New Custom UCMR4 Standard for EPA Method 525.3

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 csreps@restek.com or phone 800-356-1688 ext. 3 to place your order (items are not available at Restek.com)

Cat# 572261 – Method 525.3 UCMR4 Standard – Eight Pesticides and One Pesticide Manufacturing Byproduct (in Methanol)

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 (MRL)

SIM Analysis of EPA 525.3 UCMR4 Standard Run at 10x Method Reporting Limit (MRL)

Peaks tR (min) MRL Conc. (µg/mL) 10x MRL Conc. (µg/mL)
1. 1,3-Dimethyl-2-nitrobenzene (SUR) 7.43 1.0 1.0
2. Acenaphthene-D10 (IS) 11.54 1.0 1.0
3. Ethoprop 13.29 0.030 0.30
4. Alpha-BHC 14.06 0.010 0.10
5. Dimethipin 14.54 0.20 2.0
6. Pentachlorophenol-13C6 (IS) 14.65 2.0 2.0
7. Phenanthrene-D10 (IS) 15.05 1.0 1.0
8. Chlorpyrifos 17.09 0.030 0.30
9. Profenofos 19.34 0.30 3.0
10. Tribufos 19.49 0.070 0.70
11. Oxyfluorfen 19.57 0.050 0.50
12. Tebuconazole 21.7 0.20 2.0
13. Triphenyl phosphate (SUR) 21.8 1.0 1.0
14. Chrysene-D12 (IS) 22.63 1.0 1.0
15. cis-Permethrin 24.98 0.017 0.17
16. trans-Permethrin 25.16 0.023 0.23
17. Benzo[a]pyrene-d12 (SUR) 26.68 1.0 1.0

 

Column Rxi-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623)
Sample 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)
Diluent: Ethyl Acetate
Injection
Inj. Vol.: 1 µL pulsed splitless (hold 1.0 min)
Liner: 4 mm Single Taper w/Wool (cat.# 23303)
Inj. Temp.: 275 °C
Pulse Pressure: 30 psi (206.8kPa)
Pulse Time: 1.05 min
Purge Flow: 60 mL/min
Oven
Oven Temp.: 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)
Carrier Gas He, constant flow
Flow Rate: 1.2 mL/min
Detector MS
Mode: SIM
SIM Program:
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
Transfer Line Temp.: 280 °C
Analyzer Type: Quadrupole
Source Type: Stainless Steel
Drawout Plate: 6 mm ID
Source Temp.: 280 °C
Quad Temp.: 180 °C
Solvent Delay Time: 1.45 min
Tune Type: DFTPP
Ionization Mode: EI
Instrument HP6890 GC & 5973 MSD

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