<< Chapter < Page Chapter >> Page >

Detector

The detector senses a physicochemical property of the analyte and provides a response which is amplified and converted into an electronic signal to produce a chromatogram. Most of the detectors used in GC were invented specifically for this technique, except for the thermal conductivity detector (TCD) and the mass spectrometer. In total, approximately 60 detectors have been used in GC. Detectors that exhibit an enhanced response to certain analyte types are known as "selective detectors".

During the last 10 years there had been an increasing use of GC in combination with mass spectrometry (MS). The mass spectrometer has become a standard detector that allows for lower detection limits and does not require the separation of all components present in the sample. Mass spectroscopy is one of the types of detection that provides the most information with only micrograms of sample. Qualitative identification of unknown compounds as well as quantitative analysis of samples is possible using GC-MS. When GC is coupled to a mass spectrometer, the compounds that elute from the GC column are ionized by using electrons (EI, electron ionization) or a chemical reagent (CI, chemical ionization). Charged fragments are focused and accelerated into a mass analyzer: typically a quadrupole mass analyzer. Fragments with different mass to charge ratios will generate different signals, so any compound that produces ions within the mass range of the mass analyzer will be detected. Detection limits of 1-10 ng or even lower values (e.g., 10 pg) can be achieved selecting the appropriate scanning mode.

Sample preparation techniques

Derivatization

Gas chromatography is primarily used for the analysis of thermally stable volatile compounds. However, when dealing with non-volatile samples, chemical reactions can be performed on the sample to increase the volatility of the compounds. Compounds that contain functional groups such as OH, NH, CO 2 H, and SH are difficult to analyze by GC because they are not sufficiently volatile, can be too strongly attracted to the stationary phase or are thermally unstable. Most common derivatization reactions used for GC can be divided into three types:

  1. Silylation.
  2. Acylation.
  3. Alkylation&Esterification.

Samples are derivatized before being analyzed to:

  • Increase volatility and decrease polarity of the compound
  • Reduce thermal degradation
  • Increase sensitivity by incorporating functional groups that lead to higher detector signals
  • Improve separation and reduce tailing

Advantages and disadvantages

GC is the premier analytical technique for the separation of volatile compounds. Several features such as speed of analysis, ease of operation, excellent quantitative results, and moderate costs had helped GC to become one of the most popular techniques worldwide.

Advantages of gc

  • Due to its high efficiency, GC allows the separation of the components of complex mixtures in a reasonable time.
  • Accurate quantitation (usually sharp reproducible peaks are obtained)
  • Mature technique with many applications notes available for users.
  • Multiple detectors with high sensitivity (ppb) are available, which can also be used in series with a mass spectrometer since MS is a non-destructive technique.

Disadvantages of gc

  • Limited to thermally stable and volatile compounds.
  • Most GC detectors are destructive, except for MS.

Gas chromatography versus high performance liquid chromatography (hplc)

Unlike gas chromatography, which is unsuitable for nonvolatile and thermally fragile molecules, liquid chromatography can safely separate a very wide range of organic compounds, from small-molecule drug metabolites to peptides and proteins.

Relative advantages and disadvantages of GC versus HPLC.
GC HPLC
Sample must be volatile or derivatized previous to GC analysis Volatility is not important, however solubility in the mobile phase becomes critical for the analysis.
Most analytes have a molecular weight (MW) below 500 Da (due to volatility issues) There is no upper molecular weight limit as far as the sample can be dissolved in the appropriate mobile phase
Can be coupled to MS. Several mass spectral libraries are available if using electron ionization (e.g., (External Link) ) Methods must be adapted before using an MS detector (non-volatile buffers cannot be used)
Can be coupled to several detectors depending on the application For some detectors the solvent must be an issue. When changing detectors some methods will require prior modification

Bibliography

  • E. F. Barry, Columns for gas chromatography: performance and selection , Wiley-Interscience, Hoboken, NJ (2007)
  • L. S. Ettre, LCGC , 2001, 19 , 120.
  • D. Filmore, Industry Facts&Figures - American Chemical Society Publications . GC: Mature and moving forward. May, 2003.
  • R. L. Grob and E. F. Barry, Modern practice of gas chromatography , 4 th edition, Wiley-Interscience, Hoboken, N.J.(2004)
  • J. V. Hinshaw, LCG , 2013, 31 , 932.
  • A.T. James, Biochem. J. , 1952, 52 , 242.
  • A. T. James and A. J. P. Martin, Biochem. J. , 1952, 50 , 679.
  • A. T. James, A. J. P. Martin, and G. H. Smith, Biochem. J. , 1952, 52 , 238.
  • A. J. P. Martin and R. L. M Synge, Biochem. J. , 1941, 35 , 1358.
  • G. McMahon, Analytical Instrumentation: A Guide to Laboratory, Portable and Miniaturized Instruments , 1 st edition, Wiley, Hoboken, N.J (2007)
  • H. M. McNair, Basic gas chromatography , Wiley, New York (1998)
  • http://www.chromatographyonline.com/
  • Sigma Aldrich Brochure. Derivatization reagents for selective response and detection in complex matrices. 2011,Sigma-Aldrich Co. Available through http://www.sigmaaldrich.com

Questions & Answers

if three forces F1.f2 .f3 act at a point on a Cartesian plane in the daigram .....so if the question says write down the x and y components ..... I really don't understand
Syamthanda Reply
hey , can you please explain oxidation reaction & redox ?
Boitumelo Reply
hey , can you please explain oxidation reaction and redox ?
Boitumelo
for grade 12 or grade 11?
Sibulele
the value of V1 and V2
Tumelo Reply
advantages of electrons in a circuit
Rethabile Reply
we're do you find electromagnetism past papers
Ntombifuthi
what a normal force
Tholulwazi Reply
it is the force or component of the force that the surface exert on an object incontact with it and which acts perpendicular to the surface
Sihle
what is physics?
Petrus Reply
what is the half reaction of Potassium and chlorine
Anna Reply
how to calculate coefficient of static friction
Lisa Reply
how to calculate static friction
Lisa
How to calculate a current
Tumelo
how to calculate the magnitude of horizontal component of the applied force
Mogano
How to calculate force
Monambi
a structure of a thermocouple used to measure inner temperature
Anna Reply
a fixed gas of a mass is held at standard pressure temperature of 15 degrees Celsius .Calculate the temperature of the gas in Celsius if the pressure is changed to 2×10 to the power 4
Amahle Reply
How is energy being used in bonding?
Raymond Reply
what is acceleration
Syamthanda Reply
a rate of change in velocity of an object whith respect to time
Khuthadzo
how can we find the moment of torque of a circular object
Kidist
Acceleration is a rate of change in velocity.
Justice
t =r×f
Khuthadzo
how to calculate tension by substitution
Precious Reply
hi
Shongi
hi
Leago
use fnet method. how many obects are being calculated ?
Khuthadzo
khuthadzo hii
Hulisani
how to calculate acceleration and tension force
Lungile Reply
you use Fnet equals ma , newtoms second law formula
Masego
please help me with vectors in two dimensions
Mulaudzi Reply
how to calculate normal force
Mulaudzi
Got questions? Join the online conversation and get instant answers!
Jobilize.com Reply

Get Jobilize Job Search Mobile App in your pocket Now!

Get it on Google Play Download on the App Store Now




Source:  OpenStax, Physical methods in chemistry and nano science. OpenStax CNX. May 05, 2015 Download for free at http://legacy.cnx.org/content/col10699/1.21
Google Play and the Google Play logo are trademarks of Google Inc.

Notification Switch

Would you like to follow the 'Physical methods in chemistry and nano science' conversation and receive update notifications?

Ask