Thermo Scientific NITON XL3t 500 User Manual page 58

Analysis of Prepared Samples – Ex Situ
Specimen Preparation -
Fused Glass Disk;
Specimen Preparation -
Pressed powder briquette
preparation;
1-44 NITON XL3 Analyzer User's Guide
The samples need to be predried for 2-6 hours in 105°C depending on the
moisture content.
1. Grind the dried samples to ~200mesh (74 µm).
2. Calcination (Ashing) the sample;
a. About 4-6 g of dry pulverized sample is calcinated in an alumina or
platinum crucible in a muffle furnace at 1000°C for 1 hour.
b. The sample is cooled in a dedicator and loss on ignition (LOD) is
calculated from weight difference before and after Calcination.
3. Weight 1.0g of calcinated sample into fusion crucible add 5.0 g of
lithium tetraborate and 0.3 lithium fluorife, and 10-20 mg lithium
bromide as a nonstick agent.
4. Fuse in a fluxer for at least 4 min in the flame.
5. The resulting disk is released from the mold, cooled the presented
to the spectrometer.
1. T
horoughly remix the sample in its jar by rotating in a figure-eight
motion with two hands
2. Weight 7.0g of sample into weighting boat by taking several
separate gram-size portions then fine grind sample using a swing
mill.
3. Add 2 small drops of propylene glycol on the top of the powder
sample in the mill as a grinding aid, grind 4min at 1000rpm to
obtain 10 µm particle size.
4. Add 0.5g binder to the sample and continue grinding for 30sec
more.
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