HS/T 62-2019Determination of copper content in printed circuit board waste and scrap -- Wavelength dispersive X-Ray fluorescence spectrometry (English PDF)

Foreword

This standard was drafted in accordance with the rules given in HS/T 1-2011 and HS/T 39-2013.

This standard was proposed by the Customs Administration Department of the General Administration of Customs of the People's Republic of China.

This standard is under the jurisdiction of the Department of Policies and Regulations of the General Administration of Customs of the People's Republic of China.

Appendix A and Appendix B of this standard are informative appendices.

This standard was drafted. Chongqing Customs, People's Republic of China.

1 Scope

This standard specifies test methods for quantitative analysis of copper content in PCB waste and scrap.

This standard is applicable to the determination of copper content in PCB waste and scrap. The measurement range is 10.0 g/100g ~ 56.0 g/100g.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies to this article Pieces. For undated references, the latest version (including all amendments) applies to this document.

GB/T 6682 National Standard for Analytical Laboratory Water JY/T 016 General rules for wavelength-dispersive X-ray fluorescence spectroscopy

3 Principle

The crusher and ring grinder are used to crush and pre-process the PCB. After homogenization, the muffle furnace is used for burning. After burning, the ball is ground.

The instrument performs secondary pulverization, and then prepares as a fuse. The measured value is obtained by X-fluorescence quantitative analysis, and then the weighing value of the sample before and after burning, the elemental ratio of copper in copper oxide and X-fluorescence quantitative measurement calculate the copper content in the PCB.

4 Reagents and materials

Unless otherwise specified, the reagents used in this method are analytical grade, and the water is grade III water specified in GB/T 6682.

4.1 Lithium tetraborate (LiB4O7).

4.2 Lithium metaborate (LiBO2).

4.3 LiBr. Prepared as a solution with a mass fraction of 18 g/100g.

4.4 Lithium nitrate (LiNO3). formulated as a solution with a mass fraction of 22 g/100g.

4.5 Corundum crucible. 100 mL volume.

5 Equipment

5.1 Wavelength dispersion X-ray fluorescence spectrum. The composition and performance of the instrument should meet the requirements of JY/T 016.

5.2 Pulverizer. Sieve with 5 cm hole size.

5.3 Ring grinder. with tungsten carbide grinding head.

5.4 Ball mill. The maximum speed is not less than 500 rpm.

5.5 Electronic balance. Sensitivity 0.1 mg.

5.6 Muffle furnace. the maximum operating temperature is not less than 850 °C, and the cavity volume is not less than 30 L.

5.7 Automatic temperature control oven. The maximum use temperature is not lower than 110 °C.

5.8 Melt sample machine. The maximum operating temperature is not less than 1150 °C, with a crucible.

5.9 Standard sieve. 100 mesh.

HS/T XXXX-XXXX

5.10 Microsampler.

6 Analysis steps

7 Result representation

7.1 The copper content in the PCB is calculated according to formula (1).

XWK= x x x (1)

In the formula.

W-copper content (calculated as copper oxide) using an X-ray fluorescence spectrometer;

K-the coefficient of copper oxide converted to copper, calculated as 0.799 (calculated according to the latest international atomic weight table);

m1-the amount of sample weighed before burning, in grams (g);

m2-the amount of sample weighed after burning, the unit is gram (g);

X-The copper content (in terms of copper) in the PCB, the unit is grams per hundred grams (g/100g).

7.2 The result is retained to one digit after the decimal point. The arithmetic mean of the results of the two determinations is taken as the final result.

8 Precision

The analysis results are as follows. in the same laboratory, the same operator uses the same equipment, according to the same test method, and in a short time the absolute difference between independent test results obtained from the same measured object must not exceed 0.8 g/100g; in different laboratories, different operators the author uses different equipment and according to the same test method, the absolute difference between the test results obtained from the same test object must not exceed 1.5 g/100g.

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Appendix A

(Informative appendix) Standard Fuse Raw Material Proportion Table

Table A.1 Proportion of oxide raw materials used to configure standard fuses

Unit. g

Group

Oxide type

CuO SiO2 Al2O3 Fe2O3 CaO MgO 10% CuO 0.0400 0.2772 0.0478 0.0167 0.0116 0.0066 30% CuO 0.1200 0.1624 0.0736 0.0296 0.0052 0.0093 40% CuO 0.1600 0.1240 0.0055 0.0152 0.0050 0.0903 50% CuO 0.2000 0.0996 0.0053 0.0130 0.0113 0.0708 70% CuO 0.2800 0.0642 0.0162 0.0174 0.0110 0.0113 Appendix B (Informative appendix) Measurement condition table

Table B.1 Table of measurement conditions

Elemental analysis line Mask mm mode Voltage kV Current mA Spectroscopic crystal 2d (Å) Collimator detector PHA Peak position 2 theta (degrees) wavelength (Å) Cu KB1-Maj 28 Vac 50 24 4.026 0.23 SC 40 ~ 250 40.461 1.392 4 Mg KA1-HR-M in

28 Vac 30 100 55.1 0.46 F-PC 50 ~ 150 20.756 9.893

Al KA1-Maj 28 Vac 30 100 8.752 0.23 F-PC 50 ~ 150 144.639 8.339 3 Si KA1-Maj 28 Vac 30 100 8.752 0.46 F-PC 50 ~ 150 109.022 7.125 4 Ca KA1-HS -M in

28 Vac 50 60 4.026 0.46 F-PC 50 ~ 150 113.141 3.358 4 Fe KA1-Maj 28 Vac 50 10 4.026 0.23 SC 50 ~ 150 57.517 1.936 Ba LA1-HR-T

28 Vac 50 60 4.026 0.23 F-PC 50 ~ 150 87.177 2.777 7 Note. The measurement conditions in Table B.1 are Bruker S8 Tiger type instruments. The requirements of the instrument for the test environment are a temperature of 17 °C ~ 29 °C and a humidity of <= 60%;

Of users recommend using their own optimal measurement conditions.