# Presentation: 182768

## 电子电气产品中有毒有害物质检测方法Determination of Levels of Six Regulated Substances (Lead, Mercury, Hexavalent Chrominum, Polybrominated Biphenyls, Polybrominated Biphenyl Ether) in Electrotechnical Products 

- 郑建国  博士
- Dr. Zheng Jianguo
- Guangdong Entry-Exit Inspection & Quarantine Bureau, P.R.China

## Comparisons of Testing methods of ISO/IEC, GB and SN for RoHS 

- 13 methods in ISO/IEC 62321
- 12 methods in GB series standards
- 22 methods in SN series standards
- _[Details in Table 1](file:///C:/Documents%20and%20Settings/Jim%20Mathews/Local%20Settings/Temp/标准体系-表1.doc)__._

## SN series Standards for RoHS 

**Testing**
**Methods**

- Procedures of
- the mechanical
-  disjointment for
-  the determination
-  of regulated
- substances in
- electrotechnical
- products

**General **
**Requirements**

- Conformity
- Assessment

**lead, mercury, cadmium, **
**chromium**

**Chromium****(****VI****)**

**PBB**、**PBDE**

**screening**

**XRF**
**Spot-test**
**Spark**
**IR**

**ICP-AES**
**AAS**
**ICP-MS**
**CVAAS**
**AFS**

**UV-VIS**
**IC**

**GC-MS**
**LC-MS**
**GC-ECD**
**GC-FID**
**HPLC**

## 15 methods in SN series standards for RoHS have been finished:

**1****、****Determination of Chromium****(****VI****)****in electrical and electronic equipment—1,5-Diphenylcarbohydrazide spectrophotometry**
-   Cr (VI) compound was extracted from sample using basic extract solution  with shaking at 90°C~95°C water bath for 1.5 hours, which can react with 1,5-Diphenylcarbohydrazide to appear a kind of amaranthine complex in acid medium. Then, this complex was detected at wavelength 540 nm with UV spectrometry.

## 15 methods in SN series standards for RoHS have been finished:

**2、****Determination of mercury in electrical and electronic equipment—Hydride generation-atomic fluorescence spectrometry**
-   As** **to metal material in electrical and electronic equipment, it was digested with routine acid digestion. And to the other material, it was digested with airtight high-temperature press bomb. After digestion, mercury in sample material can be digested into dissoluble salt. And finally, obtained digestion solution was detected using Hydride generation-atomic fluorescence spectrometry.

## 15 methods in SN series standards for RoHS have been finished:

**3、****Determination of lead, cadmium and chromium in electrical and electronic equipment—Flame atomic absorption spectrometry**
-   As to metal material in electrical and electronic equipment, it was digested with routine acid digestion with concentrated nitric acid,and for the other material, it was digested with concentrated HNO3、H2O2 and HF(specially for the glass and chinaware material)at 180±5°C for 4 hours by using airtight high-temperature press bomb. After digestion, lead, cadmium and chromium in sample material can be digested into dissoluble salt. And finally, obtained digestion solution was detected using flame atomic absorption spectrometry.

## 15 methods in SN series standards for RoHS have been finished:

**4、****Qualitative screening of lead, mercury, cadmium, chromium and bromine in electrical and electronic equipment—Wavelength dispersive X-ray fluorescence spectrometry**
-   Based on the lead, mercury, cadmium, chromium and bromine’s characteristic X-ray lines, the wavelength dispersive x-ray fluorescence spectrometry (WDXRF) can be used for qualitative screening the prepared sample. When the element’s characteristic X-ray peak appears in the qualitative screening result, it approve that the element exist in the sample. When the element’s characteristic X-ray peak doesn’t appear in the qualitative screening result, it approve that the element’s content is lower than the detection limit of WDXRF.

## 15 methods in SN series standards for RoHS have been finished:

**5、****Determination of polybrominated biphenyls and polyborminated biphenyl ethers in electrical and electronic equipment—High Performance Liquid chromatography**
-   Technical flame retardants such as polybromo biphenyls and polybromo biphenyl ethers in electrical and electronic equipment were separated and determined by high performance liquid chromatography method. The samples were extracted with 150mL toluene in a soxhlet apparatus for three hours. The HPLC separation was achieved on a reversed-phase C18 column, applying gradient elution using a mixture of aqueous phosphate buffer and methanol with ultraviolet detection in the scanning mode at 226nm.

## 15 methods in SN series standards for RoHS have been finished:

**6、****Determination of polybrominated biphenyls and polyborminated biphenyl ethers in electrical and electronic equipment—Gas chromatography/Mass spectrometry**
-   The electrical and electronic equipment samples were extracted with 150mL toluene in a soxhlet apparatus for three hours. The extracted solution was purified by silica gel column and then concentrated in rotary vacuum evaporator. The residue was taken up in 2.0 mL toluene. Polybromo biphenyls and polybromo biphenyl ethers were separated and determined by Gas chromatography/Mass spectrometry.

## 15 methods in SN series standards for RoHS have been finished:

**7、****Determination of polybrominated biphenyls and polyborminated biphenyl ethers in electrical and electronic equipment****-****GC–FID**
- The electrical and electronic equipment samples were extracted with 150mL toluene in a soxhlet apparatus for three hours. The extracted solution was purified by silica gel column and then concentrated in rotary vacuum evaporator. Internal standard in 1.0 mL toluene was added to the residue, polybromo biphenyls and polybromo biphenyl ethers in the mixture were separated and determined by Gas chromatography with flame ion detector.

## 15 methods in SN series standards for RoHS have been finished:

**8、****Qualitative screening of polybrominated biphenyls and polyborminated biphenyl ether in electrical and electronic equipment by infra-red spectrometric method**
-   The method is to collect the infra-red spectrum of plastic part of the electric or electronic equipments, analyzing the polymeric component. Comparing the spectrum of the sample with the reference spectrum of the relative polymer, to determine whether the sample spectrum contains the characteristic peaks of the C-Br bond within the 650cm-1~500cm-1 region, and, to figure out whether the sample contains PBB or PBDE.

## 15 methods in SN series standards for RoHS have been finished:

- 9、Quantitative Screening of Lead, Mercury, Chromium, Cadmium and Bromine in Electrical and Electronic Equipment-X-Ray Fluorescence Spectrometric Method
-   Wavelength dispersive X-ray fluorescence spectrometry (WD-XRF) has been applied to the direct quantitative screening of lead(Pb), mercury(Hg), chromium(Cr), cadmium(Cd), bromine(Br) in electrical and electronic equipments. It covers all material types such as polymers, metals, and other electronic assembly materials. A series of six polymers reference materials and other matrix reference materials were prepared to make calibration curves. Determination of the elemental concentrations for the references and samples was analyzed by WD-XRF.

## 15 methods in SN series standards for RoHS have been finished:

**10、****Determination of polybrominated biphenyls and polybrominated diphenyl ethers in electrical and electronic equipment With HPLC/MS-MS**
**   **A HPLC/MS-MS method for the determination of polybrominated biphenyls and polybrominated diphenyl ethers in electrical and electronic equipments was established. The polybrominated biphenyls and polybrominated diphenyl ethers was extracted with toluene using ultrasonator from samples and detected by HPLC/MS-MS.

## 15 methods in SN series standards for RoHS have been finished:

**11****、****Determination of Lead and Cadmium in in electrical and electronic equipment by AFS**
- The method is used for he determination of **lead** and **Cadmium** in a) polymers; b) metal materials made from aluminium, iron and zinc matrices and c) electronics. The sample is digested and heated to exhausting the acids, then diluted properly. Ionic Cd in the sample solution reacts with KBH4 and generates volatile gas, which is introduced to atomizer with carrier gas (Ar). The content of cadmium is determined on the basis of fluorescence intensity of the element.
- Ionic Pb(II) in the sample solution is oxidized into Pb(IV) by potassium ferricyanide, then reacts with KBH4 and generates volatile hydride PbH4, which is introduced to atomizer with carrier gas (Ar). The content of lead is determined on the basis of fluorescence intensity of the element.

## 15 methods in SN series standards for RoHS have been finished:

**12****、****Determination of Lead, Cadmium, Chromium and Mercury in electrical and electronic equipment—Inductively coupled plasma atomic emission spectrometry**
-     The samples of polymer materials (such as PP, PE, PS, ABS, PVC, etc.) and electronics (such as glasses and ceramics, etc.) from Electronic and electrical equipment were digested under pressure with nitric acid, tetrafluoroborate solution and hydrogen peroxide in a tightly sealed PTFE vessel which was then put into the corrosion resisting steel pressure dissolution can. The pressure dissolution can as a whole was heated at 180°C for 4h in a constant temperature heating oven. The samples of metallic materials (such as iron alloys, copper alloys, aluminum alloys, zinc alloys and solder alloys, etc.) from Electronic and electrical equipment were digested by heating with reflux cooler and absorption vessels. The samples of polymer materials and electronics from Electronic and electrical equipment were digested under pressure with microwave sample preparation system. The method for the simultaneous determination of Pb, Cd, Cr, Hg in polymer materials, metallic materials and electronics from Electronic and electrical equipment have been developed

## 15 methods in SN series standards for RoHS have been finished:

**13、****Determination Of Mercury In Electrical And Electronic Equipment**
**-****Cold Vapor Atomic Absorption Spectrometry**
-   This standard provides the procedure for the determination of materials used in Electrical And Electronic Equipment. These materials are polymer materials, metal materials and electronics. Metal materials in electrotechnical equipment are treated by traditional digestion using acids. Other materials, such as polymers and electronics, were digested with acids, in microwave oven or in a sealed and high pressure autoclave. The mercury in the digestion solution is reduced to the atomic state before it is analyzed, then mercury is determined by Cold Vapor Atomic Absorption Spectrometry.

## 15 methods in SN series standards for RoHS have been finished:

**14****、****Technical Requirements for the Conformity Assessment of Certain Hazardous Substances in Electrical and Electronic Equipment**
- This standard specifies the general technical requirements for the conformity assessment of certain  hazardous substances in electrical and electronic equipments. For the purpose of determining the conformity of the products with relevant laws and regulations and evaluating the validity of the test results, the following items should be assessed and certified to be fully in compliance with specific technical requirements.

## 15 methods in SN series standards for RoHS have been finished:

**15、****Procedures of the mechanical disjointment for the determination of regulated substances in electrotechnical products**
- This part specifies the procedures and requirements of the mechanical disjointment of electrotechnical products into test units for chemical determination of certain regulated substances.
- This part deals with the mechanical disjointment of electrical and electronic products (including their parts and components) with rated voltage not exceeding 1 000 volts for alternating current and 1 500 volts for direct current;

- Thank you for your attention!

- This part deals with but is not limited to the following categories of products:
- large household electrical appliances
- small household electrical appliances
- information technology equipment and telecommunication equipment
- Consumer equipment
- Lighting equipment
- Electrical and electronic tools
- Toys, leisure and sports equipment
- Medical devices
- Monitoring and control instruments
- Automatic dispensers