Nama : Muhammad Ali Akbar

NPM : 1506741114

ICP-ES/ ICP-OES

ICP-OES (Inductively coupled plasma - optical emission spectrometry) is a technique in which the
composition of elements in (mostly water-dissolved) samples can be determined using plasma and a
spectrometer. The solution to analyze is conducted by a peristaltic pump though a nebulizer into a spray
chamber. The produced aerosol is lead into an argon plasma. Plasma is the forth state of matter, next to
the solid, liquid and gaseous state. In the ICP-OES the plasma is generated at the end of a quarts torch by
a cooled induction coil through which a high frequency alternate current flows. As a consequence, an
alternate magnetic field is induced which accelerated electrons into a circular trajectory. Due to collision
between the argon atom and the electrons ionization occurs, giving rise to a stable plasma. The plasma is
extremely hot, 6000-7000 K. In the induction zone it can even reach 10000 K. In the torch desolvation,
atomization and ionizations of the sample takes place. Due to the thermic energy taken up by the
electrons, they reach a higher "excited" state. When the electrons drop back to ground level energy is
liberated as light (photons). Each element has an own characteristic emission spectrum that is measured
with a spectrometer. The light intensity on the wavelength is measured and with the calibration calculated
into a concentration.
The GI and the spin-off company B-WARE having two ICP-OES systems; iCAP 6000 (Thermo Fischer
Scientific, Bremen, Germany), and the high-end system ARCOS (Spectro Analytical, Kleve, Germany)

a. ICP-OES ICAP
The ICAP 6000 (Thermo Fisher Scientific) is equipped with a vertical torch and a radial plasma
observation. With this configuration the ICAP can measure robust, reliable and heavy matrices.
The detection limits are normally in the higher ppb (µg/L) range. For the detection the ICAP uses
mirrors and a prism to measure the light on one CCD chip.
b. ICP-OES ARCOS
The ARCOS (Spectro Analytical) is the ICP-OES of B-WARE Research Centre; if the ARCOS has an
added value compared to the ICAP the instrument can also be used for FNWI. The ARCOS can
change the plasma configuration from vertical to horizontal, and can so change the plasma
observation from true radial to true axial. The detection limits are varying by plasma
configuration, matrix and elements that are measured, but in each case they are in the low ppb
(µg/L) to high ppt (ng/L) range.

ICP-MS

ICP-MS (inductively coupled plasma-mass-spectrometry) is a technique to determine low-concentrations

(range: ppb = parts per billion = µg/l) and ultra-low-concentrations of elements (range: ptt = parts per
trillion = ng/l). Atomic elements are lead through a plasma source where they become ionized. Then,
these ions are sorted on account of their mass. The advantages of the ICP-MS technique above AAS
(Atomic Absorption Spectroscopy) or ICP-OES (inductively coupled plasma optical emission
spectrometry) are:

 Extremely low detection limits

 A large linear range

 Possibilities to detect isotope composition of elements

The ICP-MS technique has a multi-element character and a high sample throughput, like ICP-OES, but it
allows one to perform more sensitive measurements. Disadvantages and weaknesses of the ICP-MS
detection are the occurrence of spectral and non-spectral interferences and the high costs.
 a. ICP part

Like for the ICP-OES, the sample solution is introduced into the device by means of a peristaltic
pump. There it becomes nebulized in a spray chamber. The resulting aerosol is injected into an argon-
plasma that has a temperature of 6000-8000 K. Inside the plasma torch, solution is removed from the
sample and also atomization and ionization occur. Only a small amount part of the ions produced in the
plasma further penetrate to the mass-spectrometer part.

b. Mass-spectrometer part
This part consists of:
 An interface (in particular a “sampler cone” and a skimmer cone), in which a small amount of the
free ions generated by the plasma are transmitted. During this process the ions migrate from an
environment with extremely high temperature and atmospheric pressure to a compartment at room
temperature an high vacuum (< 0,001 Pa)
 Electrostatic lenses that focus (positive) ions onto the entry to the true mass-spectrometer
 The true mass-spectrometer in the GI device has a quadrupole, composed of 4 metal rods which
separate the ions on account of their mass by a kind of resonance principle
 An electro-multiplier (a specific type of detector) containing active surfaces, which enhances the
signal from one colliding ion so that a measurable pulse is generated
 Electronics that counts and sorts the pulses and relates them to the corresponding mass. This
selection can be accomplished in milliseconds, so that a complete spectrum can be acquired within
one second.

Sample preparation / how to deliver samples:

1. Solid material should be preferably destructed with nitric acid only (keep the concentration
HNO3 below 10%, ideally around 1%), or if necessary with HNO3/H2O2. This step can be
performed as a closed destruction in a microwave-oven.
2. Samples should be acidified (preferably with 1-5 % HNO3 in order to keep metals in solution)
3. Deliver samples in 12 – 15 ml tubes.
4. The content of salts in samples should be kept below 0.2% (=2 g/l)
5. HCl can cause precipitates and the sulfur in sulfuric acid interferes in the analysis.
6. The torch present at the GI is not resistant to HF.
7. Samples should not contain any organic solvents.
8. Indicate as far a possible which approximate concentration of the elements to analyse may be
expected in the samples
9. The ICP-MS can be employed to measure isotope ratios of enriched experiments, but the device
is not appropriate to analyze the differences in natural abundance of isotopes
Comparison of ICP-MS and ICP-OES Advantages and Methods

ICP MS ICP OES

ICP-MS is becoming a workhorse for metal
analysis in water not only because it offers lower
detection limit. The following features also
contribute its wide range of environmental
applications:
ICP-OES is used for all the matrices of
environmental samples especially for high-matrix
samples. The following features also contribute its
wide range of environmental applications:

 Only analytical grade reagents are sufficient

 Wide dynamic range
 Simpler method development does not need a
 Efficiently remove polyatomic spectral
specialist with highly technical expertise
interferences using collision cell technology
 Overall is a cheaper option if the elements do
 Rapid semi-quantitative analysis
not need lower detection limit that ICP-MS
 Isotopic analysis
delivers

Sumber:

 http://www.ru.nl/science/gi/facilities-activities/elemental-analysis/icp-oes/
 http://www.ru.nl/science/gi/facilities-activities/elemental-analysis/icp-ms/
 “Introduction To Mineral Exploration;: 2nd Edition” (2006), Moon, Charles J. G, Michael K. Evans,
Whatley and Anthony M. Blackwell Publishing. Australia.