Improve Semivolatiles Method Performance with Rxi-SVOCms Columns

• Ensure accuracy and sensitivity with good peak shape, response, and resolution.
• Highly inert, ultra-low bleed column provides excellent results for active compounds at trace levels.
• Increase productivity with stable calibrations and consistent column-to-column performance.

Semivolatiles methods are essential parts of environmental testing programs, yet they can be difficult for labs to run efficiently because target analyte lists are extensive, and they contain different types of reactive compounds. To accurately report semivolatiles, particularly reactive ones, highly inert columns must be used to ensure good chromatography and stable calibrations. Rxi-SVOCms columns, which are designed specifically for semivolatiles analysis, feature optimized selectivity, exceptional inertness, and very low bleed, characteristics that result in improved analytical performance and increased lab productivity.

As shown below, good peak shapes and responses are obtained for a diverse array of reactive compounds, including acidic phenols (pentachlorophenol and dinitrophenol) and amines (benzidine and pyridine), analytes that are typically problematic in semivolatiles methods. Split injection is used here and recommended because it minimizes the accumulation of active sites created by matrix components during actual sample analysis. Because the Rxi-SVOCms column is so inert, tailing is minimized, which improves peak shape and response, making accurate integration easy and reliable. Better chromatographic performance improves sensitivity and reproducibility, so calibrations pass for longer periods of time, and more samples can be analyzed before recalibration is needed.

In addition to improved performance for both basic and acidic reactive compounds, excellent resolution is seen for the neutral polycyclic aromatic hydrocarbons (PAH) that are most troublesome in semivolatiles methods. Critical pairs, such as indeno[1,2,3-cd]pyrene and dibenz[a,h]anthracene as well as benzo[b]fluoranthene and benzo[k]fluoranthene, are well resolved on the Rxi-SVOCms column, allowing for positive identification and accurate reporting. Consistent, high-quality chromatography makes using Rxi-SVOCms columns an effective way for labs to improve the performance of semivolatiles methods.

	Peaks	tR (min)
1.	(IS) 1,4-Dioxane-d8	2.30
2.	1,4-Dioxane	2.32
3.	N-Nitrosodimethylamine	2.52
4.	Pyridine	2.56
5.	Ethyl methacrylate	2.85
6.	2-Picoline	3.10
7.	N-Nitrosomethylethylamine	3.16
8.	Methyl methanesulfonate	3.42
9.	(SS) 2-Fluorophenol	3.56
10.	N-Nitrosodiethylamine	3.77
11.	Ethyl methanesulfonate	4.04
12.	Benzaldehyde	4.38
13.	(SS) Phenol-d6	4.42
14.	Phenol	4.44
15.	Aniline	4.48
16.	Bis(2-chloroethyl) ether	4.54
17.	Pentachloroethane	4.54
18.	2-Chlorophenol	4.60
19.	1,3-Dichlorobenzene	4.77
20.	(IS) 1,4-Dichlorobenzene-D4	4.83
21.	1,4-Dichlorobenzene	4.85
22.	Benzyl alcohol	4.96
23.	1,2-Dichlorobenzene	5.01
24.	2-Methylphenol	5.08
25.	Bis(2-chloroisopropyl)ether	5.12
26.	Nitrosopyrrolidine	5.22
27.	4-Methylphenol	5.24
28.	3-Methylphenol	5.24
29.	N-Nitrosodi-N-propylamine	5.25
30.	Acetophenone	5.25
31.	4-Nitrosomorpholine	5.27
32.	o-Toluidine	5.29
33.	Hexachloroethane	5.37
34.	(SS) Nitrobenzene-D5	5.42
35.	Nitrobenzene	5.44
36.	N-Nitrosopiperidine	5.60
37.	Isophorone	5.71
38.	2-Nitrophenol	5.80
39.	2,4-Dimethylphenol	5.85
40.	Benzoic acid	5.91
41.	Bis(2-chloroethoxy)methane	5.96
42.	2,4-Dichlorophenol	6.07
43.	1,2,4-Trichlorobenzene	6.18
44.	(IS) Naphthalene-D8	6.24
45.	Naphthalene	6.27
46.	4-Chloroaniline	6.33
47.	2,6-Dichlorophenol	6.34

	Peaks	tR (min)
48.	Hexachloropropene	6.37
49.	Hexachlorobutadiene	6.42
50.	α,α-Dimethylphenethylamine	6.43
51.	Caprolactam	6.71
52.	N-Nitroso-N-butylamine	6.74
53.	4-Chloro-3-methylphenol	6.91
54.	Isosafrole	6.99
55.	2-Methylnaphthalene	7.09
56.	1-Methylnaphthalene	7.21
57.	Hexachlorocyclopentadiene	7.28
58.	1,2,4,5-Tetrachlorobenzene	7.29
59.	Isosafrole	7.34
60.	2,4,6-Trichlorophenol	7.43
61.	2,4,5-Trichlorophenol	7.47
62.	(SS) 2-Fluorobiphenyl	7.54
63.	Safrole	7.62
64.	Biphenyl	7.65
65.	2-Chloronaphthalene	7.67
66.	1-Chloronaphthalene	7.70
67.	Diphenyl ether	7.79
68.	2-Nitroaniline	7.79
69.	1,4-Naphthoquinone	7.88
70.	1,2-Dinitrobenzene	7.97
71.	Dimethyl phthalate	8.03
72.	1,3-Dinitrobenzene	8.05
73.	2,6-Dinitrotoluene	8.10
74.	1,4-Dinitrobenzene	8.15
75.	Acenaphthylene	8.17
76.	3-Nitroaniline	8.29
77.	(IS) Acenaphthene-d10	8.35
78.	Acenaphthene	8.39
79.	2,4-Dinitrophenol	8.42
80.	4-Nitrophenol	8.50
81.	Pentachlorobenzene	8.55
82.	2,4-Dinitrotoluene	8.58
83.	Dibenzofuran	8.60
84.	1-Naphthalamine	8.69
85.	2,3,5,6-Tetrachlorophenol	8.69
86.	2,3,4,6-Tetrachlorophenol	8.75
87.	2-Naphthalamine	8.79
88.	Diethyl phthalate	8.90
89.	Fluorene	9.01
90.	4-Chlorophenyl phenyl ether	9.03
91.	2-Methyl-5-nitroaniline	9.03
92.	4-Nitroaniline	9.03
93.	4,6-Dinitro-2-methylphenol	9.08
94.	N-Nitrosodiphenylamine	9.17

	Peaks	tR (min)
95.	N,N-Diphenylhydrazine	9.22
96.	(SS) 2,4,6-Tribromophenol	9.30
97.	1,3,5-Trinitrobenzene	9.49
98.	Diallate	9.54
99.	Phenacetin	9.55
100.	4-Bromophenyl phenyl ether	9.62
101.	Hexachlorobenzene	9.69
102.	Atrazine	9.83
103.	Pentachlorophenol	9.93
104.	4-Aminobiphenyl	9.94
105.	Pentachloronitrobenzene	9.94
106.	Propyzamide	10.03
107.	(IS) Phenanthrene-D10	10.16
108.	Phenanthrene	10.19
109.	Anthracene	10.25
110.	Carbazole	10.45
111.	di-n-Butyl phthalate	10.91
112.	4-Nitroquinoline 1-oxide	11.13
113.	Isodrin	11.46
114.	Fluoranthene	11.64
115.	Benzidine	11.82
116.	(SS) Pyrene-D10	11.90
117.	Pyrene	11.92
118.	(SS) p-Terphenyl-d14	12.13
119.	Aramite-1	12.13
120.	Aramite-2	12.22
121.	Dimethylaminoazobenzene	12.31
122.	4,4'-Dichlorobenzilate	12.37
123.	3,3'-Dimethylbenzidine	12.72
124.	Butyl benzyl phthalate	12.75
125.	Kepone	12.77
126.	Bis(2-ethylhexyl) adipate	12.88
127.	2-(Acetylamino)fluorene	13.04
128.	3,3'-Dichlorobenzidine	13.43
129.	Benz[a]anthracene	13.46
130.	(IS) Chrysene-D12	13.47
131.	Chrysene	13.51
132.	Bis(2-ethylhexyl) phthalate	13.56
133.	Di-n-octyl phthalate	14.58
134.	Benzo[b]fluoranthene	15.14
135.	7,12-Dimethylbenzo[a]anthracene	15.14
136.	Benzo[k]fluoranthene	15.19
137.	Benzo[a]pyrene	15.70
138.	(IS) Perylene-D12	15.80
139.	3-Methylcholanthrene	16.35
140.	Dibenz[a,j]acridine	17.46
141.	Indeno[1,2,3-cd]pyrene	17.78
142.	Dibenz[a,h]anthracene	17.84
143.	Benzo[ghi]perylene	18.27

Column	Rxi-SVOCms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 16623)
Standard/Sample	Revised SV internal standard mix (cat.# 31886)
	Revised B/N surrogate mix (cat.# 31888)
	Acid surrogate mix (cat.# 31063)
	8270 MegaMix standard (cat.# 31850)
	8270 Benzidines mix (cat.# 31852)
	Benzoic acid (cat.# 31879)
	Appendix IX mix #1, Revised (cat.# 32459)
	Appendix IX mix #2 (cat.# 31806)
Diluent:	Dichloromethane
Conc.:	20 ng/µL
Injection
Inj. Vol.:	1 µL split (split ratio 10:1)
Liner:	Topaz 4.0 mm ID single taper inlet liner with wool (cat.# 23303)
Inj. Temp.:	250 °C
Split Vent Flow Rate:	12 mL/min
Oven
Oven Temp.:	40 °C (hold 0.5 min) to 280 °C at 20 °C/min to 330 °C at 6 °C/min (hold 4 min)
Carrier Gas	He, constant flow
Flow Rate:	1.2 mL/min

Detector	MS
Mode:	Scan
Scan Program:
Group Start Time (min) Scan Range (amu) Scan Rate (scans/sec) 1 1.55 35-550 5.4
Transfer Line Temp.:	280 °C
Analyzer Type:	Quadrupole
Source Type:	Extractor
Extractor Lens:	6 mm ID
Source Temp.:	330 °C
Quad Temp.:	150 °C
Electron Energy:	70 eV
Solvent Delay Time:	1.55 min
Tune Type:	DFTPP
Ionization Mode:	EI
Instrument	Agilent 7890B GC & 5977A MSD
Sample Preparation	Samples were aliquoted into amber 2 mL, 9 mm short-cap, screw-thread vials (cat.# 21143) containing glass Big Mouth inserts (cat.# 21782) and sealed with 2.0 mL, 9 mm short-cap, screw-vial closures (cat.# 23842).

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