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Saturation of GC Detectors

This technical article discusses saturation of GC detectors. It can occur when the detector receives more analyte than it was designed to handle, overwhelming the physical or chemical processes involved in detection. Saturation causes nonlinear detector response and inaccurate analyte quantification at high concentrations. The article describes causes of saturation for different detector types and provides solutions like reducing the sample amount, optimizing detector parameters, or changing the jet size.

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Salman Abuzuhaira
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265 views2 pages

Saturation of GC Detectors

This technical article discusses saturation of GC detectors. It can occur when the detector receives more analyte than it was designed to handle, overwhelming the physical or chemical processes involved in detection. Saturation causes nonlinear detector response and inaccurate analyte quantification at high concentrations. The article describes causes of saturation for different detector types and provides solutions like reducing the sample amount, optimizing detector parameters, or changing the jet size.

Uploaded by

Salman Abuzuhaira
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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TECHNICAL ARTICLE

Saturation of GC Detectors
This technical article relates to the saturation of GC detectors. It addresses the causes of saturation, what effect saturation might have on analytical
results, how to know when it is happening, and how to avoid it.

Each style of GC detector will detect compounds based on some physical or    A detector becomes “saturated” if its increase in signal as a function of
chemical characteristic of the sample. In flame ionization detectors (FID), increasing amount of analyte is less than expected. Figures 2 and 3 illustrate
organic compounds are burned in an H2/air flame and form ions that are the roll off in response at the high end of a calibration curve as the detector
collected on a polarized electrode (the “collector”). Other detectors respond saturates. Each detector will have its own root cause(s) for saturation
in different ways, but the response always ends up as an amplified electrical depending on the underlying chemical and physical phenomena relating to
signal (which then is usually digitized and stored). its response. In the case of an FID, saturation usually results from the flame
   Every detector is designed for a specific intended use paradigm that becoming “starved”; it is no longer able to completely combust the large
involves all setpoint variables and physical design characteristics. Take the amount of analyte passing through it. This lack of complete combustion can
FID, for example. The primary source of signal is the efficient combustion be influenced by many variables such as limited fuel (H2) or oxidant (air),
of column effluent in a hydrogen flame, as illustrated in Figure 1. Column not enough pre-heat, inefficient mixing, etc. An extreme indication of poor
effluent is directed to the flame and mixed with H2 as it passes through mixing and insufficient combustion is when the flame self-extinguishes
a small orifice (the “jet”). In order to yield the theoretically 6-7 orders of when the solvent peak elutes. In many cases, increasing air and/or fuel
magnitude response that are possible with an FID, all the physical aspects flows and increasing detector temperature can yield another factor of
of the detector must work together. So, the dimensions of the detector, 5-10 of proportional detector response at the high end of the calibration
the orifice size, dimensions and position of the jet, the temperature profile, curve; however these changes would at the same time make LOD worse
the flow-rates of gases, electrical and electronics design, etc. — all (increasing noise).
these parameters are designed and specified for a “typical” use paradigm.    Poor mixing of column effluent with the H2 fuel prior to entering the
Saturation occurs when some of the actual parameters of use fall outside flame can happen if the jet dimensions are not well matched to the column
the normal operating range. flow (a bigger orifice is needed for higher column flows, especially if using
packed columns). In this case, a change in jet orifice size can help. Using too
big of a jet orifice when unnecessary, on the other hand, degrades LOD if
used with lower flow columns.
Figure 1

Figure 2

Figure 1: When an FID is operating correctly, sample components are


quantitatively combusted in the flame, creating positive ions and electrons.
The positive ions are attracted to the negatively biased collector while the Figure 2: Typical FID calibration curve in log(response) vs. log(amount)
(negatively charged) electrons are repelled toward the jet. showing detection limit and the onset of saturation at high concentrations.

www.sepscience.com
Figure 3
This technical article is produced in collaboration with Dr Matthew S. Klee,
internationally recognized for contributions to the theory and practice
of gas chromatography. His experience in chemical, pharmaceutical and
instrument companies spans over 30 years. During this time, Dr Klee’s
work has focused on elucidation and practical demonstration of the many
processes involved with GC analysis, with the ultimate goal of improving
the ease of use of GC systems, ruggedness of methods and overall quality of
results.

Figure 3: Alternate view of calibration curve in Response Factor format.

   ECDs saturate because of a combination of quenching and charging


effects. By diluting the effluent (adding more makeup gas), the saturation
point can be raised (again with worse LOD).
   NPDs saturate because the plasma at the surface of the bead is stripped
of essential Rb ions (it takes time for more to diffuse to the surface from the
bulk of the bead).
   A TCD might saturate because the concentration of analyte passing
through it exceeds the boundaries for which the electronics were designed.
And so on … each detector with its own characteristic manifestations of
overload.
   In addition to saturation from what happens within the detector, one can
also get saturation of the detector electronics. The amplifiers are designed
for a given range of signal. If the signal exceeds that, the signal is limited
(“clamped”) to the board’s maximum output. Some designs require that the
user set the “range” of the board. For example, the board might be designed
for 4 orders of magnitude response, but by setting the range you are able to
position the range to low, medium, or high signal levels depending on your
needs. If you set it to the most sensitive setting (low signal levels) and a big
peak comes through, its signal will “flat top” at the maximum value of the
electronics.
   You can easily tell if the saturation is electronic vs. physical/chemical
processes in the detector. With electronic saturation, the top of the peak is
flat (the numerical value of the signal is constant across the top of the peak)
with a very abrupt transition to the flat top at the edges. With chemical/
physical saturation, the top of the peak is distorted and noisy and has round
more gradual transitions at the edges.
   The bottom line is that if you need to analyze high concentrations of
components, you have to put less sample into the GC (inject less, split more,
dilute the sample) and/or adjust the detector parameters to accommodate
the higher load (more flame gases, higher temperature, dilute with more
makeup gas, change the jet size, etc.). If you do not, the concentration
of the saturated analyte will be under reported and the detector may
become contaminated, affecting results for other analytes and requiring
maintenance or repair.

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