QC/T 941-2013 PDF English
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QC/T 941-2013 | English | 165 |
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Test Method for Mercury in Automobiles Materials
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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/QCT941-2013
QC
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 Contents
Foreword... 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... 22
Foreword
This 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 Scope
This 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 References
The 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 Spectrophotometry
3 X-ray Fluorescence Spectrometric Method
3.1 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 Method
4.1 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 Method
5.1 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 Report
Test 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.
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