Title: Shimadzu Gas ChromatographECD from Matson Lab:
1Shimadzu Gas Chromatograph(ECD) from Matson Lab
(draft sketch by S.Hall from P. Brooks, 2/02)
ECD
Inject
Load
2
Inject
Vent
11
10
5CH4/Ar (60 psi) Oven (run temp) 70C Oven
(bake temp) 140C Detector temp 295C ECD
Current 1 mA Flow rates at tank GC? Oxy
Trap on Ar/CH4 line
12
9
13
1 mL sample loop
8
14
Vent
7
1
1 m 1/16 Haysep N
6
2
5
3
4
Plugged
Parts (All fittings and lines must be stainless
steel pressure flow controllers cannot be
plastic because of offgassing issues) M1/8 OR M
Shimadzu M to 1/8 fitting 1 SS-100-R-2
1/8F to 1/16 M (Oakland Valve and fitting) 2
SS-200-6-1 1/8 to 1/16 union 3 SS-100-6
1/16 to 1/16 union 4 Shimadzu 221-22910-72 5
SS-100-3 1/16 tee 6 SS-200-R-4 1/4 F to
1/8 male union 7 SS-200-6 1/8 M unions
2 m 1/16 Haysep Q
In Load mode Gas sample injected into port 2,
fills sample loop and excess is vented from port
12. Carrier flows three ways 1) directly into
ECD, 2) into port 9, through main Haysep N
column, into port 2, to port 3, and into ECD, and
3) into port 6, to port 7, through backflush
Haysep Q column, to port 14, to port 1, and
vent. In Inject mode When the valve is turned
to the dotted (inject) position, air injected in
port 11 is vented in port 12. Carrier gas goes
from port 9 to 10, pushing the sample through the
sample loop to port 13 and 14 and through the
backflush column (Haysep N). Here acetylene,
halogens, and water are held up on the backflush
(Haysep N) column, while O2, N2, and Ar move
rapidly through the main column (Haysep Q) column
to port 2 and vent through port 1 to the
atmosphere. Meanwhile CO2 and N2O pass from the
backflush (Haysep N) column through ports 7 and
8 and onto the Haysep Q column. In Backflush
(Load) mode At the point before acetylene,
halogens, and water appear on the main Haysep Q
column (and before N2O is vented),the valve is
turned back to the load position (solid lines).
CO2 and N2O are pushed through and separated on
the Haysep Q column by carrier gas coming from
ports 9 and 8, then they go through port 3 and
pass onto the ECD detector. Acetylene, halogens,
and water are pushed backward through the
backflush (Haysep N) column by carreir gas
coming from port 6 and they are vented through
port 1.
Sample Chromatograph (integrate by peak height
rather than peak area)