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SN/T 1600-2005 English PDF (SNT1600-2005)

SN/T 1600-2005 English PDF (SNT1600-2005)

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SN/T 1600-2005: Determination for trace elements in coal by ICP-AES

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.
SN/T 1600-2005
SN
ENTRY-EXIT INSPECTIONA AND QUARANTINE INDUSTRY
STANDARD OF THE PEOPLE REPUBLIC OF CHINA
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
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. 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)
GB/T 602 Chemical Reagent ?€? Preparations of Standard Solutions for Impurity (ISO 6353-1, NEQ)
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.
3.3.4 Muffle furnace: the temperature may be controlled to (500??5) ??C.
3.3.5 Ash dish: The bottom of the rectangular ash dish is 105mm long, 50mm wide, and 15mm high.
3.3.6 Volumetric flask: 100mL.
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
3.4.1.1 Ashing of coal sample
Accurately take 2g (accurate to 0.2 mg) of the air-dried analytical coal sample prepared in accordance with the method of GB 474 in a ash dish; flatten it; and place the ash dish in a muffle furnace below 100??C; and raise the temperature to 300?? for 1 h; then raise the temperature to 500??C for 1 h; and burn at this temperature to no carbon particles.
3.4.1.2 Decomposition of ash sample
Transfer all the ash samples (3.4.1.1) to a PTFE crucible; moisten it with a little water; add 5mL of nitric acid (3.2.1), 5mL of perchloric acid (3.2.2) and 15mL of hydrofluoric acid (3.2.3); heat on a hot plate; heat at 100??C for 2h, heated at 150??C for 2h, heat at 180??C until nearly dry; cool. Add 5 mL of nitric acid (3.2.1) and 15 mL of distilled water; Heat on the hot plate to slightly boil; and keep it for 20min; dissolve the salts; cool; and transfer all the solution to a 100 mL volumetric flask; make constant volume with water; shake well and then transfer to a 100 mL plastic bottle immediately.
3.4.2 Blank test
Except for not weighing the sample, perform with the specimen according to procedure 3.4.1.
4.2.5 Boron standard stock solution (1000??g/mL): prepare standard solution according to the method of GB/T 602; or directly use certified standard solution. 4.2.6 Boron standard solution (50??m/mL): accurately pipette 5mL of the boron standard stock solution (4.2.5) into a 100 mL plastic volumetric flask; make constant volume with water; and shake well.
4.3 Apparatus
4.3.1 ICP-AES: with computer control and data processing system.
4.3.2 Balance: sensitivity is 0.0001g.
4.3.3 Muffle furnace: the temperature may be controlled to (780??5) ??C.
4.3.4 Platinum crucible: 30mL.
4.3.5 Plastic volumetric flask: 100mL.
4.3.6 Plastic beaker: 300mL.
4.3.7 Pipette: 1 mL, 10mL.
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). Put the crucible into a muffle furnace below 100??C; and raise the temperature to 500??C for 1 h, keep the temperature constant for 1h; and then raise the temperature to 780??C, keep the temperature constant for 3h.
Take the platinum crucible out of the muffle furnace and cool it to room temperature. Transfer the burnt material of the crucible into a 300mL plastic beaker containing 50mL of water. Carefully clean the inner wall of the crucible with water; pour the rinse solution into a 300 mL plastic beaker; and add 15 mL of hydrochloric acid (4.2.1); fully dissolve; the solution in the plastic beaker is filtered into a 100 mL plastic volumetric flask; and make the constant volume with water; and shake well.
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
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. Add hydrochloric acid and keep warm. After cooling and making constant volume, the test solution and sodium borohydride solution are passed into the hydride generator at the same time; and the generated arsine hydride and selenium hydride gases are carried into the inductively coupled plasma torch by the auxiliary gas for spectrum measurement.
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 (??=1.19 g/mL).
5.2.2 Argon: high purity (99.99%).
5.2.3 Eschka mixed reagent: take two portions by mass of light magnesium oxide and one portion by mass of anhydrous sodium carbonate (ground to a particle size of less than 0.2 mm); and mix well.
5.2.4 Potassium ferrocyanide solution (100g/L): take 10g of potassium ferrocyanide and dissolve it in 100mL of distilled water.
5.2.5 Sodium borohydride solution (10g/L): take 1g of sodium hydroxide and dissolve it in 100mL of water; shake well. Then add 1g of sodium borohydride; shake well; and prepare it when used.
5.2.6 Single element standard solution of arsenic and selenium (1000??g/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 100??g/mL, Se 10??g/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.
5.2.8 Mixed standard solution of arsenic and smash (As 10??g/mL, Se 1??g/mL): pipette 10mL of arsenic standard solution (5.2.7) into a 100mL volumetric flask; make constant volume with water; and shake well. The concentration of the mixed standard solution may also be selected according to the content of arsenic and selenium in the tested sample.
6.3.3 Analytical balance: sensitivity is 0.0001g.
6.3.4 Muffle furnace: temperature may be controlled to (650??5) ??C.
6.3.5 Electric heating plate: with temperature adjustment device.
6.3.6 Ash dish.
6.3.7 PTFE crucible: 30 mL, 50 mL
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. Place the ash dish in a muffle furnace lower than 100??C; half open the furnace door; and raise the temperature to 500??C for 1h, keep a constant temperature for 1 h; and then raise the temperature to 650??C until no carbon particles are present. Transfer all the burnt materials to a 30mL PTFE crucible; moisten it with water. Add 2mL of nitric acid (6.2.1), 2mL of phosphoric acid (6.2.2), 5mL of hydrofluoric acid (6.2.3). Heat it on a low- temperature electric hot plate until it is nearly dry; cool slightly. Add 10 mL of water to heat it to near boiling; keep warm for 20min; and cool; transfer all the solution into a 50mL volumetric flask; add 3mL of phosphoric acid (6.2. 2); make constant volume with water; and shake well.
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. 6.4.3 Preparation of standard series solutions
Respectively pipette 0mL, 0.5mL, 1mL, 2mL and 3mL of the germanium standard solution (6.2.7) in a 50 mL volumetric flask; dilute to the mark with a blank solution (6.4.2); and shake well.
6.4.4 Determination
Put the coal sample into an oxygen bomb to burn and decompose; absorb with nitric acid solution; convert the mercury in the coal into divalent mercury ions; use sodium borohydride to reduce the divalent mercury ions into mercury atom vapor; and use auxiliary gas to bring the generated gas into the inductively coupled plasma torch for the spectral measurement.
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 (??=1.42 g/mL) with 9 volumes of water.
7.2.2 Potassium permanganate solution (50g/L): take 5g of potassium permanganate and dissolve it in 100mL of water, and shake well. Store in a brown reagent bottle. 7.2.3 Potassium ferrocyanide solution (100g/L): take 10g of potassium ferrocyanide and dissolve it in 100mL of water; shake well; and prepare it when used. 7.2.4 Sodium borohydride solution (10g/L): take 1g of sodium hydroxide and dissolve it in 100mL of water. After shaking well, add 1g of sodium borohydride and shake well; prepare it when used.
7.2.5 Mercury standard stock solution (1000??g/mL): prepare the certified standard material according to the method of GB/T 602; or directly use the certified standard solution.
7.2.6 Mercury standard intermediate solution (10??g/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 (0.1??g/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.
7.3.2 Apparatus (oxygen bomb, combustion vessel, ignition wire, metal container) for sample combustion: follow the provisions in GB/T 213.
7.3.3 Analytical balance: sensitivity is 0.0001 g
7.3.4 Glassware: the following glassware shall be soaked in nitric acid solution (7.2.1)

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