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GB/T 14849.1-2007 English PDF (GBT14849.1-2007)

GB/T 14849.1-2007 English PDF (GBT14849.1-2007)

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GB/T 14849.1-2007: Methods for chemical analysis of silicon metal -- Part 1: Determination of iron content - 1, 10-phenanthrolion spectrophotometric method

This Part specifies the method for determination of iron content in silicon metal. This Part is applicable to the determination of iron content in silicon metal. Determination range (mass fraction): 0.10%~0.65%.
GB/T 14849.1-2007
GB
ICS 77.120.10
H 12
NATIONAL STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
Replacing GB/T 14849.1-1993
Methods for chemical analysis of silicon metal -
Part 1. Determination of Iron content - 1,
10-Phenanthrolion spectrophotometric method
ISSUED ON. OCTOBER 25, 2007
IMPLEMENTED ON. APRIL 1, 2008
Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China;
Committee of Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Method summary ... 4
3 Reagents ... 4
4 Instruments ... 5
5 Test sample ... 5
6 Analytical steps ... 5
7 Calculation of the analysis results ... 6
8 Precision ... 7
9 Quality assurance and control ... 7
Foreword
GB/T 14849 Methods for Chemical Analysis of Silicon Metal is divided into 4 parts. ?€? Part 1. Determination of iron content - 1, 10-phenanthroline spectrophotometric method;
?€? Part 2. Determination of aluminum content - chrome azurol-S spectrophotometric method;
?€? Part 3. Determination of calcium content - flame atomic absorption spectrometry, chlorophosphonazo I spectrophotometric method;
?€? Part 4. Inductively coupled plasma-atomic emission spectrometry to determine element content.
This is Part 1 of GB/T 14849.
This Part will replace GB/T 14849.1-1993 Silicon metal - Determination of iron content - 1,10-Phenanthroline spectrophotometric method. Comparison with GB/T 14849.1-1993, main changes are as follows.
?€? ?€?Repeatability?€? and ?€?quality assurance and control?€? are added.
This Part was proposed by China Nonferrous Metals Industry Association. This Part shall be under the jurisdiction of the National Technical Committee on Nonferrous Metals of Standardization.
This Part was responsibly drafted by Fushun Aluminium Co., Ltd.
Main drafters of this Part. Yang Limei, Yang Yuhong, Xu Tieling, and Ji Chunlei. The previous version of the standard replaced by this Part is as follows. ?€? GB/T 14849.1-1993
Methods for chemical analysis of silicon metal - Part 1.
Determination of Iron content - 1, 10-Phenanthrolion
spectrophotometric method
1 Scope
This Part specifies the method for determination of iron content in silicon metal. This Part is applicable to the determination of iron content in silicon metal. Determination range (mass fraction). 0.10%~0.65%.
2 Method??summary
The specimen is decomposed with hydrofluoric acid and nitric acid. Sulfuric acid?€?s smoking removes silicon, fluorine, etc. And the residue is dissolved with hydrochloric acid. USE hydroxylamine hydrochloride to reduce Fe (III) to Fe (II). In sub-acid medium of pH3-5, iron and 1, 10-phenanthroline form red complex compound. At wavelength of 510nm of the spectrophotometer, MEASURE the absorbance.
3 Reagents
3.1 Hydrofluoric acid (??1,14g/mL).
3.2 Nitric acid (1+1).
3.3 Sulfuric acid (1+1).
3.4 Hydrochloric acid (1+1).
3.5 Hydroxylamine hydrochloride solution (10g/L).
3.6 1,10-phenanthroline solution (2.5g/L). WEIGH 1.25g of 1,10-phenanthroline (C12H8O2??H2O) and PUT into a beaker. ADD 2mL of hydrochloric acid (3.4). ADD about 300mL of water. After dissolved, USE water to dilute to 500mL. MIX evenly. 3.7 Acetic acid-sodium acetate buffer solution. WEIGH 272g of sodium acetate (CH3COONa??3H2O) and PUT into a beaker. Add 500mL of water. After dissolved, FILTER into a 1000mL volumetric flask. ADD 240mL of glacial acetic acid (??1.05g/mL). USE water to dilute to the scale. MIX evenly.
3.8 Mixed chromogenic solution. Evenly MIX hydroxylamine hydrochloride solution (3.5), 1, 10-phenanthroline solution (3.6) and acetic acid-sodium acetate buffer solution (3.7) in V1 ?€? Volume of divided test solution, in unit of mL.
8 Precision
8.1 Repeatability
Under the repeatability condition, within the range of average value given as follows, for the determination values obtained from 2 independent test results, the absolute values of these 2 test results shall not exceed repeatability limit (r). The probability of exceeding repeatability limit (r) is no more than 5%. The repeatability limit (r) is obtained by linear interpolation or extrapolation according to the data in Table 2.
Table 2
Mass fraction of iron /% Repeatability limit r/%
0.184 0.017
0.334 0.023
0.502 0.023
8.2 Allowable difference
The difference value of analysis results among the laboratories shall not exceed the allowable difference listed in Table 3.
Table 3
Mass fraction of iron /% Allowable difference /%
0.100-0.300 0.030
>0.300-0.650 0.040
9 Quality??assurance??and??control
USE national standard sample or industry-level standard sample to check the validity of the analytical method standard every 6 months. When the process is out of control, FIND out the reasons. After correcting the error, REPEAT the checking.

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