HG/T 2515-1993 Analysis method for active components of organic sulfur hydrogenation catalysts
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/ T 2515 -93
Active components of organic sulfur hydrogenation catalysts
Analysis methods
Published on September 9, 1993
Ministry of Chemical Industry of the People's Republic of China
Implementation on July 1, 1994
Chemical Industry Standard of the People's Republic of China
Active components of organic sulfur hydrogenation catalysts
Analysis methods
1 Subject content and scope of application
HG/T2515-93
This standard specifies the analysis method for the cobalt and molybdenum content in organic sulfur hydrogenation catalysts. This standard is applicable to the chemical analysis of the active components cobalt and molybdenum in organic sulfur hydrogenation catalysts T201 and T (T) 203 catalyst products.
2 Reference standards
GB/T602 Preparation of standard solution for determination of impurities in chemical reagents GB/T6682 Specifications and test methods for water used in analytical laboratories 3 General provisions
The purity of the reagents used in this standard are analytically pure unless otherwise specified; the experimental water should meet the specifications of grade 3 water in GB/T6682.
4 Preparation of test specimens
Mix the experimental empty samples evenly, take about 40g by quartering, crush and grind them all in a porcelain mortar, then take about 20g by quartering, continue to grind until they can all pass through a 125μm test sieve (in accordance with GB6003, R40/3 series aperture size), put them into a weighing bottle for use.
5 Preparation of test sample solution
5.1 Summary of method
The test sample is dissolved in sulfuric acid, the acid-insoluble matter is filtered out, and diluted with water to a certain volume for use. 5.2 Reagents and solutions
Sulfuric acid (GB/T625) solution: 1+1.
5.3 Instruments
General laboratory instruments,
5.4 Preparation steps
Weigh about 0.10g of sample, accurate to 0.0001g, place in a 250㎡L beaker, and moisten with a small amount of water. Add 10mL of sulfuric acid, cover the surface blood, slowly heat until the sample is completely dissolved, rinse the surface blood and the beaker wall with water after cooling slightly, until the volume dissolved in the beaker is about 50mL, filter this solution with medium-speed filter paper into a 100mL volumetric flask, rinse the filter paper with hot water until the filtrate is no longer acidic, wait for the solution to cool to room temperature, dilute with water to the scale, shake and set aside. Approved by the Ministry of Chemical Industry of the People's Republic of China on September 9, 1993 and implemented on July 1, 1994
6 Determination of cobalt content
6.1 Summary of the method
HG/T 2515-93
The divalent cobalt in the test solution forms a red complex with the nitroso R salt under the condition of pH 5.5 to 6. The determination is carried out by spectrophotometry.
6.2 Reagents and liquid
6.2.1 Cobalt sulfate (CoSO-7H2O HG/T 3-914).6.2.2 Sulfuric acid (GB/T625) solution: 1+1.6.2.3 Sodium acetate (GB/T693) solution: 450/L6.2.4 Nitric acid (GB/T 626) Solution: 1+1.6.2.5 Cobalt standard solution: 500/mL, prepared according to GB/T602. Weigh 1.315g of anhydrous cobalt sulfate (burned with CoS02·7H2O at 500-550°C to constant weight), dissolve it in water, transfer it into a 1000mL volumetric flask, dilute it to the mark with water, and shake to hook. 6.2.6 Cobalt standard solution: 10μg/mL.
Accurately pipette 10mL of cobalt standard solution (6.2.5) into a 500mL volumetric flask, dilute to the mark with water, shake well, 6.2.7 Nitroso R salt solution: 2 g/L.
6.3 Instruments
6.3.1 General laboratory instruments.
6.3.2 Spectrophotometer,
6.4 Analysis steps
6.4.1 Drawing of working curve
Accurately pipette 0, 1.0.2.0, 4.0.6.0, 8.0mL of cobalt standard solution (6.2.6) into 6 100mL volumetric bottles, add 10mL of sodium acetate solution, 10mL of nitroso R salt solution, 5 drops of nitric acid solution into each, dilute to the mark with water, shake well. Place at room temperature for 15 minutes, use a spectrophotometer at a wavelength of 490nm, with a 2cm absorption cell and a blank solution as a reference, measure the absorbance of the standard colorimetric solution one by one, use the mass of cobalt as the horizontal axis and the absorbance as the vertical axis, and draw a working curve. 6.4.2 Determination
Accurately pipette 2.0mL of the sample solution into a 100mL volumetric flask, add t0mL of sodium acetate solution, 10mL of nitrite R salt solution, 5 drops of nitric acid solution, dilute to the scale with water, shake well, place at room temperature for 15 minutes, use a spectrophotometer to measure the absorbance of the colorimetric solution under the same conditions as the standard colorimetric solution, and find the corresponding cobalt mass from the working curve according to the absorbance value of the sudden solution. 6.5 Expression of analysis results
The cobalt content is expressed as mass percentage (X,%), calculated according to formula (I): x,
m, ×10 -6
Wherein: m,
mass of cobalt found on the working curve, g;
mass of test material, g.
The result should be expressed to two decimal places,
6.6 Allowable difference
The absolute difference between two parallel determination results should not be greater than 0.15%, 2
× 100-
HG / T 2515 93
7 Determination of molybdenum trioxide content (Methods I and II have equal validity) 7.1 Summary of the method
7.1.1 Method I
In acidic solution, thiourea is used as a reducing agent to reduce hexavalent thiocarbamide to pentavalent thiocarbamide. The hexavalent thiocarbamide reacts with sulfuric acid salt to form a brown-red complex, which is determined by spectrophotometry.
7.1.2 Method II
In an acidic solution, hexavalent molybdenum is reduced to pentavalent molybdenum with ascorbic acid. Pentavalent molybdenum forms a blood-red complex with thiocyanate, which is determined by spectrophotometry.
Trivalent iron forms a blood-red complex with thiocyanate. After adding a reducing agent, the trivalent iron is reduced to divalent iron and no longer affects the determination. The presence of a certain amount of iron can make the color development reaction complete quickly and help maintain the pentavalent state. 7.2 Reagents and solvents
7.2.1 Molybdenum trioxide.
Sodium hydroxide (GB/T629) solution: 250g/L. 7.2.21
7.2.3 Citric acid (GB/T9855) solution: 350g/L.7.2.4 Sulfuric acid (GB/T625) solution: 1+1.7.2.5 Sulfur (HG3-979) solution: 100g/L Ammonium ferric sulfate (GB/T1279) solution: 60g/L. 7.2.6
7.2.7 Sulfuric acid (GB/T 625) solution: 1+3.7.2.8 Ascorbic acid solution: 100/L, stored in a brown bottle, valid for 7 days.7.2.9 Molybdenum trioxide standard solution: 500/mL. Weigh 0.500g of aluminum trioxide into a beaker, add 10mL of sodium hydroxide solution, heat to dissolve, cool and transfer to a 1000mL volumetric flask, dilute to the mark with water, and shake the spoon. 7.2.10 Molybdenum trioxide standard solution: 100/mL. Accurately pipette 50mL of molybdenum trioxide standard solution (7.2.9) into 9250mL volumetric flasks, dilute to the mark with water, and add 7.2.11 Potassium thiocyanate (GB/T648) solution: 350g/L-7.3 Instruments
7.3.1 General laboratory instruments
7.3.2 Spectrophotometer.
7.4 Analysis of non-step
7.4.1 Method I
7.4.1.1 Drawing of working curve
Accurately pipette 0, 0.5, 1.0, 2.0, 3.0, 4.0mL of molybdenum trioxide standard solution (7.2.10) into 6 100mL volumetric flasks respectively. Add 10mL of citric acid solution, 20mL of sulfuric acid solution (7.2.4), and 10mL of thiourea solution, let stand for 5 minutes, then add 10mL of potassium thiocyanate solution, shake well, let stand for 15 minutes, add water and shake, then add water to dilute to the scale, and shake well. Let stand at room temperature for 15 minutes, use a spectrophotometer at a wavelength of 460nm, with a 2cm absorption cell and a blank solution as a reference, to measure the absorbance of the standard colorimetric solution, with the mass of sodium trioxide as the horizontal coordinate and the absorbance as the vertical coordinate. Draw a working curve. 7.4.1.2 Determination
Accurately pipette 2.0mL of the sample solution into a 100mL container bottle, add 10mL of citric acid solution, 20mL of sulfuric acid solution (7.2.4) 10 mL sulfur solution: let stand for 5 minutes, then add 10 mL potassium thiocyanate solution and mix well. Place for 15 min, dilute with water and shake, then add water to the scale, shake sentence: Place at room temperature for 15 min, use a spectrophotometer to measure the absorbance of the color developed solution under the same conditions as the standard color developing solution,
According to the absorbance value of the solution, find the corresponding mass of molybdenum trioxide from the working curve, 3
7.4.2 Method II
7.4.2.1 Drawing of working curve
HG/T2515—93
Accurately pipette 0, 0.5, 1.0, 2.0, 3.0, 4.0 mL of molybdenum trioxide standard solution (7.2.10) and place them in 6 100 mL volumetric flasks that have been added with 5 mL of ammonium sulfate solution in advance, add 10 mL of potassium thiocyanate solution, 20 mL of sulfuric acid solution (7.2.7), and 10 mL of ascorbic acid solution to each flask, dilute with water to the scale, and shake. Place at room temperature for 20 minutes, use a spectrophotometer at a wavelength of 460nm, with a 2cm absorption gap, and use the blank solution as a reference to determine the absorbance of the standard color-developing solution one by one, and use the mass of trioxide as the horizontal axis and the absorbance as the vertical axis to draw a working curve. 7.4.2.2 Determination of
Put 2.0mL of the sample solution in a 100mL volumetric flask that has been previously added with 5mL of ammonium ferric sulfate solution, add 10mL of potassium thiocyanate solution, 20mL of sulfuric acid solution (7.2.7), and 10mL of ascorbic acid solution, dilute to the scale with water, shake well, and place at room temperature for 20 minutes. Use a spectrophotometer to determine the absorbance of the color-developing solution under the same conditions as the standard color-developing solution. According to the absorbance value of the solution, the corresponding mass of trioxide can be found from the working curve. 7.5 Expression of analysis results
The content of trioxide in aluminum is Mass percentage (X2%), calculated by (2) X,
mz×10~6
Where: m2——mass of molybdenum trioxide found on the working curve, 4g; -mass of the test material, g.
The result should be expressed to two decimal places,
7.6 Allowable difference
The absolute difference between the results of two parallel determinations should not exceed 0.30%, Additional remarks:
This standard is proposed by the Science and Technology Research Institute of the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of Nanjing Chemical Industry (Group) Corporation. This standard was drafted by the Chemical Fertilizer Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Li Jide and Zhang Yalin (2)
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Chemical Industry Standard
Active components of organic sulfur hydrogenation catalysts
Analysis method
JIG/T2515-93
Editor: Chemical Industry Standard Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal code: 100013
Printer: Standardization Research Institute of Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Format: 880×12301/16 Sheet: Number of words: 8000
First edition: January 1994
First printing: January 1994
Number of copies: 1-500
1 Book fee: RMB 2.60
G/T2515-
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