Professional Documents
Culture Documents
2. Referenced Documents
1. Scope
3. Terminology
3.1 Definitions:
3.1.1 analytical column, nthe particles of the solid stationary phase fill the whole inside volume of a tube (column)
that the mobile phase passes through using the pressure
generated by the liquid chromatography system.
1
This test method is under the jurisdiction of ASTM Committee E54 on
Homeland Security Applications and is the direct responsibility of Subcommittee
E54.03 on Decontamination.
Current edition approved June 1, 2016. Published July 2016. Originally approved
in 2012. Last previous edition approved in 2012 as E2866 12. DOI: 10.1520/
E2866-12R16.
2
The MDL is determined following the Code of Federal Regulations, 40 CFR
Part 136, Appendix B utilizing solvent extraction of soil by PFE. A detailed process
determining the MDL is explained in the reference and is beyond the scope of this
Standard to be explained here.
3
Reporting range concentrations are calculated from Table 4 concentrations
assuming a 100 L injection of the lowest and highest level calibration standards
with a 40 mL final extract volume of a 10 gram soil sample. Volume variations will
change the reporting limit and ranges. The reporting limit (RL), lowest concentration of the reporting range, is calculated from the concentration of the Level 1
calibration standard as shown in Table 4.
4
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 standards Document Summary page on
the ASTM website.
5
Available from National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
www.epa.gov/epawaste/hazard/testmethods/index.htm
6
Available from U.S. Government Printing Office Superintendent of Documents,
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2866 12 (2016)
TABLE 1 Method Detection Limit and Reporting Range
Analyte
Diisopropyl methylphosphonate
Ethyl methylphosphonic acid
Ethyl methylphosphonic acid
Isopropyl methylphosphonic
acid
Isopropyl methylphosphonic
acid
Methylphosphonic acid
Pinacolyl methylphosphonic
acid
ESI
Mode
MDL
(PPB)
Reporting Range
(PPB)
Positive
Negative
Positive
Negative
2.7
2.3
1.3
5.7
40-2000
40-2000
40-2000
40-2000
Positive
2.8
40-2000
Positive
Negative
8.7
5.3
40-2000
40-2000
4.1 For OPs soil analysis, samples are shipped to the lab
between 0C and 6C. The samples are to be extracted, filtered
and analyzed by LC/MS/MS within 7 days of collection.
4.2 The OPs and the surrogates (diisopropyl
methylphosphonate-D14, pinacolyl methylphosphonic acid-13
C6 and methylphosphonic acid-D3) are identified by retention
time and one SRM transition. The target analytes and surrogates are quantitated using the SRM transitions utilizing an
external calibration. The final report issued for each sample
lists the concentration of each organophosphonate target compound and each surrogate recovery.
5. Significance and Use
5.1 This is a performance based method, and modifications
are allowed to improve performance.
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described
in this standard are allowed as long as better or equivalent
performance data result. Any modifications shall be documented and performance data generated. The user of the data
generated by this Standard shall be made aware of these
changes and given the performance data demonstrating better
or equivalent performance.
5.2 Organophosphate pesticides affect the nervous system
by disrupting the enzyme that regulates acetylcholine, a neurotransmitter. They were developed during the early 19th
century, but their effects on insects, which were similar to their
effects on humans, were discovered in 1932. Some are poisonous and were used as chemical weapon agents. Organophosphate pesticides are usually not persistent in the
environment.7,8
5.3 This test method is for the analysis of selected organophosphorous based pesticide degradation products.
3.2 Abbreviations:
3.2.1 DIMPdiisopropyl methylphosphonate
3.2.2 EMPAethyl methylphosphonic acid
3.2.3 IMPAisopropyl methylphosphonic acid
3.2.4 LCliquid chromatography
3.2.5 LCS/LCSDlaboratory control spike/laboratory control spike duplicate
3.2.6 mMmillimolar, 1 10-3 moles/L
3.2.7 MPAmethylphosphonic acid
3.2.8 MRMmultiple reaction monitoring
5.4 This method has been investigated for use with various
soils.
6. Interferences
6.1 Method interferences may be caused by contaminants in
solvents, reagents, glassware, and other apparatus producing
7
Additional information about organophosphate pesticides is available on the
Internet at http://www.epa.gov (2011).
8
Additional information about chemical weapon agents is available on the
Internet at http://www.opcw.org (2011).
E2866 12 (2016)
7.2.2 Glass Fiber Filters.14,10
7.2.3 Amber VOA Vials40 mL for sample extracts and 60
mL for PFE.
9
A Waters Acquity UPLC H-Class System was used to develop this test method
and generate the precision and bias data presented in Section 16. The sole source of
supply known to the committee at this time is Waters Corporation, Milford, MA
01757.
10
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,1 which you may attend.
11
A Waters-Atlantis dC18, 150 mm 2.1 mm, 3 m particle size, was used to
develop this test method and generate the precision and bias data presented in
Section 16. The sole source of supply known to the committee at this time is Waters
Corporation, Milford, MA 01757.
12
A Waters Quattro micro API mass spectrometer was used to develop this test
method and generate the precision and bias data presented in Section 16. The sole
source of supply known to the committee at this time is Waters Corporation,
Milford, MA 01757.
13
A Dionex Accelerated Solvent Extraction (ASE 200) system with appropriately sized extraction cells was used to develop this test method and generate the
precision and bias data presented in Section 16. The sole source of supply known to
the committee at this time is Dionex Corporation, Sunnyvale, CA 94088.
E2866 12 (2016)
TABLE 2 Gradient Conditions for Liquid Chromatography
Time
(min)
Flow
(L/min)
Percent
CH3CN
Percent
Water
Percent
2% Formic
Acid in
Water
0
4
5
9
10
13
14
20
300
300
300
300
300
300
300
300
0
0
45
45
95
95
0
0
95
95
50
50
0
0
95
95
5
5
5
5
5
5
5
5
E2866 12 (2016)
TABLE 3 Retention Times, SRM Transitions, and Analyte-Specific Mass Spectrometer Parameters
Analyte
Diisopropyl methylphosphonate
Ethyl methylphosphonic acid
Ethyl methylphosphonic acid
Isopropyl methylphosphonic acid
Isopropyl methylphosphonic acid
Methylphosphonic acid
Pinacolyl methylphosphonic acid
DIMP-D14 (Surrogate)
PMPA-13C6 (Surrogate)
MPA-D3 (Surrogate)
ESI Mode
Retention Time
(min)
Cone Voltage
(Volts)
Collision Energy
(eV)
Positive
Negative
Positive
Negative
Positive
Positive
Negative
Positive
Negative
Positive
8.8
3.6
3.6
7.5
7.5
2.0
8.6
8.8
8.6
2.0
181.2>139.1
123.0>94.9
125.0>96.9
137.0>94.9
139.1>96.9
96.9>78.8
179.1>94.9
195.2>147.1
185.1>94.9
99.9>81.8
25
30
25
28
25
45
35
23
35
40
6
12
10
13
7
15
18
7
18
15
E2866 12 (2016)
TABLE 4 Concentrations of Calibration Standards (PPB)
Analyte/Surrogate
Diisopropyl methylphosphonate
Ethyl methylphosphonic acid
Isopropyl methylphosphonic acid
Methylphosphonic acid
Pinacolyl methylphosphonic acid
DIMP-D14 (Surrogate)
PMPA-13C6 (Surrogate)
MPA-D3 (Surrogate)
LV 1
LV 2
LV 3
LV 4
LV 5
LV 6
LV 7
LV 8
10
10
10
10
10
10
10
10
25
25
25
25
25
25
25
25
50
50
50
50
50
50
50
50
100
100
100
100
100
100
100
100
200
200
200
200
200
200
200
200
300
300
300
300
300
300
300
300
400
400
400
400
400
400
400
400
500
500
500
500
500
500
500
500
complete analytical test method including any sample preservation and pretreatment steps.
12.3.2 Calculate the mean (average) percent recovery and
relative standard deviation (RSD) of the four values and
compare to the acceptable ranges of the quality control (QC)
acceptance criteria for the Initial Demonstration of Performance in Table 5.
12.3.3 This study shall be repeated until the single operator
precision and mean recovery are within the limits in Table 5.
12.3.4 The QC acceptance criteria for the Initial Demonstration of Performance in Table 5 are preliminary until a
collaborative study is conducted. Single-laboratory data is
shown in the Precision and Bias Section. The analyst shall be
aware that the performance data generated from singlelaboratory data tend to be significantly tighter than those
generated from multi-laboratory data. The laboratory shall
generate its own in-house QC acceptance criteria which meet
or exceed the criteria in this test method. References on how to
generate QC acceptance criteria are ASTM Standard E2554 or
Method 8000B in EPA publication SW-846.
E2866 12 (2016)
TABLE 5 Quality Control Acceptance Criteria (Test Concentration at 400 ppb)
Initial Demonstration of Performance
Analyte
ESI Mode
Diisopropyl methylphosphonate
Ethyl methylphosphonic acid
Ethyl methylphosphonic acid
Isopropyl methylphosphonic acid
Isopropyl methylphosphonic acid
Methylphosphonic acid
Pinacolyl methylphosphonic acid
DIMP-D14 (Surrogate)
PMPA-13C6 (Surrogate)
MPA-D3 (Surrogate)
Recovery (%)
Upper Limit
Maximum % RSD
Lower Limit
Upper Limit
70
70
70
70
70
50
70
70
70
50
130
130
130
130
130
150
130
130
130
150
30
30
30
30
30
40
30
30
30
40
70
70
70
70
70
50
70
70
70
50
130
130
130
130
130
150
130
130
130
150
+
+
+
+
+
+
where:
A =
B =
C =
Vs =
V =
P =
? A ~ V 1V ! 2 BV ?
s
CV
Recovery (%)
Lower Limit
between 200 and 800 ppb. This test method was tested at 400
ppb. The LCS is prepared following the analytical method and
analyzed with each batch of 20 samples or less. Prepare a stock
matrix spiking solution in methanol containing EMPA, MPA,
IMPA, DIMP and PMPA each at 40 ppm. An Ottawa sand
sample is spiked with the matrix spiking solution to achieve a
concentration of 400 ppb (that is, 100 L of a 40 ppm methanol
solution containing of DIMP, EMPA, IMPA, MPA and PMPA
is added to a 10 g soil sample). The results obtained for the
LCS shall fall within the limits in Table 5.
12.6.2 If the results are not within these limits, analysis of
samples is halted until the problem is corrected, and either all
samples in the batch shall be re-analyzed or the results shall be
qualified with an indication that they do not fall within the
performance criteria of the test method.
P 5 100
Precision
(1)
12.8 Duplicate:
12.8.1 To check the precision of sample analyses, analyze a
sample in duplicate with each batch of 10 or fewer samples. If
the sample contains the analyte at a level greater than 5 times
the detection limit of the method, the sample and duplicate may
be analyzed unspiked; otherwise, an MSD shall be used.
12.8.2 Calculate the relative percent difference (RPD) between the duplicate values (or MS/MSD values) as shown in
Eq 2. Compare to the RPD limit in Table 6.
12.7.4 The percent recovery of the spike shall fall within the
limits in Table 6. If the percent recovery is not within these
limits, a matrix interference may be present in the selected
7
E2866 12 (2016)
TABLE 6 MS/MSD Quality Control Acceptance Criteria
MS/MSD
Analyte/Surrogate
ESI Mode
Diisopropyl methylphosphonate
Ethyl methylphosphonic acid
Ethyl methylphosphonic acid
Isopropyl methylphosphonic acid
Isopropyl methylphosphonic acid
Methylphosphonic acid
Pinacolyl methylphosphonic acid
DIMP-D14 (Surrogate)
PMPA-13C6 (Surrogate)
MPA-D3 (Surrogate)
RPD 5
? MSR 2 MSDR?
~ MSR1MSDR! 2
+
+
+
+
+
+
3 100
Recovery (%)
400
400
400
400
400
400
400
400
400
400
Precision
Lower Limit
Upper Limit
Maximum RPD
(%)
30
30
30
30
30
30
30
30
30
30
130
130
130
130
130
130
130
130
130
130
30
30
30
30
30
30
30
30
30
30
(2)
where:
RPD
= relative percent difference,
MSR
= matrix spike recovery, and
MSDR = matrix spike duplicate recovery.
NOTE 1If the soil sample with the drying agent can fit into the smaller
sized cell without packing it down, the smaller sized cell should be
chosen. Do not pack the soil down into the cell, this will prevent effective
extraction. Hand-tighten the main body of the extraction cell with a cell
cap and insert a disposable glass fiber filter at the bottom of the cap. Place
the prepared sample into each cell.
13.8 Fill any void volume in the cell with the drying agent
or Ottawa sand. Assemble each extraction cell by handtightening the cell caps on each end. Do not use a wrench or
other tool to tighten the cap. If the extraction cells are packed
tightly, an over-pressurized condition can cause the system to
shut down. Prior to using the cell caps, verify that the white
O-rings are in place and in good condition. Check the polyether
ether ketone (PEEK) seals inside the caps and replace if
necessary.
13.9 Load the cells in numerical order and hang the cells
vertically in the tray slots from their top caps. The bottom cap
contains the glass fiber filter.
8
E2866 12 (2016)
concentrations or column degradation this is not a concern if
the analyte specific SRM transitions are employed. DIMP and
PMPA both have parent ion of 181.2 m/z, and both will
produce the same product fragment under certain conditions. In
ESI negative mode, PMPA will produce a parent ion of 179.1
m/z, but DIMP will not. Therefore, the optimum transition for
PMPA is in the ESI negative mode using 179.1>94.9. In ESI
positive mode, the DIMP parent ion 181.2 m/z will produce a
139.1 m/z product ion by loss of one isopropyl moiety, whereas
PMPA is not able to lose that fragment. Therefore, the optimum
SRM transition for DIMP is in the ESI positive mode using
181.2>139.1.
15. Report
15.1 Determine the results in units of g/kg (ppb) in a soil
sample. Calculate the concentration in the sample using the
linear or quadratic calibration curve generated. All data that do
not meet the specifications in the test method shall be appropriately qualified.
14.2 Data for EMPA and IMPA are collected both in ESI
positive and ESI negative modes. Both ESI positive and ESI
negative quantitative results shall be reported for all samples
including method blanks, laboratory control samples and
matrix spikes.
14.3 DIMP and PMPA may be overlapping in this test
method. If there is overlap encountered due to poor chromatography which may be caused by a variation in elution solvent
18
Reference to the ASTM soils and soil reports can be found at: http://
www.durhamgeo.com/downloads/ASTM%20Soil%20Reports.html (2011)
E2866 12 (2016)
TABLE 7 Surrogate Recovery Data
Measured ppb from 400 ppb Spikes
Precision and
Accuracy
Samples
Sand
Georgia
Nebraska
Method Blank
1
2
3
4
5
6
7
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
608.0
505.6
493.1
495.1
453.0
227.7
457.4
468.2
463.5
115.9
107.1
23.1
384.2
385.8
377.6
386.5
375.5
363.2
371.4
361.2
375.7
93.9
9.9
2.6
460.4
473.5
403.1
424.6
427.5
413.6
436.3
402.7
430.2
107.6
25.7
6.0
<RL
<RL
<RL
<RL
<RL
<RL
<RL
<RL
-
370.0
362.5
354.6
350.5
349.9
347.9
355.8
362.8
356.8
89.2
7.7
2.2
364.0
346.9
364.3
356.3
355.4
350.9
335.1
358.5
353.9
88.5
9.6
2.7
<
<
<
<
<
<
<
<
RL
RL
RL
RL
RL
RL
RL
RL
-
237.6
237.2
239.6
240.0
226.2
210.6
225.3
237.3
231.7
57.9
10.3
4.5
240.0
281.0
284.2
289.2
265.3
260.0
264.6
303.2
273.4
68.4
19.8
7.2
<RL
<RL
<RL
<RL
<RL
<RL
<RL
<RL
-
91.7
58.2
58.4
43.6
27.6
66.8
72.3
32.0
56.3
14.1
21.4
37.9
190.8
134.8
149.9
130.9
189.6
165.6
155.5
130.3
155.9
39.0
24.5
15.7
MPA-D3
(ESI +)
PMPA-13C6
(ESI -)
DIMP-D14
(ESI +)
MPA-D3
(ESI +)
PMPA-13C6
(ESI -)
DIMP-D14
(ESI +)
MPA-D3
(ESI +)
PMPA-13C6
(ESI -)
DIMP-D14
(ESI +)
109.6
105.0
135.8
132.4
95.4
87.8
85.8
99.0
106.3
26.6
18.9
17.8
380.4
353.9
356.5
373.5
363.7
372.2
382.8
361.3
368.1
92.0
10.8
2.9
395.4
385.2
380.6
386.0
423.2
398.2
388.0
373.8
391.3
97.8
15.0
3.8
403.5
295.2
362.4
364.0
340.5
347.4
333.3
359.4
350.7
87.7
30.9
8.8
387.3
382.9
386.0
393.8
392.8
394.0
397.5
404.8
392.4
98.1
7.0
1.8
391.9
392.2
385.8
400.0
396.8
389.2
392.2
391.2
392.4
98.1
4.4
1.1
107.2
85.2
60.4
16.0
60.4
18.4
89.2
62.8
62.5
15.6
32.4
51.9
138.4
218.8
68.0
84.0
149.6
62.4
290.0
285.2
162.1
40.5
92.8
57.3
101.6
183.2
67.6
41.6
102.0
50.0
231.2
232.0
126.2
31.5
78.4
62.2
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
419.5
407.5
423.7
401.0
160.6
381.5
380.7
367.8
92.0
92.9
25.3
<RL
411.7
421.4
379.0
359.7
335.2
361.0
377.5
377.9
94.5
30.2
8.0
<RL
375.2
377.1
387.2
364.7
347.3
363.8
351.2
366.7
91.7
14.3
3.9
<RL
417.0
415.4
415.6
367.2
361.9
381.8
374.7
390.5
97.6
24.6
6.3
<RL
378.8
374.5
383.2
366.3
364.2
372.8
359.0
371.3
92.8
8.6
2.3
<RL
374.6
371.3
387.0
372.4
361.7
368.3
360.5
370.8
92.7
8.9
2.4
<RL
424.1
357.5
367.9
365.7
354.6
365.2
342.7
368.2
92.1
26.1
7.1
16.3.4 Poor recovery for PMPA was found with CH-1 soil at
~33% and CL-1 soil at ~17%.
16.3.5 Poor recovery for DIMP was found with CH-1 soil at
~23% and CL-1 soil at~38%.
17. Keywords
17.1 liquid chromatography; mass spectrometry; organophosphonates; pressurized fluid extraction; soil
10
E2866 12 (2016)
TABLE 10 Organophosphates Recovery Data in Georgia Soil (400 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
6
7
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
<RL
<RL
<RL
<RL
<RL
<RL
<RL
-
<RL
360.8
375.8
379.8
360.0
383.4
335.5
394.2
369.9
92.5
19.5
5.3
<RL
331.7
331.1
342.1
335.4
337.1
302.0
359.1
334.1
83.5
17.1
5.1
<RL
297.4
284.4
296.0
280.1
286.8
248.2
289.1
283.1
70.8
16.6
5.9
<RL
329.8
326.7
328.7
323.5
328.3
302.2
343.4
326.1
81.5
12.3
3.8
<RL
360.8
363.4
366.8
372.7
356.6
332.2
383.6
362.3
90.6
15.9
4.4
<RL
346.9
361.2
355.9
358.3
352.1
336.4
349.6
351.5
87.9
8.3
2.4
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
< RL
< RL
< RL
< RL
< RL
< RL
< RL
-
<RL
307.6
328.4
306.1
287.2
294.9
295.5
292.6
301.8
75.4
13.8
4.6
<RL
218.4
213.2
216.4
208.3
218.4
206.9
212.0
213.4
53.3
4.6
2.2
<RL
138.4
136.0
145.2
146.3
163.1
139.6
142.1
144.4
36.1
9.0
6.3
<RL
91.0
87.4
92.6
91.8
103.4
91.5
87.6
92.2
23.0
5.3
5.8
<RL
240.1
240.0
242.6
232.3
260.2
225.8
235.0
239.4
59.9
10.8
4.5
<RL
281.3
267.8
279.4
253.8
293.9
256.4
288.3
274.4
68.6
15.5
5.6
TABLE 12 Organophosphates Recovery Data in ASTM Soil CH-1 (400 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
6
7
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 400 ppb Spikes in ASTM Reference Soil CH-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
<RL
<RL
<RL
<RL
<RL
<RL
<RL
-
<RL
183.2
57.2
106.4
144.4
91.2
316.4
318.0
173.8
43.5
105.7
60.8
<RL
147.2
39.6
84.0
121.6
69.6
264.8
272.8
142.8
35.7
92.8
65.0
<RL
160.4
51.6
94.0
130.4
78.8
277.6
285.6
154.1
38.5
93.9
61.0
<RL
123.6
30.8
71.2
101.6
59.2
221.2
227.6
119.3
29.8
77.7
65.1
<RL
147.2
34.4
87.2
117.6
69.6
270.8
280.8
143.9
36.0
96.8
67.3
<RL
111.6
27.2
49.2
71.6
45.6
228.8
218.0
107.4
26.9
83.6
77.8
11
E2866 12 (2016)
TABLE 13 Organophosphates Recovery Data in ASTM Soil CL-1 (400 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
6
7
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 400 ppb Spikes in ASTM Reference Soil CL-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
<RL
<RL
<RL
<RL
<RL
<RL
<RL
-
<RL
114.2
70.2
64.1
113.7
86.0
133.4
83.1
95.0
23.7
25.8
27.1
<RL
100.8
64.6
56.6
82.1
64.0
102.0
58.5
75.5
18.9
19.5
25.8
<RL
120.9
71.8
69.3
111.3
84.1
142.7
81.3
97.3
24.3
27.9
28.7
<RL
98.8
55.6
52.0
78.6
61.0
95.2
53.3
70.7
17.7
20.1
28.5
<RL
86.4
40.8
40.5
62.2
49.5
85.3
43.3
58.3
14.6
20.3
34.8
<RL
185.7
121.7
143.7
204.2
149.8
184.8
142.4
161.8
40.4
29.9
18.5
TABLE 14 Organophosphates Recovery Data in ASTM Soil ML-1 (400 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
6
7
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 400 ppb Spikes in ASTM Refernce Soil ML-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
343.0
291.8
339.1
328.7
358.6
337.8
289.2
326.9
81.7
26.4
8.1
<RL
456.7
464.8
463.9
473.2
469.7
477.7
474.7
468.7
117.2
7.3
1.6
<RL
391.8
388.9
399.7
399.4
401.1
413.1
416.0
401.4
100.4
10.0
2.5
<RL
411.9
425.9
409.4
414.1
411.2
419.8
418.8
415.9
104.0
5.9
1.4
<RL
373.6
368.2
367.2
375.8
375.0
394.3
394.0
378.3
94.6
11.3
3.0
<RL
403.6
409.7
413.5
413.9
419.6
428.3
433.0
417.4
104.3
10.4
2.5
<RL
416.8
415.1
416.1
414.4
409.1
420.6
414.5
415.2
103.8
3.4
0.8
TABLE 15 Organophosphates Recovery Data in ASTM Soil SP-1 (400 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
6
7
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
A
B
Measured ppb from 400 ppb Spikes in ASTM Reference Soil SP-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
87.7
119.4
116.1
74.7
65.9
65.6
75.0
86.3
21.6
22.7
26.3
47.4
423.4
437.8
435.6
439.2
441.6
489.5
459.0
446.6
111.7
21.6
4.8
37.7A,B
391.6
420.6
404.1
389.1
384.7
411.2
416.9
402.6
100.7
14.3
3.6
<RL
370.2
360.6
380.8
384.0
359.0
412.0
364.0
375.8
94.0
18.7
5.0
<RL
327.6
338.2
352.4
336.3
316.4
362.2
333.0
338.0
84.5
15.3
4.5
<RL
375.6
376.5
392.3
389.8
390.6
411.0
385.4
388.7
97.2
11.9
3.1
<RL
392.0
390.4
401.7
447.7
415.2
414.2
387.2
406.9
101.7
21.2
5.2
Blank concentrations are not subtracted from sample results, EMPA not present in Method Blank associated with 1600 ppb spiked samples for soil SP-1.
Below Reporting Limit.
12
E2866 12 (2016)
TABLE 16 Organophosphates Recovery Data in Ottawa Sand (1600 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
1136.0
1056.8
1192.0
1015.6
1058.0
1091.7
68.2
71.0
6.5
<RL
1467.6
1537.6
1493.2
1477.2
1471.2
1489.4
93.1
28.7
1.9
<RL
1542.8
1578.0
1524.0
1473.6
1504.0
1524.5
95.3
39.4
2.6
<RL
1540.8
1618.4
1545.6
1564.4
1553.6
1564.6
97.8
31.4
2.0
<RL
1576.8
1636.0
1536.0
1504.8
1505.2
1551.8
97.0
55.6
3.6
<RL
1545.6
1596.0
1541.2
1488.8
1534.0
1541.1
96.3
38.1
2.5
<RL
1504.4
1580.0
1550.0
1510.4
1545.2
1538.0
96.1
31.0
2.0
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
<RL
<RL
<RL
61.6
<RL
12.3
0.8
-
<RL
1524.0
1574.8
1596.0
1550.0
1484.4
1545.8
96.6
43.7
2.8
<RL
1396.8
1377.6
1421.2
1326.0
1273.6
1359.0
84.9
59.2
4.4
<RL
1422.0
1412.4
1462.8
1364.8
1311.2
1394.6
87.2
58.2
4.2
<RL
1307.6
1316.4
1326.8
1252.8
1232.4
1287.2
80.5
41.9
3.3
<RL
1415.2
1403.2
1425.6
1307.2
1326.0
1375.4
86.0
54.7
4.0
<RL
1614.0
1587.2
1621.2
1607.2
1578.0
1601.5
100.1
18.3
1.1
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
<RL
<RL
<RL
<RL
<RL
-
<RL
1979.6
1966.0
1925.6
2004.4
1964.4
1968.0
123.0
28.6
1.5
<RL
1126.8
1065.2
1073.2
1066.8
999.2
1066.2
66.6
45.3
4.2
<RL
401.2
410.0
452.0
444.4
396.8
420.9
26.3
25.5
6.1
<RL
211.6
213.6
214.0
215.6
181.2
207.2
13.0
14.6
7.0
<RL
972.8
953.6
913.2
923.2
823.6
917.3
57.3
57.5
6.3
<RL
1326.0
1283.6
1274.4
1340.4
1236.0
1292.1
80.8
41.9
3.2
TABLE 19 Organophosphates Recovery Data in ASTM Soil CH-1 (1600 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 1600 ppb Spikes in ASTM Reference Soil CH-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
134.4
80.4
189.6
358.4
226.4
197.8
12.4
105.5
53.3
<RL
1600.8
1060.8
730.4
359.6
296.0
809.5
50.6
538.9
66.6
<RL
975.6
588.4
390.8
180.0
138.8
454.7
28.4
342.3
75.3
<RL
1412.8
927.6
647.6
302.0
234.4
704.9
44.1
484.2
68.7
<RL
794.4
499.2
355.6
167.6
124.8
388.3
24.3
272.2
70.1
<RL
969.2
613.2
424.8
190.0
140.0
467.4
29.2
338.8
72.5
<RL
744.0
232.8
156.4
260.4
84.0
295.5
18.5
260.0
88.0
13
E2866 12 (2016)
TABLE 20 Organophosphates Recovery Data in ASTM Soil CL-1 (1600 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 1600 ppb Spikes in ASTM Reference Soil CL-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
<RL
<RL
<RL
<RL
<RL
-
<RL
390.8
336.8
427.6
579.2
322.0
411.3
25.7
103.0
25.0
<RL
380.4
314.8
398.8
549.2
320.8
392.8
24.6
94.8
24.1
<RL
361.2
287.6
349.6
490.8
282.0
354.2
22.1
84.2
23.8
<RL
380.8
315.6
390.4
530.4
289.2
381.3
23.8
93.7
24.6
<RL
326.0
256.0
316.0
458.0
213.2
313.8
19.6
92.7
29.6
<RL
561.2
524.4
541.2
671.6
545.6
568.8
35.6
58.9
10.4
TABLE 21 Organophosphates Recovery Data in ASTM Soil ML-1 (1600 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 1600 ppb Spikes in ASTM Reference Soil ML-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
887.6
1022.4
845.6
1017.2
842.4
923.0
57.7
90.1
9.8
<RL
1644.0
1694.0
1669.6
1566.0
1615.6
1637.8
102.4
49.6
3.0
<RL
1458.8
1439.6
1406.8
1378.0
1302.8
1397.2
87.3
61.2
4.4
<RL
1552.4
1550.4
1537.2
1440.4
1481.2
1512.3
94.5
49.5
3.3
<RL
1356.4
1322.0
1232.4
1202.0
1173.2
1257.2
78.6
78.7
6.3
<RL
1395.2
1349.2
1305.2
1266.4
1263.6
1315.9
82.2
56.3
4.3
<RL
1414.8
1598.8
1503.2
1331.2
1446.4
1458.9
91.2
99.9
6.8
TABLE 22 Organophosphates Recovery Data in ASTM Soil SP-1 (1600 ppb Spike)
Precision and Accuracy
Samples
Method Blank
1
2
3
4
5
Average Recovery:
Average % Recovery:
Standard Deviation:
% Relative SD
Measured ppb from 1600 ppb Spikes in ASTM Reference Soil SP-1
MPA
(ESI +)
EMPA
(ESI +)
EMPA
(ESI -)
IMPA
(ESI +)
IMPA
(ESI -)
PMPA
(ESI -)
DIMP
(ESI +)
<RL
1307.6
1288.4
1222.0
1194.8
1279.2
1258.4
78.7
47.8
3.8
<RL
1604.8
1631.2
1653.2
1576.4
1673.6
1627.8
101.7
38.5
2.4
<RL
1657.2
1702.0
1610.0
1570.8
1658.8
1639.8
102.5
50.5
3.1
<RL
1574.0
1610.8
1584.0
1502.4
1590.4
1572.3
98.3
41.3
2.6
<RL
1574.0
1638.8
1588.8
1525.6
1410.0
1547.4
96.7
86.8
5.6
<RL
1466.0
1439.6
1438.0
1392.0
1466.0
1440.3
90.0
30.2
2.1
<RL
1540.4
1585.2
1490.4
1451.2
1604.8
1534.4
95.9
64.1
4.2
APPENDIX
(Nonmandatory Information)
GA
Soil
NE
Soil
46%
22%
32%
5.0
0.2%
6%
60%
34%
5.6
2.1%
14
E2866 12 (2016)
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15