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Summary
Concurrent solvent recondensation–large
volume splitless injection (CSR-LVSI) with
an unmodified Agilent-style split/splitless
GC inlet is a viable approach for analyzing
1,4-dioxane in drinking water. While large
volume injection usually involves special-
ized equipment, using it with a completely
unmodified inlet provides a cost-effective
way to meet ever decreasing detection limits.
For the complete version of this technical
article, visit
Figure 1: 1,4-Dioxane extracted ion chromatogram from a 10 µL CSR-LVSI of a 0.5 pg/µL
fortified drinking water extract (5 pg on-column). Note that the 1,4-dioxane quantifica-
tion ion (m/z 88) and confirmation ion (m/z 58) are fully separated from matrix interfer-
ences and good peak responses were obtained.
6.00 6.20 6.40 6.60
5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80 7.00
Time (min)
7.20 7.40 7.60 7.80 8.00 8.20 8.40
1
2
3 5
4
4
m/z 88.00
m/z 58.00
EIC
GC_EV1263
Peaks
1. Tetrahydrofuran-d8 (IS)
2. Co-extracted material
3. 1,4-Dioxane-d8 (SS)
4. 1,4-Dioxane
5. Co-extracted material
Figure 2: 1,4-Dioxane extracted ion chromatogram from a standard splitless 1 µL injection
of a 0.5 pg/µL fortified drinking water extract (0.5 pg on-column). Peaks are barely distin-
guishable from background noise.
5.20 5.40 5.60 5.80 6.00 6.20
3
5.10
Time (min)
m/z 88.00
m/z 58.00
EIC
3.60 3.80 4.00 4.20 4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80 7.00 7.20 7.40 7.60 7.80 8.00 8.20 8.40
GC_EV1264
• Signal-to-noise = 16 (m/z 88)
• Baseline separation from
matrix interferences
Standard splitless injection
produces poor response.
Matrix Fortified Sample
Conc. (µg/L)
Volume of Sample
Extracted (L)
Theoretical Extract
Conc. (pg/µL)
Recovery
(pg/µL)
1,4-Dioxane
% Recovery
Surrogate
% Recovery
Bottled drinking
water 0.0050 1.0 0.50 0.40 80 125
Bottled drinking
water 0.20 0.50 10 9.2 92 102
Bottled drinking
water 0.20 1.0 20 18 87 96
Reagent water 0.020 0.50 1.0 1.0 100 88
Reagent water 0.20 0.50 10 8.4 84 92
Reagent water 0.0 0.50 0.0 - - 86
Table II: CSR-LVSI resulted in good recovery of both 1,4-dioxane and surrogate
1,4-dioxane-d8 from extracted fortified samples. Restek Recommends
Our CSR-LVSI setup:
Rxi®-624Sil MS Columns &
Rxi® Retention Gaps
Press-Tight® Connectors
Sky™ Inlet Liners
Instrument Setup for CSR-LVSI:
Column:
Rxi®-624Sil MS, 30 m, 0.25 mm ID, 1.40 μm (cat.# 13868) usingRxi®
guardcolumn5m,0.25mm ID(cat.#10029)withuniversalangledPress-
Tight®connectors(cat.#20446-261)
Sample:
Extractof drinking water fortified at 0.5 pg/µL with 1,4-dioxane
(cat.# 30287) and at 10 pg/µL with internal standard tetrahydro-
furan-d8 (cat.# 30112) and surrogate standard 1,4-dioxane-d8
(cat.# 30614)
Injection:
10 μL splitless (hold 1 min); Liner: Sky™ 4 mm single taper w/wool
(cat.# 23303.5); Inj. Temp.: 120 °C; Purge Flow: 80 mL/min
Oven:
35 °C (hold 1 min) to 120 °C at 12 °C/min (hold 1 min)
Carrier Gas:
He,constantflow,1.4mL/min;LinearVelocity:30.556cm/sec@35°C
Detector:
MS, SIM mode
For complete conditions and SIM program, visit
and enter GC_EV1263 in the search.
1,4-dioxane
References
[1] U.S. EPA, Unregulated Contaminant Monitoring
Rule 3.
ucmr/ucmr3/index.cfm (accessed March 2, 2012).
[2] P. Magni, T. Porzano, Concurrent Solvent
Recondensation Large Sample Volume
Splitless Injection, J. Sep. Sci. 26 (2003) 1491.
[3] Patent No: US 6,955,709 B2.
[4] P. Grimmett, J. Munch, Method Development for
the Analysis of 1,4-Dioxane in Drinking Water
Using Solid-Phase Extraction and Gas
Chromatography-Mass Spectrometry, J. of
Chromatographic Science 47 (2009) 31.