Failure analysis using the Rigaku ZSX Primus wavelength-dispersive X-ray fluorescence spectrometer and SQX standardless analysis
Failure analysis can involve many analytical techniques to determine the cause for failure. WDXRF has been proven to be a very useful method to aid in failure analysis since in many cases elemental composition can be central to determining the failure mode. With today's modern semi-quantitative methods, which operate without needing elemental standards, the analysis can be performed quickly and easily.
As an example we analyzed a sediment deposited in a water chiller thought to be important for the potential failure of an X-ray instrument in our own laboratory. In this case only two grams of powdered sample was recovered for analysis. The sample was prepared by drying and placing it into a plastic sample cell with Prolene film as the surface analyzing window, as seen in Figure 1.

Figure 1
The sample was then loaded on Rigaku's Primus WDXRF system and run in a vacuum atmosphere. The analysis was done using Rigaku's standardless SQX program and EZ scan routine. The window for the EZ Scan setup can be seen in Figure 2 depicting the five questions needed to perform a full semi-quantitative elemental analysis.

Figure 2
The resulting elemental data from the sediment scan can be seen in Table 1.
|
Elemental |
Concentration |
Measuring |
Detection |
Elemental |
Intensity |
Concentration |
|
AI203 |
0.14 |
mass% |
0.02 |
Al-Kα |
0.10 |
0.12 |
|
Si02 |
0.12 |
mass% |
0.02 |
Si-Kα |
0.08 |
0.11 |
|
P205 |
0.05 |
mass% |
0.01 |
P-Kα |
0.05 |
0.05 |
|
SO3 |
0.06 |
mass% |
0.01 |
S-Kα |
0.08 |
0.05 |
|
K2O |
0.11 |
mass% |
0.01 |
K-Kα |
0.33 |
0.10 |
|
TiO2 |
0.05 |
mass% |
0.02 |
Ti-Kα |
0.04 |
0.05 |
|
Cr2O3 |
0.04 |
mass% |
0.01 |
Cr-Kα |
0.08 |
0.03 |
|
Fe2O3 |
0.05 |
mass% |
0.01 |
Fe-Kα |
0.29 |
0.04 |
|
NiO |
0.06 |
mass% |
0.01 |
Ni-Kα |
0.38 |
0.05 |
|
CuO |
97.60 |
mass% |
0.03 |
Cu-Kα |
629.19 |
88.74 |
|
ZnO |
1.73 |
mass% |
0.02 |
Zn-Kα |
15.69 |
1.57 |