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GB/T 33351.2-2021: Determination of arsenic, beryllium, antimony in electrical and electronic products - Part 2: Inductively coupled plasma optical emission spectrometry
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Determination of arsenic, beryllium, antimony in electrical and electronic products - Part 2: Inductively coupled plasma optical emission spectrometry
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GB/T 33351.2-2021
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Basic data | Standard ID | GB/T 33351.2-2021 (GB/T33351.2-2021) | | Description (Translated English) | Determination of arsenic, beryllium, antimony in electrical and electronic products - Part 2: Inductively coupled plasma optical emission spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | L10 | | Word Count Estimation | 9,919 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 33351.2-2021: Determination of arsenic, beryllium, antimony in electrical and electronic products - Part 2: Inductively coupled plasma optical emission spectrometry
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Determination of arsenic, beryllium, antimony in electrical and electronic products-Part 2.Inductively coupled plasma optical emission spectrometry
ICS 31.020
L10
National Standards of People's Republic of China
Determination of arsenic, beryllium and antimony in electronic and electrical products
Part 2.Inductively coupled plasma emission spectrometry
Released on 2021-04-30
2021-11-01 implementation
State Administration of Market Supervision and Administration
Issued by the National Standardization Management Committee
Foreword
GB/T 33351 "Determination of Arsenic, Beryllium and Antimony in Electronic and Electrical Products" is divided into the following parts.
---Part 1.Inductively coupled plasma mass spectrometry;
---Part 2.Inductively coupled plasma emission spectrometry.
This part is Part 2 of GB/T 33351.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents.
This part is proposed and managed by the National Environmental Standardization Technical Committee for Electrical and Electronic Products and Systems (SAC/TC297).
Drafting organizations of this section. China Electronics Standardization Institute, Shenzhen Saixi Information Technology Co., Ltd., China National Certification for Conformity Assessment
Ke Center, China Academy of Information and Communications Technology, China Household Electrical Appliances Research Institute, BOE Technology Group Co., Ltd., Zibo Product Quality Supervision
Supervise the inspection office.
The main drafters of this section. Cheng Tao, Liu Jia, Cao Rui, Gao Jian, Zhao Junsha, Li Yue, Gao Yaxin, Lu Chunyang, Cao Yanxin, Li Jianghao, Wang Lian.
Determination of arsenic, beryllium and antimony in electronic and electrical products
Part 2.Inductively coupled plasma emission spectrometry
Warning---The personnel using this section should have practical experience in formal laboratory work. This section does not point out all possible safety issues
question. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.
1 Scope
This part of GB/T 33351 specifies the inductively coupled plasma emission spectroscopy (ICP-
OES) Measuring method.
This section applies to the determination of arsenic, beryllium and antimony in electronic and electrical products.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
IEC 62321-2 Determination of certain substances in electrical products Part 2.Disassembly, disassembly and mechanical sample preparation (Determination of
certainsubstancesinelectrotechnicalproducts-Part 2.Disassembly,disjointmentand mechanical
samplepreparation)
3 Principle
Microwave digestion is used for polymer, ceramic and glass samples in electronic and electrical products, and acid digestion is used for metal samples.
Process to obtain sample digestion solution. Then use an inductively coupled plasma emission spectrometer to determine the arsenic, beryllium, and antimony in the sample digestion solution.
The external standard method was used for quantification.
4 Reagents or materials
Except for the special provisions of this section, all reagents of analytical grade and above are used, and the experimental water should meet the secondary water specified in GB/T 6682.
4.1 Nitric acid (HNO3). ρ=1.40g/mL.
4.2 Hydrogen peroxide (H2O2). ρ=1.10g/mL, 30% (mass fraction).
4.3 Hydrochloric acid (HCl). ρ=1.19g/mL.
4.4 Hydrofluoric acid (HF). ρ=1.18g/mL.
4.5 Mixed acid. Take 1 volume of nitric acid (see 4.1) and 3 volumes of hydrochloric acid (see 4.3) and mix.
4.6 Standard solution of single element of arsenic. 100μg/mL.
4.7 Beryllium single element standard solution. 100μg/mL.
4.8 Antimony single element standard solution. 100μg/mL.
5 Equipment
5.1 Analytical balance. the accuracy is 0.0001g.
5.2 Microwave digestion apparatus. Equipped with sample holder and polytetrafluoroethylene/tetrafluoroethylene (PTFE/T FM) or perfluoroalkoxy polymer/tetrafluoroethylene
High pressure vessel of ethylene (PFA/T FM) or other fluorocarbon materials.
5.3 Electric heating plate.
5.4 Acid catcher.
5.5 Glass measuring tools. Class A or equivalent products with acceptable precision and accuracy. Other capacity equipment (such as automatic diluter) as long as it has
It can also be used with the same precision and accuracy.
5.6 Pipette.
5.7 Inductively coupled plasma emission spectrometer (ICP-OES). consists of a hydrofluoric acid-resistant sampling system, plasma torch tube, atomization chamber, atomizer,
It is composed of optical components, detectors, system control and data output devices.
5.8 Argon. The purity is greater than 99.99% (volume fraction).
6 samples
6.1 Mechanical pretreatment
The samples used for the determination should be mechanically pretreated.
IEC 62321-2 specifies the method to complete.
6.2 Chemical treatment
6.2.1 Polymer samples
6.2.1.1 Acid digestion method
Weigh 0.5g~1g (accurate to 0.0001g) sample, put it into a 100mL beaker, add 25mL mixed acid (see 4.5), cover the table
Flour bowl, heat to dissolve. After the dissolution is complete and cooled, transfer the solution into a 25mL volumetric flask, and wash the watch glass and the wall of the cup with water at least three times.
And transfer the washing liquid to the volumetric flask, add water to the volumetric flask scale, mix well, and wait for the test.
6.2.1.2 Microwave digestion method
Weigh 0.1g~0.2g (accurate to 0.0001g) sample, put it in the digestion tank, add 9mL nitric acid (see 4.1), 1mL peroxygen
Hydrogen (see 4.2), put it into the microwave digestion apparatus and perform microwave digestion on the sample according to the set digestion program. Refer to Appendix A for the digestion procedure. Such as
If a few samples are not completely digested, after the digestion tank is cooled to room temperature, add 1 mL of nitric acid (see 4.1) and 0.5 mL of peroxygen to it.
Hydrogen (see 4.2), put it into the microwave digestion apparatus and run the digestion program again to ensure that the sample is completely digested. After the digestion is complete, wait for the solution to cool to the room
Warm, transfer the solution to a 25mL volumetric flask, wash the inner wall of the digestion tank at least three times with water, transfer the washing solution to the volumetric flask, and add water
To the scale of the volumetric flask, mix well, and wait for measurement.
Note. Hydrogen peroxide can only be added when the reaction components of the sample are known. Hydrogen peroxide can react quickly and violently with easily oxidizable materials. If so
If the product contains a lot of easily oxidizable organic components, hydrogen peroxide should not be added. The type and volume of the acid used for digestion can be based on the sample matrix, the amount of the sample, and the amount used.
Microwave digestion apparatus, etc. are different. For example, for samples containing Si, Zr, W and other elements, adding 1 mL of HF will help complete the digestion.
6.2.2 Metal samples
Using the acid digestion method, the digestion reagents include nitric acid (see 4.1), hydrogen peroxide (see 4.2) and hydrochloric acid (see 4.3) and other reagents or
Several types can be adjusted according to the composition of the matrix. Weigh 0.5g~1g (accurate to 0.0001g) metal sample and put it into a 100mL beaker
in. Solder samples, use 25mL nitric acid (see 4.1) and 5mL hydrogen peroxide (see 4.2) for digestion. The sample of copper matrix adopts
10mL water and 10mL nitric acid (see 4.1) for digestion. The iron matrix sample uses 25mL hydrochloric acid (see 4.3) and 15mL hydrogen peroxide
(See 4.2) for digestion. The sample of zinc matrix is digested with 25 mL of hydrochloric acid (see 4.3). Transfer the solution after the sample is completely dissolved
Into a 25mL volumetric flask, and wash the watch glass and the wall of the cup with water at least three times, transfer the washing liquid to the volumetric flask, and add water to the volumetric flask.
Degree, mixing, to be tested.
6.2.3 Ceramic and glass samples
Using microwave digestion method. Take 0.1g~0.2g (accurate to 0.0001g) ceramic or glass sample in the digestion tank, add 5mL nitric acid
(See 4.1), 1mL of hydrofluoric acid (see 4.4), 1mL of hydrogen peroxide (see 4.2), cover the sealing plug, and put it into the microwave digestion apparatus to digest according to the setting
The program microwave digestion of the sample, see Appendix B for the microwave digestion program. After the digestion program is finished, wait for the digestion tank to cool to room temperature, and use
The water cleans the inner wall of the digestion tank at least three times, and the solution is combined and placed on the acid scavenger to heat the acid to make the sample solution slowly evaporate to about 1 mL.
Right, then transfer the sample to a 25mL volumetric flask, wash the inner wall of the digestion tank with water at least three times, and transfer the washing liquid to the volumetric flask.
Add water to the scale of the volumetric flask, mix well, and wait for measurement.
6.2.4 Blank solution
Except that no sample is added, the blank solution is prepared according to the above pretreatment steps.
7 Preparation of standard curve
Use a pipette to pipette a certain amount of arsenic single element standard solution (see 4.6), beryllium single element standard solution (see 4.7), antimony single element standard solution
(See 4.8). Dilute with dilute nitric acid to form standard solutions of different concentrations. The concentration of dilute nitric acid should match the sample matrix. Measure and draw standard work
Draw a curve, and the specific concentration of the standard series is shown in Table 1.The standard solution series are prepared for immediate use, or used within the verified validity period. for
For high-salt samples, the standard solution should match the matrix of the sample, or use the internal standard method for testing.
Table 1 Standard series concentration
8 Determination
Turn on the ICP-OES instrument and optimize the instrument condition parameters. For working parameters, please refer to Appendix C. It should be noted that the instrument used
The working parameters may be different depending on the conditions. The set parameters should ensure the effective measurement of the elements to be tested. After the instrument is stable,
Standard and sample digestion solutions are measured. When using ICP-OES for measurement, the wavelengths of the measured elements arsenic, beryllium, and antimony should be selected as
188.98nm, 313.11nm, 206.84nm, for the test solution containing hydrofluoric acid content, the use of hydrofluoric acid resistant injection system. If the result is determined
If it exceeds the calibration curve range, the sample solution should be diluted to an appropriate concentration. For the blank test, except for no sample, the other tests are all according to
The above steps are carried out.
9 Result calculation
The content of arsenic, beryllium, and antimony in the sample is calculated by mass fraction X, and the unit is expressed in milligrams per kilogram (mg/kg), calculated according to formula (1).
Where.
c1---The concentration value of the measured element in the sample solution, in milligrams per liter (mg/L);
c0---The concentration value of the measured element in the method blank, in milligrams per liter (mg/L);
V---The volume of the test solution during the measurement, in milliliters (mL);
f---The dilution factor of the sample solution (test solution);
m---The weight of the sample, in grams (g).
The result retains 3 significant digits.
10 Precision and method detection limit
10.1 Precision
In the same laboratory, the same operator uses the same equipment, according to the same test method, and compares the same object under test in a short period of time.
The absolute difference between the two independent test results obtained by mutually independent tests is not greater than the arithmetic mean of the two measured values
Of 10%.
10.2 Method detection limit
The detection limits of arsenic, beryllium, and antimony are shown in Table 2.
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