EPA Method 525.3 UCMR4 Standard on Rxi-5Sil MS at 10x the Method Reporting Limit (SIM Analysis)

	Peaks	t_R (min)	Conc. (µg/mL)
1.	1,3-Dimethyl-2-nitrobenzene (SS)	7.43	1.0
2.	Acenaphthene-d10 (IS)	11.54	1.0
3.	Ethoprop	13.29	0.30
4.	α-Hexachlorocyclohexane (α-HCH)	14.06	0.10
5.	Dimethipin	14.54	2.0
6.	Pentachlorophenol-¹³C₆ (IS)	14.65	2.0
7.	Phenanthrene-d10 (IS)	15.05	1.0
8.	Chlorpyrifos	17.09	0.30

Injection
Column	Rxi-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623)
Standard/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
Inj. Vol.:	1 µL pulsed splitless (hold 1.0 min)
Liner:	Topaz 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 to 320 °C at 7 °C/min (hold 3 min)
Carrier Gas	He, constant flow
Flow Rate:	1.2 mL/min

Detector

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:

Instrument

HP6890 GC & 5973 MSD

Notes

The EPA Method 525.3 UCMR4 standard analyte concentrations vary to simplify preparing ICAL levels based on the minimum method reporting levels.

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