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Gas Chromatography/Mass Spectrometry (GC/MS)

Description

The Gas Chromatography/Mass Spectrometry (GC/MS) instrument separates chemical mixtures


(the GC component) and identifies the components at a molecular level (the MS component). It
is one of the most accurate tools for analyzing environmental samples. The GC works on the
principle that a mixture will separate into individual substances when heated. The heated gases
are carried through a column with an inert gas (such as helium). As the separated substances
emerge from the column opening, they flow into the MS. Mass spectrometry identifies
compounds by the mass of the analyte molecule. A library of known mass spectra, covering
several thousand compounds, is stored on a computer. Mass spectrometry is considered the
only definitive analytical detector.

Applicability

GC/MS is a technique that can be used to separate volatile organic compounds (VOCs) and
pesticides. Portable GC units can be used to detect pollutants in the air, and they are currently
used for vapor intrusion investigations. However other uses of GC or MS, combined with other
separation and analytical techniques, have been developed for radionuclides, explosive
compounds such as Royal Demolition Explosive (RDX) and Trinitrotoluene (TNT), and metals.
Some of these are described below.

A type of spectrometry can also be used to continuously monitor incinerator emissions, in place
of a standard method that collects samples from a gas stream for laboratory analysis. That
standard method has a relatively long turn around time, and it does not provide information
that catastrophic releases have occurred or that there is a system failure. With real-time,
continuous monitoring, all releases are monitored, and if there is a system breakdown, the
system can be turned off and/or the nearby community can be notified.

Limitations and Concerns

Sample analysis is often time consuming. Newly developed portable GC/MS models may offset
this concern.

GC-MS actually comprises two basic units: Gas Chromatograph and Mass Spectrometer.

Gas chromatography is a chromatographic technique that can be used to separate organic


compounds that are volatile. In early 1900s, Gas chromatography (GC) was discovered by
Mikhail Semenovich Tsvett as a separation technique to separate compounds. A gas
chromatograph consists of a flowing mobile phase, an injection port, a separation column
containing the stationary phase, a detector, and a data recording system. The organic
compounds are separated due to differences in their partitioning behavior between the mobile
gas phase and the stationary phase in the column.
Mass spectrometry (MS) is an analytical technique that measures the mass-to-charge ratio of
charged particles.[1] It is used for determining masses of particles, for determining the elemental
composition of a sample or molecule, and for elucidating the chemical structures of molecules,
such as peptides and other chemical compounds. The MS principle consists of ionizing chemical
compounds to generate charged molecules or molecule fragments and measuring their mass-to-
charge ratios. In a typical MS procedure:

1. A sample is loaded onto the MS instrument, and undergoes vaporization


2. The components of the sample are ionized by one of a variety of methods (e.g., by
impacting them with an electron beam), which results in the formation of charged
particles (ions)
3. The ions are separated according to their mass-to-charge ratio in an analyzer by
electromagnetic fields
4. The ions are detected, usually by a quantitative method
5. The ion signal is processed into mass spectra

Instrumentation:

Gas Chromatography:

A typical gas chromatograph consists of an injection port, a column, carrier gas flow control
equipment, ovens and heaters for maintaining temperatures of the injection port and the
column, an integrator chart recorder and a detector (here feed to Mass spectrometer).

1. Sample Injection

A sample port is necessary for introducing the sample at the head of the column. Modern
injection techniques often employ the use of heated sample ports through which the sample can
be injected and vaporized in a near simultaneous fashion. A calibrated microsyringe is used to
deliver a sample volume in the range of a few microliters through a rubber septum and into the
vaporization chamber.

2. Carrier Gas

The carrier gas plays an important role, and varies in the GC used. Carrier gas must be dry, free
of oxygen and chemically inert mobile-phase employed in gas chromatography. Helium is most
commonly used because it is safer than, but comprable to hydrogen in efficiency, has a larger
range of flow rates and is compatable with many detectors. Nitrogen, argon, and hydrogen are
also used depending upon the desired performance and the detector being used. All carrier
gasses are available in pressurized tanks and pressure regulators, gauges and flow meters are
used to meticulously control the flow rate of the gas. Most gas supplies used should fall between
99.995% - 99.9995% purity range and contain a low levels (< 0.5 ppm) of oxygen and total
hydrocarbons in the tank.

3. Column Oven

The thermostatted oven serves to control the temperature of the column within a few tenths of
a degree to conduct precise work. The oven can be operated in two manners: isothermal
programming or temperature programming. In isothermal programming, the temperature of
the column is held constant throughout the entire separation. The optimum column
temperature for isothermal operation is about the middle point of the boiling range of the
sample.

4. Open Tubular Columns and Packed Columns

Open tubular columns, which are also known as capillary columns, come in two basic
forms. The first is a wall-coated open tubular (WCOT) column and the second type is a support-
coated open tubular (SCOT) column. WCOT columns are capillary tubes that have a thin later of
the stationary phase coated along the column walls. In SCOT columns, the column walls are first
coated with a thin layer (about 30 micrometers thick) of adsorbant solid, such as diatomaceous
earth, a material which consists of single-celled, sea-plant skeletons. The adsorbant solid is then
treated with the liquid stationary phase. While SCOT columns are capable of holding a greater
volume of stationary phase than a WCOT column due to its greater sample capacity, WCOT
columns still have greater column efficiencies.

The Mass Spectrometry Unit

Mass Spectrometer (MS) detectors are most powerful of all gas chromatography detectors. In a
GC/MS system, the mass spectrometer scans the masses continuously throughout the
separation. When the sample exits the chromatography column, it is passed through a transfer
line into the inlet of the mass spectrometer . The sample is then ionized and fragmented,
typically by an electron-impact ion source. During this process, the sample is bombarded by
energetic electrons which ionize the molecule by causing them to lose an electron due to
electrostatic repulsion. Further bombardment causes the ions to fragment. The ions are then
passed into a mass analyzer where the ions are sorted according to their m/z value, or mass-to-
charge ratio. Most ions are only singly charged.

The Chromatogram will point out the retention times and the mass spectrometer will use the
peaks to determine what kind of molecules are exist in the mixture. The figure below represents
a typical mass spectrum of water with the absorption peaks at the appropriate m/z ratios.

MS instruments consist of three modules:

An ion source, which can convert gas phase sample molecules into ions (or, in the case of
electrospray ionization, move ions that exist in solution into the gas phase)
A mass analyzer, which sorts the ions by their masses by applying electromagnetic fields
A detector, which measures the value of an indicator quantity and thus provides data for
calculating the abundances of each ion present
Additional Schematic diagram of GC/MS (any one to be used)

Figure: Schematic of the GC/MS system


Applications

Environmental Monitoring and Cleanup


GC-MS is becoming the tool of choice for tracking organic pollutants in the environment. The
cost of GC-MS equipment has decreased significantly, and the reliability has increased at the
same time, which has contributed to its increased adoption in environmental studies. There are
some compounds for which GC-MS is not sufficiently sensitive, including certain pesticides and
herbicides, but for most organic analysis of environmental samples, including many major
classes of pesticides, it is very sensitive and effective.
Criminal Forensics
GC-MS can analyze the particles from a human body in order to help link a criminal to a crime.
The analysis of fire debris using GC-MS is well established, and there is even an established
American Society for Testing Materials (ASTM) standard for fire debris analysis. GCMS/MS is
especially useful here as samples often contain very complex matrices and results, used in court,
need to be highly accurate.
Law Enforcement
GC-MS is increasingly used for detection of illegal narcotics, and may eventually supplant drug-
sniffing dogs.[1] It is also commonly used in forensic toxicology to find drugs and/or poisons in
biological specimens of suspects, victims, or the deceased.
Security
A post-September 11 development, explosive detection systems have become a part of all US
airports. These systems run on a host of technologies, many of them based on GC-MS. There are
only three manufacturers certified by the FAA to provide these systems,[citation needed] one of which
is Thermo Detection (formerly Thermedics), which produces the EGIS, a GC-MS-based line of
explosives detectors. The other two manufacturers are Barringer Technologies, now owned by
Smith's Detection Systems, and Ion Track Instruments, part of General Electric Infrastructure
Security Systems.
Food, Beverage and Perfume Analysis
Foods and beverages contain numerous aromatic compounds, some naturally present in the
raw materials and some forming during processing. GC-MS is extensively used for the analysis
of these compounds which include esters, fatty acids, alcohols, aldehydes, terpenes etc. It is also
used to detect and measure contaminants from spoilage or adulteration which may be harmful
and which is often controlled by governmental agencies, for example pesticides.
Medicine
Dozens of congenital metabolic diseases also known as Inborn error of metabolism are now
detectable by newborn screening tests, especially the testing using gas chromatography-mass
spectrometry. GC/MS can determine compounds in urine even in minor concentration. These
compounds are normally not present but appear in individuals suffering with metabolic
disorders. This is an increasingly becoming a common way to diagnose IEM for earlier diagnosis
and institution of treatment eventually leading to a better outcome. It is now possible to test a
newborn for over 100 genetic metabolic disorders by a urine test at birth based on GC/MS