Journal of Chromatographic Science, Vol.

32, November 1994

Gas Chromatography Problem Solving and Troubleshooting

Question:

What is the best method to clean and deactivate injector liners?

Answer:

It is usually easier and more economical to replace an injector liner than to clean and deactivate one. Some liners have
complex inner surfaces, making them difficult to properly clean. The residues on most liners are high-molecular-weight
substances subjected to prolonged exposure to high temperatures. These residues adhere to the glass surfaces and will not
rinse off with solvents or become dislodged with ultrasonication. Harsh conditions are often necessary to remove the
residues. Unfortunately, these conditions also render the liner unsuitable for G C use without subsequent deactivation
(silylation). Eventually, all liners become active upon use and need to be deactivated or replaced.

If a rigorous liner cleaning is needed, the following method can be used. Place the liner in a clean tube or small glass
container (one that can be sealed is best). Cover the liner with 1Ν nitric or hydrochloric acid. Let the liner remain in the acid
solution for at least 8 hours. If the solution is highly discolored after 8 hours, repeat the process. Carefully remove the liner
from the acid solution and thoroughly rinse the liner with water and then methanol. Dry the liner at temperatures between
100-150°C. The liner must be silylated after an acid cleaning.

There are two techniques for silylating liners. The solution method is easier than the gas-phase method, but it is not as
good. The solution method involves placing the liner in a screw-cap test tube or small container. Cover the liner with 10%
trimethylchlorosilane or dimethyldichlorosilane in dry toluene. Seal the tube with a Teflon-lined cap. Let the liner remain in
the solution for at least 8 hours (longer times are not harmful). Carefully remove the liner from the solution and thoroughly
rinse with toluene and methanol. Dry the liner in an oven between 100-150°C.

The gas-phase method involves placing the liner in a glass test tube that can be easily flame-sealed. Heat the neck of the
tube until only a 2-3-mm opening remains. Add 2-3 drops of diphenyltetramethyldisilazane to the tube. Immediately flush
the tube with dry nitrogen, then flame-seal the tube. Caution should be exercised because the disilazane is flammable. Heat
the tube for at least 3 hours at 300°C. After cooling to room temperature, open the tube in a hood and thoroughly rinse the
liner with hexane or pentane. If desired, the liners can be stored in the sealed tubes until needed.

Numerous liners can be simultaneously cleaned and silylated with either method. After silylation, the liners can be stored
for future use. This may make cleaning and deactivating liners more reasonable than replacing them, especially if liners are
frequently changed and discarded.

The purpose of Chromatography Problem Solving and Troubleshooting is to have selected experts answer chromatographic questions
in any of the various separation fields (GC, GC-MS, HPLC, TLC, SFC, HPTLC, open column, etc.). If you have questions or problems that
you would like answered, please forward these to the Journal editorial office with all pertinent details: instrument operating conditions,
temperatures, pressures, columns, support materials, liquid phases, carrier gas, mobile phases, detectors, example chromatograms, etc. In
addition, if you would like to share your expertise or experience in the form of a particular question accompanied by the answer, please
forward to JCS Associate Editor, Chromatography Problem Solving and Troubleshooting, P.O. Box 48312, Niles, IL 60714. All
questions/answers are reviewed to ensure completeness. The Journal reserves the right not to publish submitted questions/answers.
Dean Rood
Associate Editor

523