HG/T 2512-1993 Chemical composition analysis method of zinc oxide desulfurizer
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T 2512 93
Chemical composition of zinc oxide desulfurizer
Analysis method
1993-09-09
Ministry of Chemical Industry of the People's Republic of China
Implementation on 1994-07-01
Chemical Industry Standard of the People's Republic of China
Chemical composition of zinc oxide desulfurizer
Analysis method
1 Subject content and scope of application
HG/T 2512-93
Replaces HG/T 1-1S45-84
This standard specifies the analysis method for the chemical composition of zinc oxide desulfurizers of types T302Q, T(T)303.T304-1 and T305. This standard is applicable to the determination of zinc oxide, magnesium oxide and manganese dioxide contents in zinc oxide desulfurizers. 2 Reference standards
GB/T601 Preparation of standard solutions for chemical reagent titration analysis (volume analysis) GB/T602 Preparation of preparations and products used in chemical tests: test methods GB/T6682 Specifications and test methods for water used in analytical laboratories GB6003 Test sieves
3 Preparation of test samples
Take about 40 samples by quartering method and consider the sample uniform. Grind them in a mortar until they can all pass through the test sieve with a diameter of 150 μm. Sieve: add two more portions, keep one portion for future reference, put the other portion in a weighing bottle, and bake in an oven at 105 °C for 2 hours. Take it out and put it in a desiccator for chemical analysis: 4 Dissolution of sample
4.1 Dissolution of T302Q sample
4.1.1 Method summary
Use acetic acid to dissolve zinc oxide and magnesium oxide in the sample, and filter out insoluble matter. 4.1.2 Reagents and solutions
4.1.2. 1 Ice Z saddle (GB/T 676). :4.1.2.2 Acetic acid dissolving bottle: 1+50
4.1.3 Operation steps
Weigh 1g of sample (accurate to 0.D00), measure 2L of flask, moisten with ice, add 10mL of glacial acetic acid, dilute with water to about 50mL, heat slowly and boil slightly for 10min, after zinc oxide and magnesium oxide are completely dissolved, remove the insoluble matter, filter, collect the filtrate in a 250ml volumetric flask, wash the insoluble matter with hot acetic acid solution for 8 to 10 times, after the solution is cooled, dilute with water to the scale, shake well, this solution is test solution A.
4.2 Dissolution of T (T) 303, T304-1 and T305 type test specimens 4.2.1 Method Summary
The test specimen is dissolved in hydrochloric acid solution,
2, reduced and
4 2.2.1 Hydrochloric acid (GB/T622) solution: 1+ Ministry of Chemical Industry of the People's Republic of China 1993-09-09 Approved 1994-07-01 Implementation
HG/T 2512-93
4.2.3 Operation steps
Weigh 1g of the sample (accurate to 0.0001g), place it in a 250mL beaker, moisten it with a small amount of water, add 20mL of hydrochloric acid solution, and slowly heat until the sample is completely dissolved. After cooling, transfer it to a 250mL volumetric flask, dilute it to the scale with water, and check it. This solution is test solution B.
5 Determination of zinc oxide content
5.1 Summary of method
The sample solution is titrated with EDTA standard titration solution in hexamethylenetetramine buffer solution at pH 5.5 and using xylenol orange as indicator.
Add hydroxylamine hydrochloride and potassium sodium tartrate to eliminate the interference of trace iron and aluminum. 5.2 Reagents and solutions
5.2.1 Hydroxylamine hydrochloride (GB/T 6685).
5.2.2 Potassium sodium tartrate (GB/T1288). 5.2.3 Hydrochloric acid (GB/T 622) solution: 1+1.5. 2.4 Ammonia (GB/T 631) solution: 1+1. 5.2.5 Hexamethylenetetramine (GB/T1400) buffer solution: pH 5.5, see Appendix A for preparation method. 5.2.6 Xylenol orange indicator solution: 2g/L, prepared according to GB/T603. 5.2.7 Disodium ethylenediaminetetraacetic acid (EDTA) (GB/T1401) standard titration solution: C (EDTA) = 0.02 mol/L, prepared and calibrated according to GB/T601.
5.3 Analysis stepsbzxZ.net
Accurately pipette 10 mL of test solution A or test solution B, place it in a 250 mL conical flask, dilute it with water to about 100 mL, add about 0.2 g of hydroxylamine hydrochloride and about 0.2 g of potassium sodium tartrate, adjust the pH of the test solution to between 4 and 6 with ammonia solution, add 10 mL of hexamethyltetramine satin solution and 4 drops of xylenol orange indicator solution, add EDTA standard titration solution until the test solution changes from red to bright yellow, record the volume of EDTA standard titration solution consumed V, mL.5.4 Expression of analysis results
The mass percentage of zinc oxide (X%) is calculated according to formula (1): x
V,*c × 0. 081 38
Wherein: V—volume of EDTA standard titration solution, mL; -actual concentration of EDTA standard titration solution, mol/L; 100+
m,——mass of sample taken, g:
0.08138-——the amount of zinc oxide expressed in grams when it is dissolved and filtrated with 1.00mL EDTA standard titration solution (EDTA) of 1.000mol/L,
5.5The allowable difference
The absolute difference between the results of two parallel determinations shall not exceed 0.3%. 6 Determination of magnesium oxide content
6.1 Method
In an ammonia and ammonium chloride buffer solution at pH 10, use chrome black T as the indicator and use EDTA standard titration solution to drop out the total amount of zinc and magnesium. Subtract the volume of EDTA solution consumed in the determination of zinc to calculate the magnesium content. Use hydroxylamine hydrochloride and triethanolamine to eliminate the interference of trace iron and aluminum. 6.2 Reagents and reagents
6.2.1 Hydroxylamine hydrochloride (GB/T 6685). 6.2.2 Triethanolamine solution: 1+4.
6.2.3 Ammonia (GB/T 631) solution 1+I.6.2.4 Ammonium chloride (GB/T658)
HG/T 2512 --- 93
6.2.5 Eriochrome black T indicator solution: 5g/L, prepared according to GB/T6036.2.6 Ammonia-ammonium nitride buffer solution: PH10, prepared according to GB/T6036.2.7 Disodium ethylenediaminetetraacetic acid (EDTA) (GB/T1401) standard titration solution: c(EDTA)=0.02mol/L, prepared according to GB/T 601 Preparation and calibration.
6.3 Analysis steps
Accurately pipette 10 mL of test solution A or test solution B and place it in a 250 mL conical flask. Dilute it to 100 mL with water. Add about 0.2 g of hydroxylamine hydrochloride and 5 mL of triethanolamine solution. Adjust the pH of the solution to 10 with ammonia solution. Then add 10 mL of ammonia-ammonium chloride buffer solution and 6 drops of black T indicator solution. Use EDTA standard titration solution until the test solution changes from purple to blue. Record the volume of EDTA solution V, which is the total amount of zinc and magnesium. Subtract the corresponding volume of EDTA solution V consumed when determining zinc alone in item 5 to obtain the volume of EDTA solution V consumed by magnesium.-
6.4 Expression of analysis results
The mass percentage of magnesium oxide (X,%) is calculated according to formula (2): X,
V, * c × 0. 040 31
× 100 -
Wherein: V2——the difference between the volume of the titrated zinc bond and the volume of the EDTA standard solution for zinc titration alone, mL, Vz= V. -V: V—the volume of the EDTA standard solution consumed for the combined amount of zinc and magnesium titration, mL; V——the volume of the EDTA standard solution for zinc titration alone, mL: C——the actual concentration of the EDTA standard titration solution, mol/L; the mass of the sample taken, g;
0. 040 31-
6.5 plus the allowable difference
-with 1. 00 mL EDTA standard titration solution c(EDTA)=1. 000 mol/L Equivalent, the mass of magnesium oxide expressed in grams, the absolute difference between two parallel determination results is not greater than 0.2%. 7 Determination of manganese dioxide content 7.1 Method After the sample is dissolved in phosphoric acid, silver ions are used as catalysts, low-valent manganese is oxidized to permanganate ions with ammonium persulfate, N-phenyl anthranilic acid is used as an indicator, and ammonium ferrous sulfate standard solution is used for titration. 7.2 Reagents and solutions 7.2.1 Phosphoric acid (GB/T 1282), 7.2.2 Ammonium persulfate (GB/T 655), 7.2.3 Silver nitrate (GB/T 670) solution: 10 μL. 7.2.4 Hydrogen peroxide (GB/T 6684) solution: 1 + 97.2.5 N-phenylamine formic acid indicator solution: 2 mol/L, see Appendix A for preparation method. 7.2.6 Ammonium ferrous sulfate (GB/T 661) cL (NH4+), Fe(SO4)2·6H2O) = 0.1 mol/L standard titration solution: prepared and calibrated according to GB/T 601,
7.3 Analysis steps
Weigh 0.5 μg (accurate to 0.0001 g) of the sample prepared in Section 3 in a bowl and place it at 500 mL flask, moisten with a small amount of water, such as 15 mL phosphoric acid, 10 mL hydrogen peroxide solution, slowly heat until the sample is completely dissolved, boil for 0.0 min, use 150 mL rice, such as 5 mL silver nitrate solution, about 2 g ammonium persulfate, place for 10 min, boil for 5-7 min, incubate at room temperature, use ammonium ferrous sulfate standard titration solution until the sample solution turns light red, add N-amino acid to indicate 34%, continue to drip until the solution turns bright green as the end point, record the volume of ammonium ferrous sulfate standard titration solution, 7.4. Expression of analysis results
The percentage of manganese dioxide (X,%) is calculated according to formula (3): X, -
c5007739
or use sulfuric acid to titrate the solution, L× 100 -
The actual concentration of the standard solution of sulfuric acid,
m—Weigh the sample,
001739 and 00m ZnSO4 standard solution NHe (S0<0) ±1.0000014, the mass of manganese dioxide expressed in grams. 7.5 Tolerance
The absolute difference between the results of two parallel determinations shall not exceed 0.2%. 4
A1 Hexamethylenetetramine solution, pH 5.5; HG/ T 2512 —93
Attachment A
Preparation of solution
(Supplement)
Weigh 200g of hexamethylenetetramine, dissolve in 200mL of water, add 40mL of concentrated hydrochloric acid, dilute to 1000mL with water, stir well, A2N-phenylanthranilic acid indicator solution, 2g/L; weigh 0.20g of N-phenylanthranilic acid, dissolve in 100mL of sodium carbonate solution (concentration is 2g/L), stir well. Additional remarks:
This standard is proposed by the Department of Science and Technology of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Nanjing Chemical Industry (Group) Corporation Research Institute. This standard is drafted by Nanjing Chemical Industry (Group) Corporation Research Institute. The main drafters of this standard are Yang Rongtai and Zhang Yuanlao. People's Republic of China
Chemical Industry Standard
Analysis Method of Chemical Composition of Zinc Oxide Desulfurizer HG/T 2512-93
Editor: Chemical Industry Standards Department
(Institute of Standardization, Ministry of Chemical Industry)
Postal Code: 100013
Printing: Standardization Institute, Ministry of Chemical Industry
Proprietary and No Reproduction
Printing No. 9000
Format 880×1230 1/16
First Edition in December 1993
First Printing in January 1994
Print Quantity 1-500
Cost 3.00 Yuan
2512-93
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