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Pages in this section: C42 C43 C44 C45 C46
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Applications - Thermal Desorption
C44
Scientific Instrument Services, Inc.
™
Phone: 908-788-5550
www.sisweb.com/catalog/08/C44
1. benzene
2. toluene
3. tetra chloro ethane
4. 2- Fluorocarboxaldehyde
5. ethyl benzene
6.00
7.00
8.00
9.00
10.00
11.00
12.00
13.00
200000
400000
600000
800000
1000000
1200000
1400000
1600000
1800000
2000000
2200000
2400000
2600000
2800000
3000000
0
Time
2
3
4
6
7
1
5
6. xylene
7. xylene
8. xylene
1. Diallyl Sulfide
2. 2,5 Dimethyl
Thiophene
3. Methyl,
Allyl Disulfide
4. P-Cymene
5.Diallyl Disulfide
1
2
5
5 : 0 0
1 0 : 0 0
1 5 : 0 0
2 0 : 0 0
2 5 : 0 0
3 0 : 0 0
3 5 : 0 0
0 . 0
0 . 5
1 . 0
4
3
Technique: Sampler Oven for Larger Solid Samples
Sample: 1.0 gram garlic was flushed with N
2
(50°C) in the sampler oven and the
eluted compounds trapped on a Tenax trap. Data courtesy CAFT, Rutgers University.
Thermal Desorption: Block temperature: 220°C, Purge flow:10.0 ml/min He,
Desorption time: 5.0 min. Initial column trap temperature: Injection Port Split: 10:1
Column: 60 meter x 0.32 mm I.D. DB-1, 0.25u film, -20°C to 280°C at 10°C /min.
Technique: Sampler Oven for Larger Solid Samples
Sample: 2.0 gram soil was flushed with N
2
(70°C) in the sampler oven and the
eluted compounds trapped on a Tenax trap.
Thermal Desorption: Block temperature: 220°C, Purge flow: 2.0 ml/min He,
Desorption time: 10.0 min. Initial column trap temperature: -40°C
Column: DB-5, 25 meter x 0.25 mm I.D., 0.25 u film, -40° to 280°C at 10°/min.
1. Hexanal
2. Methyl Pyrazine
3. 2-Pentyl Furan
4. Nonanal
1 .0
0 .5
0 .0
5 :00
10 :00
15 :00
20 :00
25 :00
30 :00
35 :00
40 :00
1
2
3
4
Technique: Sampler Oven for Larger Solid Samples
Sample: 10.0 gram corn meal was flushed with N
2
(160°C) in the sampler oven and the
eluted compounds trapped on a Tenax trap. Data courtesy CAFT, Rutgers University.
Thermal Desorption: Block temperature: 220°C, Purge flow:10.0 ml/min He,
Desorption time: 5.0 min. Initial column trap temperature: Injection Port Split: 10:1
Column: 60 meter x 0.32 mm I.D. DB-1, 0.25u film, -20° to 40°C at 10°/min., then to
280° at 4° / min.
Technique: Sampler Oven for Larger Solid Samples
Sample: 0.5 gram cherry wood was flushed with N
2
(70°C) in the sampler oven and the
eluted compounds trapped on a Tenax trap.
Thermal Desorption: Block temperature: 220°C, Purge flow:10.0 ml/min He,
Desorption time: 5.0 min. Initial column trap temperature: -40°C
Column: DB-5, 25 meter x 0.25 mm I.D., 0.25 u film, -40° to 280°C at 10°/min.,
3e+07
2.5e+07
2e+07
1.5e+07
1e+07
5000000
6.00
8.00
10.00
12.00
14.00
16.00
18.00
20.00
22.00
24.00
26.00
terpenes
sesqui
terpenes
Time
1. Alpha Creosol
2. toluene
1
2
Corn Meal
Garlic
Soil
Wood Sample
Sample Collection System
T
he Sample Collection System permits the analysis of
solid samples which are too large to fit inside the GLT
desorption tubes directly. For instance when analyzing for
residual concentrations in the ppm and ppb range, and for the
analysis of samples which contain appreciable concentrations of
water which would form ice plugs if desorbed directly into the GC
column. Samples from 0.5 to 50 grams in size are placed inside a
long glass tube between two glass wool plugs. The tube is insert-
ed into the Solid Sampler oven, which can be heated to any tem-
perature up to 250°C, depending on the boiling point of the residual
volatiles the analyst wishes to detect. Carrier gas is purged in one
end of the heated tube and a desorption tube packed with Tenax or
other suitable adsorbent resin is attached at the opposite end. The
packed desorption tube has been previously cleaned and condi-
tioned to remove any contaminants from the adsorbent resins. If
the sample contains appreciable amounts of water, an optional dry
purge or makeup gas may be added just before the desorption
tube. This gas prevents the saturation of the adsorbent packing
with water and helps purge the water from the adsorbent resin
(Tenax has a low affinity for water). Samples are normally purged
with high purity Nitrogen or Helium at flow rates of 10 to 60 ml/min
for 10 to 60 minutes. The oven temperature is normally maintained
at 50 to 80°C for most volatiles such as benzene and toluene but
can be raised to higher temperatures for higher molecular weight
compounds.
Dry Make Up
Gas Flow (Opitional)
Carrier Gas
Flow
Sample
Heater Block
GLT Desorption
Tube
with Tenax
S.S. Connector, 0.5" to
Desorption Tube
with Purge Gas Inlet
S.S. Connector, 0.5"
to 1/8" Swagelok
Sample for
Analysis
Quartz Wool
Plug
1/4" or 1/2" x 14" Long Glass Tube
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