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Simultaneous analysis of 10 trihalomethanes at nanogram per liter levels in water using solid-phase microextraction and gas chromatography mass-spectrometry.

Journal of chromatography. A (2012-04-13)
Sebastien Allard, Jeffrey W A Charrois, Cynthia A Joll, Anna Heitz
ABSTRACT

Trihalomethanes are predominantly formed during disinfection of water via reactions of the oxidant with natural organic matter. Even though chlorinated and brominated trihalomethanes are the most widespread organic contaminants in drinking water, when iodide is present in raw water iodinated trihalomethanes can also be formed. The formation of iodinated trihalomethanes can lead to taste and odor problems and is a potential health concern since they have been reported to be more toxic than their brominated or chlorinated analogs. Currently, there is no published standard analytical method for I-THMs in water. The analysis of 10 trihalomethanes in water samples in a single run is challenging because the iodinated trihalomethanes are found at very low concentrations (ng/L range), while the regulated chlorinated and brominated trihalomethanes are present at much higher concentrations (above μg/L). An automated headspace solid-phase microextraction technique, with a programmed temperature vaporizer inlet coupled with gas chromatography-mass spectrometry, was developed for routine analysis of 10 trihalomethanes i.e. bromo-, chloro- and iodo-trihalomethanes in water samples. The carboxen/polydimethylsiloxane/divinylbenzene fiber was found to be the most suitable. The optimization, linearity range, accuracy and precision of the method are discussed. The limits of detection range from 1 ng/L to 20 ng/L for iodoform and chloroform, respectively. Matrix effects in treated groundwater, surfacewater, seawater, and secondary wastewater were investigated and it was shown that the method is suitable for the analysis of trace levels of iodinated trihalomethanes in a wide range of waters. The method developed in the present study has the advantage of being rapid, simple and sensitive. A survey conducted throughout various process stages in an advanced water recycling plant showed the presence of iodinated trihalomethanes at ng/L levels.

MATERIALS
Product Number
Brand
Product Description

Supelco
Tenax® TA / Carboxen® 1018, glass TD tube, preconditioned, O.D. × L 1/4  in. × 3 1/2  in., Sealed with (Swagelok® End-Fittings), pkg of 10 ea
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Sigma-Aldrich
Iodoform, 99%
Supelco
ORBO 78 HBr on Carboxen® 564 specially cleaned (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
ORBO 90 Carboxen® 564 (20/45), 160/80 mg, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 563, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: (300 mg), cartridge volume 3 mL, pkg of 10 ea
Supelco
ORBO-93 Sorbent Tube, matrix Carboxen® 1000, ORBO tube I.D. × L 6 mm × 95 mm, Bed B 90 mg, Bed A 180 mg, 60/80 mesh, pkg of 25 ea
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), for use with manual holder, needle size 24 ga
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
Carboxen® 569, O.D. × L 1/4  in. × 3 1/2 , glass TD tube, fritted, Sealed with Brass Endcaps, preconditioned, pkg of 10 ea
Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), needle size 23 ga, for use with manual holder
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with manual holder/autosampler
Supelco
Carboxen® 569, glass TD tube, fritted, O.D. × L 1/4  in. × 3 1/2  in., preconditioned, pkg of 10 ea
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, pack of 144 × 290 mg
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), needle size 24 ga, for use with autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm (CAR/PDMS), needle size 23 ga, for use with autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder/autosampler, fiber L 2 cm