GB/T 14849.4-2008 English PDF (GB/T14849.4-2008)

GB/T 14849.4-2008: Methods for chemical analysis of silicon metal -- Part 4: Determination of elements content Inductively coupled plasma atomic emission spectrometric method
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GB/T 14849.4-2008
GB
ICS 77.120.10
H 17
National Standard
of the People’s Republic of China
Methods for chemical analysis of silicon metal - Part 4.
Determination of elements content inductively coupled
plasma atomic emission spectrometric method
ISSUED ON. JUNE 9, 2008
IMPLEMENTED ON. DECEMBER 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  Sample ... 5 
6  Analytical steps ... 5 
7  Calculation of the analysis results ... 7 
8  Precision ... 7 
Annex A ... 9 
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 Part is Part 4.
Appendix A of this Part is informative.
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.
Responsible drafting organizations of this Part. Zhengzhou Research Institute of
CHALCO, and Quality Research Institute of China Nonferrous Metals Industry Standard
and Measurement.
Participating drafting organizations of this Part. Northeast Light Alloy Co., Ltd., Baotou
Aluminium Co., Ltd. Southwest Aluminum (Group) Co., Ltd., and Shanxi Jinneng Group
Datong Energy Development Co., Ltd.
Main drafters of this Part. Li Yueping, Shi Lei, Zhang Shuchao, Zhang Jie, Wu Yuqiang,
Zhou Bing, Jiang Wei, Jin Jianhua, Liu Shuangqing, Mou Lijuan, and Zhang Aifen.
Methods for chemical analysis of silicon metal - Part 4.
Determination of elements content inductively coupled
plasma atomic emission spectrometric method
1  Scope 
This Part species the determination method for iron, aluminum, calcium, titanium,
manganese, and nickel content in silicon metal.
This Part applies to the determination of iron, aluminum, calcium, titanium, manganese,
and nickel content in silicon metal. The determination range is shown in Table 1.
Table 1
Element Mass fraction /% Element Mass fraction /%
Iron 0.020-1.00 Nickel 0.0050-0.50
Aluminum 0.020-0.50 Manganese 0.0050-0.50
Calcium 0.020-1.00 Titanium 0.0050-0.10
2  Method summary 
The specimen is decomposed with hydrofluoric acid and nitric acid. Perchloric acid’s
smoking removes silicon, fluorine, etc. And the residue is dissolved with hydrochloric acid.
Test solution is introduced into plasma–spectrometer. Under selected optimal
determination conditions, MEASURE the content of each element in the test solution.
3  Reagents 
3.1 Perchloric acid (ρ1.67g/mL), Guaranteed reagent.
3.2 Hydrofluoric acid (ρ1.14 g/mL), Guaranteed reagent.
3.3 Nitric acid (1+1), Guaranteed reagent.
3.4 Hydrochloric acid (1+1), Guaranteed reagent.
3.5 Standard storage solution. Preparation of each analytical element’s standard storage
solution is shown in Appendix A. It may also use the certified series of national standard
Mass fraction /% 0.0050 0.0100 0.050 0.100 0.50 1.00
Allowable difference R/% 0.0007 0.0020 0.0050 0.012 0.030 0.07
2 Quality assurance and control
In each month, the self-made control standard sample (the standard samples at national
level or industry level shall be used in priority) is used to check the effectiveness of
analysis method of this standard. When the process is out of control, FIND out the
reasons. After correcting the error, REPEAT the checking.
Annex A 
(Informative) 
Preparation of standard storage solution 
A.1 Iron standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of metallic iron (≥99.99%) into the flask. ADD 40mL of
hydrochloric acid (3.4) to completely dissolve by heating. TAKE it down for cooling.
PIPETTE into 1000mL volumetric flask. AMEND 30mL of hydrochloric acid (3.4). DILUTE
to the scale with water. MIX evenly. 1mL of this solution contains 1.0mg of iron.
A.2 Aluminum standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of metallic aluminum (≥99.99%) into the
polytetrafluoroethylene flask. ADD 20mL of water and 3g of sodium hydroxide
(guaranteed reagent). After completely dissolved, NEUTRALIZE slowly with hydrochloric
acid (3.4), until the precipitation appears, and with excessive 20mL. HEAT to dissolve.
COOL it. PIPETTE into 1000mL volumetric flask. DILUTE to the scale with water. MIX
evenly. 1mL of this solution contains 1.0mg of aluminum.
A.3 Calcium standard storage solution (1.0mg/mL).
Accurately WEIGH 2.4971g of calcium carbonate (standard reagents or guaranteed
reagent) which has been pre-dried at 105°C. PLACE in the flask. COVER with dish. ADD
10mL of water. ADD hydrochloric acid (3.4) drop-by-drop until completely dissolved. Then
ADD 10mL of hydrochloric acid (3.4). BOIL to remove carbon dioxide. TAKE down for
cooling. PIPETTE into 1000mL volumetric flask. DILUTE to the scale with water. MIX
evenly. 1mL of this solution contains 1.0mg of calcium.
A.4 Manganese standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of manganese (≥99.99%). PLACE in the 400mL flask.
COVER with the dish. ADD 40mL of hydrochloric acid (3.4). HEAT slowly until completely
dissolved. TAKE down for cooling. PIPETTE the solution into 1000mL volumetric flask.
DILUTE to the scale with water. MIX evenly. 1mL of this solution contains 1.0mg of
manganese.
A.5 Titanium standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of metallic titanium (≥99.99%) into the platinum crucible. ADD
a little of water. ADD hydrofluoric acid slowly drop-by-drop to dissolve the sample. ADD
nitric acid to fully oxidize the low valent titanium. ADD 10mL of sulfuric acid (3.8). SHAKE
evenly. HEAT and EVAPORATE until the white smoke of sulfuric acid just appears. TAKE
down for cooling, PIPETTE the solution into 1000mL volumetric flask. DILUTE to the scale
with water. MIX evenly. 1mL of this solution contains 1.0mg of titanium.
A.6 Nickel standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of nickel (≥99.99%). PLACE in the 400mL flask. COVER with
the dish. ADD 40mL of hydrochloric acid (3.4). HEAT slowly until completely dissolved.
TAKE down for cooling. PIPETTE the solution into 1000mL volumetric flask. DILUTE to
the scale with water. MIX evenly. 1mL of this solution contains 1.0mg of nickel.
GB/T 14849.4-2008
GB
ICS 77.120.10
H 17
National Standard
of the People’s Republic of China
Methods for chemical analysis of silicon metal - Part 4.
Determination of elements content inductively coupled
plasma atomic emission spectrometric method
ISSUED ON. JUNE 9, 2008
IMPLEMENTED ON. DECEMBER 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  Sample ... 5 
6  Analytical steps ... 5 
7  Calculation of the analysis results ... 7 
8  Precision ... 7 
Annex A ... 9 
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 Part is Part 4.
Appendix A of this Part is informative.
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.
Responsible drafting organizations of this Part. Zhengzhou Research Institute of
CHALCO, and Quality Research Institute of China Nonferrous Metals Industry Standard
and Measurement.
Participating drafting organizations of this Part. Northeast Light Alloy Co., Ltd., Baotou
Aluminium Co., Ltd. Southwest Aluminum (Group) Co., Ltd., and Shanxi Jinneng Group
Datong Energy Development Co., Ltd.
Main drafters of this Part. Li Yueping, Shi Lei, Zhang Shuchao, Zhang Jie, Wu Yuqiang,
Zhou Bing, Jiang Wei, Jin Jianhua, Liu Shuangqing, Mou Lijuan, and Zhang Aifen.
Methods for chemical analysis of silicon metal - Part 4.
Determination of elements content inductively coupled
plasma atomic emission spectrometric method
1  Scope 
This Part species the determination method for iron, aluminum, calcium, titanium,
manganese, and nickel content in silicon metal.
This Part applies to the determination of iron, aluminum, calcium, titanium, manganese,
and nickel content in silicon metal. The determination range is shown in Table 1.
Table 1
Element Mass fraction /% Element Mass fraction /%
Iron 0.020-1.00 Nickel 0.0050-0.50
Aluminum 0.020-0.50 Manganese 0.0050-0.50
Calcium 0.020-1.00 Titanium 0.0050-0.10
2  Method summary 
The specimen is decomposed with hydrofluoric acid and nitric acid. Perchloric acid’s
smoking removes silicon, fluorine, etc. And the residue is dissolved with hydrochloric acid.
Test solution is introduced into plasma–spectrometer. Under selected optimal
determination conditions, MEASURE the content of each element in the test solution.
3  Reagents 
3.1 Perchloric acid (ρ1.67g/mL), Guaranteed reagent.
3.2 Hydrofluoric acid (ρ1.14 g/mL), Guaranteed reagent.
3.3 Nitric acid (1+1), Guaranteed reagent.
3.4 Hydrochloric acid (1+1), Guaranteed reagent.
3.5 Standard storage solution. Preparation of each analytical element’s standard storage
solution is shown in Appendix A. It may also use the certified series of national standard
Mass fraction /% 0.0050 0.0100 0.050 0.100 0.50 1.00
Allowable difference R/% 0.0007 0.0020 0.0050 0.012 0.030 0.07
2 Quality assurance and control
In each month, the self-made control standard sample (the standard samples at national
level or industry level shall be used in priority) is used to check the effectiveness of
analysis method of this standard. When the process is out of control, FIND out the
reasons. After correcting the error, REPEAT the checking.
Annex A 
(Informative) 
Preparation of standard storage solution 
A.1 Iron standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of metallic iron (≥99.99%) into the flask. ADD 40mL of
hydrochloric acid (3.4) to completely dissolve by heating. TAKE it down for cooling.
PIPETTE into 1000mL volumetric flask. AMEND 30mL of hydrochloric acid (3.4). DILUTE
to the scale with water. MIX evenly. 1mL of this solution contains 1.0mg of iron.
A.2 Aluminum standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of metallic aluminum (≥99.99%) into the
polytetrafluoroethylene flask. ADD 20mL of water and 3g of sodium hydroxide
(guaranteed reagent). After completely dissolved, NEUTRALIZE slowly with hydrochloric
acid (3.4), until the precipitation appears, and with excessive 20mL. HEAT to dissolve.
COOL it. PIPETTE into 1000mL volumetric flask. DILUTE to the scale with water. MIX
evenly. 1mL of this solution contains 1.0mg of aluminum.
A.3 Calcium standard storage solution (1.0mg/mL).
Accurately WEIGH 2.4971g of calcium carbonate (standard reagents or guaranteed
reagent) which has been pre-dried at 105°C. PLACE in the flask. COVER with dish. ADD
10mL of water. ADD hydrochloric acid (3.4) drop-by-drop until completely dissolved. Then
ADD 10mL of hydrochloric acid (3.4). BOIL to remove carbon dioxide. TAKE down for
cooling. PIPETTE into 1000mL volumetric flask. DILUTE to the scale with water. MIX
evenly. 1mL of this solution contains 1.0mg of calcium.
A.4 Manganese standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of manganese (≥99.99%). PLACE in the 400mL flask.
COVER with the dish. ADD 40mL of hydrochloric acid (3.4). HEAT slowly until completely
dissolved. TAKE down for cooling. PIPETTE the solution into 1000mL volumetric flask.
DILUTE to the scale with water. MIX evenly. 1mL of this solution contains 1.0mg of
manganese.
A.5 Titanium standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of metallic titanium (≥99.99%) into the platinum crucible. ADD
a little of water. ADD hydrofluoric acid slowly drop-by-drop to dissolve the sample. ADD
nitric acid to fully oxidize the low valent titanium. ADD 10mL of sulfuric acid (3.8). SHAKE
evenly. HEAT and EVAPORATE until the white smoke of sulfuric acid just appears. TAKE
down for cooling, PIPETTE the solution into 1000mL volumetric flask. DILUTE to the scale
with water. MIX evenly. 1mL of this solution contains 1.0mg of titanium.
A.6 Nickel standard storage solution (1.0mg/mL).
Accurately WEIGH 1.0000g of nickel (≥99.99%). PLACE in the 400mL flask. COVER with
the dish. ADD 40mL of hydrochloric acid (3.4). HEAT slowly until completely dissolved.
TAKE down for cooling. PIPETTE the solution into 1000mL volumetric flask. DILUTE to
the scale with water. MIX evenly. 1mL of this solution contains 1.0mg of nickel.