Emission Spectroscopy Line

DOE-HDBK-3010-94

Appendix B; Production Support Lab

The same types of counting devices found in the liquid sample line rooms are found in the

metal sample line rooms.

3.2.4 E m ission S p ectroscop y L in e

The emission spectrometer is used primarily to measure impurities in plutonium metal. It is

also used to prepare samples for the x-ray diffraction analysis unit installed in the room. The

line consists of three major stations: (1) the diffraction sample preparation station, (2) the

spectrometer sample preparation station, and (3) the emission spectrometer station.

The diffraction sample preparation station has a storage rack capable of holding 10 sample

vials. A metal storage container that can hold up to five sample vials awaiting return to H-1

for recycle into the main process is located at this station as well. A mortar and pestle are

provided in the station to grind non-metallic samples into fine powder. The sample obtained

is sealed in a plastic pipe cap by Teflon or Mylar film before being removed from the

glovebox via the hood box on the entry end of the line. It is examined for contamination in a

separate laboratory hood and then taken to the diffractometer sample chamber. The x-ray unit

is operated in accordance with ANSI standards and is equipped with warning lights that

activate in the room and in the hallway when the unit is on. Respirators are worn whenever

the sealed sample is in transit in the room, and a contamination check is made before

removing the respirator after transfer.

The spectrometer sample preparation station also has a storage rack capable of holding 10

sample vials. The first step in preparation is to dissolve the sample in acid and then

precipitate the sample in a slurry form. The slurry is dried under an infrared lamp and

converted to oxide in a small muffle furnace. In the final step of sample preparation, the

oxide obtained is pelletized in a sodium fluoride matrix.

Individual pellets are introduced into the emission spectrometer station and inserted in the

unit's electrode rod. The pellet is vaporized once it is in place, and impurities are detected

from their spectral emissions. The emission spectrometer itself is built into the glovebox,

with the physical bulk of the unit outside the box.

3.2.5 M ass S p ectrom etry L in e

Like the emission spectrometer, the mass spectrometer is built into the mass spectrometry

glovebox with the bulk of the unit outside the glovebox. The line receives small liquid

samples from the liquid or solid sampling lines and is equipped with a 20-position storage

rack. Analysis is performed on small samples dried and oxidized with a heated filament.

These samples are transferred through a vacuum lock into the automated mass spectrometer.

Page B-95