GB/T 33351.2-2021Determination of arsenic, beryllium, antimony in electrical and electronic products—Part 2: Inductively coupled plasma optical emission spectrometry (English PDF)

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.

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 document. 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). rho=1.40g/mL.

4.2 Hydrogen peroxide (H2O2). rho=1.10g/mL, 30% (mass fraction).

4.4 Hydrofluoric acid (HF). rho=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.

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.

5.4 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

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.

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