection until
sample extraction. At the laboratory, the samples and extracts
are stored in the refrigerator at ≤6 °C while not being analyzed.
Holding times have not yet been established for these analytes
in the various matrices or the extracts. The extracts are
normally analyzed the day of preparation or within seven days
if multiple dilutions and analysis are required.
11. Sample Preparation and Analysis
11.1 Sample Preparation: Step I—Each batch of samples
(20 or less) shall contain at least a method blank, laboratory
control sample and laboratory control sample duplicate, matrix
spike and matrix spike duplicate (if enough sample is
available), and an RLCS. The sample is mixed in the laboratory
with a clean spatula to have a homogeneous subsample.
11.1.1 Method Blank—The method blank is prepared by
measuring ~2 g of Ottawa sand in a 40-mL VOA vial and then
taken through the sample preparation Step II in 11.2.
11.1.2 Laboratory Control Sample/Laboratory Control
Sample Duplicate—A ~2-g amount of Ottawa sand is added to
each of two 40-mL VOA vials. The samples are spiked with
100 µL of a target spike solution containing BPA at 12.5 mg/L;
NP, OP, and NP2EO at 25 mg/L; and NP1EO at 375 mg/L and
then taken through the sample preparation Step II in 11.2.
11.1.3 RL Check—A ~2-g amount of Ottawa sand is added
to a 40-mL VOA vial. The sample is spiked with 50 µL of a RL
check solution containing BPA at 2 mg/L; NP, OP, and NP2EO
at 4 mg/L; and NP1EO at 60 mg/L and then taken through the
sample preparation Step II in 11.2.
11.1.4 Sample and Sample Duplicate—A ~2-g amount of
sample is added to each of two 40-mL VOA vials. The samples
are taken through the sample preparation Step II in 11.2. The
sample is mixed in the laboratory with a clean spatula to try
and have a homogeneous subsample taken for analysis.
11.1.5 Matrix Spike/Matrix Spike Sample Duplicate—A
~2-g amount of sample is added to each of two 40-mL VOA
vials. The samples are spiked with 100 µL of a TP target spike
solution containing BPA at 12.5 mg/L; NP, OP, and NP2EO at
25 mg/L; and NP1EO at 375 mg/L and then taken through the
sample preparation Step II in 11.2.
11.2 Sample Preparation: Step II:
11.2.1 A surrogate standard solution containing Br-OP,
n-NP, BPA-D6, and n-NP2EO is added to each sample. Refer to
8.3.4.1.
11.2.2 After addition of the surrogate, 7.5 mL of acetone is
added, tumbled on a rotator for 2 h, and centrifuged at
1900 rpm for 10 min.
11.2.3 All the samples are filtered through a PVDF filter
unit using the cleaned glass syringe.
NOTE 1—It is important that this syringe is cleaned with water and
organic solvents as discussed in Section 7. The filters require rinsing with
10 mL acetonitrile followed by 10 mL methanol before use. These
chemicals are found in facilities that manufacture filter units. Nonylphenol
is used in the polypropylene housing to extend shelf life and make the
plastic pliable and less brittle. It is important to wash the nonylphenol off
the filter unit.

9
 D8310 − 20
11.2.4 To the extract, 2.5 mL of ASTM Type 1 water is 12.3 Calibration:
added and mixed. If precipitation is seen after adding water, the 12.3.1 Initial Calibration—The initial calibration contains
samples shall be filtered again through a PVDF filter unit. an eight-point curve. Depending on instrument type, the
11.2.5 An aliquot of that solution is transferred to an LC vial sensitivity and calibration curve responses may vary. At a
and a cap is applied. The final volume of the solution is 10 mL minimum, a five-point linear or a six-point quadratic calibra-
for quantitation purposes. tion curve will be used for all analytes. A calibration curve and
11.2.6 The analyte concentration for all samples will be an instrument blank will be analyzed at the beginning of each
reported in microgram/kilogram based on a dry-weight basis. run or daily to ensure instrument stability. A new curve will be
generated daily. The calibration method is saved and used to
12. Calibration and Standardization quantify all samples. Acceptance limit for calibration curve is
12.1 Calibration of Mass Spectrometer—The triple quadru- mentioned in 13.2.3 and 14.1.5.
pole mass spectrometer is calibrated monthly or when mass 12.3.2 CCC or End Calibration Check, or Both—The CCC
shifts of more than 0.2 Dalton are noticed by the analyst. The or end calibration check needs to be performed at the end of the
calibration file is saved in the software file folder. The batch and within 24 h of the initial calibration of that same
calibration solution normally used is a mixture of NaCsI. Other analytical batch. The CCC or end calibration check standard is
calibration solutions can also be used per manufacturer’s at or near the midpoint of the calibration curve. A QC
specifications. acceptance criterion for CCC is included in 14.2.7. A new
12.2 Instrument Operating Conditions—Analytical condi- calibration shall be generated every 24 h regardless of a
tions for LC and the mass spectrometer are: passing CCC.
12.2.1 Liquid Chromatographic Conditions: 12.4 Autosampler Schedule/Analytical Sequence—Prepare a
12.2.1.1 Analytical Column—UPLC BEH C18, 2.1 × sequence that includes all QC samples and field samples. The
100 mm, 1.7 µm particle size. first sample to be analyzed is a reagent blank sample. The
12.2.1.2 Injections of all standards and samples are nor- calibration standard’s levels are analyzed next. The next
mally made at a 10-µL volume. Other injection volumes may samples to be analyzed should be in the following sequence:
be used to optimize conditions. Standards and samples shall be reagent blank, method blank, RLCS, LCS/LCSD, diluted
in 75:25 acetone:water. In the case of extreme concentration samples, samples, duplicates, MS/MSD, and CCC.
differences among samples, it is wise to analyze a blank after
a concentrated sample and before a diluted sample to minimize 13. Procedure
carryover of analytes from injection to injection. However,
there should not be carryover between samples. The UPLC has 13.1 Sample Analysis Procedure:
a flow-through LC needle design. The gradient conditions for 13.1.1 Instrument conditions for LC/MS/MS are described
liquid chromatography are shown in Table 20. in 12.2. The target compound is identified by comparing the
12.2.2 Mass Spectrometer Conditions—To acquire the sample SRM transition to the known standard SRM transition.
maximum number of data points per SRM channel while Confirmatory transitions are available for BPA and BPA-D6
maintaining adequate sensitivity, the tune parameters shall be (Table 2 and Table 22). The RT for the analytes of interest shall
optimized according to the instrument. Each peak should have also agree with the RT of the mid-level standard by 65 %. The
at least ten scans per peak for adequate quantitation. This test target compound is quantitated using the SRM transition of the
method contains five target compounds and four surrogates that target compound using external calibration. The final report
are optimized in SRM experiment windows to acquire an issued for each sample lists total concentration of TPs, if
optimum number of scans and sensitivity. Variable parameters detected, or non-detect at the RL, if not detected, in
regarding retention times, SRM transitions, and cone and microgram/kilogram on a dry-weight basis.
collision energies are shown in Table 2. Mass spectrometer 13.1.2 If the absolute amount of a target compound in a
parameters used in the development of this test method are sample exceeds the working calibration range, the sample is
listed in Table 21. The instrument is set in the electrospray diluted and reanalyzed. This should be done by diluting the
ionization source setting. sample with 75:25 acetone:water.
13.2 Qualitative and Quantitative Analysis:
TABLE 20 Gradient Conditions for LC 13.2.1 The quantitation of the target analyte is accomplished
Percent Percent 100 mM
with the appropriate software. No internal standards are used.
Time, Flow, Percent
min µL/min CH3CN
95 % Water: NH4OAc in 95 % Refer to Table 22 for the SRM transitions and RTs. The SRM
5 % CH3CN Water: 5 % CH3CN analysis provides confirmation by isolating the precursor ion,
0 300 0 95 5
1 300 0 95 5 fragmenting it to the product ion, and also relating the
3 300 50 45 5 transition RT data. The software manual should be consulted to
4 300 60 35 5 use the software correctly. The quantitation method is set as an
6 300 70 25 5
7 300 70 25 5 external calibration using the peak areas in µg/L units.
9 300 95 0 5
13 300 95 0 5 NOTE 2—If suitable internal standards or isotopes of the native analytes
14 300 0 95 5 are identified, they can be used for isotope dilution or internal standard
16 300 0 95 5 quantitation. If these quantitation types are utilized, the recoveries must
meet the lower and upper control limits shown in Table 3. Any deviations

10
 D8310 − 20
TABLE 21 MS Tune ParametersA
Electrospray Positive Mode Electrospray Negative Mode
Capillary Voltage: 3.5 kV Capillary Voltage: 1 kV
Cone: Variable depending on analyte (Table 1) Cone: Variable depending on analyte (Table 1)
Extractor: 2 V Extractor: 3 V
RF Lens: 0.1 V RF Lens: 0.1 V
Source Temperature: 150 °C Source Temperature: 150 °C
Desolvation Temperature: 450 °C Desolvation Temperature: 450 °C
Desolvation Gas Flow: 900 L/h Desolvation Gas Flow: 900 L/h
Cone Gas Flow: 200 L/h Cone Gas Flow: 300 L/h
Low Mass Resolution 1:9 Low Mass Resolution 1:8
High Mass Resolution 1:15 High Mass Resolution 1:14
Ion Energy 1: –0.1 V Ion Energy 1: 0.9 V
Entrance Energy: –1 V Entrance Energy: –1 V
Collision Energy: Variable depending on analyte (Table 1) Collision Energy: Variable depending on analyte (Table 1)
Exit Energy: 1 V Exit Energy: 0 V
Low Mass Resolution 2:9 Low Mass Resolution 2:7
High Mass resolution 2:15 High Mass resolution 2:13
Ion Energy 2: 1.0 V Ion Energy 2: 1.5 V
Multiplier: 700 V Multiplier: 700 V
Inter-Channel Delay: 0.02 s Inter-Channel Delay: 0.02 s
Inter-Scan Delay: 0.02 Inter-Scan Delay: 0.02
Repeats: 1 Repeats: 1
Span: 0.2 Dalton Span: 0.2 Dalton
Collision Gas Flow (mL/min): 0.25 Collision Gas Flow (mL/min): 0.35
Dwell: 0.1 to 0.105 s to optimize scans Dwell: 0.1 to 0.105 s to optimize scans
A
A Waters Quattro Premier XE mass spectrometer was used to develop this standard.

TABLE 22 RT and SRM Ions

Retention Time, SRM Mass Transition
Analyte ESI Mode
min (Parent > Product)
BPA negative 5.58 227.1 > 211.9
BPA confirmatoryA negative 5.58 227.1 > 132.7
OP negative 8.53 205.1 > 132.7
NP negative 9.70 219.3 > 133.1
NP1EO positive 9.71 282.3 > 126.9
NP2EO positive 9.65 326.3 > 182.9
BPA-D6 (surrogate) negative 5.57 233.3 > 214.9
BPA-D6 confirmatoryA (surrogate) negative 5.57 233.3 > 137.8
Br-OP (surrogate) negative 9.56 283.1 > 78.6
n-NP (surrogate) negative 10.71 219.3 > 105.6
n-NP2EO (surrogate) positive 10.69 326.4 > 88.8
A
Confirmatory transitions are optional but should be included for added qualitative information.

outside these limits must be fully documented and accompany the data
generated.
13.2.2 If there are two or more analyses for a particular
sample because of sample dilution, the analyst shall determine
which is best to report on the sample summary results sheet
based on evaluation of all available data relevant to a given
sample. The target compound is identified by comparing the
sample primary SRM transition. Confirmatory transitions are
available for BPA and BPA-D6 only (Table 2 and Table 22). If
a co-eluting peak is present that interferes with the primary
transition, a confirmatory transition may be used for quantita-
tion. This change shall be documented in the case narrative.
These changes should be rare exceptions.
13.2.3 Regression fits should exclude the point of origin (X
= 0, Y = 0) and be weighted by 1/concentration to increase the
accuracy of the curve at the lower concentrations. For linear
regression to be used, the coefficient of determination, r2,
should be >0.98 for each analyte and, for quadratic regression,
the r2 should be >0.99. Upon inspection of the calibration
curves, if one of the calibration standard injections, other than
the high or low, skews the curve such that the r2 is
unacceptable, this point shall be re-injected and replaced in the
calibration curve or a new calibration curve shall be made. If
the low or high point is excluded, a six-point curve is
acceptable for quadratic fit and five-point for a linear fit, but the
calibration range and reporting limits shall be modified to
reflect this change. Only the high or low point may be
excluded, and internal calibration points may not be excluded.
13.2.4 The RT window of the SRM transitions shall be
within 5 % of the RT of the analyte in a Level 4 to 6 calibration
standard. If this is not true, the calibration curve needs to be
reanalyzed to see if there was a shift in RT during the analysis
and the sample needs to be re-injected. If the RT is still
incorrect in the sample, the analyte is referred to as an
unknown. If the RT is drifting more than 5 %, this will be
noticed in the end calibration check and shall be noted in the
case narrative.

11

14. Quality Control
14.1 Minimum Requirement:
14.1.1 An analyst shall have an approved analyst demon-
stration of capability (ADOC)6 before reporting data from a
method. These studies evaluate whether the RLs and calibra-
tion standard concentrations are appropriate. MDL studies shall
be performed annually for each method if values are reported
below the RL. An RL check standard shall be analyzed with
each batch of 20 samples or less.
14.1.2 Demonstration of Capability (DOC):
14.1.2.1 An initial demonstration of the laboratory capabil-
ity to generate data of acceptable quality is made. A precision
and accuracy (P&A) study shall be performed whenever a
major modification is made to this test method. The average
percent recovery (X), individual percent recovery, and the
standard deviation (σ) of the recoveries are calculated for each
analyte. QC confidence limits at 99.7 %, or three times the
standard deviation of the replicates (3σ), are established. QC
acceptance criteria for the P&A study are shown in Table 3.
14.1.2.2 For a P&A study, four samples containing
1250 µg ⁄L for OP, NP, and NP2EO; 625 µg/L for BPA; and
18 750 µg/L for NP1EO shall be analyzed as replicates. These
samples are then analyzed according to the method described
in Section 11.
14.1.3 MDL Test—The MDL test is performed using the
procedure outlined in 40 CFR Part 136, Appendix B as a guide.
MDL data for this test method are shown in Table 23. The
MDL criteria are not required to meet the criteria in 40 CFR
Part 136 because this SOP only reports to the RL and this is not
a regulatory method. MDL studies will be repeated at least
yearly if any data are reported between the MDL and RL.
14.1.4 Example Calculation of Sample Concentration
Reported—The concentration of sample is calculated using Eq
1 and Eq 2 if dilution is required.
@ C i ~ µg/L! # 3 @ V s ~ L ! #
C s ~ µg/kg! 5
@ W d ~ kg! #
where:
Cs = concentration of target analyte in sample,
Ci = concentration of target analyte in sample from
instrument,
Vs = volume of sample extract, and
Wd = dry weight of the sample.
Vf
5 ~ C u! 5 C f
Vi
6
An example of demonstration of capability is in the following link: https://
nelac-institute.org/docs/2003nelacstandard.pdf.
D8310 − 20
where:
Vf = final volume,
Vi = initial volume (before dilution),
Cu = uncorrected concentration (before dilution), and
Cf = final concentration (corrected for dilution).
14.1.5 Calibration Range—The initial calibration contains
an eight-point curve. Depending on instrument type, the
sensitivity and calibration curve responses may vary. At a
minimum, a five-point linear or six-point quadratic calibration
curve will be used for all analytes. The coefficient of the
determination (r2) of the linear fit shall be greater than or equal
to 0.98. The r2 of the quadratic curve shall be greater than or
equal to 0.99. The calibration points used to generate the curve
should not be deviated more than 630 % from the curve. A
new calibration curve will be generated daily.
14.2 QC Acceptance Criteria—All control limits are pre-
liminary because this is a new standard and collected data are
insufficient to determine historical acceptance criteria over the
course of a longer period. Preliminary QC acceptance criteria
will be addressed when the standard is renewed or when
additional validation data become available.
14.2.1 Matrix Spike:
14.2.1.1 As part of a QC program, spike accuracy for each
matrix is monitored and updated regularly. Records are main-
tained of spiked matrix analyses, and the average percent
recovery (X) and the standard deviation of the percent recovery
are calculated. This procedure maintains a 99.7 % confidence
interval from X 6 3σ control limits for spike compounds. The
acceptance criteria that should be used are shown in Table 3
until more matrix spike data are obtained.
14.2.1.2 Calculate the percent recovery of the spike (P)
using:
SSR 2 SR
P 5 100 3 (3)
SA
(1) where:
SSR = MS/MSD spike sample result,
SR = unspiked sample result,
SA = spike concentration, and
P = percent recovery.
14.2.2 Surrogates—As part of a QC program, all samples
are spiked with surrogate standard spiking solution as de-
scribed in Section 11. The percentage recovery limit for each
surrogate compound is updated regularly based on historical
(2)
recovery data and is based on 99.7 % confidence interval from
X 6 3σ to establish control limits for surrogate compounds.
The acceptance criteria are shown in Table 3. These values are
currently set to 70 to 130 % until more data are acquired.

TABLE 23 MDL Study

Spike Level, Number of Mean Recovery, Mean Recovery, Standard
Analyte Percent RSD MDL,A µg/kg
µg/kg Samples µg/kg % Deviation
BPA 50.0 9 36.9 73.9 14.5 5.3 15.5
OP 100.0 9 105.0 105.0 14.5 15.3 44.2
NP 100.0 9 108.0 108.0 9.7 10.5 30.4
NP1EO 1500.0 9 1472.2 98.1 21.8 321.6 931.2
NP2EO 100.0 9 90.1 90.1 2.8 2.6 7.4
A
MDL (µg/kg) = standard deviation × t (n – 1.1 – α = 0.99).

12
 D8310 − 20
14.2.3 Duplicates—The relative percent difference (Eq 4)
for the duplicate sample should be <30 % RPD. If greater, the
associated sample concentration is qualified, estimated, and
noted in the case narrative.
14.2.4 Reagent Blank—A reagent blank is prepared with
75:25 % acetone and water for every 20 samples to investigate
for system/laboratory contamination. This solution is also used
to make the calibration curve standards and dilute samples, if
required. The concentration of the target analyte in the blank
shall be less than half the RL.
14.2.5 Method Blank—A method blank for every 20
samples will be prepared in Ottawa sand to investigate for
contamination during sample preparation and extraction. The
concentration of target analytes in the blank shall be less than
half the RL.
14.2.6 MS/MSD—An MS/MSD is extracted with each ma-
trix at a frequency of at least one MS/MSD pair for every 20
samples to investigate for matrix interferences. If the labora-
tory has not received MS/MSD samples for site-specific P&A
data, the site data quality will be evaluated solely on the LCS
criteria. Tables 4-17 display recoveries in different soils.
14.2.7 CCC or End Calibration Check, or Both:
14.2.7.1 Analyze a mid-level continuing calibration stan-
dard at the end of each batch. All analytes should be within
630 % of their expected values. If not, a separately prepared
CCC may be analyzed. If the second CCC fails the criteria,
630 % of the expected analyte value, the data may be reported
qualified as estimated or, if sample and time are available, be
reanalyzed with a new calibration curve and end CCC check. If
any data are reported with any failing QC, it shall be explained
in the case narrative and properly qualified according to your
laboratory’s quality management plan.
14.2.7.2 The percent difference (%D) between the calcu-
lated and expected concentration in the continuing calibration
verification standard is calculated using:
Calculated concentration 2 Expected concentration
%D 5 3 100 (4)
Expected concentration
14.2.8 LCS/LCSD—As part of requirement of a QC
program, spike accuracy for water is monitored with each
batch. At least one LCS/LCSD pair for every 20 samples is
extracted and analyzed. The percent recovery limits for the
target compound are updated regularly based on historical
recovery data and are based on a 99.7 % confidence interval
from X 6 3σ as control limits. The acceptance criteria are
shown in Table 3.
14.2.9 RLCS—For each batch or within the 24-h analysis
window, an RLCS shall be analyzed. The RLCS is processed
like an LCS and spiked at or near the lowest RL. This sample
is to verify that, if the analytes were present at the RL, they
would be confidently identified. The recovery criteria for the
RLCS is 50 to 150 %.
14.3 Immediate Corrective Actions—All control limits are
preliminary because this is a new standard and collected data
are insufficient to determine acceptance criteria based on
historical data. If the QC criteria are not met, the samples may
be reanalyzed to ensure the best possible results are reported. If
the QC samples are reanalyzed and continue to fail, the site
13
samples may be re-extracted into a new batch including all new
batch QC. As stated in 14.2.7, if an end calibration check fails,
the samples should be reanalyzed if possible. All reported
exceedances of QC criteria need to be discussed in the case
narrative.
14.3.1 LCS—As part of a QC program, spike accuracy for
each matrix sample is monitored with each batch. Records are
maintained of spiked sample analyses, and the average percent
recovery and the standard deviation of the percent recovery are
calculated. This procedure maintains a 99.7 % confidence
interval from X 6 3σ control limits for spike compounds.
Criteria for LCS/LCSD samples are shown in Table 3. All
reported exceedances of QC criteria need to be discussed in the
case narrative and data appropriately qualified according to
your laboratory’s quality management plan requirements.
14.3.2 Matrix Spike Samples—As part of a QC program,
spike accuracy for each matrix sample is monitored with each
batch. Records are maintained of spiked sample analyses, and
the average percent recovery and the standard deviation of the
percent recovery are calculated. This procedure maintains a
99.7 % confidence interval from X 6 3σ control limits for spike
compounds. Criteria for MS/MSD samples are shown in Table
3 (LCS/LCSD criteria). All reported exceedances of QC
criteria need to be discussed in the case narrative and data
appropriately qualified according to your laboratory’s quality
management plan requirements. These criteria pertain only to
the native unspiked sample.
14.3.3 Method Blank and Reagent Blank Samples—The
concentration of target analyte in the blank shall be less than
half the RL or the data shall be qualified that there is possible
interference from the blank, or the RL for the associated
sample(s) shall be raised to at least three times above the blank
contamination concentration. Since a quadratic fit is often used,
the concentrations below the RL are not accurate; therefore, the
response/area count of the blank should be less than half the
response/area count in the associated sample(s).
14.3.4 RLCS—The recovery criteria for the RLCS is 50 to
150 %. If the analytes are not detected or biased low in the
RLCS, then the data for all non-detects are qualified according
to your quality management plan and the QC failure is
explained in the narrative accompanying the data.
14.3.5 Duplicate Samples:
14.3.5.1 A duplicate sample is analyzed with every batch of
20 samples. The relative percent difference in the duplicate
shall be less than 630 %. If not, the native sample is qualified
estimated. For problematic matrices, it is recommended that
the frequency of duplicate analyses be increased above this
criteria.
14.3.5.2 Calculate the relative percent difference (RPD)
using:
RPD 5
? @ S # 2 @ DS # ? 3 100 (5)
~ @ S # 1 @ DS # ! ⁄ 2
where:
S = concentration of the sample, and
DS = concentration of the duplicate sample.
14.3.6 Surrogates—Br-OP represents OP and NP, BPA-D6
represents BPA, and n-NP2EO represents NP1EO and NP2EO.
 D8310 − 20
n-NP is not representative of NP or OP but is included as a
monitoring compound. n-NP is the straight chain analog that
does not mimic the branched. If the recovery for n-NP is low,
this does not indicate that the recovery for NP or OP is low
based on historical data. Qualification of data generated with
this method should follow your laboratory’s quality manage-
ment plan.
15. Data and Records Management
15.1 Calculations and Documentation:
15.1.1 Refer to Eq 1 on how the final concentration is
calculated.
15.1.2 Use of professional judgment in the data reduction
and verification process shall be documented.
15.1.3 All QA/QC data and final results are reported.
15.2 Reporting Result Procedure:
15.2.1 The concentration in the sample is calculated using
the linear or quadratic calibration curve. The sample results are
reported to the RL in microgram per kilogram based on
dry-weight basis. These results are reported without any
corrections for recovery data. All QC data obtained are
included in the data packages.
16. Troubleshooting
16.1 Symptom—Inadequate Abundance or Sensitivity Prob-
able Causes:
16.1.1 Dirty or contaminated ion source, electron multiplier,
or quadrupole rod surfaces.
16.1.2 Potentials of ion source elements at wrong values
because of open or short circuits.
16.1.3 Faulty ion source electronics, detector electronics, or
power supply.
16.2 Symptom—High Background Probable Causes:
16.2.1 Carryover—There is the possibility that some previ-
ously injected sample can still be present in the vacuum system
long after it was thought to be evacuated. This phenomenon
depends on sample volatility, temperature, and so forth.
16.2.2 Contamination in a Recently Cleaned Vacuum
System—After any venting of a vacuum system for
maintenance, there is the potential for introducing new sub-
stances into the vacuum system. Some substances can be
readily removed by evacuation, while others require more
cleaning or baking.
16.2.2.1 Solvents Used in the Cleaning Process—These may
be present for a short time and should be pumped out to the
vacuum system.
16.2.2.2 Water Absorbed on the Metal Surfaces While
Vented—This will pump out.
16.3 Symptom—Mass Spectrometer Does Not Respond
Probable Cause:
16.3.1 Mass Spectrometer Electronics Are Not On—Check
the switch.
16.3.2 Secondary Fuse Blown—Check the secondary fuses
on the rear of the mass spectrometer and replace the faulty fuse
or fuses.
16.3.3 Board failure.
16.3.4 Communication Loss—Reboot mass spectrometer,
PC, and LC.
17. Preventive Maintenance
17.1 A logbook for recording preventive maintenance and
repair work of LC/MS should be located near the instrument
with dates of repair and initials. The reagents and standards are
recorded in the analyst’s data logbook.
17.2 The instrument manual should be located on the
instrument computer associated with the instrument software.
18. Precision and Bias
18.1 This standard has been tested on Ottawa sand, four
ASTM soil types, biosolid sample, and one commercial soil
(results shown in Tables 4-17). The QC acceptance criteria are
listed in Table 3.
19. Keywords
19.1 Bisphenol A; LC/MS/MS; liquid chromatography;
mass spectrometry; nonylphenol; octylphenol; sediment; soil

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