Professional Documents
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Instructions
GC
Capillary
Columns
M171c
Table Of Contents
! Warning!
1.0 GC Preparation . . . . . . . . . . . . . . . . . 3
2.0
3.0
4.0
5.0
6.0
Gas Purification . . . . . . . . . . . . . . . . . .
Injection Port . . . . . . . . . . . . . . . . . . . .
Detectors . . . . . . . . . . . . . . . . . . . . . .
Ferrule Selection . . . . . . . . . . . . . . . . . .
3
3
3
3
3
4
4
4
5
7.0
8.0
9.0
10.0
11.0
1.1
1.2
1.3
1.4
6
7
7
8
8
13.0 Storage . . . . . . . . . . . . . . . . . . . . . . 9
14.0 Troubleshooting Guide . . . . . . . . . . . 1011
1.0 GC Preparation
0.10mm
0.18mm
0.25mm
0.32mm
0.45mm
0.53mm
Ferrule i.d.
0.4mm
0.4mm
0.4mm
0.5mm
0.8mm
0.8mm
Slip the nut and then the ferrule over the injector end of the
capillary column and slide them 6 inches down the column. Then
cut off a two inch section of column from the injector end. This
eliminates the possibility that ferrule fragments have entered the
column.
The ends must be cut square, with none of the polyimide coating
projecting beyond the ends. Inspect the ends with a 20X magnifier
to make sure the cut is square. If the end is not square, make a
small scratch about 1-inch from the end with a diamond-tipped
or ceramic scriber. Hold the column between the thumb and
forefinger, one hand on either side of the scratch. Place the scratch
away from you and apply slight pressure with your thumbs. The
column should snap easily and cleanly. Avoid making any scratches
elsewhere on the column as this can cause your column to break.
Injection
Port
Nut
Ferrule
Nut
Capillary Column
For an FID, the column is usually inserted all the way to the tip of
the detector jet and then pulled back about 2mm. This distance is
close enough to prevent dead volume, but far enough away from
the jet that it prevents the column from being crushed against the
jet when the nut is tightened.
Detector
Nut
Ferrule
Nut
Capillary Column
AT-35, AT-35ms
Phase
AT-50
AT-210
AT-225
AT-WAX, EC-WAX,
AT-WAXms
AT-1701
AT-Pesticide
AT-502.2
AT-624
Drug 1,2,& 3
AT-Silar 90
AT-Silar 100
AT-Amine
AT-Amino Acid
AT-CAM
AT-1, EC-1
AT-1ht
AT-1ms
AT-2887
AT-3710
AT-Petro
AT-Sulfur
AT-5, EC-5
AT-5ms
AT-20, EC-20
Film Thickness
0.10-1.20m
1.50-2.50m
2.65-5.00m
0.10m
0.10-1.00m
1.20m
5.00m
0.50m
4.00m
0.10-1.20m
1.50-2.50m
2.65-5.00m
0.10-1.00m
0.25-0.75m
1.00-1.20m
Temperature
350C
330C
300C
380C
350C
350C
300C
350C
350C
350C
330C
300C
350C
320C
300C
AT-AquaWax
AT-AquaWax-DA
AT-1000, EC-1000
AT-FAME
AT-1301
Film Thickness
0.10m
0.25-0.50m
1.00-1.20m
2.00-2.65m
0.25m
0.50m
1.00m
0.15-0.50m
1.00-1.20m
0.15-0.30m
0.50-1.20m
0.10-0.40m
0.50-2.00m
2.50-5.00m
0.25m
0.25m
0.20-1.20m
0.25m
0.25m
1.00m
0.20-1.20m
0.25-0.60m
1.40-3.00m
1.40-3.00m
0.25-1.20m
0.25m
0.25m
0.25m
1.20m
0.25-1.00m
Temperature
350C
320C
300C
280C
325C
300C
280C
260C
240C
240C
220C
280C
260C
250C
260C
250C
250C
280C
280C
260C
280C
240C
270C
260C
330C
250C
250C
200C
350C
250C
FID/TCD
NPD
ECD
ELCD
MS
PID
u = L/t
The linear velocity should be adjusted to
20-25cm/sec for helium carrier gas by increasing or decreasing
the carrier gas head pressure. See Table 4 for approximate head
pressures for various lengths and internal diameters using helium
or hydrogen as the carrier gas.
Compound
methane
acetonitrile vapors
methylene chloride vapors
dichlorodifluoromethane vapors
air
ethylene
a
0.10mm
27psig
54psig
0.18mm
Column i.d.
0.25mm 0.32mm
0.45mm
0.53mm
Once it has been determined that the column has been installed
properly and the optimum linear velocity has been set, a test
probe mixture should be run to evaluate the performance of the
column and the system as a whole. This test should be repeated
periodically and a record kept to monitor column performance.
Table 5 contains a complete list of test mixes for Alltech capillary
columns.
Grob Mix
For AT-1, EC-1
For AT-5, AT-1701, EC-5, AT-20, EC-20,
AT-502.2
For AT-1000, EC-1000, AT-AquaWax-DA
For AT-WAX, EC-WAX, AT-AquaWax
For AT-225
For AT-624
For AT-50
For AT-35
For AT-35 (0.53)
Highest Polarity
Part No.
41761
441700
441701
AT-210
441704
441716
441705
441707
441708
441709
441710
AT-1701
AT-50
AT-35, AT-35ms
AT-20, EC-20
AT-1301
AT-5, EC-5, AT-5ms
AT-1, EC-1, AT-1ms, AT-1-ht
Lowest Polarity
Figure 5 Relative Stationery Phase Polarity
0.1m
10ng
20-30ng
30-40ng
50-70ng
80-100ng
100-120ng
Film Thickness
0.25m
0.5m
30-40ng
60-80ng
125-175ng
200-250ng
300-400ng
400-500ng
1.0m
50-70ng
100-200ng
100-150ng 250-350ng
175-250ng 400-500ng
250-350ng 600-800ng
400-500ng 800-1000ng
500-700ng 1000-1500ng
13.0 Storage
Always place the column on a clean, dirt-free surface, preferably
in the original shipping container, when not in use. All columns,
especially Carbowax and cyano-containing stationary phases,
should have their ends sealed to prevent oxidation. Oxidation can
show up as a noisy or rising baseline.
Possible Solution:
Possible Cause:
Possible Solution:
Possible Cause:
Possible Solution:
Defective syringe
Detector off or not functioning
Injection port temperature too low
Oven temperature too low
No carrier flow
Column broken
Fronting Peaks
Column overloaded
Two compounds co-eluting
Sample condensation
Sample decomposition
Tailing Peaks
Active sample adsorbing on injection
port liner or column
Column or injection port temperature too
low
Two compounds co-eluting
Column deteriorating
Column contaminated
Ghost Peaks
Possible Cause:
Possible Solution:
Possible Cause:
Possible Solution:
Replace liner. If that does not solve the problem remove 1-2 coils from the inlet end of the
column and reinstall.
Try new syringe with clean solvent. If ghost peaks disappear, clean syringes more thoroughly.
Lower injection amount.
Use rapid, smooth injection technique.
Possible Solution:
Possible Cause:
Possible Solution:
Replace liner. If that does not solve the problem, remove 1-2 coils from the inlet end of
the column and reinstall.
Clean detector and/or injection port.
Change septum and check for column leaks.
Check carrier gas supply for sufficient pressure. Replace tank if 500 psig pressure.
Change gas tank, use gas purifiers, and clean metal tubing.
Measure flows and verify against manual specifications.
Possible Solution:
11
Differences:
Construction:
Recommend For:
ALLTECH and HELIFLEX are trademarks, registered in the United States and/or other countries, of Alltech Associates, Inc. AT, EC, and ECONO-CAP are trademarks of Alltech Associates, Inc. AQUAWAX is a trademark of Alltech Associates, Inc. GRACE, and GRACE
DAVISON are trademarks, registered in the United States and/or other countries, of W. R. Grace & Co.-Conn. GRACE DAVISON DISCOVERY SCIENCES is a trademark of W. R. Grace & Co.-Conn. SILAR is a trademark of Silar Laboratories, Inc. CARBOWAX is a
trademark, registered in the United States and/or other countries, of Union Carbide Chemicals & Plastics Technology Corporation. VESPEL is a trademark, registered in the United States and/or other countries, of E. I. Du Pont De Nemours and Company. This trademark list has
been compiled using available published information as of the publication date of this brochure and may not accurately reflect current trademark ownership. Alltech Associates, Inc. is a wholly owned subsidiary of W. R. Grace & Co.-Conn. Grace Davison Discovery Sciences is a
product group of W. R. Grace & Co.-Conn., which now includes all product lines formerly sold under the Alltech brand. Copyright 2007 Alltech Associates, Inc. All rights reserved.