Assignment 2 GC-MS FFF

INTRODUCTION
Gas chromatography- mass spectroscopy (GC-MS) is one of the so called hyphenated

analytical techniques. It is a method that combines the features of gas chromatography and
mass spectrometry to identify different substances within the sample. Additionally, it can trace
elements in materials that were previously thought go undetected by other technologies. Gas
chromatography separates the components of a mixture and mass spectroscopy characterizes
each of the components individually. By combining the two techniques, an analytical chemist
can both qualitatively and quantitatively evaluate a solution containing a number of chemicals.
In general, chromatography is used to separate mixtures of chemicals into individual
components. Once separated, the components can be evaluated.
Gas chromatography
In all chromatography, separation occurs when the sample mixture is introduced or injected into
a mobile phase. In gas chromatography (GC), the mobile phase is an inert gas such as helium.
In liquid chromatography, the mobile phase is solvent.
The mobile phase carries the sample through what is referred as a stationary phase. The
stationary phase is a usually chemical that can selectively attract components in a sample
mixture and contained in a tube that referred as column. The columns can be glass or stainless
steel of various dimensions.
The mixture of compounds in the mobile phase will interacts with the stationary phase. Each
compound in the mixture interacts at a different phase. The difference in the chemical properties
between different molecules in a mixture will separate the molecules as the sample travel down
the length of column. Compounds that interact fastest will exit the column first and the slowest
will exit the column last. Different mixtures of chemicals can be separated by changing the
characteristics of the mobile phase and stationary phase. And this separation can be further
refine by changing the temperature of the stationary phase by the used of oven or the pressure
of the mobile phase.
As the compounds are separated, they exit from the column and enter a detector. The detector
is capable of creating an electronic signal whenever the presence of compounds is detected.
The greater the concentration in the sample, the bigger the signal. The signal then processed by
a computer and generates a graph from the signal. The time when the injection of sample
mixture is made to when elution occurs is referred to as the retention time (RT). The graph
generates called a chromatogram. Each peak in chromatogram represents the signal created
when the compound elutes from the column into detector.
Figure 1: Chromatrogram generatd by a CG

By knowing the retention time (RT) for a given compound, assumptions about the identity of the
compounds can be made. However, some compounds that have similar properties may have
the same retention time. Therefore, further analysis is made to make true identification of the
compounds in a sample containing unknown components.
Mass spectroscopy
When gas chromatography separates the components of a mixture, mass spectroscopy
characterizes each of the components individually. As the individual compounds exit from the
GC column, they enter the electron ionization detector. There, they are bombarded with a
stream of electrons causing them to break apart into fragments. The fragments are charged ions
with a certain mass. The mass of the fragments divided by the charge is called the mass to
charge ratio (M/Z). The mass-to-charge ratio of a cation is equal to the mass of the cation
divided by its charge.
masscharge ration=
mass of cation
charge of cation
Since most fragments have a charge of +1, the M/Z usually represents the molecular weight of
the fragment.
masscharge ration=
mass of cation
+1
mass of cation
The mass of the molecular ion is equal to the molecular weight of the compound. Thus, the
mass-to-charge ratio of the molecular ion is equal to the molecular weight of the compound. The
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detector in the mass spectrometer counts the number of ions with a specific mass. This
information is sent to a computer and a mass spectrum is created. The mass spectrum is a
graph of the number of ions with different masses that travelled through the filter.
Figure 2: Mass-spectrum generated by MS

Gas chromatography-mass spectroscopy (GS-MS)
Figure 3: 3D depiction of GC-MS output

Figure 3 represents a three-dimensional graph generated when the GC is combined with the
MS.
INSTRUMENTAL COMPONENT
Figure 4: GC-MS
Carrier gas
The carrier gas used is inert gas which is helium, argon and carbon dioxide. Usually, the carrier
gas is chosen based on the type of detector used. It is also contains a molecular sieve to
remove impurities and water.
Sample injection port
A micro syringe is used to inject sample through a rubber septum into a flash vapouriser port at
the head of the column. The temperature of the sample is usually 50C higher than the boiling
point of the least volatile component of the sample.
The injector can be used in two ways namely split and splitless. It contains a heated chamber.
The carrier gas enters the chamber and leave. The sample vaporizes to form a mixture of
carrier gas, vaporized solvent and vaporized solutes. It then moves along the column.
Columns
There are two types of columns packed and capillary. The capillary column is more efficient
than the packed columns.
Column temperature
The optimum column temperature is dependent upon the boiling point of the sample.
Detectors
Different detectors give different types of selectivity. A non-selective detector responds to all
compounds except the carrier gas, a selective detector responds to a range of compounds with
a common physical or chemical property and a specific detector responds to a single chemical
compound.
HOW DOES IT WORK?

The Gas Chromatography Mass Spectrometer (GC-MS) instrument is made up of two
components which is;
1. Gas Chromatography (GC)
2. Mass Spectrometer (MS)
The GC functions as its separate the chemical mixture into pulses of pure chemicals while MS
will identifies and quantifies the chemicals.
Schematic of GC-MS
1. Gas Chromatography (GC)

Injection port a small amount of the chemical mixture is injected into the GC
and the sample is carried by inert gas through the instrument. The inert gas
usually used is helium (He). Next, the inject port is heated to 300 C for the
chemicals in the sample to vaporize and become gas.
Oven A specialized oven is built as one of the outer part of the GC. The column
is heated to move the molecules through it. The average temperature of the oven
is around 40 C to 320 C.
Column The column which is coated with a special polymer coating on the
inside and 30 meter thin tube is situated inside the oven. The mixture of the
chemicals is separated based on their votality and carried through the column by
helium. Lighter or smaller molecules will travel faster and quicker through the
column than the heavier or larger molecules that is low in votality.
2. Mass Spectrometer (MS)
Ion Source From the GC, the chemical molecules is then entered the MS.
Here, ionization occurred as the molecules are bombarded with electrons. This
result in the breakdown of the molecules into fragments and positively charged
particles called ions.
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Filter the ions travel through an electromagnetic field that will filters the ions
based on their respectively masses. The filter then scans through the range of
masses as the ions stream come from the ion source.
Detector the detector counts the number of ions with a specific mass. The
information collected then passed to the computer and mass spectrum is
created. A graph of mass spectrum showing the number of ions with different
masses that traveled through the filter.
ANALYSIS
MS is utilized in one of two ways: full scan or selected ion monitoring (SIM). The typical GC-MS
instrument can perform in both ways depending on the setup of the instrument.
The objective of the instrument analysis is to quantify an amount of substance. It is done by
comparison between the relative concentration and the atomic masses in the generated
spectrum. There are two kind of analysis which is comparative and original. Comparative
analysis is works by comparing the given spectrum to a spectrum library to see if its
characteristics are present for some sample in the library. Usually, this is done by computer
because it can correlate more data to more accurately relate certain data.
Other method is by measuring the peaks in relation to one another. In this method, the tallest
peak is assigned 100% of the value while other values and peaks are assigned proportionally.
The total mass of the unknown compound is usually the indicated by the parent peak. The
isotope pattern that exists in certain compounds can be used to detect the various element
presences. Once the chemical formula gas been matched to the spectrum, the molecular
structure and bonding can be identified, and consistent with the characteristics recorded by the
GC-MS.
A full spectrum analysis considers all the peaks within a spectrum. SIM conversely only
monitoring selected ions associated with a specific substance. At given retention time, a set of
ions is characteristic of a certain compound is predicted. This is more fast and efficient analysis.
SIM allows for a smaller quantity of a compound to be detected and measured, but the degree
of certainty about the identity of the compound is reduced.
Using full scan mode in collecting data, a target range of mass fragments is determined. An
example of a typical broad range of mass fragments is between m/z 50 400. Then a MS
should not be set to look for mass fragments too low. Large scan range resulted in less
sensitivity of the instrument since it needed to detect wide range of mass fragments. Full scan is
used to detect the unknown compounds in a sample. It gives more information than SIM.
In SIM certain ion fragments are inserted into the instrument method and only those mass
fragments are detected by the mass spectrometer. The advantages of SIM are the detection
limit is lower since the instrument is only looking at a small number of fragments during each
scan.
APPLICATION
Medication
Drug detection
Fire investigation
Environmental analysis
Explosives investigation
Identification of unknown samples
REFERENCES
1. Gas Chromatography-Mass Spectroscopy Background. Retrieved 23 November, 2013
from http://www.gmu.edu/depts/SRIF/tutorial/gcd/gc-ms2.htm
2. Gas chromatography-Mass spectrometry. Retrieved 23 November, 2013 from
http://www.smithsdetection.com/gc-ms.html
3. Mass-to-Charge
Ratio.
Retrieved
23
November,
2013
from
http://science.uvu.edu/ochem/index.php/alphabetical/m-n/mass-to-charge-ratio/
4. Gas
Chromatography.
Retrieved
23
November,
2013
from
http://teaching.shu.ac.uk/hwb/chemistry/tutorials/chrom/gaschrm.htm.
5. Amirav, A.; Gordin, A. Poliak, M. Alon, T. and Fialkov, A. B. (2008). "Gas
Chromatography Mass Spectrometry with Supersonic Molecular Beams". Journal of
Mass Spectrometry 43: 141163.

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INTRODUCTION

Gas chromatography- mass spectroscopy (GC-MS) is one of the so called hyphenated

Figure 1: Chromatrogram generatd by a CG

Figure 2: Mass-spectrum generated by MS

Figure 3: 3D depiction of GC-MS output

HOW DOES IT WORK?

1. Gas Chromatography (GC)

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