XRF
 
 
ZSX Primus II Application Byte

 

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 
component

Concentration
w/ normalization

Measuring
unit 

Detection 
limit 

Elemental
line measured 

Intensity
(kcps)

Concentration
w/o normalization

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

Table 1: Sediment failure analysis 

The high elemental concentrations of both copper and zinc indicate a copper waterline degradation to the instrument in question.

As shown in this example, the XRF data can provide clues to determine where a failure has or may take place. This method can be instrumental in maintaining equipment and forecasting problems in a process prior to an actual failure.

Tags: XRF, Primus, WDXRF, standardless, failure, analysis