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TECHNICAL NOTE 12
1 Principle of atomic emission For a liquid sample, the atomization process can
be illustrated as follows.
1.2 Plasma
TECHNICAL NOTE 12
TECHNICAL NOTE 12
Precision: Corresponds to repeatability and repro- In figure 5 the second case is better than the third,
ducibility. even though the result seems bad (high relative
standard deviation).
Quantification limit: Concentration corresponding to 3
a given repeatability (for example 5%).
ICP OPTICAL EMISSION SPECTROSCOPY
TECHNICAL NOTE 12
2.4.2 Detection limits (LOD), Quantification limit expressed in multiples of standard deviation.
(LOQ)
Figure 8 shows the influence of the coefficient k on
Here, we assume that the fluctuation of the spec- the percentage of error.
tral background follows a Gaussian distribution
defined by its standard deviation.
TECHNICAL NOTE 12
2.4.3 Robustness
I
Depending on the composition of the matrix, the
same concentration of an element will not give the
same signal.For example, 5 ppm of Mg in water or
in NaCl 10 g/L does not give the same net intensi-
ty.
Therefore, for k = 3, RSD = 47%. The higher the ratio, the more robust is the plasma.
A plasma is robust when the ratio of magnesium is
To define the quantification limit, you define the greater than 6. In this case, the plasma is in ther-
maximum desired RSD, for example 5 or 10%. modynamic equilibrium.
RSD = 10%, for LOQ = 4.5 LOD
RSD = 5%, for LOQ = 10 LOD
RSD = 2% for LOQ = 30 LOD 3 Sample Preparation
Generally, the minimum LOQ used = 3 LOD.
The samples are usually introduced into the plasma
The detection limit is an estimation. in solution form but solids, finely divided, can also
The quantification limit is a measurement. be used. Care should be taken in obtaining a solu-
tion of a solid sample since there is a risk of loss of
The detection limit can be calculated in water or in element, or contamination. The final solution
a special matrix. It is very important to know the obtained by the analyst depends on the nature of
detection and quantification limits for each of the the sample and the concentration of elements to be
applications. determined.
Two main types of sample preparation are used for
ICP analysis:
- Acid Digestion.
- Dry attack.
5
ICP OPTICAL EMISSION SPECTROSCOPY
TECHNICAL NOTE 12
Acids, whether singly or in a mixture, use their oxi- - Whatever the type of solution, the quantity of acid
dising or reducing properties. Care must be taken or flux must be as low as possible to ensure mini-
with respect to possible loss of volatile elements. mum perturbation of the plasma. Certain acids are
For example, loss of As, Se, Sn in the form of chlo- preferable to others as they perturb the plasma
ride in the presence of HCl. Creation of precipitates less.
of Ca, Ba, Pb also represents a possible error in the
presence of H2SO4. Open and closed microwave Order of preference (from more favorable to least
systems are increasingly used in laboratories. favourable): HNO3, HCl, HCLO4, H2SO4, H3PO4.