GB/T 4324.24-1984 Chemical analysis of tungsten - Beryllium as carrier precipitant - Molybdenum blue photometric method for determination of phosphorus content
Some standard content:
National Standard of the People's Republic of China
Chemical analysis method of tungsten
Methods for chemical analysis of tungstenTheberylium as carrier precipitation agent-molybdenum blue photometric method forthe detcrmination of phosphorus contentUDC 669.27:543
42:546.1B
GB 4324.24---B4
This standard is applicable to the determination of phosphorus in pigeon powder, tungsten bar, tungsten trioxide, tungstic acid and ammonium tungstate. The determination range is: 0.0002~0.018%. This standard is in accordance with the Standard (B147-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products"). 1. Method Summary
Platinum powder and platinum strips are decomposed with hydrogen peroxide (tungsten monoxide, tungstic acid and ammonium tungstate are dissolved with hydroxide) and the main aluminum is complexed. It is adjusted to ammoniacal with ammonium nitrate. Impurities such as iron, manganese, copper and magnesium are complexed with disodium ethylenediaminetetraacetic acid in 2.2N sodium hydroxide solution. Phosphorus is carried with beryllium and separated from other impurities. In sulfuric acid as a medium, phosphorus and ammonium tungstate form phosphomolybdenum yellow heteropoly acid, which is extracted with a mixed solvent of n-butanol-chlorinated ethane to form chlorinated Tin is converted into phosphorus blue, and its photometric value is measured. 2 Reagents
2.1 Potassium chloride.
Peroxide (specific gravity 1.10).
Ammonium hydroxide (specific gravity 0.90).
Sulfuric acid (1.2N)
Hydrochloric acid (1+1).
Sodium ethanoate solution (%).
P-nitrophenol solution (1%).
Potassium hydroxide solution (20%).
Beryllium sulfate solution (2%): Weigh 20g of sulfuric acid and dissolve it in sulfuric acid (2.5). And add sulfuric acid ( 2.5) Dilute to 10 (0.01% ethanol, transfer to 2000ml separatory tube, add 40ml ammonium sulfate (2.11) with a pipette, mix, let stand for 30min, add ethanol (2.2) to saturate (add 7-8ml ethanol to every 100ml liquid), shake 1mm on charcoal, add 40ml trinitroethanol extractant (2.12), shake for 2.5min, let stand to separate, discard the organic phase, repeat the extraction - times, transfer the aqueous phase to the test condensation bottle, each 2.11
ammonium potassium hydroxide solution (10%).
n-butanol-dichloro Methane mixed solvent: 1 volume of 1-hydroxyethyl alcohol (2.2) and 3 volumes of trichloromethane mixed, stannous chloride solution (10%): weigh 1g of tin nitride and dissolve it in 10ml of hydrochloric acid (2.6), prepare it when needed. Precipitation solution: add 5ml of ammonium hydroxide (2.4) and 1g of ammonium chloride to 1000ml of water, mix, and set aside 2.14
Single distilled water (this method uses this water). National Bureau of Standards 1984·04-12 IssuedWww.bzxZ.net
1985-03-01 Implemented
2.16 Phosphorus solution
GB 4324.24—84
2.16.1 Weigh 4393g potassium difluorophosphate standard reagent which has been dried at 105-110℃ for 1h, dissolve it in 100ml of water, transfer it to a 1000ml volumetric flask, dilute it to the mark with water, and mix it. 1ml of this solution contains 0.10mg phosphorus. 2.16.2 Transfer 5.00m! phosphorus standard solution (2.t6.1) to a 100ml volumetric flask, dilute it to the mark with water, and mix it. 1ml of this solution contains 5g phosphorus.
The strips should be crushed and passed through a 120 self-sieve.
4 Analysis steps
4. Determination of the number of samples
The analysis state should weigh a sample for determination. If the determination value is within the allowable error in the room, take the average. 4.2 Sample area
According to the report! Take the sample.
Phosphorus, %
0.0002-0.001
0.01~0.002
~0.002~1.010
9.010 - 0.018
Empty point test
Empty point test with sample.
4.4 Determination
4.4,1 Sodium powder, sodium strip
4.4.1.1 Place the sample (4.2) in a 250ml beaker, add 10ml hydrogen peroxide (2.3), heat slowly, stop the intense speed, continue to heat to decompose the sample completely, boil until large bubbles (volume controlled below 5m), remove, wash off the stigma and cup with water, dilute to 40ml, add 1 drop of nitro powder solution Liquid (2.8), adjust to alkaline with ammonium hydroxide (2.4b) and pass through 16ml, add 2ml sodium ethylenediaminetetradecanoate solution (2.?), mix well, dilute with water to 10ml. 4.1. Add 10ml of aqueous acid solution (2.10) (stirring while adding) to make the precipitate free of gold, move to an electric stove, heat and boil, keep boiling for 5min, remove, cool for 30min, filter with rapid quantitative filter paper, wash the beaker 3-4 times with washing solution (2.14), Wash the precipitate 5-7 times. Dissolve the precipitate with sulfuric acid (2.5) in a 125ml separatory funnel and dilute to 50ml, mix well. 4.4.1.4 Add 10ml of ammonium leucate solution (2.11), mix well, let stand for 10min, saturate the solution with 4ml of n-1 alcohol (2.2), shake for 1min, add 14ml of n-1 alcohol chloroform to filter and extractant (2.12), shake for 2.5min, let stand to separate, transfer the organic phase to a 50ml "dry" tube, Dilute to 25 ml with n-butanol (2.2), mix well, add 1 drop of stannous chloride solution (2:13), mix well. 4.4.1.5 Transfer part of the solution into a 3 cm colorimetric tube, use n-butanol (2.2) as reference, and measure its absorbance at a wavelength of 620 mm on a spectrophotometer.
4.4.1.6 Subtract the absorbance of the sample. Find the corresponding phosphorus content from the working curve. 2 Tungsten oxide, tungstic acid, ammonium tungstate
GB $324.24--84
4.4.2.1 Place the sample (4.2) in a 251 ml beaker, add 10 ml of copper hydride solution (2.9), heat until the sample is completely dissolved and remove. Rinse the surface and the wall of the beaker with water (the volume is controlled to be about 4 ml at this time), add 0.5 g of chloride 2.1, and boil until the gas rate is below 30%.
4.4.2.2 Rinse the table and the cup wall with boiling water, add 5ml hydrogen peroxide (2.3), stir vigorously, add 2ml sodium diquaternary acid solution (2.7), mix, and cool slightly.
4.4.2.3 Add 1 drop of p-nitrophenol solution (2.8), neutralize with hydrochloric acid (2.6) until colorless, then adjust to alkalinity with ammonium nitrate (2.4), and add 16ml excess, dilute with water to 100ml. The following is carried out according to 4.4.1.3~4.4.1.6. 4.5 Drawing of working curve
Pipette 0.00, 0.20, 0.60, 1.00, 1.40, 1.80, 2.40ml phosphorus standard solution (2.16.2), measure into 125ml separatory funnel respectively, add 10ml sulfuric acid (2.5), and dilute with water to 50ml. Follow the steps in 4.4.1.4 to 4.4.1.5, measure the absorbance of H, subtract the absorbance of the reagent chamber, and plot the three curves using the absorbance of the sample as the vertical axis. Calculation of analysis results
Calculate the percentage of phosphorus according to the following formula:
P (%) =
6 Allowable error
Phosphorus content obtained from the following test:
A sample weight, g,
The difference in the results of the scale analysis between the experiments shall not be less than that listed in Table 2. Allowable error:
Q.00020~0.00040
.m080.0015
30.0015~0.0030
h.0030o.6045
Additional instructions:
This standard was proposed by the Ministry of Metallurgy of the People's Republic of China. This standard was drafted by Zhuzhou Cemented Carbide Association. This standard was drafted by Zhuzhou Cemented Carbide Association. Phosphorus
>0.0045~0.1060
>0.0068~0.0980
t.0089--9.01 20
0.012-,018
The main drafter of this standard is Dong Zhuifan.
Since the implementation of this standard, the former Ministry of Metallurgical Industry Standard YH895-77 "Tungsten Chemical Analysis Method" will be invalid 93
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