ICP-MS

The ICP-MS of the GI department is a model Xseries I from Thermo Fisher Scientific.

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.

Principle
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.

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

 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.
 Samples should be acidified (preferably with 1-5 % HNO3 in order to keep metals in
solution)
 Deliver samples in 12 – 15 ml tubes.
 The content of salts in samples should be kept below 0.2% (=2 g/l)
 HCl can cause precipitates and the sulfur in sulfuric acid interferes in the analysis.
 The torch present at the GI is not resistant to HF.
 Samples should not contain any organic solvents.
 Indicate as far a possible which approximate concentration of the elements to analyse
may be expected in the samples
 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