GB 3654.1-1983 Chemical analysis method of ferroniobium - Paper chromatography gravimetric method for determination of niobium and tantalum

This standard is applicable to the determination of niobium and tantalum in ferroniobium. Determination range: niobium 50-8%, tantalum 0.4-1.5%. GB 3654.1-1983 Chemical analysis method for ferroniobium - Determination of niobium and tantalum by paper chromatography separation gravimetric method GB3654.1-1983 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of ferroniobiumThe paper chromatograph-gravimetric method forthe determinaiion of niobium and tantalumUDC 669.15'293
543.2T:546
GB 3654.1-83
This standard is applicable to the determination of energy and tantalum in low-energy iron. Determination range: 50~80%, 0.4~1.5%. This standard complies with GB1467-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
Saw and other impurities are separated based on palladium, but on the chromatographic paper coated with ammonium nitrate, when methyl isobutyl ketone-ketone hydrofluoric acid-nitric acid is used as the developing agent, the R value of vanadium is about 0.94, the R value of saw is about 0.60, and other impurities stay in place or move very little to achieve separation. Use dansyl acid to dissolve the color on the free-layer paper. Cut off the niobium and color ribbons respectively, incinerate, burn and weigh, and then get the niobium and niobium. 2 Reagents and Materials
2.1 Hydrogen fluoride (specific gravity 1.15).
2.2 Hydrofluoric acid (1 + 1).
2.3 Nitric acid (specific gravity 1.42).
2.4 Tannic acid solution (2%)).
2.5 Waist-opening agent: benzyl isobutyl ketone + methyl ketone + hydrofluoric acid nitric acid (44+44+6+6). 2.6 Chromatographic paper, Xinhua No. 3 chromatographic paper, cut into 20cm wide and 26cm long, two-thirds of its length is set with 10% ammonium nitrate solution and then dried.
3 Instruments
3.12ml plastic pipette.
3.2 Chromatographic box, a cylindrical plastic tube with a diameter of 25cm and a height of 35cm, with a lid. 3.3 Sprayer.
1.4 Humidity controller: Place a cup of warm water and place a 10-humidity thermometer. 3.5 Neutralizer: Ammonium hydroxide (specific gravity 0.90) is placed under the sieve plate of the large desiccator. 4 Analysis steps
4,1 Sample
Weigh 0.100hg of sample.
,4.2 Quebai test
Use the sample as a blank.
4.3 Determination
4.3.1 Place the test sample in a crucible, add 2-3ml of hydrochloric acid (2.1), add nitric acid (2.3) dropwise until the sample is completely dissolved, then place it on a sand bath and heat it, and evaporate it to about 1ml. National Bureau of Standards issued on May 2, 1983
Implementation on March 1984bZxz.net
GB 3654.183
1.3.2 Remove, use a plastic pipette to transfer the test solution, and apply it to the lower part of the chromatographic paper that has not been immersed in the ammonium nitrate solution. When applying the test solution, try to apply it evenly and straightly, and keep a distance of 2cm from the bottom edge of the chromatographic paper. After applying the test solution, wash the crucible twice with hydrofluoric acid (2.2) and twice with distilled water, using about 0.5㎡1 each time, and evenly apply the washing solution on the chromatographic paper. After low-temperature drying, roll it into a cylindrical shape, fix it with a paper clip, and stand it upright in a humidity controller with a humidity of 80%. After leaving it for 15 minutes, take it out and immediately put it in the developing agent (2.5). The thickness of the liquid layer is about 1cm chromatographic box, sealed and developed for about 2-3h. When the solution rises to 1-2cm from the top of the chromatographic paper (2.6), take it out, dry it, place it in a neutralizer, place it for 15min, take it out, and dry it for ten minutes. 4.3.3 Spray the monoacid solution (2.4) on the chromatographic paper and dry it for ten minutes. The star-yellow color band on the upper part is vanadium, and the orange-red color band in the middle is niobium. Cut them out separately, measure the width of the vanadium color band, place them in a crucible of known mass, place them on a hot plate for low-temperature ash treatment, move them into a high-temperature furnace at 850-900℃ and burn them for 30min, take them out, place them in a dryer to cool to room temperature, and weigh niobium and vanadium oxides respectively. 5 Calculation of analysis results
Calculate the percentage of saw and barium according to formula (1), (2): (m,-m2) - (my=mg) ×0.6991×100.Nb (%) =
Formula, mi-
Where: m5
6 Allowable difference
Mass of platinum and vanadium pentoxide, more,
Mass of platinum crucible, g
Mass of platinum and the sample blank, B3 Mass of platinum crucible with the sample blank, gt
Sample weight, gi
Conversion factor for converting saw pentoxide to saw. (mg-mg) - (mz-ma)×0.8189
Mass of platinum pile and molybdenum pentoxide, g;
Mass of platinum crucible, gt
Mass of molybdenum crucible with blank sample, g
Mass of platinum crucible with blank sample, g
Sample volume, 1
Conversion factor for converting molybdenum pentoxide to molybdenum. The extreme value of the analysis result should not be greater than the allowable difference listed in the table below. Contains
50 ~70
Additional remarks:
Allowable difference
This standard was proposed by the Ministry of Industry of the People's Republic of China. This standard was drafted by Jilin Ferroalloy Factory. This standard was drafted by Jilin Ferroalloy Factory.
The main drafter of this standard is Yang Wanbao.
0.40 ~1.0
>1.0~1.50
Allowable difference
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