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 %

«« Back to Applications