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Analysis of odorous trichlorobromophenols in water by in-sample derivatization/solid-phase microextraction GC/MS.

Analytical and bioanalytical chemistry (2006-08-10)
Alfredo Díaz, Francesc Ventura, Maria Teresa Galceran
ABSTRACT

The simultaneous determination of several odorous trichlorobromophenols in water has been carried out by an in-sample derivatization headspace solid-phase microextraction method (HS-SPME). The analytical procedure involved their derivatization to methyl ethers with dimethyl sulfate/NaOH and further HS-SPME and gas chromatography-mass spectrometry (GC/MS) determination. Parameters affecting both the derivatization efficiency and headspace SPME procedures, such as the selection of the SPME fiber coating, derivatization-extraction time and temperature, were studied. The commercially available polydimethylsiloxane (PDMS) 100 microm and Carboxen-polydimethylsiloxane-divinylbenzene (CAR-PDMS-DVB) fibers appeared to be the most suitable for the simultaneous determination of these compounds. The precision of the HS-SPME/GC/MS method gave good relative standard deviations (RSDs) run-to-run between 9% and 19% for most of them, except for 2,5-diCl-6-Br-phenol, 2,6-diCl-3-Br-phenol and-2,3,6-triBr-phenol (22%, 25% and 23%, respectively). The method was linear over two orders of magnitude, and detection limits were compound dependent but ranged from 0.22 ng/l to 0.95 ng/l. The results obtained for water samples using the proposed SPME procedure were compared with those found with the EPA 625 method, and good agreement was achieved. Therefore, the in-sample derivatization HS-SPME/GC/MS procedure here proposed is a suitable method for the simultaneous determination of odorous trichlorobromophenols in water.

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®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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® 1003, 40-60 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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® 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
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm (CAR/PDMS), needle size 24 ga, for use with manual holder, StableFlex fiber