Table 3
Summary of successful Gas Liquid Chromatographie Procedures
Pollutant Type and
Air Sample Volume
Collection and
Displacement Techniques
GLC Column Details
Detection Details
Notes
Group 2: Oils &
Solvent
(a) Simple hydrocarbons 25ß.
(b) Chlorinated
Hydrocarbons
10«.
Collected at atmospheric
temperature on to activated
carbon; transferred by
extraction with CS2.
As above but extracted with
hexane.
(i) 4 mm glass x 4-ft. long
packed 2% Silicone 30 on
Chromosorb W
(ii) 3 mm S.S. x 6-ft. long
packed with 0.5% NPG on
Chromosorb W
(iii) 3 mm Teflon x 2-ft. long
packed Porapak Q60/80 mesh
4 mm glass x 3-ft. long
packed Chromosorb 103
(porous polymer).
1 - Carrier 50 ml/min N2
70°C to 130°C programmed
5 C rise/min.
1 - Carrier 60 ml/min N2
at 100°C.
2 - Carrier mixed
50 ml/min N2 + 30 ml/min.
H
2 at 150°C.
16 peaks defined, identified
as Cg to C14 isomers
do.
4 marked peaks with good
characteristics for quantitative
identification.
5 components identified and
determined quantitatively.
Group 4:
(a) Sulphides lOOfi.
(b) Alkylamines 100«.
(c) Aldehydes 500ß.
Absorption on solid HgCl2
impregnated into fibre glass
discs, (i) regenerated into air
with hot HC1 and absorbed in
ethyl benzene.
Absorption into coned H2SO4
impregnated fibre glass discs,
released by alkali into methanol.
Absorption in 1% NaHSC>3
ana
"
direct injection through Solid
Na2C(>3 pre-column.
(i) and (ii)
3 mm Teflon x 2-ft. long
packed Porapak Q
80/100 mesh
(i) 3 - 50 ml/min. N
2 +
30 ml/min. H
2 at 120°C.
(ii) 1 - 80 ml/min. N
2 at
130°C.
3 mm S.S. x 6-ft. long packed
15% Carbowax 400, 2% TEP,
2% NaOH on Chromosorb W
3 mm Teflon x 6-ft. long packed
Porasil R.
1 - 60 ml/min. N
2 at 100 C.
1 - 5 0 ml/min. N
2 at 150 C.
Methane thiol & dimethyl
sulphide with traces ethanethiol. H
2 S also identified
and measured.
(ii) Only methanethiol
identified.
Trimethylamine with small
amounts of dimethylamine
and diethylamine.
3 peaks defined but only
butyraldehyde identified.
Notes:
Detector, 1 - Flame lonization, 2 - Election Capture, 3 - Flame Photometer. Two chromatographs were used, either tracor Mikrotek 220 or Phillips
4000.
NPG is Nonyl Polyglycol Sebacate; TEP is Tetra Ethylene Pentamine.
D.K.B. Thistlethwayte and E.E. Goleb
Summary of successful Gas Liquid Chromatographie Procedures
Pollutant Type and
Air Sample Volume
Collection and
Displacement Techniques
GLC Column Details
Detection Details
Notes
Group 2: Oils &
Solvent
(a) Simple hydrocarbons 25ß.
(b) Chlorinated
Hydrocarbons
10«.
Collected at atmospheric
temperature on to activated
carbon; transferred by
extraction with CS2.
As above but extracted with
hexane.
(i) 4 mm glass x 4-ft. long
packed 2% Silicone 30 on
Chromosorb W
(ii) 3 mm S.S. x 6-ft. long
packed with 0.5% NPG on
Chromosorb W
(iii) 3 mm Teflon x 2-ft. long
packed Porapak Q60/80 mesh
4 mm glass x 3-ft. long
packed Chromosorb 103
(porous polymer).
1 - Carrier 50 ml/min N2
70°C to 130°C programmed
5 C rise/min.
1 - Carrier 60 ml/min N2
at 100°C.
2 - Carrier mixed
50 ml/min N2 + 30 ml/min.
H
2 at 150°C.
16 peaks defined, identified
as Cg to C14 isomers
do.
4 marked peaks with good
characteristics for quantitative
identification.
5 components identified and
determined quantitatively.
Group 4:
(a) Sulphides lOOfi.
(b) Alkylamines 100«.
(c) Aldehydes 500ß.
Absorption on solid HgCl2
impregnated into fibre glass
discs, (i) regenerated into air
with hot HC1 and absorbed in
ethyl benzene.
Absorption into coned H2SO4
impregnated fibre glass discs,
released by alkali into methanol.
Absorption in 1% NaHSC>3
ana
"
direct injection through Solid
Na2C(>3 pre-column.
(i) and (ii)
3 mm Teflon x 2-ft. long
packed Porapak Q
80/100 mesh
(i) 3 - 50 ml/min. N
2 +
30 ml/min. H
2 at 120°C.
(ii) 1 - 80 ml/min. N
2 at
130°C.
3 mm S.S. x 6-ft. long packed
15% Carbowax 400, 2% TEP,
2% NaOH on Chromosorb W
3 mm Teflon x 6-ft. long packed
Porasil R.
1 - 60 ml/min. N
2 at 100 C.
1 - 5 0 ml/min. N
2 at 150 C.
Methane thiol & dimethyl
sulphide with traces ethanethiol. H
2 S also identified
and measured.
(ii) Only methanethiol
identified.
Trimethylamine with small
amounts of dimethylamine
and diethylamine.
3 peaks defined but only
butyraldehyde identified.
Notes:
Detector, 1 - Flame lonization, 2 - Election Capture, 3 - Flame Photometer. Two chromatographs were used, either tracor Mikrotek 220 or Phillips
4000.
NPG is Nonyl Polyglycol Sebacate; TEP is Tetra Ethylene Pentamine.
D.K.B. Thistlethwayte and E.E. Goleb