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O determination in copper samples

閱讀:5741      發(fā)布時間:2015-05-15
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  Suitable analyzers
n ON 900
n OH 900
n ONH 2000
Used accessories
n Graphite crucibles (90190)
n Suitable calibration material (NIST or other)
Settings
n Comparator level: 20 mV
n Minimum time: 15 sec
n Maximum time: 1:30 min
n Post waiting: 10 sec
n Base line deviation: 200 mV;
Step: 16 mV; Time: 10 sec
n Mode: continuous
n Outgas
Time: 45 sec
Power: 3.5 kW
n Time
Purge: 20 sec
Stability: 45 sec
n Integration delay
IR cell: 2 sec
TC cell: 10 sec
n Analyse (1)
Time: 75 sec
Power (1): 3.0 kW
Power (2): 3.0 kW

Sample preparation
Make sure that the surface of the copper is free from
contaminations; otherwise clean the sample with acetone
p.a. and let dry at atmosphere. In case of very low oxygen
concentrations (< 5 ppm) rinse the sample in nitric acid
(HNO3) first, than water, last with acetone. Let this sample
dry at atmosphere and analyze immediay.
Procedure
n Prepare ELTRA analyzer (exchange anhydrone, sodium
hydroxide, copper oxide or Schuetze reagent when
necessary), clean furnace, sample drop mechanism,
electrode tip
n Run three blanks with empty crucibles
n Calibrate the analyzer with suitable calibration
material (NIST or other)
(1) Place empty crucible (90190) on the electrode tip,
close furnace (F2 Button)
(2) Weigh calibration material (usually pins)
(3) Place calibration material in the sample drop
mechanism and start analysis (F5 Button)
Repeat steps (1) – (3) at least three times;
Mark the results and use the calibration function in the
software.


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