SN/T 0803.6-1999Oil bearing materials for import and export. Method for the inspection of impurities (English PDF)

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.

4.1 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 (rho=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.

5.1 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 (rho=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).

6.1 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 (rho=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).

7.1 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 (rho=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

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.

4.1 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 (rho=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.

5.1 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 (rho=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).

6.1 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 (rho=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).

7.1 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 (rho=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.

......