Determination of methanol in biodiesel by headspace solid phase microextraction.

Determination of methanol in biodiesel by headspace solid phase microextraction.

Bioresource technology (2007-11-27)

Maria C Paraschivescu, Earl G Alley, William T French, Rafael Hernandez, Kevin Armbrust

ABSTRACT

A new direct gas chromatography procedure (headspace solid phase microextraction) was developed for the quantitative determination of methanol in biodiesel. The analysis was performed by exposing a carboxen-polydimethylsiloxane SPME fiber assembly to the headspace of the biodiesel sample. The gas chromatography used a HP-5 capillary column and flame ionization detection. A polynomial relationship was observed between the methanol concentration and its peak area. This method showed good reproducibility (average relative standard deviation 7.06%) and recovery (average recovery 100.2%).

MATERIALS

Product Number

Brand

Product Description

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

57348-U

Supelco

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

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

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

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

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

57343-U

Supelco

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

10477-U

Supelco

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

25467

Supelco

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

10269

Supelco

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

10478-U

Supelco

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

25461

Supelco

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

10471

Supelco

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

24241-U

Supelco

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

24246

Supelco

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

57318

Supelco

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

57319

Supelco

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

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

11324-U

Supelco

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

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

54041-U

Supelco

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

11048-U

Supelco

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

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

54294-U

Supelco

Carboxen^® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea

20355

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

28718-U

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

20358

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)