Data Sheet DCP-2

Grace Davison Discovery Sciences

GC Packed Column Information

Preconditioning Instructions
To precondition a GC packed column, install the column to the The preconditioning should continue for 4-48 hours at the
injection port only. Do not attach the column to the detector desired temperature. Overnight conditioning is usually
port. Initiate a flow of carrier gas that would be normal for the sufficient, but for some phases and sensitive electron capture
column. (i.e. 25cc/min for 1/8" metal or 2mm i.d. glass; work, the full 48 hours may be necessary. Cool the column
50cc/min for 1/4" metal or 4mm i.d. glass). The carrier gas completely with carrier gas flowing. At this time the column can
should be free of moisture, oils and oxygen. We highly be connected to the detector for use.
recommend the use of the Alltech® Gas Purifier and Oxy-Trap™ If a column has been out of use for a while it should be
for this purpose. reconditioned briefly. This time, it can be connected to the
The preconditioning should proceed at room temperature for 30 detector. Purge with pure carrier gas for 30 minutes, then
minutes. You may then program (either automatically or program up to the desired temperature (carrier gas still flowing)
manually) to the desired temperature. The upper temperature and hold for 30 minutes to 2 hours before starting analysis.
should be 25°C lower than the upper temperature limit listed on Exception - Molecular Sieve columns should be
the column tag. Alternatively, for longer column life, condition at preconditioned for 4-16 hours at 300°C. If you have any
25°C above the maximum operating temperature used in your further questions regarding column handling, please call our
analysis as long as this doesn’t exceed the upper temperature Technical Support Department at 1-800-255-8324.
limit minus 25°C. For example, AT-1000 has an upper
temperature limit of 250°C. The maximum recommended
temperature for preconditioning is 225°C. If however, your
analysis will be conducted at 115°C, precondition at 140°C and
your column will last longer.

Troubleshooting Common Problems

Unresolved Peaks on a Column Which Worked Well in the Past

Possible Cause Possible Solution

1. Wrong column temperature. 1. Check and adjust temperature.
2. Wrong carrier gas flowrate. 2. Check and adjust flowrate.
3. Sample size too large. 3. Reduce sample size.
4. Poor injection technique (too slow). 4 Use a rapid, smooth injection technique.
5. Column contaminated or deteriorated. 5. Recondition column, repack first 6" of column, or replace column.

Tailing Peaks

Possible Cause Possible Solution

1. Active sample adsorbing on injection port, transfer 1. Use more inert system: Deactivated surfaces.
lines, column, or glass wool.
2. Column or injection port temperature too low. 2. Increase temperature (do not exceed maximum temperature for
column). Injection port should be 25°C greater than the highest
boiling point in sample.
3. Two compounds coeluting. 3. Increase sensitivity and reduce sample size. Lower temperature
10-20°C to resolve peaks.
4. Needle hitting packing in column inlet. 4. Remove some packing.
5. Column deteriorating. 5. Replace column.
6. Column contaminated. 6. Recondition.
Troubleshooting Common Problems Continued

Irregular or Unstable Baseline

Possible Cause Possible Solution
1. Column bleed or contamination. 1. Recondition column.
2. Contaminated detector or injection port. 2. Clean detector and/or injection port.
3. Carrier gas leak. 3. Change septum and check for column leaks.
4. Inconsistent carrier gas regulation. 4. Check carrier gas supply for sufficient pressure. Replace
tank if ≤500psig pressure.
5. Gas impurities or contaminated gas line. 5. Change gas tank, use gas purifiers, and clean metal tubing.
6. Gas flows not within minimum / maximum limits of 6. Measure flows and verify against manual specifications.
the instrumentation (including hydrogen and air on FID),
or poorly regulated flow.
7. Defective detector. 7. Troubleshoot detector.
8. Septum bleed. 8. Condition septum or replace septum.

Ghost Peaks
Possible Cause Possible Solution
1. Column adsorption and subsequent desorption of sample 1. Try more inert packing material.
2. Contaminated syringe 2. Try new syringe with clean solvent. If ghost peaks disappear,
clean syringes more thoroughly.
3. Adsorption in transfer line 3. Use glass-lined stainless steel for transfer lines.
4. Poor injection technique 4. Use rapid, smooth injection technique.

Retention Times Longer (or Shorter) on Same Column

Possible Cause Possible Solution
1. Column temperature too low or too high. 1. Check and adjust temperature.
2. Carrier gas flowrate too low or too high. 2. Measure flowrate with a properly calibrated source of
measurement atcolumn exit and adjust.
3. Septum or column leak. 3. Check and correct if needed.
4. Column contaminated or deteriorated. 4. Recondition column or replace column.
5. Sample overload. 5. Reduce sample size.
6. Recorder defect. 6. Check Recorder.

Fronting Peaks
Possible Cause Possible Solution
1. Column overload. 1. Decrease sample size.
2. Two components coeluting. 2. Decrease sample size, decrease temperature, and
increase sensitivity.
3. Sample condensation. 3. Check injection port and column temperatures. Increase
if necessary.
4. Sample decomposition. 4. Use inert system and deactivated packing.

Broad Solvent Peaks

Possible Cause Possible Solution
1. Dead volume in injection port. 1. Use smaller volume injection liner and/or on-column injection.
2. Using extremely dilute samples. 2. Adjust sample or decrease oven temperature to condense
solvent then program up.
3. Poor injection technique. 3. Use rapid, smooth injection techniques.
4. Injection port temperature too low. 4. Increase injection port temperature.
5. Sample solvent interacts with the detector. 5. Change sample solvent.
6. Sample solvent retained by column. 6. Change sample solvent.

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ALLTECH® is a trademark, registered in the United States and/or other countries, of Alltech Associates, Inc. OXY-TRAP™ 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. 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 2008 Alltech Associates, Inc. All rights reserved.

The information presented herein is derived from our testing and experience. It is offered for your consideration and verification. Since operating
conditions vary significantly, and are not under our control, we disclaim all warranties on the results that may be obtained from the use of our products.
Grace reserves the right to change prices and/or specifications without prior notification. Printed in the USA.