JB/T 9220.9-1999 JB/T 9220.9-1999 Chemical analysis method of acidic slag of foundry cupolane Phosphorus, vanadium, molybdenum and yellow Methyl isobutyl ketone extraction spectrophotometric method for determination of phosphorus pentoxide JB/T9220.9-1999 Standard download decompression password: www.bzxz.net

JB/T 9220.9--1999
This standard is a revision of JB/Z284.9--87 "Chemical analysis method of acidic slag of foundry cupolatograph furnace - determination of phosphorus pentoxide by phosphorus vanadium molybdenum yellow-methyl isobutyl ketone extraction photometric method". During the revision, the original standard was edited and the main technical content remained unchanged. This standard replaces JB/2.284, 9-87 from the date of implementation. This standard was proposed and assigned by the National Technical Committee for Foundry Standardization. The drafting units of this standard are: Shanghai Diesel Engine Factory, Nanchang Diesel Engine Factory, Guiyang Foundry, Shenyang Foundry, Shanghai Tractor Company, Huafeng Iron and Steel Factory, Wuxi Diesel Engine Factory, Changzhou Diesel Engine Factory, etc. The main drafters of this standard are: Wang Zhihan, etc. 452
1 Scope
Standard of the Machinery Industry of the People's Republic of China
Chemical analysis methods for acid slay of cupolaDetermination of phosphorus pentoxide by extractionmolybdophosphate yellow using methyl isobutyl ketonespectrophotometic method of vanadiumJB/T 9220.9 1999
Replaces JB/Z28.1.987
This standard specifies the determination of phosphorus pentoxide in chemical analysis methods. Determination range: 0.005%~0.30%. This standard is applicable to the analysis of the composition of acid slag of cupola. 2 Test conditions
The sample is dissolved with hydrochloric acid-nitric acid and hydrofluoric acid, and the silicon is evaporated. The perchloric acid smokes to drive away the fluoride ions, converting phosphorus into vanadium phosphate, arsenic is complexed with citric acid, and vanadium molybdenum yellow salt is extracted with methyl isobutyl ketone, and its absorbance is measured. 3 Reagent preparation
3.1 Hydrochloric acid-nitric acid mixture: hydrochloric acid (density 1.19g/ml.) + nitric acid (density 1.42g/mlL) (4+1). 3.2 Hydrofluoric acid (density 1.15g/mlL.). 3.3 Perchloric acid (density 1.67g/mL).
3.4 ​​Nitric acid (1+2).
3.5 Ammonium vanadate solution (0.25%): Dissolve 2.5g ammonium vanadate in water, heat to dissolve it completely, add 30ml nitric acid (density 1.19g/mL) after cooling, dilute with water to 1000ml., and mix well. 3.6 Ammonium molybdate solution (15%): Prepare when needed. 3.7 Citric acid solution (50%).
3.8 Methyl isobutyl ketone [4-methyl-pentanone (2)]. 3.9 Phosphorus pentoxide standard solution
3.9.1 Weigh 0.1918g of standard potassium dihydrogen phosphate (pre-dried at 105°C to constant weight). Dissolve with appropriate amount of water, add 10 ml of nitric acid (density 1.42 g/mL), transfer to a 1000 ml volumetric flask, dilute to scale with water, and mix. This solution contains 100 μg of phosphorus pentoxide in 1 ml.
3.9.2 Transfer 50.00 ml of phosphorus pentoxide standard solution (3.9.1). Place in a 200 ml volumetric flask, dilute to scale with water, and mix. This solution contains 25 ug of phosphorus pentoxide in 1 ml. 4 Instruments
Spectrophotometer:
Approved by the State Bureau of Machinery Industry on June 24, 1999 and implemented on January 1, 2000
5 Analysis steps
5.1 Sample quantity
Weigh the sample quantity according to Table 1.
Phosphorus pentoxide content, %bzxz.net
0. 005 ~~0. 05
>0. 05～0.15
>0. 15～0.30
5.2 Blank test
Carry out a blank test together with the sample.
5.3 Determination
JB/T9220.9—1999
5.3.1 Weigh two portions of the sample (5.1) and place them in 250ml polytetrafluoroethylene beakers respectively. Wet the samples with a small amount of water respectively, add 25ml of hydrochloric acid-nitric acid mixture (3.1), heat, and add 10ml of hydrofluoric acid (3.2) to dissolve at low temperature after most of the sample is dissolved. After the sample is dissolved, remove it and cool it slightly, add 10ml of perchloric acid (3.3) and heat it until thick white perchloric acid smoke is emitted for 3~~5min, remove it and cool it, rinse the inner wall with water, continue to heat and emit thick white perfluoric acid smoke until 4~5ml of solution remains in the cup. Note: The temperature of the heated decomposition sample should not be too high. 5.3.2 Remove it and cool it separately, rinse the inner wall with 20ml of water, add 15ml of nitric acid (3.4), and cool it to about 20℃. 5.3.3 Add 10mL of ammonium vanadate solution (3.5) and 15mL of ammonium molybdate solution (3.6) to one solution, let stand, transfer the solution to a 250mL separatory funnel with a 100mL scale, dilute with water to 100mL, mix, add 10mL of citric acid solution (3.7), mix, immediately add 40.00mL of methyl isobutyl ketone (3.8), and shake for 1min. After the two phases are separated, discard the lower aqueous phase and pour out the organic phase from the bottle mouth. This is the color developing solution.
In another solution, except for not adding ammonium molybdate solution (3.6), the other operations are the same as the color developing solution. This is the compensation solution. Note
1 Avoid too high a temperature of the solution during color development to avoid interference from silicon. The color development temperature should not exceed 40. 2 Color development time: 15 to 20 minutes at room temperature at 10 to 20°C; 7 to 15 minutes at 20 to 35°C; 2 minutes above 35°C for complete color development. 5.3.4 Transfer part of the solution to a 2 cm colorimetric dish, use the compensation solution as a reference, measure its absorbance at a wavelength of 390 nm on a spectrophotometer, subtract the absorbance of the blank made with the sample, and find the corresponding amount of phosphorus pentoxide from the working curve. 5.4 Drawing of working curve
Into 8 250ml polytetrafluoroethylene beakers, transfer 0.00, 1.002.00, 4.00, 6.00, 8.00, 10.00, 12.00mL of phosphorus pentoxide standard solution (3.9.2) respectively, add 25mL of hydrochloric acid-nitric acid mixture (3.1) and heat, and then proceed as in 5.3.1 to 5.3.4, taking the reagent blank as reference and measuring its absorbance. Drawing working curve with phosphorus pentoxide as the abscissa and absorbance as the ordinate. 6 Calculation of analysis results
Calculate the percentage of phosphorus pentoxide according to formula (1): P:0, =\×100%
Where: m.--phosphorus pentoxide amount found from the working curve, g; m---sample amount, g.
7 Tolerance
The difference in analysis results between laboratories shall not exceed the tolerances listed in Table 2. When calibrated with standard samples, the deviation shall not exceed 1/2 of the tolerances listed in Table 2.
Phosphorus pentoxide content
0.0050~~0.0100
>0.0100～0.0300
>0.0300～0.100
JB/T 9220.9... 1999
Phosphorus pentaamine content
>0, 100~0. 200
≥0.20~0. 30
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.