SN/T 1600-2005 PDF English
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SN/T 1600-2005: Determination for Trace Elements in Coal by ICP-AES---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/SNT1600-2005
SN
ENTRY-EXIT INSPECTIONA AND QUARANTINE INDUSTRY
Determination for Trace Elements in Coal by ICP-AES
Issued on. MAY 20, 2005
Implemented on. DECEMBER 01, 2005
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Determination of Barium, Beryllium, Cadmium, Cobalt, Chromium, Copper,
Gallium, Manganese, Molybdenum, Nickel, Lead, Strontium, Vanadium, Zinc,
Zirconium... 5
4 Determination of Boron... 8
5 Determination of Arsenic and Selenium... 11
6 Determination of Germanium... 14
7 Determination of Mercury... 16
Appendix A (Informative) Working Conditions of the Instrument... 20
Foreword
The Appendix A of this Standard is informative.
This Standard was proposed by and under the jurisdiction of the Certification and
Accreditation Administration of the People’s Republic of China.
Drafting organization of this Standard. Qinhuangdao Entry-Exit Inspection and
Quarantine Bureau of the People’s Republic of China.
Drafting staffs of this Standard. Wang Jielin, Zhong Yali, Zhao Xiuhong, Gao Jianwen,
Zhang Bo, Ren Xinyu, Fu Hong, and Wang Guifang.
This Standard is the entry-exit inspection and quarantine industry standard that is first-
time published.
Determination for Trace Elements in Coal by ICP-AES
1 Scope
This Standard specifies the inductively coupled plasma atomic emission spectroscopy
(ICP-AES for short) of barium, beryllium, cadmium, cobalt, chromium, copper, gallium,
manganese, molybdenum, nickel, lead, strontium, vanadium, zinc, zirconium, boron,
arsenic, selenium, germanium and mercury in coal.
This Standard is applicable for the determination of barium, beryllium, cadmium, cobalt,
chromium, copper, gallium, manganese, molybdenum, nickel, lead, strontium,
vanadium, zinc, zirconium, boron, arsenic, selenium, germanium and mercury in coal.
Coke may also refer to for use.
The detection limits of 20 elements in this Standard are shown in Table 1.
Table 1 – Determination of Detection Limit of the Elements Unit. µg/mL
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
who reach an agreement based on this Standard are encouraged to study if the latest
versions of these documents are applicable. For undated references, the latest edition
of the referenced document applies.
GB 474 Methods for the Preparation of Coal Sample (eqv ISO 1988)
GB/T 213 Determination of Calorific Value of Coal (ISO 1928, NEQ)
3 Determination of Barium, Beryllium, Cadmium,Cobalt, Chromium, Copper, Gallium, Manganese, Molybdenum, Nickel,
Lead,Strontium, Vanadium, Zinc, Zirconium
3.1 Principle
The coal sample is ashed and decomposed by nitric acid, perchloric acid, and
hydrofluoric acid; and kept warm in a medium of nitric acid. After making the constant
volume, it is measured by inductively coupled plasma atomic emission spectrometer.
3.2 Reagents and materials
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with the equivalent purity.
3.3 Apparatus
3.3.1 ICP-AES. with computer control and data processing system.
3.3.2 Analytical balance. sensitivity is 0.0001g
3.3.3 Electric heating plate. temperature is controllable.
3.3.7 Pipette. 0.5mL, 5mL, 10mL.
3.3.8 PTFE crucible. 50mL.
3.3.9 Plastic bottle. 100mL.
3.4 Test Procedures
3.4.1 Preparation of specimen solution
3.5 Calculation of result
Calculate the content of the measured element according to Formula (1).
3.6 Precision
The precision data can refer to Table 3.
4 Determination of Boron
4.1 Principle
Mix and burn the coal sample and the Eschka mixed reagent; the burnt material is
dissolved with hydrochloric acid; and the specimen solution is sprayed into the
inductively coupled plasma torch to perform spectrum measurement.
4.2 Reagents and materials
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with equivalent purity.
4.2.1 Hydrochloric acid (ρ=1.19 g/mL).
4.3 Apparatus
4.3.1 ICP-AES. with computer control and data processing system.
4.3.2 Balance. sensitivity is 0.0001g.
4.4 Test procedures
4.4.1 Preparation of specimen solution
Accurately weigh 1g (accurate to 0.0001g) of the air-dried analytical coal sample
prepared in accordance with GB 474; and put it into a platinum crucible containing 1.0g
of Eschka mixed reagent (4.2.3); mix carefully; and then cover with 1.0g of Eschka
mixed reagent (4.2.3).
4.4.2 Blank test
Except for not weighing the sample, the others shall be carried out according to the
procedures of 4.4.1.
4.4.3 Preparation of standard series solutions
Respectively pipette 0mL, 1mL, 2mL, 3mL, 4mL, and 5 mL of the standard solution
(4.2.6) into 100 mL volumetric flasks; and add 20 mL of Eschka mixed reagent solution
(4.2.4) to each volumetric flask; make constant volume with water, and shake well.
4.4.4 Determination
data processing system.
4.5 Calculation of the results
According to Formula (2), calculate the boron element content in the air-dried analytical
coal sample.
4.6 Precision
The precision data can refer to Table 4.
5 Determination of Arsenic and Selenium
5.1 Principle
Mix and burn coal sample and Eschka mixed reagent; and the burnt material is
dissolved by hydrochloric acid.
5.2 Reagents and materials
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with equivalent purity.
5.2.1 Hydrochloric acid (ρ=1.19 g/mL).
5.2.2 Argon. high purity (99.99%).
5.2.6 Single element standard solution of arsenic and selenium (1000µg/mL). the
certified standard material is prepared according to the method of GB/T 602, or directly
use the certified standard solution.
5.2.7 Arsenic and selenium mixed intermediate standard solution (As 100µg/mL, Se
10µg/mL). pipette 10mL of arsenic standard solution (5.2.6) and 1mL of selenium
standard solution (5.2.6) into 100mL volumetric flask. Add 5 mL of hydrochloric acid
(5.2.1); make constant volume with water; and shake well.
5.3 Apparatus
5.4 Determination procedures
5.4.1 Preparation of specimen solution
Accurately take 1g (accurate to 0.0001g) of the air-dried analytical coal sample
prepared in accordance with GB 474; and put it into a 30mL porcelain crucible
containing 1.5g of Eschka mixed reagent (5.2.3); mix carefully. Then cover it with 1.5g
of Eschka mixed reagent (5.2.3). Put the crucible into the muffle furnace below 100°C;
slowly raise the temperature to 500°C, keep the temperature constant for 1h; then raise
the temperature to 750°C, keep the constant temperature 3h.
5.4.4 Determination
5.4.4.1 Drawing of standard series working curve
Connect the hydride generator to the ICP-AES; and select the optimal parameters of
the instrument (see Appendix A). Inject the sodium borohydride solution (5.2.5) and
the standard series solution (5.4.3) into the hydride generator at the same time; inject
the generated hydride gas into the plasma torch; and determine the spectral intensity
of the standard series solution in sequence (5.4.3). Draw the working curve through
the computer data processing system.
5.5 Calculation of the results
Calculate the content of arsenic and selenium in the air-dried analytical coal sample
according to Formula (3).
6 Determination of Germanium
6.1 Principle
The coal sample is ashed and dissolved by nitric acid, phosphoric acid and hydrofluoric
acid.
6.2 Reagents
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with equivalent purity.
6.2.1 Nitric acid (ρ=1.42 g/mL).
6.3 Apparatus
6.3.1 ICP-AES. with computer control and data processing system.
6.3.2 Hydride generator. matched with ICP-AES.
Repeatability limit r Reproducibility limit R Content rangeElement
6.3.3 Analytical balance. sensitivity is 0.0001g.
6.3.8 Volumetric flask. 50 mL, 250 mL
6.3.9 Beaker. 250 mL
6.3.10 Pipette 0.5mL, 1mL, 2mL, 5mL.
6.4 Determination procedures
6.4.1 Preparation of specimen solution
Accurately take 1g (accurate to 0.2mg) of the air-dried coal sample prepared according
to the method of GB 474; put it in an ash dish; and spread it flat.
6.4.2 Preparation of blank solution
Add 10mL of nitric acid (6.2.1), 10mL of phosphoric acid (6.2.2), 25 mL of hydrofluoric
acid (6.2.3) in a 50mL PTFE crucible; and heat it on a low-temperature electric heating
plate until it is nearly dry; cool slightly. Add 30 mL of water to heat to near boiling; kept
warm for 20min; and cool; transfer all the solution to 250 mL volumetric flask; add 15mL
of phosphoric acid (6.2.2); make constant volume with water; and shake well.
6.5 Calculation of the results
Calculate the germanium element content in air-dried coal sample according to
Formula (4).
7 Determination of Mercury
7.1 Principle
Repeatability limit r Reproducibility limit R Content range of germanium
NOTE. x – the average value of the 2 measurement values.
7.2 Reagents
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or the water with equivalent purity.
7.2.1 Nitric acid solution (1+9). mix 1 volume of nitric acid (ρ=1.42 g/mL) with 9 volumes
of water.
7.2.6 Mercury standard intermediate solution (10µg/mL). accurately pipette 1mL of
mercury standard stock solution (7.2.5) into a 100mL volumetric flask; make constant
volume with nitric acid solution (7.2.1); and shake well.
7.2.7 Mercury standard solution (0.1µg/mL). accurately pipette 1mL of mercury
standard intermediate solution (7.2.6) into a 100mL volumetric flask; make constant
volume with nitric acid solution (7.2.1); and shake well.
7.3 Apparatus
7.3.1 ICP-AES. with matching hydride generator, computer control and data
processing system.
7.4 Test procedures
7.4.1 Preparation of sample solution
7.4.1.1 Take 1g (accurate to 0.1mg) of the air-dried analytical coal sample prepared in
accordance with GB 474 in a combustion vessel; put it in an oxygen bomb previously
added with 10mL of nitric acid solution (7.2.1); and install the oxygen bomb.
7.4.2 Blank test
Except for not weighing the sample, follow the procedures in 7.4.1 with the sample.
7.4.3 Preparation of standard series solutions
Respectively pipette 0mL, 0.5mL, 1mL, 2mL, 3mL, 5mL of the mercury standard
solution (7.2.7) into a 50 mL volumetric flask. Add 40mL of nitric acid solution (7.2.1);
and titrate potassium permanganate solution (7.2.2) to make the solution change color
and stabilize for 1min. Add 1 mL of potassium ferrocyanide solution (7.2.3); and then
make constant volume with nitric acid solution (7.2.1); and shake well.
7.4.4 Determination
7.4.4.1 Drawing standard curve
Connect the hydride generator to the ICP-AES; select the optimal parameters of the
instrument (see Appendix A). Inject the sodium borohydride solution (7.2.4) and the
standard series solution (7.4.3) to the hydride generator at the same time. The
generated gas is brought by the auxiliary gas into the plasma torch; and measure the
spectral intensity of the standard series solution (7.4.3) in sequence; and draw the
working curve through the data processing system.
7.6 Precision
The precision data can refer to Table 7.
SN/T 1600-2005
SN
ENTRY-EXIT INSPECTIONA AND QUARANTINE INDUSTRY
Determination for Trace Elements in Coal by ICP-AES
Issued on. MAY 20, 2005
Implemented on. DECEMBER 01, 2005
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Determination of Barium, Beryllium, Cadmium, Cobalt, Chromium, Copper,
Gallium, Manganese, Molybdenum, Nickel, Lead, Strontium, Vanadium, Zinc,
Zirconium... 5
4 Determination of Boron... 8
5 Determination of Arsenic and Selenium... 11
6 Determination of Germanium... 14
7 Determination of Mercury... 16
Appendix A (Informative) Working Conditions of the Instrument... 20
Foreword
The Appendix A of this Standard is informative.
This Standard was proposed by and under the jurisdiction of the Certification and
Accreditation Administration of the People’s Republic of China.
Drafting organization of this Standard. Qinhuangdao Entry-Exit Inspection and
Quarantine Bureau of the People’s Republic of China.
Drafting staffs of this Standard. Wang Jielin, Zhong Yali, Zhao Xiuhong, Gao Jianwen,
Zhang Bo, Ren Xinyu, Fu Hong, and Wang Guifang.
This Standard is the entry-exit inspection and quarantine industry standard that is first-
time published.
Determination for Trace Elements in Coal by ICP-AES
1 Scope
This Standard specifies the inductively coupled plasma atomic emission spectroscopy
(ICP-AES for short) of barium, beryllium, cadmium, cobalt, chromium, copper, gallium,
manganese, molybdenum, nickel, lead, strontium, vanadium, zinc, zirconium, boron,
arsenic, selenium, germanium and mercury in coal.
This Standard is applicable for the determination of barium, beryllium, cadmium, cobalt,
chromium, copper, gallium, manganese, molybdenum, nickel, lead, strontium,
vanadium, zinc, zirconium, boron, arsenic, selenium, germanium and mercury in coal.
Coke may also refer to for use.
The detection limits of 20 elements in this Standard are shown in Table 1.
Table 1 – Determination of Detection Limit of the Elements Unit. µg/mL
2 Normative References
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
who reach an agreement based on this Standard are encouraged to study if the latest
versions of these documents are applicable. For undated references, the latest edition
of the referenced document applies.
GB 474 Methods for the Preparation of Coal Sample (eqv ISO 1988)
GB/T 213 Determination of Calorific Value of Coal (ISO 1928, NEQ)
3 Determination of Barium, Beryllium, Cadmium,Cobalt, Chromium, Copper, Gallium, Manganese, Molybdenum, Nickel,
Lead,Strontium, Vanadium, Zinc, Zirconium
3.1 Principle
The coal sample is ashed and decomposed by nitric acid, perchloric acid, and
hydrofluoric acid; and kept warm in a medium of nitric acid. After making the constant
volume, it is measured by inductively coupled plasma atomic emission spectrometer.
3.2 Reagents and materials
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with the equivalent purity.
3.3 Apparatus
3.3.1 ICP-AES. with computer control and data processing system.
3.3.2 Analytical balance. sensitivity is 0.0001g
3.3.3 Electric heating plate. temperature is controllable.
3.3.7 Pipette. 0.5mL, 5mL, 10mL.
3.3.8 PTFE crucible. 50mL.
3.3.9 Plastic bottle. 100mL.
3.4 Test Procedures
3.4.1 Preparation of specimen solution
3.5 Calculation of result
Calculate the content of the measured element according to Formula (1).
3.6 Precision
The precision data can refer to Table 3.
4 Determination of Boron
4.1 Principle
Mix and burn the coal sample and the Eschka mixed reagent; the burnt material is
dissolved with hydrochloric acid; and the specimen solution is sprayed into the
inductively coupled plasma torch to perform spectrum measurement.
4.2 Reagents and materials
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with equivalent purity.
4.2.1 Hydrochloric acid (ρ=1.19 g/mL).
4.3 Apparatus
4.3.1 ICP-AES. with computer control and data processing system.
4.3.2 Balance. sensitivity is 0.0001g.
4.4 Test procedures
4.4.1 Preparation of specimen solution
Accurately weigh 1g (accurate to 0.0001g) of the air-dried analytical coal sample
prepared in accordance with GB 474; and put it into a platinum crucible containing 1.0g
of Eschka mixed reagent (4.2.3); mix carefully; and then cover with 1.0g of Eschka
mixed reagent (4.2.3).
4.4.2 Blank test
Except for not weighing the sample, the others shall be carried out according to the
procedures of 4.4.1.
4.4.3 Preparation of standard series solutions
Respectively pipette 0mL, 1mL, 2mL, 3mL, 4mL, and 5 mL of the standard solution
(4.2.6) into 100 mL volumetric flasks; and add 20 mL of Eschka mixed reagent solution
(4.2.4) to each volumetric flask; make constant volume with water, and shake well.
4.4.4 Determination
data processing system.
4.5 Calculation of the results
According to Formula (2), calculate the boron element content in the air-dried analytical
coal sample.
4.6 Precision
The precision data can refer to Table 4.
5 Determination of Arsenic and Selenium
5.1 Principle
Mix and burn coal sample and Eschka mixed reagent; and the burnt material is
dissolved by hydrochloric acid.
5.2 Reagents and materials
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with equivalent purity.
5.2.1 Hydrochloric acid (ρ=1.19 g/mL).
5.2.2 Argon. high purity (99.99%).
5.2.6 Single element standard solution of arsenic and selenium (1000µg/mL). the
certified standard material is prepared according to the method of GB/T 602, or directly
use the certified standard solution.
5.2.7 Arsenic and selenium mixed intermediate standard solution (As 100µg/mL, Se
10µg/mL). pipette 10mL of arsenic standard solution (5.2.6) and 1mL of selenium
standard solution (5.2.6) into 100mL volumetric flask. Add 5 mL of hydrochloric acid
(5.2.1); make constant volume with water; and shake well.
5.3 Apparatus
5.4 Determination procedures
5.4.1 Preparation of specimen solution
Accurately take 1g (accurate to 0.0001g) of the air-dried analytical coal sample
prepared in accordance with GB 474; and put it into a 30mL porcelain crucible
containing 1.5g of Eschka mixed reagent (5.2.3); mix carefully. Then cover it with 1.5g
of Eschka mixed reagent (5.2.3). Put the crucible into the muffle furnace below 100°C;
slowly raise the temperature to 500°C, keep the temperature constant for 1h; then raise
the temperature to 750°C, keep the constant temperature 3h.
5.4.4 Determination
5.4.4.1 Drawing of standard series working curve
Connect the hydride generator to the ICP-AES; and select the optimal parameters of
the instrument (see Appendix A). Inject the sodium borohydride solution (5.2.5) and
the standard series solution (5.4.3) into the hydride generator at the same time; inject
the generated hydride gas into the plasma torch; and determine the spectral intensity
of the standard series solution in sequence (5.4.3). Draw the working curve through
the computer data processing system.
5.5 Calculation of the results
Calculate the content of arsenic and selenium in the air-dried analytical coal sample
according to Formula (3).
6 Determination of Germanium
6.1 Principle
The coal sample is ashed and dissolved by nitric acid, phosphoric acid and hydrofluoric
acid.
6.2 Reagents
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or water with equivalent purity.
6.2.1 Nitric acid (ρ=1.42 g/mL).
6.3 Apparatus
6.3.1 ICP-AES. with computer control and data processing system.
6.3.2 Hydride generator. matched with ICP-AES.
Repeatability limit r Reproducibility limit R Content rangeElement
6.3.3 Analytical balance. sensitivity is 0.0001g.
6.3.8 Volumetric flask. 50 mL, 250 mL
6.3.9 Beaker. 250 mL
6.3.10 Pipette 0.5mL, 1mL, 2mL, 5mL.
6.4 Determination procedures
6.4.1 Preparation of specimen solution
Accurately take 1g (accurate to 0.2mg) of the air-dried coal sample prepared according
to the method of GB 474; put it in an ash dish; and spread it flat.
6.4.2 Preparation of blank solution
Add 10mL of nitric acid (6.2.1), 10mL of phosphoric acid (6.2.2), 25 mL of hydrofluoric
acid (6.2.3) in a 50mL PTFE crucible; and heat it on a low-temperature electric heating
plate until it is nearly dry; cool slightly. Add 30 mL of water to heat to near boiling; kept
warm for 20min; and cool; transfer all the solution to 250 mL volumetric flask; add 15mL
of phosphoric acid (6.2.2); make constant volume with water; and shake well.
6.5 Calculation of the results
Calculate the germanium element content in air-dried coal sample according to
Formula (4).
7 Determination of Mercury
7.1 Principle
Repeatability limit r Reproducibility limit R Content range of germanium
NOTE. x – the average value of the 2 measurement values.
7.2 Reagents
Unless otherwise stated, the used reagents are all guaranteed reagents. The water is
deionized water or the water with equivalent purity.
7.2.1 Nitric acid solution (1+9). mix 1 volume of nitric acid (ρ=1.42 g/mL) with 9 volumes
of water.
7.2.6 Mercury standard intermediate solution (10µg/mL). accurately pipette 1mL of
mercury standard stock solution (7.2.5) into a 100mL volumetric flask; make constant
volume with nitric acid solution (7.2.1); and shake well.
7.2.7 Mercury standard solution (0.1µg/mL). accurately pipette 1mL of mercury
standard intermediate solution (7.2.6) into a 100mL volumetric flask; make constant
volume with nitric acid solution (7.2.1); and shake well.
7.3 Apparatus
7.3.1 ICP-AES. with matching hydride generator, computer control and data
processing system.
7.4 Test procedures
7.4.1 Preparation of sample solution
7.4.1.1 Take 1g (accurate to 0.1mg) of the air-dried analytical coal sample prepared in
accordance with GB 474 in a combustion vessel; put it in an oxygen bomb previously
added with 10mL of nitric acid solution (7.2.1); and install the oxygen bomb.
7.4.2 Blank test
Except for not weighing the sample, follow the procedures in 7.4.1 with the sample.
7.4.3 Preparation of standard series solutions
Respectively pipette 0mL, 0.5mL, 1mL, 2mL, 3mL, 5mL of the mercury standard
solution (7.2.7) into a 50 mL volumetric flask. Add 40mL of nitric acid solution (7.2.1);
and titrate potassium permanganate solution (7.2.2) to make the solution change color
and stabilize for 1min. Add 1 mL of potassium ferrocyanide solution (7.2.3); and then
make constant volume with nitric acid solution (7.2.1); and shake well.
7.4.4 Determination
7.4.4.1 Drawing standard curve
Connect the hydride generator to the ICP-AES; select the optimal parameters of the
instrument (see Appendix A). Inject the sodium borohydride solution (7.2.4) and the
standard series solution (7.4.3) to the hydride generator at the same time. The
generated gas is brought by the auxiliary gas into the plasma torch; and measure the
spectral intensity of the standard series solution (7.4.3) in sequence; and draw the
working curve through the data processing system.
7.6 Precision
The precision data can refer to Table 7.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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