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HST62-2019: Determination of copper content in printed circuit board waste and scrap -- Wavelength dispersive X-Ray fluorescence spectrometry
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HS/T 62-2019 | English | 179 |
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Determination of copper content in printed circuit board waste and scrap -- Wavelength dispersive X-Ray fluorescence spectrometry
| Valid |
HS/T 62-2019
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PDF similar to HST62-2019
Standard similar to HST62-2019 GB/T 40260 GB 38508 GB/T 3634.1 Basic data | Standard ID | HS/T 62-2019 (HS/T62-2019) | | Description (Translated English) | Determination of copper content in printed circuit board waste and scrap -- Wavelength dispersive X-Ray fluorescence spectrometry | | Sector / Industry | Customs Industry Standard (Recommended) | | Classification of Chinese Standard | G85/89 | | Word Count Estimation | 7,789 | | Date of Issue | 2019-12-19 | | Date of Implementation | 2020-06-01 | | Regulation (derived from) | General Administration of Customs Announcement No. 201 of 2019 | | Issuing agency(ies) | General Administration of Customs | HST62-2019: Determination of copper content in printed circuit board waste and scrap -- Wavelength dispersive X-Ray fluorescence spectrometry
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Determination of copper content in printed circuit board (PCB) waste and scrap-wavelength dispersion X-ray fluorescence spectrometry)
ICS 71.040.50
G 85/89
Customs Industry Standards of the People's Republic of China
HS
Method for determination of copper content in printed circuit board (PCB) waste and scrap
--Wavelength dispersion X-ray fluorescence spectrometry
Determination of copper content in printed circuit board waste and scrap
-Wavelength dispersive X-Ray fluorescence spectrometry
2019-12-19 released
2020-06-01 implementation
Published by the General Administration of Customs of the People's Republic of China
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.
The main drafters of this standard. Tu Jianglei, Lu Daguang, Wu Bock, Zhang Yu, Dong Jianwen, Yuan Weizhi, Li Yi, Tang Chenglin, Deng Jin, Deng
Ji Kuan and Li Dong.
Method for determination of copper content in printed circuit board (PCB) waste and scrap
--Wavelength dispersion X-ray fluorescence spectrometry
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.
4.6 Platinum-gold alloy crucible (95% P 5% Au)
4.7 Desiccator. An effective desiccant is included.
4.8 Reference materials. copper oxide (CuO), silicon dioxide (SiO2), aluminum oxide (Al2O3), iron oxide (Fe2O3), oxygen
Calcium (CaO), magnesium oxide (MgO).
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 ℃, 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 ℃.
5.8 Melt sample machine. The maximum operating temperature is not less than 1150 ℃, with a crucible.
5.9 Standard sieve. 100 mesh.
HS/T XXXX-XXXX
5.10 Microsampler.
6 Analysis steps
6.1 Sample preparation
6.1.1 Crush
A 1 kg sample was weighed and pulverized into an irregular block and powder with a maximum diameter of 5 cm by a pulverizer (5.2), and recorded as sample a.
6.1.2 Ring grinding
The sample a was put into a ring mill, and the obtained powder was passed through a 100-target sieve, and recorded as sample b.
6.1.3 Burn
The following steps are started, and two samples are tested in parallel.
6.1.3.1 Take sample b in an oven at 101 ℃ ～ 105 ℃, dry it for 2 hours, take it out, cool to room temperature in a desiccator, and weigh about 3 g.
Record the weight as m1 (to the nearest 0.1 mg).
6.1.3.2 After weighing, put it into the corundum crucible (4.5) and place it in a muffle furnace for burning. The burning temperature is 775 ℃ ～ 825 ℃. The burning time
For 10 h. After taking it out, cool it to room temperature in a desiccator and weigh it. Record the weight as m2 (accurate to 0.1 mg).
c.
6.1.4 Ball milling
The sample c was ball-milled. The rotation speed was set to 500 r/min and the ball-milling time was 2 minutes. The sample obtained by the ball-milling was recorded as sample d.
6.1.5 Fuse
6.1.5.1 Put sample d in an oven at 101 ℃ ~ 105 ℃, dry it for 2 hours, and take it out. Cool it in a desiccator to room temperature before weighing.
6.1.5.2 Prepare lithium tetraborate and lithium metaborate as a mixture of lithium borate in a ratio of 67.33; weigh 0.4 g of dry sample d (standard
To the nearest 0.1 mg), weigh 6 g of lithium borate mixed flux (accurate to 0.1 mg), mix uniformly, and drop in lithium bromide with a micro sampler.
The solution and lithium nitrate solution are each 1 mL. All weighing and mixing processes should be completed in a platinum-gold alloy crucible (4.6).
6.1.5.3 Put the crucible (4.6) with the sample into the melting sample machine. The recommended melting temperature is 1050 ℃ and the melting time is 10 minutes.
After the melting is completed, the sample in the crucible is poured into the mold, taken out after cooling, and directly formed or poured into a measurable sample piece.
6.2 Determination
6.2.1 Draw a standard curve
Refer to Table A.1 in Appendix A for the proportions of the five groups. Weigh the reference material (4.8) (accurate to 0.1 mg), mix well, and follow 6.1.5
The method was used to prepare a standard fuse, and a standard curve was measured and drawn.
6.2.2 Sample determination
Select an appropriate standard fuse (6.2.1) for instrument drift correction. The calibration interval can be determined according to the stability of the instrument. Test
The tablet is measured, and the result is calculated as copper oxide and recorded as W (four significant digits are retained). The test conditions of the instrument are shown in Table B.1 in Appendix B.
Or for those who use more advanced instruments, they should choose according to the optimization method of the instrument manufacturer.
7 result representation
7.1 The copper content in the PCB is calculated according to formula (1).
XWK (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.
HS/T XXXX-XXXX
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
θ (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 ℃ ~ 29 ℃ and a humidity of ≤ 60%;
Of users recommend using their own optimal measurement conditions.
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