Original standard number HG 1-1428-1981 HG/T 3553-1981 Chemical composition analysis method for methanol and low temperature shift catalyst HG/T3553-1981 Standard download decompression password: www.bzxz.net

Standard of the Ministry of Chemical Industry of the People's Republic of China Chemical Composition Analysis Method of Combined Alcohol and Low Temperature Shift Catalysts
HG 1--1428-81
Adjusted to: H6/ 3573-1P81
This standard is applicable to the analysis and inspection of the chemical composition of combined alcohol catalyst C207, low temperature shift catalyst B202, B204 and other catalyst products with the same chemical composition. Preparation of Analytical Samples
Mix the catalyst samples evenly, take about 40 grams by quartering, crush and grind them all in a porcelain mortar, and then take about 20 grams by quartering, continue to grind until all pass through a 100-mesh sample sieve, and place them in a weighing bottle for use. 2 Preparation of Sample Solution
2.1 Summary of Method
The sample is dissolved with hydrochloric acid, and the acid-insoluble matter is removed by filtration. The filtrate is diluted to a certain volume and set aside. 2.2 Required reagents
2.2.1 Hydrochloric acid (1 + 1)
2.2.2 Hydrochloric acid (1 + 100)
2.3 Required instruments
General laboratory instruments.
2.4 Operation steps
Accurately weigh 0.5 g of the sample, place it in a 250 ml beaker, moisten it with water, add 10 ml of (1+1) hydrochloric acid, cover it, and heat to completely dissolve the sample. After cooling, rinse the surface and beaker with water, add 50-100 ml of water, heat to 60-80℃, filter with medium-speed filter paper, wash the filter paper with hot (1+100) hydrochloric acid 6-8 times, transfer the filtrate and washing solution into a 250 ml vial, cool to room temperature, dilute with water to the scale, and operate. 3 Determination of zinc fluoride content (EDTA method) 3.1 Method summary
Under pH 5.7, use sodium thiosulfate as a mask and sodium fluoride as a mask, use xylenol orange as an indicator, and use EDTA to titrate the zinc in the sample solution.
3.2 Required reagents
3.2.1 Ammonia hydrogen water (1+ 1)
3.2.2 Sodium fluoride.
3.2.3 Sodium thiosulfate (10%).
3.2.4 Monocresol orange indicator (0.2 mL).
3.2.5 Acetic acid-sodium acetate buffer solution (pH 5.7): Weigh 100 g of sodium acetate (CH:C00Na-3H20), add 13 mL of 6N acetic acid to an appropriate amount of water, and dilute to 500 ml with water. 3.2.6 EDTA standard solution (0.02 M). 3.3 Required instruments
General laboratory instruments
3.4 ​​Operation steps
Aspirate 25 ml of the sample solution prepared in Chapter 2 of this standard, place it in a 250 ml beaker, add about 1 gram of sodium epichloride, neutralize with (1+1) hydrogen water until there is a mixture, add 10 mol of acetic acid-sodium acetate buffer solution, 10 ml of 10% sodium thiosulfate, and 4-5 drops of xylenol orange indicator, dilute with water to 100 ml, and titrate with EDTA standard solution until the solution changes from orange-red to yellow. The volume consumed by the EDTA standard solution is VI. 3.5 Calculation
The zinc oxide content X (%) is calculated as follows
V × M × 0.081 38
-Amount of EDTA standard solution, ml:
Formula: V
—Molar concentration of EDTA standard solution,
Amount of sample taken, g;
-1 liter of 1M EDTA standard solution is equivalent to the amount of zinc oxide, g. 3.6 Precision
The difference between the results of two parallel determinations should not be greater than 0.30%. 4 Determination of copper oxide content (EDTA volumetric method) 4.1 Summary of the method
Under the condition of pH 9.2, sodium fluoride is used to decompose aluminum, PAN is used as the indicator, and EDTA is used to complex the copper and zinc in the sample. The copper content minus the zinc content is the copper content. ·4.2 Required reagents
4.2.1 Ammonia water (1+1).
4.2.2 Ethanol.
4.2.3 Sodium hydroxide.
4.2.4 Ammonium hydroxide buffer solution (pH 9.2): weigh 27 g ammonium hydroxide, add appropriate amount of water to dissolve, add 32 ml ammonia water, and dilute with water to 500 ml.
i4.2.5 PAN indicator [1-(2-pyridinyl nitrogen) 2· phenol]: weigh 0.2 g PAN and dissolve in 100 ml ethanol. 4.2.6 EDTA standard solution (0.02M).
4.3 Instruments used
General laboratory instruments,
4.4 Operating procedures
Accurately take 25 ml of the sample prepared according to Chapter 2 of this standard, filter it into a 250 ml beaker, add about 1 g of sodium chlorite, neutralize it with (1+1) ammonia water until the solution turns blue, add 10 ml of nitrogen·nitrogen buffer solution, 5 drops of PAN indicator, and 15 ml of ethanol, and titrate with EDTA standard solution until the solution changes from purple to yellow-green, which is the end point. 4.5. Calculation of the consumption volume of EDTA standard solution V24.5. Calculate the copper oxide content (%) according to the following formula: (VV.) × MX0.07955 Where: V---the amount of EDTA standard solution used to titrate the copper and zinc, ml; Vi--the amount of EDTA standard solution used to titrate zinc, ml; M---the molar concentration of EDTA standard solution;
--the amount of sample, g;
1 ml of 1M EDTA standard solution is equivalent to the amount of copper oxide, g. 4.6 Precision
The difference between two determination results should not be greater than 0.30%. 12
HG1—1428—81
5 Determination of aluminum oxide content (EDTA volumetric method) 5.1 Method summary
At pH 5.7, add EDTA to complex the lead and other metal ions in the sample solution. The EDTA complexed with aluminum is replaced by sodium fluoride by back-titration with zinc solution. The released EDTA is titrated with zinc standard solution. 5.2 Required reagents
5.2.1 Ammonia water (1+1).
5.2.2 Sodium fluoride.
5.2.3 Xylenol orange indicator (0.2%).
5.2.4 Acetate Sodium acetate buffer (pH 5.7): Weigh 100 g of sodium acetate (CH,COONa-3H20), dissolve it in an appropriate amount of water, add 13 ml of 6N acetic acid, and dilute to 500 ml with water. 5.2.5 EDTA standard solution (0.02M).
5.2.6 Zinc standard solution (0.02M).
5.3 Required instruments
General laboratory instruments.
5.4 Operation steps
Accurately pipette 25 ml of the sample bath solution prepared in accordance with Section 2 of this standard, place it in a 250-liter conical flask, add 35 ml of EDTA standard solution and 10 drops of xylenol orange indicator, neutralize with (1+1) ammonia water until the solution turns blue-purple, then add 10 liters of acetic acid-sodium acetate buffer solution, heat and boil for 3 minutes, cool and titrate with zinc standard solution until the solution changes from yellow-green to light brown. Add about 1 gram of sodium fluoride, heat and boil for 3 minutes, cool and titrate with zinc standard solution, the titration end point is the same as the first titration end point, record the volume of zinc standard solution used for the second titration. 5.5 Calculation
The aluminum oxide content X, (%) is calculated as follows: X3
Wherein: V-
V x M ×0.050 98
-the amount of zinc standard solution used in the second titration, ml; M-the molar concentration of zinc standard bath solution;
the amount of sample taken, g;
-1 ml of 1M zinc standard solution is equivalent to the amount of aluminum oxide, g. 5.6 Accurate determination
The difference between the results of two parallel determinations should not be greater than 0.20%. Determination of ferric chloride content (atomic absorption method-1 method)
6.1 Method summary
Use atomic absorption method, air-acetylene flame, 2483 angstrom analytical line to determine the iron in the sample solution, and use the standard curve method for quantification. The coexisting elements have no interference with the determination.
6.2 Required reagents
6.2.1 Hydrochloric acid (1 + 1).
6.2.2 Ferric oxide standard solution (1 ml contains 100 μg of ferric oxide): Weigh 0.1000 g of ferric oxide (FeO2) burned to constant weight at 900℃, place in a 250 ml beaker, add 20 ml of (1+1) hydrochloric acid, heat to completely dissolve, transfer to a 1000 ml volumetric flask, cool to room temperature, dilute with water to the mark, and shake to hang. 6.3 Instruments
6.3.1 General laboratory instruments.
HG1-1428--81
6.3.2 Atomic absorption spectrophotometer: with iron hollow cathode lamp. 6.4 Operation steps
6.4.1 Drawing of standard curve: Accurately pipette 1 ml of 100 micrograms of ferric oxide standard solution 0, 0.5, 1, 2, 3, 4, 5 ml, respectively, into 100 ml volumetric flasks, add (1+1) salt solution 0.4 ml each, dilute to 100% with water, and shake. According to the working conditions of the instrument, use air acetylene flame and 2483 angstrom analytical line to measure the absorbance of the standard series, and draw the standard curve. 6.4.2 Sample analysis: Directly use the sample solution prepared in Chapter 2 of this standard to measure the absorbance under the same conditions as the standard series. Find the concentration of ferric oxide in the solution to be tested from the standard curve. .5 Calculation
The content of ferric cyanide X4 (%) is calculated as follows: X4
C × V × 10 -6
Wherein: C is the concentration of ferric oxide in the solution to be tested, μg/ml, the volume of the solution to be tested, ml,
Weigh the sample, g.
Master.6 Accuracy
The difference between the results of two parallel determinations should not be greater than 0.005%. 7 Determination of ferric oxide content (o-phenanthroline spectrophotometry 7.1 Method Summary
Method II)
Under pH 4 conditions, hydroxylamine hydrochloride is used to reduce ferric iron to divalent iron, and divalent iron and o-phenanthroline form a red complex. The absorbance is measured at a wavelength of 51U nanometers by spectrophotometry. The iron content in the colorimetric band is in the range of 0 to 50 μg/liter and conforms to Beer's law. Copper interferes with the determination, so add citric acid to eliminate it. 7.2 Required Reagents
7.2.1 Hydroxylamine hydrochloride (10%).
7.2.2 Citric acid (15%): Weigh 15 g of citric acid, dissolve it in water and dilute to 100 ml, and adjust to pH 4.0 with 30% sodium hydroxide.
7.2.3 O-phenanthroline (1.5%): Weigh 1.5 g of o-phenanthroline, dissolve it with appropriate amount of water and 1 ml of hydrochloric acid, and dilute to 100 ml with water.
7.2.4 Acetic acid-sodium acetate buffer solution (pH 4): Weigh 27 g of sodium acetate (CHCOONa-3HzO), dissolve it in appropriate amount of water, add 50 ml of glacial acetic acid, and dilute to 500 ml with water. 7.2.5 Standard solution of ferric nitride (1 ml contains 100 μg of ferric oxide): Weigh 0.1000 g of ferric oxide (Fez0,) burned to constant weight at 900℃, place in a beaker, add 20 ml of (1+1) hydrochloric acid, heat to dissolve completely, transfer to a 1000 ml volumetric flask, cool to room temperature, dilute with water to the mark, and shake the hook. 7.2.6 Standard solution of ferric oxide (1 ml contains 10 μg of ferric oxide): Accurately pipette 10 ml of 1 ml of standard solution containing 100 μg of ferric oxide, place in a 100 ml volumetric flask, dilute with water to the mark, and shake the hook. 7.3 Required instruments
7.3.1 General laboratory instruments.
7.3.2 Spectrophotometer.
7.4 Operation steps
7.4.1 Drawing of standard curve: Accurately pipette 1 ml of 10 μg ferric oxide standard solution 0, 0.5: 12, 3, 45 ml, respectively, into 50 ml volumetric flasks, add 10 ml of 15% citric acid, 5 ml of acetic acid-sodium acetate buffer solution, 4 ml of 10% hydroxylamine hydrochloride, 10 ml of 1.5% o-phenanthroline, dilute with water to scale, shake, and leave for half an hour. Use a spectrophotometer at a wavelength of 510 nanometers of water, with the reagent blank as the reference, and use a 3 cm colorimetric III to measure the absorbance of the standard series and draw a standard curve. 14
HG 1--1428--81
7.4.2 Sample analysis: Accurately absorb 10 ml of the sample solution prepared in Chapter 2 of this standard, place it in a 50 ml container, add 10 ml of 15% citric acid, 5 ml of acetic acid-sodium acetate grade solution, 4 ml of 10% hydroxylamine hydrochloride, 10 liters of 1.5% non-thermal solution, dilute to full scale with water, operate the hook, and leave it for half an hour. Measure the absorbance under the same conditions as the standard series, and infer the iron oxide content of the solution from the standard curve:
.7.5 Calculate the iron oxide content X. (%) is calculated as follows: S×10 6 Formula: S-1-1 From the standard curve, the content of Fe2O3 in the sample solution is obtained, μg: g-1. The difference between the results of two parallel determinations should not be greater than 0.005%. Determination of sodium content (atomic absorption method - 1 method) 8:1 Method Summary: Atomic absorption method is used with air-acetylene flame, 5890 angstroms per minute to determine the sodium in the sample solution, and the standard curve is used for quantitative analysis. The coexisting elements zinc, aluminum and zinc have no interference with the determination. 8.2 Required Reagents
8.2.1 Sodium hydroxide standard solution (1 ml contains 1 mg sodium hydroxide): weigh 1.8859 g sodium chloride (NaCl) burned to constant weight at 500-600°C, dissolve with water, transfer to a 1000 liter volumetric flask, dilute to scale with water, and transfer to a plastic bottle. 8.2.2 Caustic soda standard solution (1 ml contains 100 μg sodium hydroxide): accurately pipette 1 ml of 1 mg sodium hydroxide standard solution 10 liters, place in a 1000 liter volumetric flask, dilute to scale with water, and add. 8.3 Required Instruments
8.3.1 Laboratory-General Instruments.
8,3,2 Atomic absorption spectrophotometer: with steel hollow pole lamp 8.4 Operation steps
8.4.1 Drawing of standard curve: Accurately pipette 1 liter of 0, 0.5, 1.2, 4, 6, 8 liters of standard solution containing 100 micrograms of sodium hydroxide, respectively, into 100 ml bottles, dilute to the scale with water, and then add water. According to the working conditions of the instrument, use air-acetylene flame and 5800 angstrom analytical line to measure the absorbance of the standard series, and finally make a standard curve. 8.4.2 Trial extension: Directly use the sample solution prepared according to Chapter 2 of this standard, and measure the absorbance under the same conditions as the standard series. Find the concentration of sodium hydroxide in the test solution from the standard curve. 8.5 Calculation of sodium hydride content X (%) Calculate as follows: Cx V × 10-6 Wherein: (~- Obtain the concentration of sodium hydride in the test solution from the standard curve, μg/ml, volume of the test solution, and the amount of sample weighed. 8.6 Precision When the sodium hydride content is between 0.1% and 1%, the difference between the results of two parallel determinations should not be greater than (,033); When the sodium hydride content is between 0.01% and 1%, the difference between the results of two parallel determinations should not be greater than 0.015. 9 Determination of sodium hydride content (flame photometry) 9.1 Summary of the method HG 1--1428—81
Use flame photometry to directly determine the sodium in the sample solution and use the standard curve method for quantification. The coexisting elements copper, zinc, and lead have no interference with the determination. The acidity of the standard series and the sample solution should be controlled to be consistent. 9.2 Required Reagents
9.2.1 Hydrochloric acid (1 +1).
9.2.2 Sodium oxide standard solution (1 ml contains 1 mg of sodium oxide). Weigh 1.8859 g of sodium chloride (NaCl) burned to constant weight at 500-600°C, dissolve with appropriate amount of water, transfer to a 1000-liter volumetric flask, dilute to scale with water, shake and put in a plastic bottle. 9.2.3 Sodium oxide standard solution (1 ml contains 100 μg of sodium hydroxide): Accurately pipette 10 ml of 1 ml of sodium oxide standard solution containing 1 mg of sodium oxide, place in a 100-liter volumetric flask, dilute to scale with water, shake and put in a plastic bottle. 9.3 Unnecessary instruments
9.3,1 Laboratory-General instruments,
9.3.2 Flame Photometer: Equipped with a pin interference filter. 9.4 Operating steps
9,4.1 Drawing of standard curve: Accurately pipette 0, .5, 1, 2, 4, 6, 8 liters of 1 ml of 100 microgram sodium oxide standard solution into 100 ml volumetric flasks, add 4 ml of (1+1) hydrochloric acid to each, dilute to the mark with water, and shake well. According to the working conditions of the instrument, use a flame photometer to measure the emission intensity of the sodium spectral line of the standard series and draw a standard curve. 9.4.2 Sample analysis: Directly use the sample solution prepared in Chapter 2 of this standard, and measure the emission intensity of the sodium spectral line under the same conditions as the standard series, and find the sodium ion concentration in the test solution from the standard curve. 9.5 Calculate the sodium oxide content (%) as follows: X-
Wherein: C
C xVx10-6
The concentration of sodium oxide in the melt to be tested is obtained from the Chengya curve, micrograms/ml; the volume of the solution to be tested, ml;
-Weigh the sample amount, grams.
9.6 Accuracy
When the sodium oxide content is between 0.1% and 1%, the difference between the two parallel determination results should not be greater than 0.03%. When the sodium oxide content is between 0.010.1%, the difference between the two parallel determination results should not be greater than 0.015%. 16
HG1-1428—81wwW.bzxz.Net
Appendix A
Preparation of standard solution
(Supplement)
A10.M Disodium ethylenediaminetetraacetic acid standard solution A.1.1 Reagents
Al.t, 1 Ammonia water (1 +1).
A.1.1.2 Eriochrome black T indicator (0.5%): weigh 0.5 g chromium black T and 2 g hydroxylamine hydrochloride and dissolve in ethanol, dilute to 100 ml with ethanol.
A-1.1.3 Ammoniacal chloride buffer solution (pH 10): weigh 27 g chromium chloride, dissolve in 100 ml boiled water, add 175 ml boiled ammonia water, and dilute to 500 ml with water.
A.1.1.4 Disodium ethylenediaminetetraacetic acid.
A, 1.1.5 Zinc standard solution (0.02M): Weigh 1.6276 g zinc oxide (ZnO) burned to constant weight at 800°C, place in a 300-liter beaker, moisten with water, add 20 ml (1+1) hydrochloric acid, slowly heat to dissolve, cool to room temperature after complete dissolution, transfer to a 1000 ml volumetric flask, dilute to scale with water, and shake well. A.1.2 Preparation steps
A.1.2.1 Preparation of solvent: Weigh 7.8 g disodium ethylenediaminetetraacetic acid (C10HN20gNa·2II:0), dissolve in 1000 ml water, shake, and wait for weighing.
A.1.2.2 Calibration method: Take 20 ml of 0.02M zinc standard solution and place it in a 250 ml beaker, add water to about 100 ml, add (1+1) ammonia water until precipitation appears, add 10 ml of ammonia-ammonia chloride buffer solution and 5 drops of chrome black T indicator, and titrate with the EDTA drop to be calibrated. The end point is when the purple in the solution changes to pure blue. A.1.3 Calculate the molar concentration of the EDTA standard solution:
Where: M-
V-Amount of EDTA standard solution: ml;
M1-molar concentration of zinc standard solution;
V.-Amount of zinc anti-epileptic bath solution, ml. A.20.02M zinc standard solution
A.2.1 Required reagents
A.2.1.1 Ammonia-ammonium oxide buffer bath solution (pH 10): weigh 27 g ammonium fluoride, dissolve in 100 ml water, add 175 ml water, dilute to 500 ml with water.
A.2.1.2 Black T indicator (U.5%): weigh 0.5 g chrome black T and 2 g hydroxylamine hydrochloride, dissolve in ethanol, dilute to 100 ml with ethanol.
A-2.1.3. EDTA standard bath solution (0.02M). A.2.2 Preparation steps
.A.2.2.1 Preparation of drop solution: weigh 2.8 g zinc chloride (ZnCl2), dissolve in appropriate water, add 0.5 ml hydrochloric acid, transfer to a 1000 liter volumetric bottle, dilute to the scale with water, average, and wait for calibration. A.2.2.2 Calibration method: Accurately pipette 20 ml of the zinc standard solution to be calibrated, place it in a 25U ml beaker, add water to about 100 ml, 10 ml of ammonia-ammonium chloride buffer solution, and 5 drops of chrome black T indicator, and titrate with 0.02M EDTA standard solution. The end point is when the liquid changes from 17
purple to pure blue.
A.2,3 Calculation
In the formula, M
concentration of zinc standard solution
amount of zinc standard solution, ml;
HG 1-1428—81
concentration of -EDTA standard solution;
amount of -EDTA standard solution, ml.
Additional instructions:
This standard was proposed by the Jiangsu Provincial Department of Petrochemical Industry and is under the jurisdiction of the Nanjing Chemical Industry Corporation Research Institute. This standard was drafted by the Nanjing Chemical Industry Corporation Research Institute. The main drafters of this standard are Sun Xian and Xu Fenglan.
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