HG/T 2511-1993 Chemical composition analysis method of methanation catalyst
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG /T 2511 — 93
Chemical Composition of Methanation Catalysts
Analysis Method
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
Analysis Method of Chemical Composition of Methanation Catalysts Subject Content and Applicable Scope
HG/T2511—93
This standard specifies the analysis method of the chemical composition of J101, J105 and J106Q methanation catalysts. This standard applies to Used for the analysis of chemical components such as aluminum oxide, magnesium oxide content and total amount of rare earth oxides in alkylation catalysts.
2 Reference standards
GB/T601 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T603 Preparation of preparations and products used in chemical reagent test methods GB/T6682 Specifications and test methods for water used in analytical laboratories 3" Reagents and materials
The purity of the reagents used in this standard is analytical pure unless otherwise specified; the experimental water should meet the specifications of grade 3 water in GB/T6682.
4 Preparation of test samples
Mix the laboratory samples evenly, take about 40g by quartering method, crush and grind them all in a porcelain mortar, take about 20g by quartering method, continue to grind until the sample can pass through the 125μm test sieve, and put it into a weighing bottle. 5 Preparation of sample solution
5.1 Method summary
The sample is dissolved in sulfuric acid, and the acid insoluble matter is removed by filtration. The filtrate is diluted to a certain volume. 5.2 Reagents and solutions
5.2.1 Sulfuric acid (GB/T 625) solution: 1+1.5.2.2 Sulfuric acid (GB/T625): 1+200.
5.2.3 Hydroxylamine hydrochloride (GB/T6685) solution: 50g/L5.3 Operation steps
For J101 and J105 catalysts, weigh 0.5g of sample: For J106Q catalyst, weigh 1g of sample. Both are accurate to 0.0001g. Place in a 250mL beaker, moisten with a little water, add 10mL of sulfuric acid solution (5.2.1), 2mL of hydroxylamine hydrochloride solution, cover the surface with blood, and heat to dissolve the sample completely. Add water to 50-60mL, stir to dissolve any salts that may be folded out, and heat to about 50°C if necessary. Filter into a 250L pan bottle with medium-speed filter paper, wash the beaker and filter paper with sulfuric acid solution (5.2.2) for 6-8 hours, cool to room temperature, dilute to the scale with water, shake the hook, and remove the mixture. 6 Determination of nickel content
6.1 Method Summary
Approved by the Ministry of Chemical Industry of the People's Republic of China on September 9, 1993 and implemented on July 1, 1994
HG/T 2511 — 93
Mask aluminum and rare earth with sodium fluoride, accurately add excess EDTA standard titration solution, adjust to pH 5-6, use xylenol orange as indicator, and back titrate with zinc chloride standard titration solution. 6.2 Reagents and solutions
6.2.1 Sodium chloride (GB/ T 1264),
6.2.2 Hydrogenated water (GB/ T. 631) solution: 1+1, 6.2.3 Acid-sodium acetate buffer solution (pH 5.7) Weigh 100g sodium acetate (CH,COONa·3H,O) (GB/T693), dissolve in appropriate amount of water, accurately add 4.5mL glacial acetic acid (GB/T676), dilute with water to 1000mL, shake and mix. 6.2.4 EDTA (GB/T1401) Standard titration solution: c(EDTA)=0.02m01/L, prepare and Calibration
6.2.5 Zinc chloride (HG/T3-947) standard titration solution, c(ZnCl)=0.02mol/L Prepare and calibrate according to GB/T601,
6.2.6 Xylenol orange indicator solution: 2g/L, prepare according to GB/T603 6.3 Analysis steps
Accurately pipette 25.0mL of sample solution into a 250mL conical flask, add 1g of fluoride, add water to about 50mL, shake well. Add 15.0mL of DTA standard titration solution, 4~5 drops of xylenol orange indicator solution, and drop nitrogen water solution (6.2.2) until the solution just turns orange. Add 10mL of acetic acid-sodium acetate buffer solution. Titrate with zinc chloride standard titration solution until the solution just turns from yellow to white, and record the volume consumed.
6.4 Expression of analysis results
The mass percentage of nickel (x) is calculated according to formula (1), x,
wherein: V—
0. 058 69-
(V, - c, V, c,)x 0. 058 69
The volume of EDTA standard titration solution added, mL: The actual concentration of EDTA standard titration solution, mol/L: The volume of zinc chloride standard titration solution consumed, mL: The actual concentration of zinc chloride standard titration solution, mol/L; The mass of the sample taken, g;
X 100-
and 1.00mL EDTA standard titration solution <c(EDTA)=1. 000mol/L L) is the mass of the corresponding ingot expressed in grams.
6.5 Allowable difference
The absolute difference between the results of two parallel determinations should not be greater than 0.3%. 7 Determination of aluminum oxide content (applicable to J101 and J105 methanation catalysts) 7.1 Method summary
In a solution with pH 5-6, add an excess of EDTA standard titration solution to make it complex with aluminum, nickel, rare earth ions, etc., back-titrate the excess EDTA with zinc oxide standard titration solution, add sodium fluoride, and remove the EDTA complexed with aluminum and rare earth. The released EDTA is titrated with zinc oxide standard titration solution. The titrated volume is the total volume of EDTA consumed by aluminum and rare earth. Then remove the EDTA consumed by rare earth. Volume can be used to calculate the amount of lead. 7.2 Reagents and solutions
Same as 6.2.
7.3 Analysis steps
Pipette 25.0mL of sample solution and place it in a 500mL conical flask, add 40mL of LEDTA standard titration solution, and dilute it to about 120mL with water 2
HG / T 2511 93
. Add 5-6 drops of xylenol orange indicator solution, add ammonia solution (6.2.2) until the solution changes from yellow to orange, add 10 mL of acetic acid-sodium acetate to rinse the solution, boil for 3 min, cool to room temperature, and titrate with zinc chloride standard titration solution until the yellow changes to orange.
Add about 1 g of sodium fluoride, boil for 3 mi, cool to room temperature, and titrate with zinc chloride standard titration solution. The end point color is the same as the end point of the first titration. Note the volume of zinc chloride standard titration solution consumed in the second titration. 7.4 Expression of analytical results
The mass percentage of aluminum oxide (x) is calculated according to formula (2): x
(V, +c2 -Va:c,)× 0.05098
Wherein: V3 Volume of zinc chloride standard titration solution consumed in the second soft titration, mL: (2)
Actual concentration of zinc chloride standard titration solution, mol/LC2
V.—Volume of EDTA standard titration solution consumed by the total amount of rare earth oxides in 25.0mL sample solution (see Chapter 8), mL;
\.5Allowance difference
-Actual concentration of EDTA standard titration solution, mol/L; Mass of sample, g:
-Mass of aluminum oxide in grams equivalent to 1.00mL EDTA standard titration solution [c(EDTA)=1.000mol/L).
The absolute difference between two parallel determination results should not exceed 0.3%. 8 Determination of total tert-butyl oxides
8.1 Method Summary
Under the condition of pH 5-6, use o-phenanthroline to mask nickel, sulfosalicylic acid to mask aluminum, use azodicarbonamide III as indicator, and titrate rare earth with EDTA:
8.2 Reagents and solutions
8.2.1 Hydrogenated water (GB/T 631) solution: 1+1.8.2.2 Sulfosalicylic acid (GB/T10705) solution: 200g/L8.2.3. o-phenanthroline (GB/T1293) solution: 50g/L Weigh 5g o-phenanthroline, moisten with appropriate amount of water, add 4mL hydrochloric acid solution (1+1), and dilute with water to 100mL8.2.4 Acetic acid-sodium acetate buffer solution (pH~5. 7) Prepare the same as 6.2.3,
8.2.5 EDTA (GB/T1401) standard titration solution: c(EDTA)=0.02mol/L, prepared and calibrated according to GB/T60I. The determination of the titration degree of this solution for rare earth oxides is shown in Appendix A. 8.2.6 Azosol III (HG/T3-1007) indicator solution: 2 ml/L 8.3 Analysis steps
Accurately pipette 25.0 mL of sample solution into a 250. mL beaker, add 5 mL of o-filament solution, 5 mL of sulfosalicylic acid solution (double the amount when analyzing J106Q type), stir and add 3-4 drops of azosol III indicator solution, add ammonia solution (8.2.1) until the solution changes from purple-red to dark green, add 10 mL of acetic acid-sodium acetate buffer solution, dilute with water to about 100 mL, use a high-precision burette, and titrate with EDTA standard titration solution until the dark edge color changes to purple-red. 8.4 Expression of analysis results
The mass percentage (z) of the total amount of rare earth oxides is calculated according to formula (3): 3
HG/T 2511 —93www.bzxz.net
Wherein: V is the volume of EDTA standard titration solution consumed, mL: T
8.5 allowable difference
-the mass of the sample taken for the titration of rare earth oxides.
The absolute difference between the two parallel determination results should not exceed 0.2% for J105 catalyst and 0.07% for J106Q catalyst.
9 Determination of magnesium oxide content (applicable to J105 methanation catalyst) 9.1 EDTA titration method (arbitration method)
9.1.1 Method summary
Use hexamethylenetetramine, ammonium carbonate and copper reagent to precipitate and separate aluminum, nickel and rare earth. In a solution of pH ~ 10, use chrome black T as an indicator and use EDTA standard titration solution to titrate magnesium. 9.1.2 Reagents and solutions
9. 1. 2: 1 ammonium carbonate (GB / T 662).9.1.2.2 Ammonia (GB/T631) solution: 1+19.1.2.3 Hydrochloric acid (GB/T622) solution: 1+1.9.1.2.4 Hexadecane (GB/T1400) solution: 300g/L9.1.2.5 Copper reagent (GB/T10727) solution: 50g/L Weigh 5&copper reagent into a 250mL beaker, add appropriate amount of water to dissolve, add 10 drops of ammonia solution (9.1.2.2), dilute with water to 100mL and prepare.
9.1.2.6 Ammonia-ammonium buffer solution A (pH 10), prepared according to GB/T603, 9.1.2.7 EDTA (GB/T1401) standard titration solution, c(EDTA)=0.02mo)/L, prepared and calibrated according to GB/T601.
9.1.2.8 Chrome black T indicator solution: 5g/L, prepared according to GB/T603. 9.1.3 Analysis steps
Accurately pipette 25.0mL of sample solution into a 250mL beaker, add water to about 100mL, heat to boiling, add ammonia solution (9.1.2.2) dropwise until turbidity appears, then add hydrochloric acid solution (9.1.2.3) until the precipitate is just dissolved, add 5mL of methylenetetramine solution, heat to boiling, cool to about 60°C, add 0.5g of ammonium carbonate, add 10mL of copper reagent solution, stir, cool to 40°C, transfer to a 250mL volumetric flask, dilute to the scale with water, and shake. Dry filter, discard the first few milliliters of filtrate, accurately pipette 100.0mL of filtrate into a 250mL conical flask, add 10mL of ammonia-ammonium chloride buffer solution A, 5 drops of EDTA indicator solution, titrate with EDTA standard titration solution until pure blue, record the volume of EDTA consumed, and perform blank test at two times. 9.1.4 Expression of analytical results
The mass percentage of magnesium oxide (x) is calculated according to formula (4): x
(Vs V,) . c, × 0. 040 31
Where: V-the volume of EDTA standard titration solution consumed during titration, mL; V-the volume of EDTA standard titration solution consumed in blank test, mL; c
-the actual volume of EDTA standard titration solution, Ⅱo1/L; the mass of the sample taken,:
HG / T 2511 —93
-The mass of magnesium oxide expressed in grams equivalent to 1.00mL EDTA standard titration solution [c(EDTA)=1.000mol/L],
9.1.5 Allowable difference
The absolute value of two parallel determination results should not be greater than 0.2%. 9.2 Atomic absorption method
9.2.1 Summary of method
The atomic absorption method is used with an air-acetone fast oxidizing flame and a 285.2nm analytical line to determine the magnesium in the sample solution. The standard addition method is used to overcome the influence of sulfuric acid and other interfering factors. 9.2.2 Reagents and solutions
9.2.2.1 Magnesium oxide (GB/T9857) standard solution (1 mL solution contains 1.00 mg MgO) Weigh 1.000 g of magnesium oxide burned at 800°C to constant weight, place it in a beaker, moisten it with water, add 20 mL of hydrochloric acid solution (1+1), transfer it to a 1000 mL volumetric flask after dissolution, dilute it to the scale with water, shake well, and store it in a plastic bottle. 9.2.2.2 Magnesium oxide standard solution (1mL solution contains 20.0g MgO)
Accurately pipette 10.0mL magnesium oxide standard solution (9.2.2.1) and place it in a 500mL volumetric flask, dilute to scale with water, and use 9.2.3 Instrument
Atomic absorption spectrometer (with magnesium hollow cathode lamp) 9.2.4 Analysis steps
Accurately pipette 10.0mL sample solution and place it in a 100mL volumetric flask, dilute to scale with water, and shake. Then accurately pipette 10.0mL of the diluted solution in three portions and place them in 100mL volumetric flasks one, two, and three respectively; accurately add 0.0, 10.0, and 20.0mL magnesium oxide standard solution (9.2.2.2) to the three volumetric flasks, dilute to scale with water, and shake. According to the working conditions of the instrument, use air-acetylene oxidizing flame and 285.2nm analytical line. First, adjust the instrument with water to zero absorbance, and then measure the absorbance of the solutions in the three volumetric flasks respectively:
The concentration of magnesium oxide in the solution in the first volumetric flask is calculated according to formula (5): Pamo) (2.00+400) × (4, A,)+(4, -A1)A
Wherein: P(Mgo) is the concentration of magnesium oxide in the solution in the first volumetric flask, μg/mL; 2.00 is the concentration of magnesium oxide increment in the solution in the second volumetric flask, /mL; 4.00 is the concentration of magnesium oxide increment in the solution in the third volumetric flask, g/mL; A, A2, As are the absorbances of the solutions in the first, second and third volumetric flasks respectively. 9.2.5 Expression of analysis results
The mass percentage of magnesium oxide (xs) is calculated according to formula (6): x, -
Pmro) :Yg × 10 -6
× 100
Wherein: P(Mzo)—magnesium oxide concentration in the solution in the first volumetric flask, nom/mL, see (5); V—volume of the solution in the first volumetric flask, mL; m2—mass of the sample taken, g.
9.2.6 Allowable difference
The absolute difference between the results of two parallel determinations should not be greater than 0.4%, (5)
A1 Reagents and solutions
HG / T 2511 - 93
Appendix A
Determination of the titer of rare earth oxides with EDTA standard titration solution (supplement)
A1.1 Hydrochloric acid (GB/T622) solution: 1+1. A1.2 Ammonia (GB/T631) solution: 1+1. A1.3 Oxalic acid (GB/T9845) solution: 100g/L. A1.4 Oxalic acid (GB/T9845) solution: 10g/L. A1.5 Hydroxylamine (GB/T6685) solution: 50g/L. A1.6 Acetic acid-sodium acetate buffer solution (pHα5.7): Preparation is the same as 6.2.3. A1.7 EDTA (GB/T 1401) standard titration solution: c(EDTA)=0.02mol/L, according to GB/T 601 Preparation and calibration,
A1.8 Methyl orange indicator: 1g/L,
A1.9 Azodicarbonamide III (HG/T3-1007) indicator: 2g/L. A2 Purification of rare earth oxides
Weigh about 1g of the raw material of rare earth oxide for preparing the catalyst, place it in a 250mL beaker, add 10mL of hydrochloric acid solution (A1.1) and 2mL of hydroxylamine hydrochloride solution, heat until completely dissolved, dilute with water to about 80mL, if salts precipitate, heat until all the salts are dissolved, filter with medium-speed filter paper, collect the filtrate in a 400mL beaker, add 2 drops of methyl orange indicator, neutralize with ammonia solution (A1.2) until the solution changes from red to orange-yellow, then add hydrochloric acid solution (A1.1) until it just appears red and add 5 drops in excess, heat to nearly boiling, add 50mL of oxalic acid solution (A1.3), and leave at room temperature for 4h.Filter with medium-speed quantitative filter paper, wash the precipitate with oxalic acid solution (A1.4) several times, put the precipitate together with the filter paper into a porcelain, burn in a high-temperature furnace at 850℃ for 1.5h after the paper is incinerated, take it out and place it in a desiccator to cool to room temperature,
A3 Determination of titer
Weigh 0.5g (accurate to 0.000ig) of the purified rare earth oxide, place it in a 250mL beaker, add 2mL of hydrochloric acid solution (A1.1), 2mL of hydroxylamine hydrochloride solution, heat to completely dissolve it, cool it, transfer it to a 250mL volumetric flask, dilute it to the scale with water, shake it
Accurately draw 25.0mL of the above solution, place it in a 250mL beaker, add 2 drops of azo spleen blood indicator solution, and adjust it with ammonia solution (A1.2) until the solution changes from purple-red to blue-green. Add 10mL of acetic acid-sodium acetate buffer solution, and use EDTA Titrate the solution with standard titration solution until the solution changes from blue-green to purple-red. A4 calculates
wherein. T---the titration degree of EDTA standard titration solution on rare earth oxide, name/mL; m
mass of rare earth oxide after purification, g
volume of EDTA standard titration solution consumed, mL. (7)
Additional instructions:
HG/T2511—93
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Research Institute of Nanjing Chemical Industry (Group) Corporation. This standard is drafted by Sichuan Chemical General Plant. The main drafters of this standard are Liu Fujin, Huang Songsheng and Yang Chengzhang. From the date of implementation of this standard, the former Ministry of Chemical Industry of the People's Republic of China Standard HG/T1-1429—84 "Analysis Method of Chemical Composition of Methane Catalyst" shall be invalid.
People's Republic of China
Chemical Industry Standards
Methanation Catalyst Chemical Composition Analysis Method HG/T 2511 -- 93
Editor Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printed by Standardization Research Institute of Ministry of Chemical Industry
Copyright reserved and no reproduction or reprinting
Format 880×12301/[6 Sheets 5% Number of Words 13000 First Edition December 1993
First Printing December 1993
Print Quantity [—500
Cost 5.00 Yuan
HG/T 2511—9
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