A method for determining the content of free aluminum in silicon carbide refractories
A technology of refractory materials and silicon carbide, applied in the field of chemical detection, can solve the problems of cumbersome operation, large consumption of chemical reagents, pollution of the environment, etc., and achieve good stability, convenient operation, and reliable methods
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[0020] 1) According to the preparation method of the sample solution in step A, prepare 7 blank sample solutions and transfer them into 50ml volumetric flasks;
[0021] 2) Precisely weigh 0.5000g of pure aluminum with a purity greater than 99.9%, use 30ml of 200g / L sodium hydroxide solution in a water bath at 80~90°C for 20~30min to obtain solution c, and add 0.2~0.4 times the volume ratio to solution c Concentrated nitric acid, heat and boil at 80~90°C for 3~5min until the solution is transparent, cool to room temperature, add distilled water or secondary deionized water to dilute to obtain 1.0mg / ml solution d, pipette solution d, add volume ratio 0.2~0.4 times concentrated nitric acid, add distilled water or secondary deionized water to dilute to obtain 10μg / ml aluminum standard stock solution;
[0022] 3) Add 0ml, 1.00ml, 2.00ml, 5.00ml, 10.00ml, 15.00ml, and 20.00ml of aluminum standard stock solutions to the volumetric flasks of the aforementioned 7 blank sample solutions...
Embodiment １
[0040] Prepare aluminum standard solution as usual:
[0041] 1. Preparation of aluminum standard solution:
[0042] 1A. Add 30 mL of sodium hydroxide solution with a concentration of 200 g / L to 0.5000 g of commercially available metallic aluminum (99.99%) at 60 mL / g of metallic aluminum, and heat and dissolve in a water bath to obtain a solution;
[0043] 1B. Add commercially available analytically pure nitric acid to the solution in step 1A to make the solution acidic, then excess 10mL, heat and boil to make the solution transparent, cool to room temperature, add water to dilute to a 1.0mg / mL aluminum solution, and obtain an aluminum standard solution ;
[0044] 1C. Pipette the aluminum standard solution in step 1B, add 5 mL of commercially available analytical pure nitric acid, and dilute with water to obtain a 10 μg / mL aluminum standard solution.
[0045] 2. Preparation of aluminum standard working solution:
[0046]2A. Pipette 0.00mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL, 15...
Embodiment 2
[0054] Determination of free aluminum in silicon carbide refractories to be tested:
[0055] 1. Preparation of sample solution for silicon carbide refractories to be tested:
[0056] 1A. According to the amount of 100mL / g sample, add 50mL of ferric sulfate solution to 0.5000g of silicon carbide refractory material sample, the concentration of the ferric sulfate solution is 50g / L, cover with a watch glass, and soak in a water bath at 100°C 1h, stirring once every 15min to obtain a solution;
[0057] 1B. Cool the solution in step 1A, filter it with medium-speed quantitative filter paper, and collect the filtrate in a beaker. According to the amount of 20mL / g sample, add 10mL of commercially available analytical pure nitric acid to the filtrate, heat and boil at 100°C for 1min, cool to room temperature, dilute the filtrate to 250mL with water, and obtain the solution;
[0058] 1C. Pipette 10.00 mL of the solution in step 1B, add 5 mL of commercially available analytically pure ...
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