GB/T 14849.3-2020 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 14849.3-2020 | English | 155 |
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Methods for chemical analysis of silicon metal - Part 3: Determination of calcium content
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| GB/T 14849.3-2007 | English | 140 |
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Industrial silicon chemical analysis -- Part 3: Determination of calcium content
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| GB/T 14849.3-1993 | English | 239 |
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Silicon metal. Determination of calcium content
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GB/T 14849.3-2020: Methods for chemical analysis of silicon metal - Part 3: Determination of calcium content
---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/GBT14849.3-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.040.30
H 17
Replacing GB/T 14849.3-2007
Methods for chemical analysis of silicon metal - Part
3.Determination of calcium content
Issued on. MARCH 06, 2020
Implemented on. FEBRUARY 01, 2021
Issued by. State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Flame atomic absorption spectrometry... 5
4 Chlorophosphonazo I spectrophotometry... 9
5 Quality assurance and control... 13
6 Test report... 13
Foreword
GB/T 14849 “Methods for chemical analysis of industrial silicon” consists of the
following 11 parts.
- Part 1.Determination of iron content;
- Part 2.Determination of aluminum content - Chrome azurol S
spectrophotometric method;
- Part 3.Determination of calcium content;
- Part 4.Determination of elements content Inductively coupled plasma
atomic emission spectrometric method;
- Part 5.Determination of elements content—Analysis using an X-ray
fluorescence method;
- Part 6.Determination of carbon-Infrared absorption method;
- Part 7.Determination of phosphorus content - Phosphorus molybdenum
blue spectrophotometry;
- Part 8.Determination of copper content - Atomic absorption spectrometric
method;
- Part 9.Determination of titanium content - Diantipyryl methane
spectrophotometry;
- Part 10.Determination of mercury content - Atomic fluorescence
spectrometric method;
- Part 11.Determination of chromium content - Diphenylcarbazide
spectrophotometric method.
This Part is Part 3 of GB/T 14849.
This Part was drafted in accordance with the rules given in GB/T 1.1-2009.
This Part replaces GB/T 14849.3-2007 “Methods for chemical analysis of silicon
metal - Part 3.Determination of calcium content”. Compared with GB/T
14849.3-2007, in addition to editorial modifications, the main technical changes
are as follows.
- added warning;
- modified range of determination from 0.020%~0.30% to 0.0050%~0.55%
(see Clause 1 of this Edition, Clause 1 of Edition 2007);
- added normative references (see Clause 2 of this Edition);
- modified method summary (see 3.1 and 4.1 of this Edition, Clause 2 and
Clause 11 of Edition 2007);
- added requirements for analysis reagents and water (see 3.2 and 4.2 of
this Edition);
- modified precision (see 3.7 and 4.7 of this Edition, Clause 8 and Clause 17
of Edition 2007);
- added test report (see Clause 6 of this Edition).
This Part was proposed by China Nonferrous Metals Industry Association.
This Part shall be under the jurisdiction of National Technical Committee on
Non-ferrous Metals of Standardization Administration of China (SAC/TC 243).
The drafting organizations of this Part. Aluminum Corporation of China
Zhengzhou Nonferrous Metal Research Institute Co., Ltd., Kunming
Metallurgical Research Institute, Guangdong Industrial Analysis and Testing
Center, Guizhou Institute of Analysis and Testing, South China University of
Technology, Xi'an Hantang Analysis and Testing Co., Ltd., Changsha Research
Institute of Mining and Metallurgy Co., Ltd., Chinalco Shanxi New Materials Co.,
Ltd., Chinalco Luoyang Copper Processing Co., Ltd., North Mine Testing
Technology Co., Ltd., Chinalco Mining Co., Ltd., Shenzhen Zhongjin Lingnan
Nonferrous Metals Co., Ltd., Baotou Aluminum Industry Co., Ltd., Shandong
Nanshan Aluminum Industry Co., Ltd.
Main drafters of this Part. Shi Lei, Huang Puying, Liu Yingbo, Cui Hao, Hu
Zongxi, Zhang Xiaoping, Wang Zhengqiang, Dai Fengying, Han Xiao, Yang Xin,
Li Shaowen, Zhang Yingying, Wang Huihui, Yang Binghong, Gu Li, Cui Junfeng,
Zhang Xiaoguang, Wang Xue.
Versions of standard substituted by this Part are.
- GB/T 14849.3-1993, GB/T 14849.3-2007.
Methods for chemical analysis of silicon metal -
Part 3.Determination of calcium content
Warning - The personnel using this Part shall have practical experience
in formal laboratory work. This Part does not point out all possible
security issues. The user is responsible for taking appropriate safety and
health measures and ensuring compliance with the conditions stipulated
by relevant national laws and regulations.
1 Scope
This Part of GB/T 14849 specifies the method for determination of calcium
content in silicon metal.
This Part is applicable to determination of calcium content in silicon metal. The
range for determination is. 0.0050%~0.55%.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 8170, Rules of rounding off for numerical values & expression and
judgement of limiting values
3 Flame atomic absorption spectrometry
3.1 Method summary
Use hydrofluoric acid and nitric acid to dissolve test material. Perchloric acid
smokes to remove silicon and fluorine. Use nitric acid to dissolve the residue.
Use lanthanum salt to suppress aluminum interference. At a wavelength of
422.7nm of flame atomic absorption spectrometer, use air-acetylene flame to
measure the absorbance of calcium. Calculate the mass fraction of calcium.
3.2 Reagents and materials
Unless otherwise specified, in the analysis, it shall only use the confirmed
analytically-pure reagent AND distilled water or deionized water or equivalent-
pure water.
3.2.1 Perchloric acid (ρ=1.67g/L).
3.2.7 Calcium standard solution. Pipette 25.00mL of calcium standard stock
solution (3.2.6) in a 250mL volumetric flask. Use water to dilute to the scale.
Mix well. 1mL of this solution contains 50μg of calcium.
3.3 Instruments
3.3.1 Atomic absorption spectrometer, attached with calcium hollow cathode
lamp. Under the best working conditions of the instrument, any atomic
absorption spectrometer that can achieve the following indicators can be used.
3.3.2 Platinum dish, 100mL.
3.3.3 Teflon beaker, 250mL.
3.4 Specimen
The specimen shall be able to pass through a 0.149mm standard sieve. Use
magnet to remove iron.
3.5 Test steps
3.5.1 Test material
Weigh 0.50g of specimen (3.4), to the nearest of 0.0001g.
3.5.2 Number of determinations
Do two tests in parallel.
3.5.3 Blank test
Conduct blank test with test material (3.5.1).
3.5.4 Determination
3.6 Processing of test data
Calculate the mass fraction of calcium wCa according to formula (1).
3.7 Precision
3.7.1 Repeatability
Obtain the measured value of two independent test results under repeatability
conditions. Within the average range given in Table 2, the absolute difference
between the two test results does not exceed the repeatability limit (r).
4 Chlorophosphonazo I spectrophotometry
4.1 Method summary
Use hydrofluoric acid and nitric acid to decompose the test material. Perchloric
acid smokes to remove silicon and fluorine. Use hydrochloric acid to dissolve
the residue. Use triethanolamine, 1,10-phenanthroline, and acetylacetone to
mask interference elements. At pH10~pH10.5, calcium and chlorophosphonazo
I form a colored complex. Take the faded solution of EGTA-Pb as a reference.
4.2 Reagents and material
Unless otherwise specified, in the analysis, it shall only use the confirmed
analytically-pure reagent AND distilled water or deionized water or equivalent-
pure water.
4.2.1 Hydrofluoric acid (ρ=1.14g/mL).
4.2.2 Nitric acid (1+1).
4.2.3 Perchloric acid (1+1).
4.2.4 Hydrochloric acid (1+1).
4.2.5 Triethanolamine (1+3), stored in polyethylene bottles.
4.2.11 Calcium standard stock solution. Weigh 2.4970g of calcium carbonate
that has been dried at 105°C and cooled to room temperature in a dryer
(reference reagent, ≥99.95%). Place in a beaker. Add about 200mL of
water. Then add hydrochloric acid (4.2.4) dropwise to completely dissolve.
4.3 Instruments
4.4 Specimen
The specimen shall be able to pass a 0.149mm standard sieve. Use magnet to
remove iron.
4.5 Test steps
4.5.1 Test material
Weigh 1.0g of specimen (4.4), to the nearest of 0.0001g.
4.5.5 Drawing of working curve
4.5.5.1 Pipette 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL,
6.00mL of calcium standard solution (4.2.12) to respectively place in a set of
50mL volumetric flasks. The following shall be carried out according to
4.5.4.4~4.5.4.5.
5 Quality assurance and control
In analysis, use standard sample or control sample to verify. Or at least use
standard sample or control sample to verify the analysis method once every
year.
6 Test report
The test report shall give at least the following information.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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