QC/T 943-2013 PDF English
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QC/T 943-2013: Test methods of lead and cadmium 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/QCT943-2013
QC
ICS 43.020
T 05
INDUSTRY STANDARD
QC/T 943-2013
Test methods of lead and cadmium 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
1 Scope... 8
2 Normative references... 8
3 X-ray fluorescence spectrometry... 9
4 Measure the lead and cadmium in the materials of steel, copper and
copper alloy, aluminum and aluminum alloy - photoelectric direct reading
spectrometry... 11
5 Atomic absorption spectrometry, inductive coupling plasma atomic
emission spectroscopy or inductively coupled plasma mass
spectrometry - measure lead and cadmium... 14
6 Test report... 19
1 Scope
This Standard specifies the test method of lead and cadmium content in automobiles
materials.
"X-ray Fluorescence Spectrometry�� applies to the screening and rapid determination of
lead and cadmium content in automobiles materials.
��Photoelectric Direct Reading Spectrometry for the Determination of Lead, Cadmium in
Steel, Copper and Copper Alloys, Aluminum and Aluminum-Alloys�� applies to quantitative
detection of lead and cadmium content of steel, copper and copper alloys, aluminum and
aluminum alloy rods or aluminum alloy bulks in automobiles materials.
��Methods of atomic absorption spectrometry, inductively coupled plasma atomic emission
spectroscopy, or inductively coupled plasma mass spectrometry for the determination of
lead, cadmium content in automobiles materials�� applies to the quantitative detection of
lead and cadmium content in automobiles materials.
2 Normative references
The articles contained in the following documents have become part of this Standard
when they are quoted herein. For the dated documents so quoted, all the modifications
(Including all corrections) or revisions made thereafter shall be applicable to this Standard.
GB/T 602 Chemical reagent -- Preparations of standard solutions for impurity
GB/T 4336-2002 Standard test method for spark discharge atomic emission
spectrometric analysis of carbon and low-Alloy steel (routine method)
GB/T 7999-2007 Optical emission spectrometric analysis method of aluminum and
aluminum alloys
GB/T 8170 Rules of rounding off for numerical values & expression and judgement of
limiting values
GB/T 20066 Steel and iron -- Sampling and preparation of samples for the
determination of chemical composition
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
YS/T 482-2005 Methods for analysis of copper and copper alloys - The atomic
emission spectrometry
IEC 62321.2008 Ed.1.0 Electrotechnical products - Determination of levels of six
regulated substances (lead, mercury, cadmium, hexavalent chromium,
polybrominated biphenyls, polybrominated diphenyl ethers)
3 X-ray fluorescence spectrometry
3.1 Principle
Place the prepared samples in X-ray fluorescence spectrophotometer sample chamber.
According to the selected analytical model, conduct X-ray fluorescence spectroscopy
analysis for the lead and cadmium content in the samples. According to the screening
values, judge if the lead and cadmium content is qualified in the samples, and if it is
required for further accurate determination.
3.2 Reagents and materials
3.3 Instruments and equipment
3.3.1 X-ray fluorescence spectrophotometer.
3.3.2 Cutting machine.
3.3.3 Crushing equipment. Pulverizer, grinder.
3.3.4 Tableting machine. Working pressure is not less than 20Mpa.
3.4 Sample preparation
3.4.1 Principle of sample preparation.
3.4.2 Sample preparation method
3.4.2.1 Solid samples. Homogeneous samples may be determined directly by the X-ray
fluorescence spectrophotometer. The sample size must meet the requirements of X-ray
fluorescence spectrophotometer. In case of the sample is too big, it shall be processed
into a smaller size of ��10mm - �� 40mm, and with a smooth surface.
3.4.2.2 Fluid sample. PIPETTE a certain volume of liquid sample into the special plastic
cup. USE the polyester film of 6mm in thickness to support the bottom of sample cup.
COVER the cup with an aperture plastic cap. The thickness of the sample is not less than
15mm.
3.5 Analytical steps
3.5.1 Instrument preparation
TURN on the instrument in accordance with the operational specifications of the
instrument. PREHEAT the instrument to be stable.
3.5.2 Analyze the spectral line
For X-ray fluorescence spectrometry, the analysis spectral line is recommended to select
lead ; Cadmium.
3.5.3 Drawing of working curve
SELECT different content��s lead and cadmium standard substances that match the tested
sample matrix and have no less than 5 points. MEASURE the fluorescence intensity of
lead and cadmium in the standard substances in accordance with the measurement
conditions of X-ray fluorescence spectrometer. DRAW the working curve in accordance
with the given standard values by the standard substances and the measured
fluorescence intensity values by the spectrometer.
3.6 Analysis of result
3.6.1 Calculation of result
According to the selected analysis mode, CALCULATE the lead and cadmium content in
the sample, based on the measured spectral line intensity of elements lead and cadmium.
4 Measure the lead and cadmium in the materials of steel, copper and copper
alloy, aluminum and aluminum alloy - photoelectric direct reading spectrometry
4.1 Determination range of measuring the lead and cadmium in the materials of steel,
copper and copper alloy, aluminum and aluminum alloy by photoelectric direct reading
spectrometry is shown in Table 2.
4.2 Principle
After the processed sample is excited by light source, the radiated light enters into the
beam splitting system through the entrance slit to disperse into spectrum. CONDUCT the
photovoltaic conversion for the selected spectral lines by the photo-translating system and
measuring system. And measure the spectral line intensity. MEASURE the mass fraction
of elements lead and cadmium, according to the working curve made by corresponding
standard substances (standard samples).
4.3 Auxiliary materials
4.3.1 Standard substance (standard sample). It shall be a national or recognized
authoritative standard substance (standard sample). In principle, the standard substance
(standard sample) shall be basically consistent with the chemical composition and
metallurgical casting process of the analytical sample.
4.3.2 Control sample. The standard sample that has the exact constant value and has
a similar matrix and organization structure with the sample to be tested.
4.4 Instruments and equipment
4.4.1 Photoelectric direct reading spectrometer
4.4.2 Sample processing equipment. Grinding machine (sandpaper millstone, abrasive
band grinding machine), lathe or milling machine.
4.5 Sample preparation
Sample shall be prepared according to the requirements of GB/T 20066.The surface of
the taken sample shall ensure that it can excite 2 points without overlapping. And it can
completely cover the excitation hole, so as to ensure that the excitation chamber does not
leak gas.
4.6 Analytical steps
4.6.1 TURN on the instrument in accordance with the requirements of instrument
specifications. PREHEAT the instrument to be stable.
4.6.2 Before analysis, firstly USE a sample for continuous excitation and good
reproducibility. CONFIRM the instrument is in the best working condition.
4.6.3 According to the material type of sample, SELECT the corresponding
appropriate standard substances (standard samples).
4.6.4 According to the type of sample and alloy designation, SELECT the analytical
procedure.
4.6.5 Analysis of drift correction of curve. According to the type of sample to be tested,
SELECT the control sample. The control sample is continuously excited and has good
reproducibility. STORE the mean value, so as to confirm whether the analytical curve is
drifted.
4.6.6 Sample analysis
The sample shall be excited to measure at least twice. The mean value shall be used as
analysis results when the data is stable. The content is expressed by mass fraction (%).
Rounding off value is in accordance with GB / T 8170.
4.7 Precision
4.7.1 Repeatability
For the measured values of 11 independent test results obtained under repeatability
conditions, within the given measured range as follows, their relative standard deviation
shall not exceed the provisions of Table 3.
5 Atomic absorption spectrometry, inductive coupling plasma atomic emission spectroscopy or inductively
coupled plasma mass spectrometry - measure lead and cadmium
5.1 Principle
WEIGH appropriate amount of sample. USE dissolved acid to completely digest the
sample. PREPARE homogeneous solution. USE atomic absorption spectrometry,
inductive coupling plasma atomic emission spectroscopy, or inductively coupled plasma
mass spectrometry to measure lead and cadmium concentration in the solution.
5.2 Reagents and materials
Unless otherwise specified, in analysis, only USE recognized analytical pure reagent and
distilled water or deionized water or water with equivalent purity.
5.3 Instruments and equipment
5.4 Sample preparation
5.4.1 Metal material
The sample is processed to debris with a thickness not more than 1mm.
5.5 Analytical steps
5.5.1 Sample
WEIGH 0.10g -1.00g of specimen, accurate to 0.0001g.
5.5.2 Determination number of times
PERFORM twice independent determination. TAKE the average values.
5.5.3 Blank test
MAKE a blank test along with the specimen.
5.5.4 Determination
5.5.4.1 Preparing solution of metal material. PLACE the sample (5.5.1) in 250mL beaker.
ADD appropriate amount of dissolved acid to heat to dissolve. After the sample to be
tested is completely dissolved, REMOVE it into 100mL volumetric flask. DILUTE to the
scale with water and mix evenly.
5.5.4.2 Preparation of polymer solution. PLACE the specimen (5.5.1) into microwave
digestion tank. Respectively ADD 5mL of concentrated nitric acid, 1.5mL of tetrafluoro
boric acid solution and 1.5mL of hydrogen peroxide. For samples containing more
siliceous, it is required to add 1mL of tetrafluoro borate solution. If the sample contains a
large number of easily oxidized organic ingredients, it cannot add hydrogen peroxide.
CLOSE the digestion tank.
5.5.4.3 Preparation of coating solution
5.5.4.4 Preparation of rubber solution.
5.5.4.5 Measurement of specimen solution. MEASURE the absorbency and intensity
values of the lead and cadmium in the blank test solution along with the specimen and the
specimen solution WITH the atomic absorption spectrometer, inductive coupling plasma
atomic emission spectrometer, and inductively coupled plasma mass spectrometry. And
CHECK out the content of the lead and cadmium from the working curve.
5.5.5 Drawing of working curve
5.5.5.1 Preparation of standard solution working curve. According to the content of lead
and cadmium, PREPARE the standard solutions not less than 5 points and with different
concentration of lead and cadmium. If the sample matrix has interference on the
measured elements, it can use matrix matching method to eliminate the interference.
DILUTE with water to the scale. SHAKE evenly.
5.5.5.2 Preparation of working curve of standard substance. According to the material of
the sample to be tested, CHOOSE the standard substances not less than 5 points and
with different content of lead and cadmium. In accordance with the preparation method of
analysis specimen, PREPARE standard substance solutions. DILUTE to the scale with
water and mix evenly.
5.5.5.3 Measurement. ARRANGE the solutions of the standard solution working curve
and the solutions of standard substance working curve, based on the sequence from low
concentration to high concentration. MEASURE the absorbency or intensity value of the
lead and cadmium WITH the atomic absorption spectrometer, inductive coupling plasma
atomic emission spectrometer, and inductive coupling plasma mass spectrometer. TAKE
mass of lead and cadmium as the abscissa; and absorbance and intensity value as the
ordinate. DRAW the working curve.
5.6 Result calculation
According to Equation (1), CALULATE the mass fraction (%) of the lead and cadmium.
The calculated result is rounded in accordance with GB/T 8170.
5.7 Precision
Under the repeatability conditions, the absolute difference value between the 2
independent determination results shall not exceed 10% of the arithmetic mean value.
6 Test report
The test report shall include the following contents.
a) Sample description, laboratories, test date and other information;
b) The degree of complying the provisions of this standard;
c) Test results and its expression;
d) Abnormal phenomena observed in the test process.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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