Introduction |
This application note gives all recommended data for the described analytical task including the list of measured values based on certified reference samples. |
|
Alloy system Au-Ag-Pd-Cu-Zn
Au-Ag-Cu-Zn-Ni
|
|
The Analytical problem |
Analysis of gold alloys is an important task in the jewellery industry for determination of alloy composition and monetary value. |
|
The five component alloys examined here are typical for white gold, although Nickel is now unusually as it is allergenic. However, many older alloys did contain Nickel. |
|
Palladium white golds are common and have higher content of „precious“ elements.
From the analytical point of view the overlapping of Au, Cu, Zn- and Ni-peaks and also of the Ag- and Pd-lines are the essential problems.
|
|
The analytical instrument |
Measurements are made with the benchtop spectrometers |
|
 |
X-Ray ComPact |
|
 |
X-Ray Karatmeter |
|
|
A low power tube is used in either instrument in excitation mode. A special collimator reduces the exciting beam down to 0.5 mm diameter. In this way, analysis of irregular or filigree samples will be possible. This is very important for jewellery manufacturers. |
|
Energy dispersive measurement is made with a proportional counter. Despite the limited resolution of this type detector, highly precise analysis is possible if the qualitative composition of the sample is known. Good statistical measurement guarantees high reproducibility. |
|
Max. Layer Thickness: approx. 10 µm |
|
Sample preparation |
The surface of the samples should be thoroughly cleaned free of contaminants. This will enable the irradiated area to be representative of the whole. |
|
Further preparation is not necessary as the very small excited area and the use of normalised intensities reduce the geometric influence on the signal. |
|
The irradiated area must be homogeneous. Non-homogenities can produce insufficient reproducibility of measurement. |
|
Excitation conditions |
| Voltage |
40 kV |
| Power |
approx. 15 W |
|
|
Program Parameters |
| Program |
SRX Vers. 4.104 |
| Evaluation program |
ALLOY.EXE |
| Measuring time for references |
180 s |
| Measuring time for analysis |
120 s |
| Normalisation parameter |
1 |
| Number of calibration ranges |
1 |
|
|
Au-Ag-Pd-Cu-Zn |
|
| Parameter |
Au |
Ag |
Pd |
Cu |
Zn |
| Deconvol |
ON |
ON |
ON |
ON |
ON |
| Cmin |
50 |
0 |
0 |
0 |
0 |
| Cmax |
90 |
40 |
20 |
20 |
5 |
| ROI Intmin |
188 |
365 |
347 |
130 |
140 |
| ROI Intmax |
212 |
404 |
385 |
150 |
160 |
| ROI Decmin |
100 |
300 |
300 |
100 |
100 |
| ROI Decmax |
270 |
480 |
480 |
270 |
270 |
|
|
Au-Ag-Cu-Zn-Ni |
|
| Parameter |
Au |
Ag |
Cu |
Zn |
Ni |
| Deconvol |
ON |
ON |
ON |
ON |
ON |
| Cmin |
30 |
0 |
0 |
0 |
0 |
| Cmax |
90 |
15 |
60 |
20 |
20 |
| ROI Intmin |
188 |
364 |
130 |
140 |
119 |
| ROI Intmax |
212 |
404 |
150 |
160 |
139 |
| ROI Decmin |
100 |
350 |
100 |
100 |
100 |
| ROI Decmax |
270 |
450 |
270 |
270 |
270 |
|
|
Calibration |
Calibration is made in one range. Ten reference samples were used. |
Analytical results |
|
Accuracy |
Au-Ag-Pd-Cu-Zn: |
Calibration curve |
|

|
|
Error of fit |
In the calibration of different elements, there are the following errors of the fit, σ:
|
|
| Element |
Au |
Ag |
Pd |
Cu |
Zn |
| σ [Wt. %] |
0.10 |
0.25 |
0.13 |
0.12 |
0.15 |
|
|
That means, that the analytical error for the described analytical problem is in the range of 0.20 Wt.% for gold. |
|
The strong overlapping of the peaks of Ag and Pd reduced the limit of detection for these elements to 1%. |
|
Au-Ag-Cu-Zn-Ni: |
Calibration curve |
|

|
|
Error of fit |
In the calibration of different elements, there are the following errors of the fit, σ:
|
|
| Element |
Au |
Ag |
Cu |
Zn |
Ni |
| σ [Wt. %] |
0.15 |
|
|
|
|
|
|
This means, that the analytical error for the described analytical problem is in the range of 0.20 Wt % for gold. |
|
Reproducibility |
Repeated measurements on the same sample with measuring times of 120 s give the following results: |
|
Standard deviation |
| Gold concentration |
0.08 % Wt. % |
| Rel. Standard deviation
Gold intensity
|
0.15 % |
|
|