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QC/T 941-2013: Test Method for Mercury in Automobiles Materials---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/QCT941-2013QC Automobile Industry Standard of the People’s Republic of China ICS 43.040 T 05 Test Method for Mercury in Automobiles Materials Issued on. OCTOBER 17, 2013 Implemented on. MARCH 1, 2014 Issued by. Ministry of Industry and Information Technology of the People's Republic of China Table of ContentsForeword... 6 Introduction... 7 1 Scope... 8 2 Normative References... 8 3 X-ray Fluorescence Spectrometric Method... 9 4 Cold Atomic Absorption Spectrometric Method, Atomic Fluorescence Spectrometric Method, Inductively Coupled Plasma Atomic Emission Spectrometric Method or Inductively Coupled Plasma Mass Spectrometric Method... 12 5 Direct Mercury Determination Method... 19 6 Test Report... 21 Annex A (Informative) Instrument Parameters Setting... 22ForewordThis Standard was drafted in accordance with the rules given in GB/T 1.1-2009, Directives for Standardization – Part 1.Structure and Drafting of Standards. This Standard includes 3 methods. Method 1, “X-ray Fluorescence Spectrometric Method”, was drafted by reference to GB/Z 21277-2007, Rapid Screening of Lead, Mercury, Chromium, Cadmium and Bromine of Regulated Substances in Electrical and Electronic Equipment – X-Ray Fluorescence Spectrometry; Method 2, “Cold Atomic Absorption Spectrometric Method, Atomic Fluorescence Spectrometric Method, Inductively Coupled Plasma Atomic Emission Spectrometric Method or Inductively Coupled Plasma Mass Spectrometric Method”, was drafted by reference to IEC 62321.2008 Ed. 1.0, Electrotechnical Products – Determination of Levels of Six Regulated Substances (Lead, Mercury, Cadmium, Hexavalent Chromium, Polybrominated Biphenyls and Polybrominated Diphenyl Ethers); and Method 3, “Direct Mercury Determination Method”, was drafted by reference to EPA 7473.2007, Determination of Mercury in Solids and Solutions by Thermal Decomposition, Amalgamation and Atomic Absorption Spectrophotometry. Annex A of this Standard is informative. This Standard was proposed by and shall be under the jurisdiction of the National Technical Committee of Auto Standardization (SAC/TC 114). The drafting organizations of this Standard. Chery Automobile Co., Ltd., China Automotive Technology & Research Center, Centre Testing International Group Co., Ltd., SGS Standards Technical Services Co., Ltd. and Pony Test Group Co., Ltd. The main drafters of this Standard. Song Xianzhi, Liu Yanrong, Gao Junhua, Wei Changqing, Lei Shuangshuang, Zhang Chunrong, Guo Miao, Guo Yong, Li Weidong and Song Wei.1 ScopeThis Standard specifies the test method for mercury in automobiles materials. The “X-ray Fluorescence Spectrometric Method” applies to screening and rapid determination of mercury contents in automobile materials. The “Cold Atomic Absorption Spectrometric Method, Atomic Fluorescence Spectrometric Method, Inductively Coupled Plasma Atomic Emission Spectrometric Method or Inductively Coupled Plasma Mass Spectrometric Method” applies to quantitative determination of mercury contents in automobile materials. The “Direct Mercury Determination Method” applies to quantitative determination of mercury contents of automobile materials.2 Normative ReferencesThe following documents are essential to the application of this standard. For dated references, only the dated editions apply to this standard. For undated references, the latest edition (including all amendments) applies to this standard. GB/T 8170 Rules of Rounding off for Numerical Values and Expression and Judgement of Limiting Values GB/T 30512-2014 Requirements for Prohibited Substances on Automobiles GB/Z 21277-2007 Rapid Screening of Lead Mercury Chromium Cadmium and Bromine of Regulated Substances in Electrical and Electronic Equipment – X-Ray Fluorescence Spectrometry IEC 62321.2008 Ed. 1.0, Electrotechnical Products – Determination of Levels of Six Regulated Substances (Lead, Mercury, Cadmium, Hexavalent Chromium, Polybrominated Biphenyls and Polybrominated Diphenyl Ethers) EPA 7473.2007, Determination of Mercury in Solids and Solutions by Thermal Decomposition, Amalgamation and Atomic Absorption Spectrophotometry3 X-ray Fluorescence Spectrometric Method3.1 Principle Place a sample prepared in the sample chamber of X-ray fluorescence spectrometer; carry out X-ray analysis for the sample in accordance with the analysis mode selected. Determine whether the mercury content (Hg) in the sample is acceptable in accordance with the screening limits of mercury element and whether further tests will be needed. 3.2 Reagents and materials 3.3 Instruments and equipment. 3.3.1 X-ray fluorescence spectrometer. 3.3.2 Cutter. 3.3.3 Liquid nitrogen low-temperature mill. 3.3.4 Grinder. wolfram carbide (WC) abrasive tools. 3.3.5 Tablet press. working pressure not lower than 20 MPa. 3.4 Sample preparation 3.4.1 Principles for sample preparation. 3.5.4 Calibration Before a sample is tested each time, use the standard substance (3.2.3) to calibrate standard curves. 3.5.5 Sample testing Place the sample prepared into the sample chamber; and carry out X-ray analysis for the sample in accordance with the selected mode, at least two times for each sample. 3.6 Result analysis 3.6.1 Result calculation Calculate the content of mercury element in the sample in accordance with the selected analysis mode, using the intensity of the spectral lines of mercury element measured.4 Cold Atomic Absorption Spectrometric Method, Atomic Fluorescence Spectrometric Method, Inductively Coupled Plasma Atomic Emission Spectrometric Method or Inductively Coupled Plasma Mass Spectrometric Method4.1 Principle Weigh an appropriate amount of sample; make a homogeneous sample solution after treatment by microwave digestion or wet reflux digestion. 4.2 Reagents and materials Unless otherwise specified, only reagents confirmed to be of analytical grade and distilled water or deionized water or equivalent water shall be used in the analysis. 4.2.1 Nitric acid. ρ is 1.40 g/mL. 4.2.2 Hydrochloride acid. ρ is 1.19 g/mg. 4.2.11 25 g/L potassium dichromate solution. weigh 2.5 g of potassium dichromate to dissolve in 100 mL of water. 4.2.12 Nitric acid-potassium dichromate solution. weigh 0.5 g of potassium dichromate to dissolve in water; add 50 mL of nitric acid solution (4.2.1); transfer to a 1000 mL volumetric flask; use water to dilute to scale; and shake up. 4.2.13 1% sodium hydroxide-3% sodium borohydride. use water to dissolve 1.0 g of sodium hydroxide in a 1000 mL plastic volumetric flask; add 3.0 g of sodium borohydride; stir to dissolve; use water to dilute to scale; and use immediately after preparation. 4.2.14 0.05% sodium hydroxide-1% potassium borohydride. use water to dissolve 0.05 g of sodium hydroxide in a 100 mL plastic volumetric flask; add 1.0 g of potassium borohydride; stir to dissolve; use water to dilute to scale; and use immediately after preparation. 4.3 Instruments and equipment 4.3.1 Microwave digestion system. 4.3.2 Cold Vapour atomic absorption spectrometer (CVAAS). 4.3.3 Atomic fluorescence spectrometer (AFS). 4.3.4 Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES/OES). 4.3.5 Inductively coupled plasma source mass spectrometer (ICP-MS). 4.3.6 Liquid nitrogen low-temperature mill. 4.4 Sample preparation 4.4.1 Sample pulverization Make a sample into test pieces of not larger than 1 mm x 1 mm x 1 mm or direct come to the next step of work for the metallic materials or inorganic non-metallic materials in other materials; use a liquid nitrogen low-temperature mill (4.3.8) to continue to pulverize into power of grain size smaller than 0.5 mm for the polymer materials and electronic materials in other materials and come to the next step of work after mixing up. 4.4.2 Sample solution preparation. 4.4.2.1 Preparation of sample solution for metallic materials. 4.5 Analytical procedure 4.5.1 Preparation of mercury standard solution. Use (5 + 95) nitric acid solution (4.2.7) to dilute mercury standard stock solution (4.2.16) [If a dissolved mercury oxide is used as the mercury stock solution, 0.5 mL of potassium dichromate (4.2.11) shall be added]; and prepare at least 5 concentrations of standard solution. 4.5.5 Sample determination After establishing the calibration curve, test blank solution and sample solution. Look up the corresponding concentrations from the calibration curve based on the signal readings of each sample. Each sample shall be tested independently twice at least. Take one sample at least in each batch of samples to conduct the test of adding standard recovery, the recovery rate between 90% and 110%. In the case of the cold atomic absorption spectrometric method or atomic fluorescence spectrometric method, mercury (Hg) shall be reduced to an atomic state with an appropriate method prior to analysis.5 Direct Mercury Determination Method5.1 Principle Weigh an appropriate amount of sample; place into an oxidation and decomposition furnace; use the heat and chemical action to decompose sample; absorb mercury in sample selectively before heating to release; use single-wavelength atomic absorption spectrophotometer to test the content of mercury in sample. 5.4 Sample preparation Take 100 mg (accurate to 0.1 mg) of a solid sample for general polymers and organic coatings to conduct tests, 500 mg at most. In the case of a liquid sample, take 100 μL (accurate to 1 μL) to conduct tests, 500 μL at most. 5.5 Analytical procedure 5.6 Result calculation The content of mercury in a solid sample is calculated in accordance with Formula (2). The content of mercury in a liquid sample is calculated in accordance with Formula (3). In the formula.6 Test ReportTest report shall include the following content. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. |
