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Combination Run of U.S. EPA Methods 521 and 522, Nitrosamines and 1,4-Dioxane, on Rxi®-5Sil-MS by CSR-LVSI

PeaksConc.
(ng/mL)
1.Tetrahydrofuran-d8 (IS) 100
2.Tetrahydrofuran50
3.1,4-Dioxane-d8 (SS) 200
4.1,4-Dioxane50
5.N-Nitrosodimethylamine-d6 (SS) 20
6.N-Nitrosodimethylamine2.5
7.N-Nitrosomethylethylamine5.0
PeaksConc.
(ng/mL)
8.N-Nitrosodiethylamine5.0
9.N-Nitrosodi-n-propylamine-d14 (IS) 10
10.N-Nitrosopyrrolidine5.0
11.N-Nitrosodi-n-propylamine5.0
12.N-Nitrosomorpholine2.5
13.N-Nitrosopiperidine5.0
14.N-Nitrosodi-n-butylamine5.0
image
GC_EV1334
ColumnRxi®-5Sil MS, 30 m, 0.25 mm ID, 1.00 µm (cat.# 13653)
using Rxi® guard column 10 m, 0.53 mm ID (cat.# 10073)
with SGE® µ-union
SampleN-Nitrosodimethylamine-d6 (cat.# 33910)
1,4-Dioxane-d8 (cat.# 30614)
N-Nitrosodi-n-propylamine-d14 (cat.# 33911)
Tetrahydrofuran-d8 (cat.# 30112)
Nitrosamine calibration mix, Method 521 (cat.# 31898)
Appendix IX mix #1, revised (cat.# 32459)
Diluent:Dichloromethane
Injection
Inj. Vol.:50 µL splitless (hold 1.5 min)
Liner:Custom Premium single taper 4 mm ID liner with 15 mg quartz wool
Inj. Temp.:275 °C
Purge Flow:100 mL/min
Oven
Oven Temp.:35 °C (hold 1.5 min) to 50 °C at 50 °C/min (hold 7.1 min) to 320 °C at 11.12 °C/min (hold 1.5 min)
Carrier GasHe, flow program
Flow Program:5.08 mL/min (hold 8.9 min) to 2.0 mL/min at 1.0 mL/min/min
DetectorMS
Mode:SIM
SIM Program:
GroupStart Time
(min)
Ion(s) (m/z)Dwell (ms)
19.942, 46, 71, 72, 78, 80 20
210.558, 62, 64, 88, 96 20
311.242, 43, 46, 48, 74, 80 20
41243, 56, 88, 102 30
515.558, 68, 70, 78, 86, 100, 116, 130, 144 20
617.484, 99, 114, 116, 141, 158 20
Transfer Line Temp.:320 °C
Analyzer Type:Quadrupole
Source Temp.:230 °C
Quad Temp.:150 °C
Solvent Delay Time:9.9 min
Tune Type:BFB
Ionization Mode:EI
InstrumentAgilent 7890A GC & 5975C MSD
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