Technological University of the Philippines Taguig Campus

Km. 14 East Road South Superhighway, Taguig

INDUCTIVELY-
COUPLED PLASMA
MASS SPECTROMETRY
REPORTERS:
DIESTRO, CHRISTIAN
ANGELES, RICA
2B2
 INDUCTIVELY- COUPLED
PLASMA MASS SPECTROMETRY
Is a type of mass spectrometry which is capable of
detecting metals and several non-metals at concentrations
as low as one part in 1015 (part per quadrillion, ppq) on
non-interfered low-background isotopes.
This is achieved by ionizing the sample with inductively
coupled plasma and then using a mass spectrometer to
separate and quantify those ions.
 An inductively coupled plasma is a plasma that is energized
(ionized) by inductively heating the gas with
an electromagnetic coil, and contains a sufficient concentration
of ions and electrons to make the gas electrically conductive.
Even a partially ionized gas in which as little as 1% of the
particles are ionized can have the characteristics of a plasma
(i.e., response to magnetic fields and high electrical
conductivity. The plasmas used in spectrochemical analysis are
essentially electrically neutral, with each positive charge on an
ion balanced by a free electron. In these plasmas the positive
ions are almost all singly charged and there are few negative
ions, so there are nearly equal amounts of ions and electrons in
each unit volume of plasma.
INDUCTIVELY- COUPLED PLASMA
MASS SPECTROMETRY
 USES AND APPLICATION
One of the largest volume uses for ICP-MS is in the
medical and forensic field, specifically, toxicology
and environmental field.
Samples collected for analysis can range from whole
blood, urine, plasma, serum, to even packed red
blood cells.
 It is also used widely in the geochemistry field
for radiometric dating, in which it is used to
analyze relative abundance of different isotopes,
in particular uranium and lead. ICP-MS is more
suitable for this application than the previously
used thermal ionization mass spectrometry, as
species with high ionization energy such
as osmium and tungsten can be easily ionized.
 In the field of flow cytometry, a new technique uses ICP-
MS to replace the traditional fluorochromes. Briefly,
instead of labelling antibodies (or other biological probes)
with fluorochromes, each antibody is labelled with a
distinct combinations of lanthanides. When the sample of
interest is analyzed by ICP-MS in a specialized flow
cytometer, each antibody can be identified and
quantitated by virtue of a distinct ICP "footprint". In
theory, hundreds of different biological probes can thus
be analyzed in an individual cell, at a rate of ca. 1,000
cells per second. Because elements are easily
distinguished in ICP-MS, the problem of compensation in
multiplex flow cytometry is effectively eliminated.
 In the pharmaceutical industry,
ICP-MS is used for detecting
inorganic impurities
inpharmaceuticalsand their
ingredients.
PARTS AND FUNCTIONS
 Spray Chamber - In spray chambers or spray
towers water is sprayed or dispersed in fine
droplets, normally via sprayers or nozzles at
the top of the scrubber, while gas is fed
tangentially from underneath thus forming
counter-current flow. Due to the centrifugal
effect, there will already be a pre-separation of
larger particles in the column. It is also possible
to place spray-towers in co-current or cross-
current set-up.
 Carrier Gas - A carrier gas is the gas used
in the mobile phase of gas-liquid
chromatography. These types of gases are
injected manually by a known volume
injector (micro-injector) and are
responsible for carrying vapors. Carrier
gases are chosen depending upon the
application and which help to achieve the
best separation in the whole process.
 Auxiliary Gas - Gas used in a spray ion
source in addition to the nebulizing gas to aid
in solvent removal.

Detector - tool for trace detection of metals

in solution, in which a liquid sample is
injected into argon gas plasma contained by a
strong magnetic field.
 Ion lens An electrostatic lens is a device
that assists in the transport of charged
particles. ... An electrostatic lens can also
be used to focus an ion beam, for example
to make a micro beam for irradiating
individual cells.
 Quadrupole The quadrupole mass
analyzer (QMS) is one type of mass analyzer used
in mass spectrometry. It is also known as
a transmission quadrupole mass
spectrometer, quadrupole mass filter,
or quadrupole mass spectrometer.

Nebulizer Analytical nebulizers are a special

category in that their purpose is to deliver a fine
mist to spectrometric instruments for elemental
analysis.
 OPERATION

Samples to be analyzed passes through the ICP.

Due to its high temperature, the sample is ionized.
The ions then enters into an electric
field and are separated according to
their mass-to-charge ratio.
 CALIBRATION
Verification that the nebulizer is operating properly is
made visually by checking the aerosol production,
operating pressure, and mass-flow controller reading
prior to igniting the plasma. If the torch has been
repositioned for any reason the torch-box position
must be re-optimized using the vertical and horizontal
adjustments while monitoring the signal from 100
g/L 63Cu through pathway (<> denote computer
software modules) and the scan parameter set.
 Calibration is performed through the analysis of multiple
element standard solutions within a set of unknown and
reference samples from the path and qa parameter set. Select
a unique dataset, calibration, and report name. While
constructing your dataset use 'template' dataset as a guide. The
calibration file must generate equations based on a linear
regression through zero. Reference standards should be
analyzed after every 6 to 8 samples. Include the calcium
standards identified as 'CA50' and 'CA100' at the end of the
sample set. These two standards represent calcium
concentrations of 50 and 100 g/mL, respectively, and are used
to generate interference corrections for Co and Ni. Load
samples into the sampler and switch to the "automatic" mode to
start the analyses.
TROUBLESHOOTING/MAINTENANCE

One of the most frequent forms of routine maintenance is

replacing sample and waste tubing on the peristaltic pump.
Other parts that will need regular cleaning and/or
replacing are sample tips, nebulizer tips, sample cones,
skimmer cones, injector tubes, torches and lenses.
It may also be necessary to change the oil in the interface
roughing pump as well as the vacuum backing pump,
depending on the workload put on the instrument.
 ICPMS User Guide Instrument Startup and Daily Performance
Check
1. Turn on gas (Argon).
2. Check gas pressure in tank (Argon). The delivery pressure
should be at least 60psi. The instrument is always on.
3. Place sample line in beaker with Mili Q water (disconnect from
autosampler if necessary). Place tubing on peristaltic pump.
4. On the computer, open the ELAN icon.
5. File Open Workspace Daily Performance Instrument tab
Start (Plasma). The vacuum pressure should be less than 10 5
torr. Check that water is being drawn up the tube. When the
ignition sequence is complete, the diagram of the instrument in
the window should be green; if not green (e.g. if gas is not in line
after changing tank), repeat.
6. The Ready and Plasma lights on the instrument (by the beakers)
should be green.
7. Wait 1015 minutes for the plasma to warm up before performing
Daily Performance Check.
8. Fill the beaker labeled daily performance (a quarter to a half) with
Daily Performance Check solution (ELAN 6100 Setup Solution).
9. Switch the feed tube from the beaker of Mili Q water to the beaker
with Daily Performance Solution. Analyze Sample (Start).
10. When the run is complete, a report will print. To view on screen
select Rpt View. In this report:
11. If (d) and (e) are not satisfied, wait 515 minutes and run again.
12. Fill in values in the Log book (Populate all fields, including your
name and the date). Place the printed report in the Log and Daily
Performance binder located next to the computer.
 REFERENCES
https://
wwwbrr.cr.usgs.gov/projects/SW_inorgan
ic/download/MSMethod.pdf
https://
en.wikipedia.org/wiki/Inductively_coupl
ed_plasma_mass_spectrometry
http://
www.ecs.umass.edu/eve/facilities/equi
pment/ICPMS/ICPMS%20quick%20guide.pdf
https://