Introduction

The EUs directives on the Restriction of the use of certain Hazardous Substances (RoHS) and Waste Electrical and Electronic Equipment (WEEE) set limits on the use of Cd, Pb, Hg, Br and Cr6+ in diversely plastic products or in each homogeneous component of electrical and electronic products, for example plastic cable insulation and solder joints on a printed circuit board (PCB). EDXRF is a well-suited analytical method for direct RoHS compliance testing of various samples such as metals, plastic, powder with minimal sample preparation.

The Analytical Instrument

The X-ray MaXXi 5/PIN analyzer offered by Röntgenanalytik Messtechnik GmbH has been especially optimized for the WEEE and RoHS analysis in plastics and solder. The large sample chamber allows non-destructive measurement of large plastic parts or PCB with various shapes.

Excitation conditions

Tube W-Microfocus-Be-window
Voltage 50 kV
Power approx. 50 W
Collimator 1.0 mm in diameter
Primary Filters Mo 75 µm, Ni 10µm
Measuring time for analysis 120-300 s

Program Parameters

Program XMaster Vers. 2.5.3.2
Application Cd, Pb, Br, Hg in Plastic

Fig. 1. Application example: printed circuit board.

Sample Preparation

The surface of the samples should be as much as possible even. Further preparation is not necessary as the small excited area reduce the geometric influence of the signal. The following Figure 2 shows the X-ray spectrum of polyethylene standard measured with Mo primary filter.

Fig. 2. Spectrum of the PE standard BCR-680.

Calibration

The using of special multi-mode non-linear calibration for thickness, background and matrix correction allows measuring of hazardous elements with high accuracy in PCB and different plastic materials with various shapes. The Figure 3 plotted a typical calibration curve for Cd

Fig. 3. Calibration curve for Cd in Plastic.

Analytical Features

Table 1 shows the analytical features of RoHS analysis of restricted elements Cd, Br, Hg and Pb in diverse plastic materials using X-ray MaXXi 5/PIN analyzer.

Feature

Cd,
ppm

Br,
ppm

Hg,
ppm

Pb,
ppm

lower meas limit

20

20

20

20

RoHS law limit

100

1000

1000

1000

accuracy

+/-10

+/-10

+/-10

+/-10

meas time, min.

5

3

3

3

Limits of detection

Different filters optimized for measuring of Cd, Br, Pb and Hg allow to decrease the detection limits down to 20 ppm, that is one order of magnitude less than the RoHS limit for Cd and yet two order of magnitude less for other elements.

Accuracy of analysis

The high accuracy of ± 10 ppm can be achieved within an analysis time of 3 min for Br, Pb Hg and 5 min for Cd.

Reproducibility

For determination of reproducibility a 10 repeated measurements with a measuring time of 180 s have been realised on a few standard samples. Mean measured values and relative standard deviations are shown in the table 2.

Sample

Br, ppm

Pb, ppm

Hg, ppm

Cd, ppm

given

meas

StD,%

given

meas

StD,%

given

meas

StD,%

given

meas

StD,%

BCR-680

808

812

1.11

108

118

4.76

25

34

13.51

141

144

11.81

BCR-681

98

104

14

23

5

6

22

22

PE high

1100

1099

1.19

1200

1200

1.02

1100

1100

1.82

300

310

4.92

PVC-3

837

846

5.95

85

85

7.32

PVC high

1101

1101

7.01

1201

1195

8.90

1101

1101

7.4

300

300

PVC low

500

500

400

402

200

195

100

102

10.78

Measurement report

Results of analysis can be summarized either in an easy measurement report or in a report file in Word format with a visualisation of measuring points and spectra imaging. The several report file templates can be generated and verified on the report template list.

Conclusion

The X-ray MaXXi 5/PIN analyzer allows rapid non-destructive direct measurement and quantification of regulated substances covered by environmental legislation, e.g. the RoHS and WEEE directives, in various plastic and powder materials and is well suited for screening and analysis of electrical instruments and components.

«« Back to Applications