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GB/T 37354-2019

Chinese Standard: 'GB/T 37354-2019'
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GB/T 37354-2019English169 Add to Cart Days<=3 Analytical method of chemical composition for activated carbon mercury removal catalyst Valid GB/T 37354-2019
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Detail Information of GB/T 37354-2019; GB/T37354-2019
Description (Translated English): Analytical method of chemical composition for activated carbon mercury removal catalyst
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: G74
Classification of International Standard: 71.100.99
Word Count Estimation: 10,194
Date of Issue: 2019-03-25
Date of Implementation: 1/2/2020
Drafting Organization: Sinopec Nanjing Chemical Research Institute Co., Ltd., Beijing Sanju Environmental Protection New Materials Co., Ltd., Wuhan Kelin Fine Chemical Co., Ltd., Xi-An Xiangyang Aerospace Materials Co., Ltd., Shandong Xunda Chemical Group Co., Ltd.
Administrative Organization: National Chemical Standardization Technical Committee (SAC/TC 63)
Proposing organization: China Petroleum and Chemical Industry Federation
Issuing agency(ies): State Administration of Markets and China National Standardization Administration


GB/T 37354-2019
Analytical method of chemical composition for activated carbon mercury removal catalyst
ICS 71.100.99
G74
National Standards of People's Republic of China
Chemical composition analysis method of activated carbon mercury removal catalyst
Analyticalmethodofchemicalcompositionforactivatedcarbon
Mercuryremovalcatalyst
Published on.2019-03-25
2020-02-01 implementation
State market supervision and administration
China National Standardization Administration issued
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China Petroleum and Chemical Industry Federation.
This standard is under the jurisdiction of the National Chemical Standardization Technical Committee (SAC/TC63).
This standard was drafted. Sinopec Nanjing Chemical Research Institute Co., Ltd., Beijing Sanju Environmental Protection New Materials Co., Ltd., Wuhan Colin
Fine Chemical Co., Ltd., Xi'an Xiangyang Aerospace Materials Co., Ltd., Shandong Schindler Chemical Group Co., Ltd.
The main drafters of this standard. Li Zhongyu, Li Min, Zhao Wentao, Wang Guoxing, Wang Guoni, Hu Wenbin, Sun Guoshuang, Wang Ze, Hou Yanan, Zhang Xianmao.
Chemical composition analysis method of activated carbon mercury removal catalyst
Caution - Some of the reagents used in this standard are toxic or corrosive and some operations are dangerous. This standard does not reveal the
There are potential safety issues, and users should exercise caution and be responsible for taking appropriate safety and health measures.
1 Scope
This standard specifies the chemical composition analysis method of activated carbon mercury removal catalyst.
This standard applies to the determination of sulfur (S), calcium (Ca), magnesium (Mg), iron (Fe), aluminum (Al) mass fraction in activated carbon mercury removal catalyst.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
Preparation of standard solution for GB/T 602 chemical reagent impurity determination
Preparation of preparations and products used in GB/T 603 chemical reagent test method
GB/T 6003.1 Test sieves - Technical requirements and testing - Part 1
GB/T 6679 Solid Chemical Products Sampling General
GB/T 6682 Analytical laboratory water specifications and test methods
3 General regulations
The reagents and water used in this standard refer to the analytical reagents and the tertiary water specified in GB/T 6682 when no other requirements are indicated. test
The standard solutions, preparations and products used for the determination of impurities used in the test shall be in accordance with GB/T 602 and GB/T 603 when no other requirements are specified.
Preparation of the provisions.
4 sampling
4.1 Laboratory samples
Obtained according to the provisions of GB/T 6679.
4.2 Sample
The laboratory samples were uniformly mixed, and about 40 g was taken by a quarter method, and the fines were ground in a porcelain mortar. Then use the quartering method to take about 20g, followed by
Continue to study until the sample passes through the 150μm test sieve (according to R40/3 series in GB/T 6003.1), placed in the crucible, at 105 °C~
Dry at 110 ° C for 2 h, remove and put in a desiccator to cool to room temperature, and set aside.
4.3 Preparation of sample solution
4.3.1 Reagents
4.3.1.1 Hydrochloric acid.
4.3.1.2 Nitric acid.
4.3.1.3 Perchloric acid.
4.3.2 Operation steps
Weigh about 0.2g sample, accurate to 0.0001g, placed in a.200mL beaker, wet with water, add 10mL hydrochloric acid in a fume hood,
10mL nitric acid, 8mL perchloric acid, covered with a watch glass, slowly heated (maintaining micro-boiling) to dissolve the sample until the white smoke disappears, and the sample is completely transparent.
Clear, remove the cooling, dilute to about 60mL with water, filter with medium speed filter paper, rinse the surface dish and the inner wall of the beaker 6 times ~ 8 times with water, filtrate and
The washing solution was incorporated into a 250 mL volumetric flask, diluted to the mark with water, and shaken.
5 Determination of sulfur (S) mass fraction
5.1 Principle
Mix the sample with the mixed flux to burn, convert all the sulfur into soluble sulfate, add barium chloride solution to make the sulfate form sulfate
In the lake, the sulfur content in the sample is calculated based on the mass of barium sulfate.
5.2 Reagents
5.2.1 Mixing flux. Take 2 parts of light magnesium oxide and 1 part of anhydrous sodium carbonate, mix well and store in a closed container.
5.2.2 Hydrochloric acid solution. 1 1.
5.2.3 Barium chloride solution. 100g/L.
5.2.4 Silver nitrate solution. 10g/L. 1 g of silver nitrate was dissolved in 100 mL of water, and 2 to 3 drops of nitric acid were added and stored in a brown bottle.
5.2.5 Methyl orange indicator solution. 2g/L.
5.3 Test procedure
5.3.1 Weigh about 0.2g sample (see 4.2), accurate to 0.0001g, placed in 50mL porcelain crucible, add 2g mixed flux, mix, top
1 g of mixed flux was placed. Put the crucible into the muffle furnace and gradually heat it from room temperature to 800 °C ~ 850 °C within 1h~2h, and at this temperature
Keep it for 1 hour. Remove and cool to room temperature. Use a glass rod to carefully loosen the burning material in the crucible, then transfer the burning to 400mL.
In the beaker, rinse the inner wall of the crucible with hot water, add the washing solution to the beaker, and add 100 mL to 150 mL of freshly boiled distilled water and mix well.
5.3.2 Filter with medium-speed qualitative filter paper by pouring, rinse with hot water for 3 times, then transfer the residue to filter paper and carefully wash with hot water until
10 times less, the total volume of washing liquid is about 250mL~300mL. 2 drops to 3 drops of methyl orange indicator solution were added to the filtrate, and hydrochloric acid solution was added thereto.
The filtrate turned from yellow to red with an excess of 2 mL. The solution is heated to boiling, and 15 mL of a cerium chloride solution is slowly added under constant stirring, and
Maintained for about 2 h under microboiling conditions, the final volume of the solution was approximately.200 mL. After the solution is cooled or left to stand overnight, it is filtered with a slow quantitative filter paper, and
Wash with hot water until there is no chloride ion (no silver turbidity in the silver nitrate solution). Transfer the filter paper with sediment to a porcelain crucible of known quality.
After ashing the filter paper, burn it in a muffle furnace at a temperature of 850 ° C ~ 900 ° C for 40 min, remove the porcelain crucible, and put it into a desiccator to cool it to
Weighed after room temperature.
5.3.3 When preparing a batch of mixed flux or replacing any other reagent, two or more blank tests shall be carried out, taking the arithmetic mean
The value is a blank value.
5.4 Test data processing
Sulfur (S) mass fraction w1, calculated according to formula (1).
W1=
M1-m2( )×0.1374
M3 ×
100% (1)
In the formula.
The value of the mass of m1 --- barium sulfate precipitate, in grams (g);
M2 --- the value of the mass of the barium sulfate precipitate obtained in the blank test, in grams (g);
M3 --- the value of the mass of the sample, in grams (g);
0.1374---The coefficient of sulfur is converted from barium sulfate.
The arithmetic mean of the results of two parallel determinations is the measurement result, and the absolute difference of the parallel determination results should be no more than 0.30%.
6 Determination of calcium (Ca) mass fraction---Atomic absorption spectrophotometry
6.1 Principle
Under acidic conditions, using an atomic absorption spectrophotometer, using an air-acetylene flame, at a wavelength of 422.7 nm, the sample solution is measured.
The absorbance of calcium is quantified using a working curve method or a linear regression equation. The addition of cerium chloride eliminates the interference of coexisting elements.
6.2 Reagents
6.2.1 Hydrochloric acid solution. 1 1.
6.2.2 Barium chloride solution. 150g/L.
6.2.3 Calcium standard solution. 0.1mg/mL.
6.3 Instruments and equipment
Atomic absorption spectrophotometer. with a hollow hollow cathode lamp.
6.4 Test procedure
6.4.1 Drawing of the working curve
6.4.1.1 Take five 100mL volumetric flasks and add calcium standard solutions 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL. in
Add 2 mL of cesium chloride solution and 2 mL of hydrochloric acid solution to each volumetric flask, dilute to the mark with water, and shake well.
6.4.1.2 According to the working conditions of the instrument, use air-acetylene flame to zero the blank solution without calcium standard solution at the wavelength of 422.7nm.
The absorbance of the solution was measured.
6.4.1.3 The mass concentration of calcium in the above solution (in micrograms per milliliter) is the abscissa, and the corresponding absorbance value is the ordinate.
Make a curve or calculate a linear regression equation.
6.4.2 Determination
Measure 10.00 mL of the sample solution, place it in a 50 mL volumetric flask, add 1 mL of cesium chloride solution, dilute to the mark with water, and shake well.
Determine the absorbance of the solution according to the provisions of 6.4.1.2, find out from the working curve or calculate the quality of calcium in the measured solution by linear regression equation
Volume concentration.
6.5 Test data processing
Calcium (Ca) mass fraction w2, calculated according to formula (2).
W2=ρ
1V1×10-6
M4 ×
100% (2)
In the formula.
Ρ1 --- Calculate the value of the mass concentration of calcium in the measured solution from the working curve or by linear regression equation, the unit is micro
Grams per milliliter (μg/mL);
V1 --- the value of the volume of the sample solution, in milliliters (mL);
M4---The value of the mass of the sample taken in grams (g).
The arithmetic mean of the results of the two parallel determinations is taken as the measurement result, and the relative deviation of the parallel measurement results is not more than 5%.
7 Determination of Magnesium (Mg) Mass Fraction---Atomic Absorption Spectrophotometry
7.1 Principle
Under acidic conditions, using an atomic absorption spectrophotometer, using an air-acetylene flame, at a wavelength of 285.2 nm, the sample solution is measured.
The absorbance of magnesium is quantified using a working curve method or a linear regression equation. The addition of cerium chloride eliminates the interference of coexisting elements.
7.2 Reagents
7.2.1 Hydrochloric acid solution. 1 1.
7.2.2 Barium chloride solution. 150g/L.
7.2.3 Magnesium standard solution. 0.1mg/mL.
7.2.4 Magnesium standard solution. 10μg/mL. Measure 5.00 mL of magnesium standard solution (see 7.2.3) in a 50 mL volumetric flask and dilute with water until
Scale and shake.
7.3 Instruments and equipment
Atomic absorption spectrophotometer. with a magnesium hollow cathode lamp.
7.4 Test procedure
7.4.1 Drawing of the working curve
7.4.1.1 Take 5 100mL volumetric flasks and add magnesium standard solution (see 7.2.4) to 0mL, 1.00mL, 2.00mL, 3.00mL,
4.00mL. Add 2 mL of cesium chloride solution and 2 mL of hydrochloric acid solution to each volumetric flask, dilute to the mark with water, and shake well.
7.4.1.2 According to the working conditions of the instrument, use air-acetylene flame to zero the blank solution without adding magnesium standard solution at the wavelength of 285.2nm.
The absorbance of the solution was measured.
7.4.1.3 The mass concentration of magnesium in the above solution (in micrograms per milliliter) is the abscissa, and the corresponding absorbance value is the ordinate.
Make a curve or calculate a linear regression equation.
7.4.2 Determination
Measure 10.00 mL of the sample solution, place it in a 100 mL volumetric flask, add 2 mL of cesium chloride solution, dilute to the mark with water, and shake well.
Determine the absorbance of the solution according to the provisions of 7.4.1.2, find out from the working curve or calculate the quality of magnesium in the tested solution by linear regression equation
Volume concentration.
7.5 Test data processing
Magnesium (Mg) mass fraction w3, calculated according to formula (3).
W3=ρ
2V2×10-6
M5 ×
100% (3)
In the formula.
Ρ2 --- the value of the mass concentration of magnesium in the measured solution calculated from the working curve or calculated by the linear regression equation, in units
Micrograms per milliliter (μg/mL);
V2---The value of the volume of the sample solution, in milliliters (mL);
M5---The value of the mass of the sample taken in grams (g).
The arithmetic mean of the results of the two parallel determinations is taken as the measurement result, and the relative deviation of the parallel measurement results is not more than 5%.
8 Determination of iron (Fe) mass fraction---Atomic absorption spectrophotometry
8.1 Principle
Determination of the sample solution under acidic conditions using an atomic absorption spectrophotometer using an air-acetylene flame at a wavelength of 248.3 nm
The absorbance of iron is quantified using a working curve method or a linear regression equation.
8.2 Reagents
8.2.1 Hydrochloric acid solution. 1 1.
8.2.2 Iron standard solution. 0.1 mg/mL.
8.3 Instrument
Atomic absorption spectrophotometer. attached with an iron hollow cathode lamp.
8.4 Test procedure
8.4.1 Drawing of the working curve
8.4.1.1 Take 5 100mL volumetric flasks and add 0mL, 0.50mL, 1.00mL, 1.50mL, 2.00mL of iron standard solution. in
Add 2 mL of hydrochloric acid solution to each volumetric flask, dilute to the mark with water, and shake well.
8.4.1.2 According to the working conditions of the instrument, use air-acetylene flame to zero the blank solution without adding iron standard solution at a wavelength of 248.3 nm.
The absorbance of the solution was measured.
8.4.1.3 Take the mass concentration of iron in the above solution (in micrograms per milliliter) as the abscissa, and the corresponding absorbance value as the ordinate.
Make a curve or calculate a linear regression equation.
8.4.2 Determination
Measure 10.00 mL of the sample solution, place it in a 100 mL volumetric flask, dilute to the mark with water, and shake well. Determined according to the provisions of 8.4.1.2
The absorbance of the solution is determined from the working curve or the linear regression equation is used to calculate the mass concentration of iron in the solution to be tested.
8.5 Test data processing
Iron (Fe) mass fraction w4, calculated according to formula (4).
W4=ρ
3V3×10-6
M6 ×
100% (4)
In the formula.
Ρ3 --- the value of the mass concentration of iron in the measured solution calculated from the working curve or calculated by the linear regression equation, in units
Micrograms per milliliter (μg/mL);
V3 --- the value of the volume of the sample solution, in milliliters (mL);
M6---The value of the mass of the sample, in grams (g).
The arithmetic mean of the results of the two parallel determinations is taken as the measurement result, and the relative deviation of the parallel measurement results is not more than 5%.
9 Determination of mass fractions of calcium (Ca), magnesium (Mg), iron (Fe) and aluminum (Al)---inductively coupled plasma optical emission spectrometry
9.1 Principle
Under acidic conditions, a high purity argon flame is used to atomize the solution into an inductively coupled plasma to determine calcium, magnesium, iron,
The analytical line signal intensity of aluminum is quantified by the working curve method.
9.2 Reagents
9.2.1 Hydrochloric acid solution. 1 1.
9.2.2 Calcium standard solution. 0.1 mg/mL.
9.2.3 Magnesium standard solution. 0.1 mg/mL.
9.2.4 Iron standard solution. 0.1 mg/mL.
9.2.5 Aluminum standard solution. 0.1 mg/mL.
9.3 Equipment
Inductively coupled plasma optical emission spectrometer.
9.4 Test procedure
9.4.1 Drawing of the working curve
9.4.1.1 Take 5 100mL volumetric flasks, separately transfer the corresponding standard solution, and prepare standard solution series according to Table 1, in each volumetric flask.
Add 2 mL of hydrochloric acid solution to each, dilute to the mark with water, and shake well.
Table 1 Standard solution series unit is microgram per milliliter
No. Element Standard Solution 1 Standard Solution 2 Standard Solution 3 Standard Solution 4 Standard Solution 5
1 Ca 0 2 4 6 8
2 Mg 0 1 2 3 4
3 Fe 0 2 4 6 8
4 Al 0 2 4 6 8
9.4.1.2 According to the working conditions of the instrument, use a high-purity argon plasma torch to zero the blank solution without adding the standard solution, as recommended in Table 2.
The wavelength of the analytical line signal of the element to be tested in the solution.
Table 2 Recommended wavelength
Element Ca Mg Fe Al
Wavelength/nm 393.37 279.55 259.94 396.15
9.4.1.3 Take the mass concentration of the element to be tested (in micrograms per milliliter) as the abscissa, and analyze the line signal intensity value as the vertical position.
Mark, draw the working curve.
9.4.2 Determination
Determine the intensity of the analytical line signal of the element to be tested in the sample solution according to 9.4.1.2, and find the element to be tested in the measured solution from the working curve.
Concentration.
9.5 Test data processing
The mass fraction of the element to be tested, wx, is calculated according to equation (5).
Wx=ρ
xV4×10-6
M7 ×
100% (5)
In the formula.
x --- element to be tested (calcium, magnesium, iron, aluminum);
Ρx --- The value of the mass concentration of the measured element in the sample solution is determined from the working curve, and the unit is microgram per milliliter (μg/mL);
V4 --- the value of the volume of the sample solution, in milliliters (mL);
M7 --- The value of the mass of the sample in grams (g).
The arithmetic mean of the results of the two parallel determinations is taken as the measurement result, and the relative deviation of the parallel measurement results is not more than 5%.
Related standard:   GB/T 37355-2019  GB/T 37359-2019
   
 
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