We recently stocked a custom EPA Method 525.3 standard made specifically for labs participating in Unregulated Contaminant Monitoring Rule 4 (UCMR4). Quantitative Certificates of Analysis with Data Packs are available for each item. Email [email protected] or phone 800-356-1688 ext. 3 to place your order (items are not available at Restek.com)
Cat# 572261 – Eight Pesticides and One Pesticide Manufacturing Byproduct
| Contaminant |
CAS Registry Number |
Minimum Reporting Level |
Standard Concentration |
|---|
| alpha-hexachlorocyclohexane |
319-84-6 |
0.01 µg/L |
10 µg/mL |
| chlorpyrifos |
2921-88-2 |
0.03 µg/L |
30 µg/mL |
| dimethipin |
55290-64-7 |
0.2 µg/L |
200 µg/mL |
| ethoprop |
13194-48-4 |
0.03 µg/L |
30 µg/mL |
| oxyfluorfen |
42874-03-3 |
0.05 µg/L |
50 µg/mL |
| profenofos |
41198-08-7 |
0.3 µg/L |
300 µg/mL |
| tebuconazole |
107534-96-3 |
0.2 µg/L |
200 µg/mL |
| total permethrin (42% cis- & 58% trans-) |
52645-53-1 |
0.04 µg/L |
40 µg/mL |
| tribufos |
78-48-8 |
0.07 µg/L |
70 µg/mL |
The analyte concentrations make it easy to prepare calibration levels based on the minimum reporting level (MRL) required by the UCMR4 program.
I’ve included example chromatograms collected at the MRL and 10x the MRL using the GC conditions taken from section 10.2.3.1 of EPA Method 525.3 version 1.0. The SIM conditions were generated using the AutoSIM feature of MSD Chemstation version D.03
SIM Analysis of EPA 525.3 UCMR4 Standard Run at Method Reporting Limit
|
Peaks |
tR (min) |
Conc. (µg/mL) |
|---|
| 1. |
1,3-Dimethyl-2-nitrobenzene |
7.43 |
1.0 |
| 2. |
Acenaphthene-d10 |
11.54 |
1.0 |
| 3. |
Ethoprop |
13.29 |
0.030 |
| 4. |
Alpha-BHC |
14.06 |
0.010 |
| 5. |
Dimethipin |
14.54 |
0.20 |
| 6. |
Pentachlorophenol-13C6 |
14.65 |
2.0 |
| 7. |
Phenanthrene-D10 |
15.05 |
1.0 |
| 8. |
Chlorpyrifos |
17.09 |
0.030 |
| 9. |
Profenofos |
19.34 |
0.30 |
| 10. |
Tribufos |
19.49 |
0.070 |
| 11. |
Oxyfluorfen |
19.57 |
0.050 |
| 12. |
Tebuconazole |
21.7 |
0.20 |
| 13. |
Triphenyl phosphate |
21.8 |
1.0 |
| 14. |
Chrysene-D12 |
22.63 |
1.0 |
| 15. |
cis-Permethrin |
24.98 |
0.017 |
| 16. |
trans-Permethrin |
25.16 |
0.023 |
| 17. |
Benzo[a]pyrene-d12 |
26.68 |
1.0 |
SIM Analysis of EPA 525.3 UCMR4 Standard Run at 10x Method Reporting Limit
|
Peaks |
tR (min) |
Conc. (µg/mL) |
|---|
| 1. |
1,3-Dimethyl-2-nitrobenzene |
7.43 |
1.0 |
| 2. |
Acenaphthene-d10 |
11.54 |
1.0 |
| 3. |
Ethoprop |
13.29 |
0.30 |
| 4. |
Alpha-BHC |
14.06 |
0.10 |
| 5. |
Dimethipin |
14.54 |
2.0 |
| 6. |
Pentachlorophenol-13C6 |
14.65 |
2.0 |
| 7. |
Phenanthrene-D10 |
15.05 |
1.0 |
| 8. |
Chlorpyrifos |
17.09 |
0.30 |
| 9. |
Profenofos |
19.34 |
3.0 |
| 10. |
Tribufos |
19.49 |
0.70 |
| 11. |
Oxyfluorfen |
19.57 |
0.50 |
| 12. |
Tebuconazole |
21.7 |
2.0 |
| 13. |
Triphenyl phosphate |
21.8 |
1.0 |
| 14. |
Chrysene-D12 |
22.63 |
1.0 |
| 15. |
cis-Permethrin |
24.98 |
0.17 |
| 16. |
trans-Permethrin |
25.16 |
0.23 |
| 17. |
Benzo[a]pyrene-d12 |
26.68 |
1.0 |
| Rxi-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623) |
| EPA Method 525.3 PAH IS Mix (cat.# 32547) |
|
Pentachlorophenol-13C6 (cat.# 32548) |
|
EPA Method 525.3 Surrogate Standard (cat.# 32549) |
|
Method 525.3 UCMR4 Standard (cat.# 572261) |
| Ethyl Acetate |
| 1 µL pulsed splitless (hold 1.0 min) |
| 4 mm Single Taper w/Wool (cat.# 23303) |
| 275 °C |
| 30 psi (206.8kPa) |
| 1.05 min |
| 60 mL/min |
| 70 °C (hold 1.5 min) to 200 °C at 10 °C/min (hold 0 min) to 320 °C at 7 °C/min (hold 3 min) |
| He, constant flow |
| 1.2 mL/min |
| MS |
| SIM |
| Group |
Start Time
(min) |
Ion(s) (m/z) |
Dwell (ms) |
|---|
| 1 |
1.546 |
77 134 |
25 |
| 2 |
9.501 |
162 164 |
25 |
| 3 |
12.423 |
97 126 139 158 |
25 |
| 4 |
13.666 |
109 181 183 219 |
25 |
| 5 |
14.288 |
53 54 274 276 |
25 |
| 6 |
14.856 |
160 188 |
25 |
| 7 |
16.087 |
97 197 199 |
25 |
| 8 |
18.205 |
57 63 97 139 169 208 252 339 361 |
25 |
| 9 |
20.652 |
77 83 125 169 250 326 |
25 |
| 10 |
22.212 |
236 240 |
25 |
| 11 |
23.813 |
163 183 |
25 |
| 12 |
25.886 |
132 164 |
25 |
|
| 280 °C |
| Quadrupole |
| Stainless Steel |
| 6 mm ID |
| 280 °C |
| 180 °C |
| 1.45 min |
| DFTPP |
| EI |
| HP6890 GC & 5973 MSD |
