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2007 vol. 4
Tech Tip
WarmUp Before You Run
Why conditioning your inlet parts after maintenance is good practice
By Scott Grossman, GC Accessories Chemist
• Eliminate background peaks and avoid
costly reanalysis.
• Improve reproducibility and system
performance.
• Demonstrate system cleanliness.
Every good coach tells athletes to warmup before
they run to make sure the body is primed for opti-
mum performance. The same principle applies to
maintaining your gas chromatograph—time spent
warming up the analytical system after mainte-
nance pays big dividends by improving accuracy
and reducing the need for reanalysis. No matter
whose products you purchase, inlet parts, just like
columns, require a brief conditioning before they
are ready for analytical work. Although it is tempt-
ing to save time by jumping directly into sample
analysis after maintenance, warming up your system
helps you ensure accurate results the first time. In
this article, we will highlight inlet liners as a perfect
example of the need to condition your inlet after
maintenance to avoid costly coelutions, irrepro-
ducible results, and avoidable reanalysis.
Sources of Contamination
Even the best liner can exhibit a small bleed pat-
tern if it is used immediately after installation.
Common sources of contaminants that can cause
bleed include plastic packaging (e.g. phthalates
used to make plastics more flexible) and fatty acids
from finger oils. To evaluate bleed from contami-
nated liners, we first established a clean baseline
with a control liner, then installed a test liner, and
ran the instrument without making an injection.
Figure 1 illustrates the effect of handling an inlet
liner with bare hands. Even some gloves will
impart hydrocarbon contamination that can be
very prominent and persistent (Figure 2). So, care
needs to be taken when handling your new liners.
Handling liners with clean forceps or lint-free
technical wipes is a good way to prevent liner
contamination.
Reduce Noise by Conditioning Your System
This contamination, also called background
“noise,” can be eliminated simply by conditioning
the GC system prior to use. You can condition the
entire inlet a variety of ways. One suggestion is to
make a few preliminary runs using the analytical
method parameters (inlet temperature, oven pro-
gram, etc.) to be used in the subsequent analyses.
We evaluated several commercially available liners
and determined that liner bleed generally will be
gone by the second or third run (Figure 3). An
Figure 2
Hydrocarbon peaks from nitrile gloves are another
example of contamination from maintenance activities that can
be eliminated by warming up the system.
Column:
Rxi
®
-5ms, 30m, 0.32mm, 0.25µm (cat.# 13424)
Sample:
no sample injected; instrument ran the method conditions with no injection.
Inj.:
no injection; splitless mode (hold 0.5 min., split flow 40mL/min.)
4mm single gooseneck liner with wool, IP deactivated (cat.# 22406).
Inj. temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
5.0mL/min.
Oven temp.:
50°C (hold 5 min.) to 320°C @ 30°C/min. (hold 10 min.)
Det.:
FID @ 330°C
GC_EX00955
Figure 1
Eliminate contamination peaks from finger oils by
warming up the system prior to sample analysis.
First Analysis
Second Analysis
Column:
Rxi
®
-5ms, 30m, 0.32mm, 0.25µm (cat.# 13424)
Sample:
no sample injected; instrument ran the method conditions with no injection.
Inj.:
no injection; splitless mode (hold 0.5 min., split flow 40mL/min.)
4mm split with wool inlet liner, IP deactivated (cat.# 20782).
Inj. temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
5.0mL/min.
Oven temp.:
50°C (hold 5 min.) to 320°C @ 30°C/min. (hold 10 min.)
Det.:
FID @ 330°C
GC_EX00956