Ni, Mo, Co, Pt, Re, Fe determination in new and spent catalysts

The test method specifies mass content determination of:
– Ni (Nickel), Mo (Molybdenum), Co (Cobalt), Pt (Platinum) and Re (Rhenium)  in new (clean) catalysts;
– Ni (Nickel), Mo (Molybdenum), Co (Cobalt), Fe (Iron), Pt (Platinum) and Re (Rhenium)  in spend (dirty) catalysts.
By X-Ray fluorescence method with “SPECTROSCAN MAKC” spectrometers.

The sample material is grinded with a disk grinder or agate mortar to the particle size about 70 microns.
Analysis includes two measurements of two samples of the same sample material.
The samples may be prepared the following two ways.

Filling the sample cup
Sample material is filled in a standard sample cup delivered with spectrometer. The powder is compressed till smooth flat surface at the cup edge level is obtained. The cup is covered with 5 micron thick polyethyleneterephtalate film. The film is fixed with rings included in the sample cup set.

Pressing in a boron acid cup
Boron acid cup is pressed out with a shaped punch being at least 3 mm deep. Sample material is put into the cup and pressed with a flat punch into a pellet.
The sample cup or the pellet put into the sample holder and then into spectrometer. Analysis is carried out automatically according to the chosen program. The program can determine all elements (oxides) listed in the test method or some of those elements by choice.
Mass content determination of all metal and metal oxides is done from one sample.

Mass content determination of the elements specified with the test method are given in the table:

Determined component Component mass content, %
MoO3 3,0 –15,0
NiO 0,5 –5,0
CoO 0,5 –5,0
Fe 0,2 – 3,0
Pt 0,10 – 0,7
Re 0,10 – 0,7