This standard specifies the determination of titanium content by diantipyrine methane spectrophotometry. This standard is applicable to the determination of titanium content in manganese ore, manganese concentrate and sintered ore. Determination range: 0.01% to 0.50% GB/T 14949.5-1994 Chemical analysis method for manganese ore Determination of titanium content GB/T14949.5-1994 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of manganese ore
Determination of titanium content
Manganese ores--Determination of titanium contentGB/T 14949.5- 94
This standard is equivalent to the international standard ISO7723-1984 "Manganese ores and concentrates-Determination of titanium content--·-4,1...antipyrine photometric method".
1 Subject content and scope of application
This standard specifies the determination of titanium content by diantipyrine methane spectrophotometry. This standard is applicable to the determination of titanium content in manganese ore, manganese concentrate and sintered ore. Determination range: 0.01%~~0.50%. 2 Method summary
The sample is decomposed with hydrochloric acid, nitric acid and sulfuric acid, and the insoluble residue is treated with sulfuric acid and hydrofluoric acid, and then melted with potassium pyrosulfate. Solution: Add diantipyrine methane to 1.0-1.2 mol/L hydrochloric acid medium 4 to form a yellow complex with titanium. Measure its absorbance at a wavelength of 385 nm on a spectrophotometer.
3 Reagents
3.1 Potassium pyrosulfate.
3.2 Hydrochloric acid (pl.19 g/ml).
3.3 Hydrochloric acid (1+1).
3.4 ​​Hydrochloric acid (1+50).
3.5 Nitric acid (pl.42 g/ml.).
3.6 Sulfuric acid (1+1).
Sulfuric acid (1+9).
3.8 Hydrofluoric acid (pl.14 g/ml).
3.9 Ascorbic acid solution (100 g/1.), prepare when needed. 3.10 Antipyrine methane (C2:H24O,N,) solution (50g/): Weigh 10g of diantipyrine methane (anhydrous) and dissolve it in 140ml of hydrochloric acid (1+10) (heat if necessary), transfer it into a 200mL volumetric flask, and dilute it to the mark with the same concentration of hydrochloric acid, mix. Filter and store in a brown bottle. Prepare when needed.
3.11 Titanium standard storage solution
This solution can be prepared by one of the following two methods. 3.11.1 Weigh 0.1670g of titanium dioxide (spectrally pure) that has been calcined at 85090°C for 40min and place it in a platinum crucible with a lid. Add 4-6g of potassium pyrosulfate (3.1), first bake it on a 300-400°C electric furnace to remove the water in the reagent, then melt it at 700-750°C and stand until the molten material is clear. Cool the crucible and place it in a 200ml beaker. Add 50ml sulfuric acid (3.7) and heat at low temperature to dissolve the sinter. Wash the crucible and cover with sulfuric acid (3.7) and remove. Transfer this solution to a 1000mL volumetric flask, dilute to scale with sulfuric acid (3.7) and mix. This solution contains 100μg titanium in 1ml.
Approved by the State Administration of Technical Supervision on January 18, 1994 828
Implementation on October 1, 1994
GB/T14949.5-·94
3.11.2 Weigh 0.1000g of titanium (99.95%) and dissolve it in 20ml sulfuric acid (3.6). Add 2~3 drops of nitric acid (3.5) when it is dissolved and evaporate until white smoke appears for 5~10 minutes and cool. Add 50ml of hot sulfuric acid (3.7) to dissolve the salts. Cool. Transfer to a 10ml volumetric flask, dilute to scale with sulfuric acid (3.7), and mix. This solution contains 100μg titanium in 1mL. 3.12 Titanium standard solution
Transfer 50.0mlL titanium standard: stock solution (3.11). Place in a 250ml volumetric flask, dilute to scale with sulfuric acid (3.7). Mix. This solution contains 20μg titanium in 1ml.
4 Instruments and equipment
Common laboratory instruments and
4.1 Platinum crucible.
4.2 Alcohol burner or muffle furnace: The temperature can be controlled within the range of 700~750C. 4.3 Spectrophotometer: A spectrophotometer with near ultraviolet and visible spectrophotometer 5 Samples
The sample should pass through a 0.100mm sieve and be air-dried under laboratory conditions. 6 Analysis steps
6.1 Sample quantity
Weigh 0.9~1.1g of sample, accurate to 0.0001g. Weigh the sample at the same time as the determination to determine the mass percentage of wet water (A). When calculating the titanium content, the result (mass percentage) should be multiplied by the conversion factor (K), which is the mass percentage of titanium content determined in the completely dry sample. 6.2 Blank test
Carry out a blank test with the sample.
6.3 Determination
Conversion factor (K) 100-A
6.3.1 Place the sample (6.1) in a 200mL beaker and wet it with a few drops of water. Add 30mL of hydrochloric acid (3.2), cover with Table III, and heat at low temperature to decompose for 30~~40min, then add 5mL of nitric acid (3.5), heat until there is no nitrogen oxide smoke, and cool. Add 20 ml of sulfuric acid (3.6). Continue heating until thick white smoke appears for about 5 to 10 minutes, then cool. Add 20mL hydrochloric acid (3.3) and 50ml hot water, and heat until the soluble discs are dissolved. 6.3.2 Filter with medium-speed filter paper containing a small amount of filter paper pulp, and use a glass rod with a piece of filter paper to wipe the precipitated particles on the wall of the beaker. Transfer all of it to the filter paper, and wash the beaker and the filter paper with residue 2-3 times with hot hydrochloric acid (3.4), and then wash it 8-10 times with hot water. The filtrate is received in a 400ml beaker and the filtrate is retained. 6.3.3 Transfer the filter paper with residue (6.3.2) to a platinum crucible, dry, ash, and burn at 700-750C until it is completely ash. Cool the crucible, add a few drops of water to moisten the residue, add 5-6 drops of sulfuric acid (3.6) and 5-6mL of hydrofluoric acid (3.8), and slowly heat until all white smoke is emitted. Cool.
6 .3.4 Add 1-2g potassium pyrosulfate (3.1) to a platinum crucible, bake at 300-400°C to remove the water, then cover the crucible with a platinum lid and melt at 700-750°C for 5-10 minutes. Place the cooled solution with lid in a 200ml beaker, add 30ml sulfuric acid (3.7), heat and leaching. Combine this solution with the filtrate (6.3.2), heat and evaporate until the solution volume is about 150ml. Cool the solution, transfer it to a 200ml volumetric flask, dilute to the mark with water and mix. When barium and lead sulfates are present, the solution should be dry filtered with slow filter paper before the solution is separated. 6.3.5 Take 1 portion of the test solution (6.3.4) and place it in a 100ml volumetric flask (the blank test solution should take the same volume as the test solution). Titanium content
2:0. 01 ~0. 10
0. 10~0. 30
0.30-~0.50
GB/T 14949. 5-94bzxZ.net
Take aliquot of the test solution (6.3.4)
Take aliquot of the titanium content in the test solution (6.3.4)
:10100
>50~150
75~125
6.3.6 Add 10mL of ascorbic acid solution (3.9), mix well, let stand for 5 minutes, add 15mL of hydrochloric acid (3.3) and 10mL of diantipyrine methane solution (3.10), dilute to the mark with water, and mix well. Let stand for 20 to 60 minutes (when the room temperature is above 20°C, leave it in the stomach mask for 20 minutes, when it is below 20°C, leave it in the buttocks for 40 to 60 minutes) to allow the color to develop completely. 6.3.7 Transfer part of the color development solution into Measure the absorbance of the 1~~3cm absorption dish with the aqueous solution as reference at a wavelength of 385nm on the spectrophotometer. Subtract the absorbance of the test blank solution and find the corresponding titanium content from the working curve. 6.4 Drawing of titanium working curve
Pipette 0, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00, 10.00mL titanium standard solution (3.12) and place them in 8 100mL containers respectively. Add 10.0, 9.5, 9.0, 8.0, 6.0, 4.0.2.0, 0mL sulfuric acid (3.7) in turn. Follow 6.3.6~~6.3.7 and subtract the absorbance of the standard blank solution from the measured absorbance. Draw the working curve with the titanium content as the horizontal axis and the absorbance as the vertical axis. Note: The colored solution of the sample, blank and titanium working curve is measured with the same absorption dish. 7 Calculation of results
7.1 The mass percentage of titanium is calculated according to formula (1): mi.v
Ti(%) =
Wherein: V—total volume of test solution, ml;
V,———volume of test solution taken, ml;
m,-——amount of titanium found from the working curve, g; m—mass of sample·g,
K—-conversion coefficient of titanium content in completely dried sample. …The mass percentage of titanium oxide is calculated according to formula (2): 7. 2
X 100 × K
Ti0,(%) = 1.668 Ti(%)
Formula 4: 1.668-
8Tolerance
Coefficient for converting titanium into titanium dioxide.
The difference in analysis results between laboratories should not be greater than the tolerance listed in Table 2. sn
（1）
（2）
Additional instructions:
≥0. 01~0. 02
>0. 02~～0. 04
>0. 04 ～ 0. 08
>0.080.15
>0.15~0. 25
>0.25~0.50
GB/T14949.5--94
This standard is proposed by the Ministry of Metallurgical Industry of the People's Republic of China. Allowable difference
This standard was drafted by the Mineral Geology Research Institute of China Nonferrous Metals Industry Corporation and the Changsha Mining and Metallurgical Research Institute of Metallurgical Industry. This standard was drafted by the Mineral Geology Research Institute of China Nonferrous Metals Industry Corporation. The main drafters of this standard are Zhang Jinian and Shu Baichong.
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