JB/T 9220.5-1999 Chemical analysis of acidic slag from foundry cupola furnaces - Sodium fluoride-EDTA volumetric method for determination of aluminum oxide content
Some standard content:
JB/T 9220.5--1999
This standard is a revision of JB/Z284.5---87 "Chemical Analysis Method of Acidic Slag of Casting Iron Cupola, Determination of Aluminium Oxide Content by Sodium Fluoride·EDTA Volumetric Method". During the revision, editorial changes were made to the original standard, and the main technical content remained unchanged. This standard replaces JB/Z284.5-87 from the date of implementation. This standard was proposed and managed by the National Technical Committee for Foundry Standardization. The drafting units of this standard are: Shanghai Diesel Engine Factory, Nanchang Diesel Engine Factory, Guiyang Foundry, Shenyang Foundry, Shanghai Tractor Engine, Huafeng Steel Factory, Wuxi Diesel Engine Factory, Changzhou Diesel Engine, etc. The main drafters of this standard are: Wang Zhihan, etc. 436
Machinery Industry Standard of the People's Republic of China
Chemical analysis methods for acid slay of cupola.--- Determination of aluminium oxide by volumetricmethod using sodium fluoride-EDTA1Scope
JB/T 9220.5:1999
Replaces JB/Z281.5.-87
This standard specifies the determination of aluminium oxide in chemical analysis methods. Determination range: 1.00%~20.00%. This standard is applicable to the analysis of the composition of acid slag of cupola. 2Test conditions
The sample is dissolved in hydrochloric acid and hydrofluoric acid, and fluoride ions are removed by fuming nitric acid and perchloric acid. Use hexamethylenetetramine to precipitate aluminum and separate it from other elements. In the presence of EDTA, use sodium hydroxide to separate and remove the coexisting interfering elements such as titanium, iron, and rare earth. Heat the leaves in a slightly acidic solution to make aluminum and residual ions complex with EDTA. At about pH 5.5, use xylenol orange as an indicator, titrate the excess FDTA with zinc standard solution, replace the EIDTA complexed with aluminum with fluoride ions, and then titrate with zinc standard solution. 3 Reagent preparation
Hydrochloric acid (density 1.19g/mL).
Hydrochloric acid (1+1)
3.3 Hydrochloric acid 2+98).
Hydrofluoric acid (density 1.15g/mL).
Nitric acid (density 1.42g/ml.).
Perchloric acid (density 1.67g/mL).
Ammonium hydroxide (1+1).
3.8 Ammonium chloride.
3.9 Ammonium chloride solution (2%): Add 12 drops of ammonium hydroxide (3.7) to every 100 ml of solution. 3.10 Hexamethylenetetramine solution (25%)
Ethylaminetetraacetic acid disodium (CHiN,O,Na2·2H0EDTA) solution (0.2M): Weigh 74.448 g EDTA, place in a 100 ml beaker, dissolve in water, transfer to a 1000 ml volumetric flask, dilute to scale with water, and mix. 3. 12
Sodium hydroxide solution (40%).
Sodium hydroxide solution (1%).
3.14 Potassium permanganate solution (2%).
3.15 Anhydrous alcohol.
3.16 p-Nitrophenol solution (0.2%)
3.17 Acetic acid-ammonium acetate buffer solution (pH 5.0-5.5): weigh 200g ammonium acetate and dissolve it in 500ml water, add 25ml glacial acetic acid (approved by the State Bureau of Machinery Industry on June 24, 1999, implemented on January 1, 2000
JB/T 9220.5--1999
concentration 1.05g/mL), dilute with water to 1000ml, and mix well. 3.18 Xylenol orange solution (0.2%): prepare with xylenol orange reagent of grade \color developer. 3.19 Zinc chloride solution (0.1M): Weigh 13.65g zinc chloride and dissolve it in water, add hydrochloric acid (3.2) dropwise to adjust to pH 3. Dilute with water to 1000ml, mix well,
3.20 Sodium fluoride solution (4%).
3.21 Zinc standard solution (0.01000M): Weigh 0.6538g pure zinc (more than 99.95%), dissolve in 20ml hydrochloric acid (3.2), add 200mL water, use ammonium hydroxide (3.7) and hydrochloric acid (3.2) to adjust the acidity until the Congo red test paper changes from blue to purple (about pH 3), cool, transfer to a 1000ml volumetric flask, dilute with water to the mark, mix well. 4 Analysis steps
4.1 Sample amount
Weigh 1.0000g sample.
4.2 Determination
4.2.1 Place the sample (4.1) in a 250mL polytetrafluoroethylene beaker, wet the sample with a small amount of water, add 20ml acid (3.1), 10ml hydrofluoric acid (3.1), heat at low temperature to dissolve, remove and cool slightly after most of the sample is dissolved, add 5ml nitric acid (3.5), 10ml perchloric acid (3.6) and heat until perchloric acid thick white smoke appears for 5-10 minutes, remove and cool, rinse the cup wall with water, add 2mL perchloric acid (3.6) and continue heating until thick white smoke of perchloric acid remains in the cup until 2~~3ml liquid is dissolved. Note: The temperature of the heated decomposition sample should not be too high, and the heating and dissolution time takes about 30 minutes. 4.2.2 Remove and cool, rinse the cup wall with water, add 20mL hydrochloric acid (3.2), heat to dissolve the salts, remove and cool, transfer the solution to a 100mL volumetric flask, dilute to scale with water, mix well, Note: This dilution can be used for the determination of lead, calcium, and magnesium systems. 4.2.3 Transfer 25.00mL of the test solution to a 400mL beaker, add 125mL of water, 1g of ammonium chloride (3.8), stir to dissolve, add ammonium hydroxide (3.7) to adjust until the precipitate just appears, then adjust with hydrochloric acid (3.2) until the precipitate just dissolves, add 20mL of hexamethylenetetramine solution (3.10) under stirring, cover with surface III, heat and boil for 1 to 2 minutes, remove, filter with fast filter paper after the precipitate settles, wash surface III and the beaker with hot ammonium chloride solution (3.9) 4 to 5 times, and precipitate 6 to 7 times. Use 25ml hot hydrochloric acid (3.2) to dissolve the precipitate on the filter paper and filter it into the original beaker. Use hot hydrochloric acid (3.3) to wash the filter paper until there is no iron ion. Note: The heating and boiling time should not be too long, otherwise the precipitate will be difficult to filter and wash. 4.2.4 Control the volume of the filtrate to about 100mL, use ammonium hydroxide (3.7) to adjust until the precipitate just appears, then use hydrochloric acid (3.2) to adjust until the precipitate just dissolves and the excess is 10 drops, add 10mL of ETA solution (3.11). Cover the surface III, heat and boil for 1min, remove, immediately wash the surface and the wall of the cup with hot water, stir while hot, add 20ml of sodium hydroxide solution (3.12), add 5 drops of potassium permanganate solution (3.14), 1~2m, anhydrous ethanol (3.15). Cool for 510 minutes, cool to room temperature with running water, transfer the solution and precipitate into a 250 ml volumetric flask, wash the beaker with sodium hydroxide solution (3.13) and dilute to the mark, mix, and dry filter with slow filter paper. 4.2.5 Transfer 100.00ml of the filtrate to a 500ml conical flask, add 2 drops of p-nitrophenol solution (3.16), adjust with hydrochloric acid (3.2) until the yellow color of the solution just fades, and add 2-3 drops in excess, heat and boil for 1-2 minutes, remove and cool, add 10ml of acetic acid-ammonium acetate buffer solution (3.17), 4 drops of xylenol orange solution (3.18), first titrate with zinc chloride solution (3.19 to near the end point, and then titrate with zinc standard solution (3.21) to light red.
4.2.6 Add 20mL of sodium fluoride solution (3.20), mix well, heat and boil for 2-3 minutes, remove and cool, add 5ml of acetic acid-ammonium acetate buffer solution (3.17) and 2 drops of p-nitrophenol solution (3.18), and use zinc standard solution (3.21) to drop The end point is when the color turns light red. 5 Calculation of analysis results
Calculate the percentage of lead trioxide according to formula (1): A1.0, VMX20.8×100%...
mX2000
（1）
5-1999
JB/T9220.5bZxz.net
The volume of zinc standard solution consumed in the second titration, mI; M—the molar concentration of zinc standard solution;
m—the amount of sample taken;
101.98——the molecular weight of lead trioxide. 6 Tolerance
The difference in analysis results between laboratories should not be greater than the tolerance listed in Table 1. When calibrating the monthly standard sample, the result deviation shall not exceed 1/2 of the tolerance listed in Table 1.
Aluminum trioxide content
1. 00~~2.00
2. 00~5. 00
Blue Aluminum Oxide Content
>5. 0010.00
10,00--20.00
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