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TCH ICPMSThirtyMinuteGuide
TCH ICPMSThirtyMinuteGuide
T E C H N I C A L
ICP Mass Spectrometry
N O T E
on ICP-MS were published in the attainable using Graphite higher productivity and obtain
1980s and PerkinElmer SCIEX Furnace Atomic Absorption lower detection limits. Let’s look at
introduced the first commercially (GFAA) with much higher what an ICP-MS instrument can do
available ICP-MS instrument in productivity. and how it does it.
1983. Since that time, many The ICP-MS instrument
■ ICP-MS can easily handle both
improvements and refinements measures most of the elements in
simple and complex sample
have been made to each generation the periodic table. The elements
matrixes.
of ICP-MS instrumentation. Today, shown in color in Figure 1 can be
PerkinElmer SCIEX is on its fifth ■ ICP-MS has detection limit analyzed by ICP-MS with detection
generation ICP-MS and the capabilities that are superior limitsa at or below the part per
technique is used daily by many to those obtained in Inductively trillion (ppt)b range. Elements that
laboratories as a routine analytical Coupled Plasma Optical are in white are either not measur-
tool. Emission Spectrometry (ICP- able by ICP-MS (the upper right
OES). hand side) or do not have
naturally occurring isotopes. The
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a The detection limits are based on a 98% confidence level (3 standard deviations).
b Identifying a single part per trillion of an element in a solution is analogous to locating a single white raisin in a house (2,700 sq. ft) full of regular raisins.
Liquid Sample
c One micron diameter (1 X 10-6 meters) is considered an ideal diameter for introduction into the plasma.
plasma to pass into the ion lens The Vacuum System – the quadrupole region. Since the
regiond. The interface (shown in Provides Correct Operating ions generated in the plasma are
Figure 5) consists of two inverted Pressure nearly all positively charged, they
funnel-like devices called cones. The distance from the interface to have a natural tendency to repel
The sampler cone is located next to the detector of an ICP-MS is each other. In order to get as many
the plasma and the skimmer cone is typically one meter or less. If an ion of the ions as possible into the
located several millimeters behind is to travel that distance, it cannot quadrupole for mass separation and
the sampler cone. Each cone has an collide with any gas molecules. eventual measurement, it is neces-
opening of approximately one- This requires removal of nearly all sary to keep the ion beam from
millimeter in diameter at the apex of the gas molecules in the space diverging. This is achieved by
that permits the ions to pass between the interface and the passing the ions through a charged
through. The cones are typically detector to create a vacuum. This metallic cylinder that acts as a
made of nickel or platinum and are task is accomplished using a focusing lens. Since the charge on
mounted into a water-cooled metal combination of turbomolecular the lens is the same as the charge on
housing to prevent damage from the pumps and mechanical roughing the ions, the ions are repelled (like
heat of the plasma. The region pumps called the vacuum system. pushing the positive poles of two
between the two cones is evacuated The turbomolecular pumps work magnets together) back toward each
to a pressure of a few Torre by a like jet turbines and are capable of other to form a focused ion beam.
mechanical roughing pump. The rapidly pumping a chamber to a The small disk located between the
holes in the cones or orifices must pressure of 1 x 10-5 Torr. The skimmer cone and the cylinder lens
be large enough to prevent un- roughing pump connected to the is the shadow stop. This device
vaporized materials from clogging interface area (where the cones are keeps the photons and unionized
them. The orifices must also be located) removes most of the excess materials emitted from the plasma
small enough to maintain a consis- sample matrix ions and gasses. from moving downstream where
tent vacuum on the other side of the Routine maintenance on the they could have an adverse effect
interface. As samples pass through vacuum system generally consists on the performance of the ICP-MS.
an ICP-MS instrument, materials of changing the oil in the roughing Again, focusing ions in a mass
will eventually deposit on these pumps every 2 to 3 months. spectrometer is like focusing light
cones and will need to be removed in an optical spectrometer. Howev-
by occasional cleaning. How often The Lens System - Focusing er, the optical spectrometer uses an
the cones require cleaning is an Ions optical lens to bend the light beam,
important maintenance item that The ion lens is positioned immedi- while the mass spectrometer uses
must be considered when selecting ately behind the interface. It is an electrical field to focus the ion
an ICP-MS. responsible for focusing ions into beam.
The Quadrupole -
Separating Ions
The mass spectrometer separates
the singly charged ions from each
other by mass, serving as a mass
filter. Three main types of mass
spectrometers are used in commer-
cial ICP-MS systems: quadrupole,
time-of-flight, and magnetic sector.
The quadrupole is the type most
commonly used in routine analyti-
cal instrumentation. A quadrupole
consists of 4 rods approximately
20 cm in length and 1 cm in
diameter arranged as shown in
Figure 6.
The quadrupole mass spectrome-
Figure 5. The ICP-MS interface. ter works by allowing only one
d
mass to pass through to the detector
"An Improved Interface for Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)”,
D. J. Douglas and J. B. French, Spectrochimica Acta,Vol. 41B, No 3, pp. 197-204, 1986.
e The Torr is a unit of pressure equal to 1-760th of an atmosphere. The Torr is named after the
physicist Evangeslista Torricelli (1608-1647) who is credited with inventing the barometer.
at any given time. The quadrupole only one mass goes through the Data Handling and System
actually sorts on the mass-to-charge quadrupole at a time. Controller
(often referred to as m/z) ratio of the Another way to think of this is All ICP instruments require com-
ions. The quadrupole does this by to compare it to AA or ICP-OES. puters and sophisticated software
setting up the correct combination Instead of using an optical grating to control the plasma and mass
of voltages and radio frequencies to in a monochrometer to separate out spectrometer as well as perform
guide the ions with the selected m/z the wavelength of light for the calculations on the data collected.
between the four rods of the element being determined, the mass The following is an overview of the
quadrupole. Ions that do not have spectrometer separates the ions on main software features provided by
the selected m/z pass out through the basis of their mass and charge. the ELAN software on all
the spaces between the rods and are PerkinElmer SCIEX ICP-MS
ejected from the quadrupole. The The Detector - instruments.
mass spectrometer can move to any Counting Ions Instrument Status and Control
m/z needed to measure the ele- The ions exiting the mass spectrom- All the parts of the ICP-MS dis-
ments of interest in the sample eter strike the active surface of the cussed above are under software
analyzed. For example, to measure detector and generate a measurable control. The software makes sure
sodium, which has a single isotope electronic signal. The active surface each part of the instrument is
at mass 23, the mass spectrometer of the detector, known as a dynode, working properly and can provide
can be set to allow ions with m/z = releases an electron each time an the operator with useful informa-
23/1 to pass. For copper, which has ion strikes it. In Figure 7, the ion tion regarding the instrument
an isotope at mass 63, the mass exiting the quadrupole strikes the status. For example, there are over
spectrometer can be set to pass ions first dynode which releases elec- 70 check points on the ELAN ICP-
with m/z = 63/1. If a doubly trons and starts the amplification MS that are monitored by the
charged ion were formed, for process. The electrons released system to ensure the instrument is
example Ba+2, the mass spectrome- from the first dynode strike a always running in a safe and
ter would need to be set for a m/z of second dynode where more elec- reliable manner.
69f to allow this ion to go through. trons are released. This cascading
Instrument Optimization
Even though the quadrupole of electrons continues until a
All the routine optimization
mass spectrometer only allows one measurable pulse is created. By
procedures performed on the ELAN
m/z to pass through the rods at any counting the pulses generated by
are controlled by the computer. Just
given time, the voltage settings on the detector, the system counts the
open the optimization window for
the rods can be changed rapidly. ions that hit the first dynode.
The quadrupole on the ELAN® Compared with AA and ICP-OES,
Series ICP-MS from PerkinElmer the detectors used in ICP-MS are
SCIEX can see from m/z = 1 to m/z not much different than the photo-
= 240 in less than 0.1 seconds. This multiplier tubes used as the
is called the scan speed of the detectors in these optical instru-
quadrupole. This is the reason ICP- ments. Instead of detecting the light
MS can determine so many differ- emitted by an analyte, the actual
ent elements quickly even though analyte ion itself is being detected.
Signal
Figure 6. Quadrupole mass filter. Out
Figure 9. Quantitative calibration curve for lead at 10, 20, and 100 ppb.
Summary elemental composition of samples. References
There are many similarities between ICP-MS generally has fewer interfer- 1. "Applications and Technology of a
ICP-MS and the other analytical tools ences than ICP-OES and is much New ICP-MS Spectrometer,"
used in the laboratory, such as faster than AA and Graphite Furnace Atomic Spectroscopy, Special
Atomic Absorption and ICP Optical AA for the determination of multiple Issue, Vol. 16, No. 1, Jan/Feb,
Emission Spectrometry. The ICP-MS analytes per sample. ICP-MS detec- 1995.
is another way to determine the tion limits are generally much lower
2. "Method Development Strategies
elemental content of samples. ICP- than those that can be achieved by
for ICP-MS," Ruth Wolf and Zoe
MS accomplishes this by counting ICP-OES and GFAA. Quadrupole
Grosser, American Environmental
the number of ions at a certain mass ICP-MS instruments are capable of
Laboratory, February 1997.
of the element instead of the light measuring as many as 35 elements in
emitted by the element, as in optical a sample in two to three minutes. 3. "Mass Spectrometry of Inductively
techniques. Sample preparation for Because the spectrometer and all the Coupled Plasmas," R.S. Houk,
ICP-MS is very similar to that used in accessories are under computer Analytical Chemistry, Vol. 58, No,
AA and ICP-OES, and in many cases control, the system can literally 1, 1986.
is identical. Standards are analyzed operate 24 hours per day, 7 days per 4. "An Improved Interface for ICP-
to generate a calibration curve and week, and analyze over 300 samples MS," D.J. Douglas and J. B. French,
the signals from unknown samples per 24-hour day. In short, no other Spectrochimica Acta Part B, Vol.
are compared against the calibration technology can provide the low 41B, No.3, 1986.
curve to determine the concentration detection limits and the high produc-
of each metal in the sample. The tivity for elemental analysis offered
software reports data and results for by ICP-MS.
quantitative, semi-quantitative, This guide is intended as a quick
isotope ratio, or isotope dilution general overview of ICP-MS. For
analyses. those interested in more details
ICP-MS has many advantages over regarding the design and operation
other technologies, such as AA and of ICP-MS instruments, additional
ICP-OES, for determining the details can be found in the scientific
literature (1 - 4).
PerkinElmer Instruments
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