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Determine the instrument blank.

a. Login a minimum of 3 Blank replicates.

b. Press the Analyze button on the instrument screen. After a short delay, the loading head slide-block will open.

c. Press the Analyze button on the instrument screen again, the loading head slide-block will close and the lower electrode will open.

d. Clean the upper and lower electrode manually, or, if applicable, remove thecrucible and press the analyze button to clean with the automatic cleaner.

e. Firmly place a graphite crucible on the lower electrode tip.

f. Press the Analyze button on the instrument screen, the lower electrode will close and the analysis sequence will start and endautomatically.

g. Repeat steps 2b through 2f a minimum of three times.

h. Set the blank following the procedure outlined in the operator's instruction manual.

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Procedure – Powder/Chip Samples

Determine the instrument blank.

Press the Analyze button on the instrument screen again, the loading head slide-block will close and the lower electrode will open.

Clean the upper and lower electrode either manually or remove the crucible and press the analyze button to clean with an automatic cleaner if applicable.

Add approximately 0.05 g of *** Graphite Powder to a 782-720 Graphite Crucible.

Firmly place the crucible on the lower electrode tip or appropriate autoloader position.

Sample Preparation

Sampling and sample preparation of refractory metals such as titanium and zirconium is somewhat different from that of steel. Unlike steel samples, hydrogen is not as mobile in this group of materials; therefore, storage in liquid nitrogen or dry ice is not required. However, it is important to keep the sample cool when cutting or sectioning. Sample preparation for oxygen and nitrogen determination has beendifferent from that of hydrogen determination.

Instrument calibration/drift correction

f. Clean the upper and lower electrode manually, or, if applicable, remove the crucible and press the analyze button to clean with the automatic cleaner.

g. Firmly place a graphite crucible on the lower electrode tip.

h. Press the Analyze button on the instrument screen, the lower electrode will close and the analysis sequence will start and end automatically.

i. Repeat steps 3b through 3h a minimum of three times for each calibration/drift standard used.

. Calibrate/drift following the procedure outlined in the operator's instruction manual.

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Procedure – Powder/Chip Samples

Instrument calibration/drift correction.

Add approximately 0.05 g of *** Graphite Powder to a***Graphite Crucible.

Firmly place the crucible on the lower electrode tip or appropriate autoloader position.

Press the Analyze button on the instrument screen,the lower electrode will close and the analysis sequence will start and end automatically.

Repeat steps 3b through 3i a minimum of three times for each calibration/drift standard used.

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