HG 2957.11-1984 Determination of titanium content in alum ore - Diantipyryl methane photometric method
Some standard content:
1 Scope of application
National Standard of the People's Republic of China
Determination of titanium content in alunite ore
Diantipyrylmethane photometric method
Alunite oresDetermimation of titanium content-Diantipyrylmethane photometric methodUDC 549.762:543
42:546.821
GB 4581.1184
For: Hah2sz.u-1f8y
This standard specifies the determination of titanium monoxide content of alunite ore ft0.01~1.00% by antipyrylmethane complex photometric method. 2 Related standards
GB4581.1-84 "General rules for analysis of alunite ore". GB4581.2-84 "Methods for sampling and preparation of analysis samples of alunite ore". 3 Method Summary
The sample is dissolved with acid, the slag is melted with potassium pyrosulfate, and then leached with water. In the 1.03.0N hydrochloric acid medium, titanium ions and diantipyrine form a yellow complex. At a wavelength of 420 nanometers, the gram molecular absorption coefficient is 1.02×101, and at a wavelength of 390 nanometers, the gram molecular absorption coefficient is 1.51×104. Titanium oxide conforms to Beer's law in the range of 0-0.08 mg/50 ml. Instrument
Spectrophotometer: wavelength 420 nanometers, 2 cm colorimetric dish; wavelength 390 nanometers, 2 cm colorimetric dish. 5 Reagents and solutions
Potassium pyrosulfate (HG3-921-76).
5.2 Hydrochloric acid (GB622-77) (ratio 1.19): 1+1. Hydrochloric acid: 2 N.
5.4 Nitric acid (GB 626-78) (specific gravity 1.42); 1+1.5.5 Sulfuric acid (GB 625-77) (specific gravity 1.84): 1+15.6
Hydrofluoric acid (GB620-77) (40%). Ascorbic acid: 2% (prepared before use). Diantipyrine: 3% 2N hydrochloric acid solution (5.3) (filtered and stored in a brown bottle). "Titanium oxide.
Titanium oxide standard solution.
5.10.1: Weigh 0.1000 g of titanium dicyanide (5.9) calcined at 950°C for 1 hour into a crucible, add 5 g of potassium pyrosulfate (5.1), place in a muffle furnace, raise the temperature from low temperature to 450°C, stay for 1 minute, then raise to 650°C, melt for 15 minutes, take out and cool. Place in a 250 ml beaker, heat with 100 ml of sulfuric acid solution (5.5) to leach the melt (the temperature should not exceed 50°C). ) After all the solution is dissolved, transfer it into a 1000 ml volumetric flask and dilute it to about 500 ml with water. After cooling, dilute it to the mark with water and shake it well. This solution contains 0.100 mg of titanium oxide per ml. 5.10.2 Pipette 100 ml of solution (5.10.1) into a 1000 ml volumetric flask and add 90 ml of sulfuric acid solution (5.5); dilute it with water. 4581.11--84
Dilute to about 500 ml, cool, and then dilute to the mark with water and shake well. This solution contains 0.010 mg of titanium dioxide per ml. 6 Determination procedures
6.1 Drawing of standard curve
Use a microburette to place 0, 1.00, 2.00, and 8.00 ml of titanium dioxide standard solution (5.10.2) in a 50 ml volumetric flask 1. Dilute to about 20 liters with water, and add ascorbic acid solution (5.7) 5 ml, place for 5 minutes, add 8 ml of hydrochloric acid solution (5.2), 12 ml of diantipyrine alkane solution (5.8), dilute with water to the scale, and mix well. Leave for 30 minutes, and measure the extinction value at a wavelength of 420 nm or 390 nm on a spectrophotometer with a 2 cm colorimetric scale. Draw a standard curve with the concentration of titanium hydride as the horizontal axis and the corresponding absorbance as the vertical axis. 6.2 Sample analysis
Weigh 0.1-0.3. g of the test column in platinum, moisten with a small amount of water, and add sulfuric acid solution ( 5.5) 1 ml, hydrochloric acid (5.6) 10 ml, distilled water (5.4) 1 ml. Heat on a hot plate without stirring until sulfuric acid smoke disappears. Remove from heat, add 3 g potassium pyrosulfate (5.1), place in a 500°C furnace, raise the temperature from low temperature to 450°C, stay for 10 minutes, and then raise to 650°C to melt for 10 minutes. Remove from heat, cool, place in a 150 ml beaker, add 15 ml of distilled water (5.2), 15 ml of water, cover with surface III, heat to leach out the melt, and wash out with hot water Vortex and heat to dissolve. After the solution cools, transfer it to a 100 ml volumetric flask and dilute it to the scale with water; shake and filter. Pipette 5-20 ml of the filtrate and place it in a 50 ml volumetric flask. Dilute it to about 20 ml with water. The following operations are the same as the drawing of the standard curve (6.11bzxz.net
Note: The melting of titanium can also be carried out on a blowtorch. The expression and calculation of the results
The percentage content (X) of titanium dioxide (Fi0) is calculated according to the following formula: Gix-
Wu City: G
× 10-
-Standard curve 1 The weight of titanium dioxide in the sample solution is found, mg: W
-The total volume of the test solution, liters;
-The volume of the sample solution, milliliters;
W--The weight of the sample, grams.
Customer tolerance
Trioxide depends on the normal,
0.010~0.050
0. 051 ~ 0.1mm
n. 11 ~0 ht
0.51 ~1.00
Tolerance (absolute tolerance),
Additional instructions:
GB 4581.11-84
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and drafted by the Chemical Industry and Mining Design and Research Institute of the Ministry of Chemical Industry. The main drafter of this standard is Cheng Maomei.
From the implementation of this standard, the original Ministry of Chemical Industry standard HG1-353·66 "Analysis method of alumite" will be invalid. 26
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