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New Custom UCMR4 Standard for EPA Method 525.3

15 Mar 2017

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.

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)

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

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	Peaks	t_R (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