Information on servicing for analysis checks of spectrometer
The function of a spectrometer is to produce analyses. The fact that spectrometers consist of components such as an energy source and stand, optics, CCD, electronics and computer and that these in turn consist of sub-component and individual parts is often only of secondary interest to users. In a comparable way, a car-driver wants to drive a car and a television viewer wants to view television.
If faults have occurred in a spectrometer
which has been commissioned in good order, these faults must be removed. It is
then necessary to test that overall operation of the spectrometer is
satisfactory by measuring the RSD of the recalibration samples.
If the user has not made a clear statement
of defects, an effort must be made to specify them. A user unaccustomed to the
terminology may understand “fluctuating” as meaning that:
1. Measurement accuracy on one and same
sample is not good, that is, for individual or for all analytes;
2. Measurements on one and the same sample
at different times do not agree.
3 . Spectrochemical analyses, in some cases
or in all cases, do not agree with chemical analyses.
There are different reasons for each of
these three variants. What is good or bad requires clear definition.
If no definite fault is reported, and no
definite defect is found on the spectrometer, its efficiency must be tested in
the form of the RSD, for which recalibration samples must be measured.
If the actual values are found to be within
the nominal values a stability test should be carried out . This long-term test
should include a pause of 1h and the start and the end of a night.
If the stability test result is within the
nominal limits, the calibration must be checked with some check or reference
samples. In so doing, so far as possible, samples should be used which were
also used for the calibration.
Note: Watch the RSD of reference for the
corresponding base, namely at least one reference line for each optics system.
The RSD should be 0.5-1%. A check on the BEC can also be useful.
If these tests leads to detection of a
defect and to work being done on the spectrometer the results of such servicing
operations should subsequently be confirmed by measuring some recalibration
samples. If these tests do not lead to detection of the fault, the user’s
criticism usually relates to non-agreement between the spectrochemical and wet
chemistry or other values. If it is a question of systematic differences, agreement
can often be obtained, with the user’s content, by a small displacement of the
recalibration HP. This should be noted in the service report and signed by the
user.
Under no circumstances should spectrometer-
specific parameters such as the electrode gap, discharge parameters,
pre-sparking and measurement times, interference equivalent etc. be altered. If
this should prove necessary in special cases, separate analysis programmes
should be established. Whenever the analysis range is to be altered or extended
the operator who carried out commissioning should first be contacted.
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