Accelerated Solvent Extraction of NIST SRM 1941b, Organics in Marine Sediment, on Rxi-PAH

	Peaks
1.	Naphthalene-d8
2.	Naphthalene
3.	2-Methylnaphthalene
4.	Biphenyl
5.	Acenaphthylene
6.	Acenaphthene-d10
7.	Acenaphthene
8.	Fluorene
9.	Dibenzothiophene
10.	Phenanthrene-d10
11.	Phenanthrene
12.	Anthracene
13.	4H-Cyclopenta[def]phenanthrene
14.	Fluoranthene
15.	Pyrene

	Peaks
16.	Benzo[c]fluorene
17.	Benzo[ghi]fluoranthene
18.	Benzo[c]phenanthrene
19.	Benz[a]anthracene
20.	Chrysene-d12
21.	Cyclopenta[cd]pyrene
22.	Triphenylene
23.	Chrysene
24.	5-Methylchrysene
25.	Benzo[b]fluoranthene
26.	Benzo[k]fluoranthene
27.	Benzo[j]fluoranthene
28.	Benzo[a]fluoranthene
29.	Benzo[e]pyrene
30.	Benzo[a]pyrene

	Peaks
31.	Perylene-d12
32.	Perylene
33.	Dibenzo[a,j]anthracene
34.	Dibenzo[a,c]anthracene
35.	Indeno[1,2,3-cd]pyrene
36.	Dibenz[a,h]anthracene
37.	Benzo[b]chrysene
38.	Picene
39.	Benzo[ghi]perylene
40.	Anthanthrene
41.	Dibenzo[b,k]fluoranthene
42.	Dibenzo[a,e]pyrene
43.	Coronene-d12
44.	Coronene
45.	Dibenzo[a,i]pyrene
46.	Dibenzo[a,h]pyrene

Injection
Column	Rxi-PAH, 60 m, 0.25 mm ID, 0.10 µm (cat.# 49317)
Sample	SV internal standard mix (cat.# 31206)
	Coronene-d12 (CIL DLM-2715)
	Benzo[a]pyrene-d12 (CIL DLM-258-0)
	Aromatics in toluene (NIST SRM-2260a)
	PAH native stock solution (Wellington PAH-STK-B)

Diluent:	Dichloromethane
Inj. Vol.:	1 µL split (split ratio 10:1)
Liner:	Premium 4 mm Precision liner w/wool (cat.# 23305.1)
Inj. Temp.:	275 °C
Split Vent Flow Rate:	19.5 mL/min
Oven
Oven Temp.:	110 °C (hold 1.6 min) to 210 °C at 24 °C/min to 295 °C at 1.9 °C/min to 350 °C at 3.7 °C/min (hold 6 min)
Carrier Gas	He, constant flow
Flow Rate:	1.95 mL/min

Detector

Mode:

SIM

SIM Program:

Group	Start Time (min)	Ion(s) (m/z)	Dwell (ms)
1	3.09	102.1, 108.1, 128.1, 136.2	40
2	5.69	115.1, 142.1	40
3	6.23	76.1, 141.1, 154.1, 156.2	40
4	6.95	75.6, 76.1, 91.1, 152.1, 153.1, 155.1, 162.2, 170.2	20
5	7.93	82.4, 165.1	40
6	9.19	139.1, 152.1, 160.2, 178.1, 184.1, 188.2	40
7	11.78	94.6, 165.1, 190.1, 192.1	40
8	14.19	101.1, 202.1	40
9	16.60	101.1, 202.1	40
10	18.49	92.1, 184.1	40
11	19.58	108, 216	40
12	22.3	196.1, 212.2	40
13	24.92	113.1, 226.1, 228.1	40
14	26.27	113.1, 114.0, 120.1, 226.1, 228.1, 240.1	40
15	28.75	154.1, 252.1	35
16	30.62	119.8, 242.2	40
17	35.29	126.1, 252.1	40
18	38.56	125.1, 252.1	40
19	39.23	126.1, 252.1	40
20	40.71	125.1, 126.1, 132.1, 252.1, 264.1	40
21	42.91	125, 132.2, 252.1, 264.1	40
22	44.35	252.1, 268.1	40
23	48.41	139.1, 139.5, 278.1, 279.1	40
24	52.13	139.1, 139.5, 278.1, 279.1	40
25	53.70	138.1, 139.1, 278.1	40
26	54.97	138.1, 276.1	40
27	55.92	138.1, 276.1	40
28	57.04	132.6, 267.1	40
29	59.69	151.0, 302.1	40
30	63.27	150, 151, 156.1, 300.1, 302.1, 312.1	40
31	64.78	151.0, 302.1	40

Transfer Line Temp.:

330 °C

Analyzer Type:

Quadrupole

Source Type:

Extractor

Extractor Lens:

9 mm ID

Source Temp.:

350 °C

Quad Temp.:

200 °C

Solvent Delay Time:

3 min

Tune Type:

DFTPP

Ionization Mode:

Instrument

Agilent 7890B GC & 5977A MSD

Notes

Performs the separation of two critical sets of isobars:
1. Cyclopenta[c,d]pyrene, triphenylene, and chrysene
2. Benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[j]fluoranthene

Download PDF