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GB/T 14849.4-2014 PDF English

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GB/T 14849.4-2014: Methods for chemical analysis of silicon metal - Part 4: Determination of impurity contents - Inductively coupled plasma atomic emission spectrometric method
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GB/T 14849.4: Evolution and historical versions

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GB/T 14849.4-2014English130 Add to Cart 0-9 seconds. Auto-delivery Methods for chemical analysis of silicon metal - Part 4: Determination of impurity contents - Inductively coupled plasma atomic emission spectrometric method Valid
GB/T 14849.4-2008English90 Add to Cart 0-9 seconds. Auto-delivery Methods for chemical analysis of silicon metal -- Part 4: Determination of elements content Inductively coupled plasma atomic emission spectrometric method Obsolete

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GB/T 14849.4-2014: Methods for chemical analysis of silicon metal - Part 4: Determination of impurity contents - Inductively coupled plasma atomic emission spectrometric method


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NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.10 H 12 Partially replacing GB/T 14849.4-2008 Methods for chemical analysis of silicon metal - Part 4.Determination of impurity contents - Inductively coupled plasma atomic emission spectrometric method Issued on. DECEMBER 05, 2014 Implemented on. AUGUST 01, 2015 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of PRC; Standardization Administration of PRC.

Table of Contents

Foreword... 3 1 Scope... 5 2 Normative references... 5 3 Summary of method... 6 4 Reagents... 6 5 Instruments... 7 6 Specimen... 7 7 Analytical procedures... 8 8 Calculation of analytical results... 10 9 Precision... 11 10 Quality assurance and control... 12 11 Test report... 12 Appendix A (Informative) Preparation of standard stock solutions... 13 Appendix B (Informative) Instrument’s working conditions... 17

Foreword

GB/T 14849 "Industrial Silicon Chemical Analysis Method" is divided into 9 parts. - Part 1.Determination of iron content - 1,10-Phenanthrolion spectrophotometric method; - Part 2.Determination of aluminum content - Chrome azurol S spectrophotometric method; - Part 3.Determination of calcium content - Flame atomic absorption spectrometric method, chlorophosphonazo I spectrophotometric method; - Part 4.Determination of impurity contents - Inductively coupled plasma atomic emission spectrometric method; - Part 5.Determination of impurity contents - X-ray fluorescence method; - Part 6.Determination of mercury content - Atomic fluorescence spectrometric 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. This part is the part 4 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 14849.4-2008 "Method for chemical analysis of silicon metal - Part 4.Determination of elements content - Inductively coupled plasma atomic emission spectrometric method". As compared with GB/T 14849.4-2008, the main technical changes are as follows. - ADD the testing of copper, chromium, vanadium, magnesium, cobalt, phosphorus, potassium, sodium, lead, zinc, boron; - ADD two sample dissolution methods; - ADD the experimental data of repeatability limit and reproducibility limit. This part shall be under the jurisdiction of the National Nonferrous Metals Standardization Technical Committee (SAC/TC 243). Responsible drafting organizations of this part. Kunming Metallurgical Research Institute, China Aluminum Corporation Zhengzhou Research Institute, Kunming Yeyan New Materials Co., Ltd. Participated drafting organizations of this part. Yunnan Entry-Exit Inspection and Quarantine Bureau Technology Center, Tongbiao Standard Technology Service Co., Ltd., Zhejiang Hesheng Silicon Industry Co., Ltd., Yunnan Yongchang Silicon Industry Co., Ltd. Main drafters of this part. Liu Weili, Wang Jinrong, Li Yueping, Zhao Deping, Yang Yi, Zhao Jianwei, Wang Yunzhou, Wang Honglei, Nie Changhong, Liu Yingbo, Lu Guohong, Wu Yuqiang, Zhang Yunhui, Tan Shaoji, Cheng Zhiwu, Zhou Jie. This standard replaces the standard previously issued as follows. - GB/T 14849.4-2008. Methods for chemical analysis of silicon metal - Part 4.Determination of impurity contents - Inductively coupled plasma atomic emission spectrometric method

1 Scope

This part of GB/T 14849 specifies the determination methods of iron, aluminum, calcium, manganese, titanium, nickel, copper, chromium, vanadium, magnesium, cobalt, phosphorus, potassium, sodium, lead, zinc, boron in industrial silicon. This part applies to the determination of iron, aluminum, calcium, manganese, titanium, nickel, copper, chromium, vanadium, magnesium, cobalt, phosphorus, potassium, sodium, lead, zinc, boron in industrial silicon. The measurement range of each element is as shown in Table 1. Table 1 -- Measurement range Element Mass fraction / % Element Mass fraction / % Iron 0.020 ~ 1.00 Magnesium 0.0010 ~ 0.50 Aluminum 0.020 ~ 1.00 Cobalt 0.0005 ~ 0.20 Calcium 0.010 ~ 1.00 Phosphorus 0.0010 ~ 0.10 Manganese 0.0050 ~ 0.50 Potassium 0.0010 ~ 0.50 Titanium 0.0050 ~ 0.50 Sodium 0.0010 ~ 0.50 Nickel 0.0050 ~ 0.50 Lead 0.0030 ~ 0.10 Copper 0.0010 ~ 0.50 Zinc 0.0010 ~ 0.50 Chromium 0.0010 ~ 0.50 Boron 0.0005 ~ 0.20 Vanadium 0.0005 ~ 0.20 - -

2 Normative references

The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this standard. GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 8170 Rules of rounding off for numerical values & expression and judgement of limiting values

3 Summary of method

The sample is dissolved by the use of hydrofluoric acid or nitric acid. The perchloric acid is smoked to remove silicon, fluorine, etc.

4 Reagents

The reagents and water used in this standard refer to, unless otherwise specified, the analytical reagents and the grade water as specified in GB/T 6682. 4.1 Perchloric acid (ρ = 1.67 g/mL), excellent grade pure. 4.9 Sodium hydroxide solution (400 g/L). 4.10 Metal iron (Fe ≥ 99.99%). 4.11 Metal aluminum (Al ≥ 99.99%). 4.12 Calcium carbonate (base reagent or excellent grade pure). 4.13 Metal manganese (Mn ≥ 99.99%). 4.14 Metal titanium (Ti ≥ 99.99%). 4.15 Metal nickel (Ni ≥ 99.99%). 4.16 Metal copper (Cu ≥ 99.99%). 4.17 Potassium dichromate (base reagent or excellent grade pure). 4.22 Potassium chloride (spectral pure). 4.23 Sodium chloride (spectral pure). 4.24 Metal lead (Pb ≥ 99.99%). 4.25 Metal zinc (Zn ≥ 99.99%). 4.26 Boric acid (Excellent grade pure). 4.29 Standard solution B. Dilute the standard stock solution (4.6) to 10 μg/mL and maintain a consistent acidity (dilute it before use) with the standard stock solution.

5 Instruments

Inductively coupled plasma optical emission spectrometer. Light source. Plasma source, using power of 750 W ~ 1750 W.

6 Specimen

The specimen shall pass through a 0.149 mm standard sieve.

7 Analytical procedures

7.1 Samples According to the preparation method (7.4) of the analytical test solution, analyze the weighed sample amount and the constant volume of different elements, which shall comply with the requirements of Table 2.The weighed sample amount is accurate to 0.0001 g. 7.2 Number of measurements Perform two measurements independently and take the average. 7.3 Blank test Carry out the blank test along with the sample. 7.4 Preparation of analytical test solution 7.5 Preparation of series standard solution 7.5.1 Add a suitable amount of standard solution B (4.29) to a set of 100 mL volumetric flask. The medium and acidity are the same as the sample solution. Use water to dilute it to the mark. Shake it uniformly. Use the specimen in which no standard solution is added as the blank solution. The content of the element to be determined shall be within the range of the plotted working curve. The amount of the series standard solution is determined by the accuracy requirements. Take at least 6 points. 7.6 Determination 7.6.1 The recommended analytical lines for each element to be tested are as shown in Table 3. 7.6.2 Determination conditions

8 Calculation of analytical results

Calculate the mass fraction of the element to be tested according to formula (1). The value is expressed in %. The value is expressed and judged according to the GB/T 8170 numerical rounding off rule and limit value.

9 Precision

9.1 Repeatability limit The measured values of two independent tests are obtained under repetitive conditions. 9.2 Reproducibility limits The absolute difference between two independent test results obtained under Mass fraction / % reproducibility conditions is not greater than the reproducibility limit (R), wherein the case in which the reproducibility limit (R) is exceeded does not beyond 5%. The reproducibility limit (R) is obtained according to the data of Table 5 by the use of linear interpolation.

10 Quality assurance and control

Use the self-made control standards (if there is national grade or industrial grade standard sample, it shall be used firstly) to check the validity of the analytical method of this standard. When the process is out of control, it shall find the cause, correct the error, carry out verification again. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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