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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.

Procedure – Powder/Chip Samples

Instrument calibration/drift correction.

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

Place the Nickel Capsule containing the sample into the open port at the top of the loading head.

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.

Sample Preparation

Sampling and sample preparation is an important issue because traditional methods used to obtain samples for oxygen and nitrogen determination are different from those recommended for hydrogen, especially when sampling molten metal. The main difference in steel sampling procedures for oxygen/nitrogen and hydrogen is due to the mobilityof hydrogen. Special precautions must be used when sampling for hydrogen. From molten steel and iron, a sample must be quickly quenched in cold water and chilled in a refrigerant such as liquefied nitrogen or a mixture of acetone and solid carbon dioxide in order to reduce losses of hydrogen from diffusion. Losses of oxygen and nitrogen from diffusion are not a problem. A sample that is taken for hydrogen and

chilled in a refrigerant can also be used for oxygen and nitrogen determination. However, a sample that is typically taken for oxygen and/or nitrogen determination is not suitable for hydrogen determination due to hydrogen loss (diffusion). Surface contamination must be removed by filing or light grinding, using care not to overheat the sample.

Procedure - Solid Samples

Determine the instrument blank.

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

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

Instrument calibration/drift correction.

Login a minimum of 3 Standard replicates.

Weigh approximately *** grams of a calibration/drift standard, enter the mass and standard identification into appropriate replicate fields.

Note: LECO Reference Materia***o not require preparation.See preparation statement on the reference material certificate.

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Instrument calibration/drift correction.

a. Login a minimum of 3 Standard replicates.

b. Weigh a ~1.000 gram of a calibration/drift standard, enter the mass and standard identification into appropriate replicate fields.

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

d. Place the calibration/drift standard into the open port at the top of the loading head.

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

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