Development of a headspace solid-phase microextraction procedure for the determination of free volatile fatty acids in waste waters.

Development of a headspace solid-phase microextraction procedure for the determination of free volatile fatty acids in waste waters.

Journal of chromatography. A (2000-04-11)

M Abalos, J M Bayon, J Pawliszyn

ABSTRACT

An analytical procedure based on headspace solid-phase microextraction (SPME) coupled to GC-flame ionization detection/Negative Chemical Ionization Mass Spectrometry has been developed for the determination of free volatile fatty acids (C2-C7) in waste water samples. Five different coatings have been evaluated and polydimethylsiloxane-Carboxen was the only fiber that allows a successful extraction of the shortest chain fatty acids (acetic and propionic). Several parameters such as extraction time and temperature, desorption conditions, agitation speed and sample volume have been optimized using the polydimethylsiloxane-Carboxen fiber. The linear dynamic range was over two-four orders of magnitude, depending on the acid. Procedural detection limits were in the low to medium microg/l levels and the RSDs were between 5.6% and 13.3%. To evaluate the applicability of the developed SPME procedure on real samples, fermented urban wastewaters were analysed.

MATERIALS

Product Number

Brand

Product Description

57912-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, Metal Alloy (1cm), needle size 23 ga, Autosampler, pk of, plain gray hub

57914-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, Metal Alloy (2cm), needle size 23 ga, Autosampler, pk of 1, plain gray hub

57906-U

Supelco

SPME Fiber Assembly, 85 μm CAR/PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, light blue hub

11072-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 572, 20-45 mesh, bottle of 10 g

57299-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub

57295-U

Supelco

SPME Fiber Assembly, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub

57319

Supelco

SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, black hub

57343-U

Supelco

SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, black hub

57344-U

Supelco

SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, black hub

10477-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1000, 40-60 mesh, bottle of 50 g

57335-U

Supelco

SPME Fiber Assembly, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, light blue hub

57328-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub

24241-U

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

11324-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 564, 20-45 mesh, pack of 144 × 290 mg

25461

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

25467

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

24246

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

10471

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1003, 40-60 mesh, bottle of 10 g

57348-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub

57329-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub

10269

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 569, 20-45 mesh, bottle of 10 g

57318

Supelco

SPME Fiber Assembly, 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub

57334-U

Supelco

SPME Fiber Assembly, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, light blue hub

10478-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1000, 60-80 mesh, bottle of 10 g

10263

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 563, 20-45 mesh, bottle of 10 g

10264

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 564, 20-45 mesh, bottle of 10 g

11048-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 569, 20-45 mesh, bottle of 500 g

54041-U

Supelco

Carboxen^® 1000 Reversible SPE Tube, 200 mg/mL, pk 30

57298-U

Supelco

SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub

23446-U

Supelco

ORBO^™-93 Sorbent Tube, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea