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       Pt-Cu

The Analytical problem

The use of Platinum alloys in jewellery has increased constantly. That means there is a need to determine the Pt-concentration in this type of alloy.

From the analytical point of view this task is not easy because the peaks of the components are strongly overlapping. On the other hand the relatively small concentration range eases the evaluation.

The Analytical instrument

Measurements are made with the benchtop spectrometers

X-Ray ComPact or

X-Ray maXXi

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 of 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. Inhomogenitis 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

Parameter

Pt

Cu

  Deconvolution

ON

ON

  Cmin

90

0

  Cmax

100

10

  ROI Int min

180

130

  ROI Int max

204

150

  ROI Decon min

100

100

  ROI Decon max

300

300

Calibration

For the small concentration range three reference samples only were used. During the production of platinum alloys there is the possibility that segregation of the different components can occur due to nonhomogenous cooling from very different melting temperatures. This segregation can produce nonhomogeneous samples. For this reason it is recommended that multiple measurements are made over the surface of the sample and the mean value taken.

Analytical results

Accuracy

Calibration table

Pt

Cu

Given

Analysed

Given

Analysed

100.00

99.99

0.00

0.00

96.00

96.08

4.00

3.78

96.30

96.22

3.70

3.92

Correlation coefficient

For this calibration, there is the following error of the fit: 0.08 Wt.%

That means, that the analytical error for the described alloy system is approximately + 0.10 Wt.%

Reproducibility

Repeated measurements (10 measurements) at the same sample position give the following results

SD (Pt-concentration):

0.09 Wt.%

RSD (Pt-intensity [1*σ]):

0.20 %

The Standard deviation of analytical results is significantly less than the standard deviation of intensities. This is a result of special evaluation of the spectra.

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