CN105300975A - Detecting method for phosphorus content in vanadium slag - Google Patents
Detecting method for phosphorus content in vanadium slag Download PDFInfo
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Abstract
The invention discloses a detecting method for the phosphorus content in vanadium slag. According to the method, a sample is smashed and dried; the sample and sodium carbonate-boric acid mixed flux are mixed uniformly, the mixture is fused for 20-25 min at the temperature of 900 DEG C+/-10 DEG C, frit is dissolved with 75 ml of hydrochloric acid, and the volume is metered to 250 ml; filtering is carried out, 20.00 ml of filter liquor is taken, three drops of paranitrophenol solution are added, a sodium hydroxide solution is dripped until the solution is yellow, hydrochloric acid is dripped until yellow fades, 5 ml of hydrochloric acid is added, 5 ml of ascorbic acid-hydroxylamine hydrochloride-bismuth nitrate mixed liquor is added, the mixed liquor is placed for 3-5 min, 5 ml of mecaammonium heptamolybdate tetrahydrate-antimony potassium tartrate mixed liquor is added, and the volume is metered to 100 ml; the mixed liquor is placed for 20 min, and with a blank as a reference, a spectrophotometer is used for measuring absorbance of developing liquid at the portion with the wavelength of 700 nm; a phosphorus standard sample with the concentration of 20 micrograms/ml is prepared, transferred and placed into volumetric flasks, water is added, hydrochloric acid is added, after developing, under the same condition, the absorbance is measured, and a working curve is drawn; the phosphorus content in the sample is calculated according to the following formula (see the formula in the description). The method is fast, efficient and particularly suitable for detecting the sample with the phosphorus content of 0.05-1.5%, and has high accuracy, repeatability and stability.
Description
Technical field
The invention belongs to technical field of chemical detection, be specifically related to the detection method of phosphorus content in a kind of vanadium slag.
Background technology
Vanadium slag is the general designation containing the bits of vanadium oxide that is that obtain through oxidation blowing in vanadium extracting process vanadium-bearing hot metal or that obtain through wet method vanadium extraction containing vanadium iron concentrate, and it is the raw material smelting and produce vanadium alloy and vanadium metal.Vanadium slag principal ingredient is V205, P205, Al203, CaO and SiO2 and Fe equal size.Owing to carrying out oxygen blast to vanadium-bearing hot metal in smelting process, while making vanadium be oxidized to vanadium pentoxide, phosphorus is also oxidized to phosphorus pentoxide and enters into vanadium slag, and the phosphorus content of molten iron is also very high, therefore cause the phosphorus content in vanadium slag higher, wherein content of vanadium higher interference phosphorus yield, and the mensuration " soda acid volumetric method and Bismuth phosphorus molybdate blue Photometric Determination of Phosphorus amount " of phosphorus content in existing metallurgy industry standard YB/T547.4-1995 vanadium slag, Bismuth phosphorus molybdate blue spectrphotometric method for measuring scope is 0.05-0.5%, soda acid volumetric determination scope is 0.3-0.8%, soda acid volumetric determination high-content phosphorus, complex operation, time-consuming, not easily grasp.Therefore, develop a kind of detection method that can solve the problem to be very important.
Summary of the invention
The object of the present invention is to provide the detection method of phosphorus content in a kind of vanadium slag.
The object of the present invention is achieved like this, comprises pre-treatment, determination step, specifically comprise:
A, pre-treatment:
1) sample is pulverized, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h, be sealed in exsiccator and be cooled to 20 ~ 25 DEG C;
2) precision takes 1) sample 0.1000 ~ 0.5000g after step process, add 5.0 ~ 6.0g sodium carbonate-boric acid mixed solvent, mixing, be placed in graphite crucible, after 890 ~ 910 DEG C of melting 20 ~ 25min, be cooled to 20 ~ 25 DEG C, add 70 ~ 80ml dissolve with hydrochloric acid solution frit, dissolve completely until frit and be cooled to 20 ~ 25 DEG C, move in 250ml volumetric flask, be diluted with water to scale, shake up rear filtration and obtain test solution a;
3) pipette in 20.00ml test solution a to 100ml volumetric flask, add 2 ~ 4 paranitrophenol solution, drip sodium hydroxide solution to solution in yellow, dropping hydrochloric acid solution is decorporated to yellow, adds 4 ~ 6ml hydrochloric acid solution, 4 ~ 6ml ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor successively again, place 3 ~ 5min, then add 4 ~ 6ml ammonium molybdate-potassium antimony tartrate mixed liquor, be diluted with water to scale after shaking up, shake up, place 15 ~ 25min, obtain nitrite ion b;
B, mensuration:
1) nitrite ion b is moved in 1cm cuvette, with blank test solution for reference, adopt spectrophotometer, in wavelength 700nm place, measure the absorbance of nitrite ion b;
2) compound concentration is the phosphorus standard specimen of 20 μ g/ml, pipette the phosphorus standard specimen of 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.00ml, 8.00ml, be placed in 100ml volumetric flask respectively, add water to 20.0ml, in with 1 after adding the colour developing of 5ml hydrochloric acid) in measure absorbance drawing curve under spectrophotometer similarity condition, in sample, phosphorus content is calculated as follows:
In formula:
M
1---according to the phosphorus quality that sample absorbance checks in from working curve, μ g;
M---sample mass, g;
V
1---the volume that test solution a pipettes, ml;
V---the cumulative volume of test solution a, ml.
Wherein the preparation of phosphorus standard specimen and the drafting of working curve comprise following concrete steps:
1) take 4.3937g in advance at 105-110 DEG C of dry 2h and the potassium dihydrogen phosphate (standard reagent) being cooled to room temperature in exsiccator in 300ml beaker, be dissolved in water, move in 1000 volumetric flasks, be diluted with water to scale and shake up, obtain standard solution a;
Pipette 20.00ml standard solution a in 1000ml volumetric flask, be diluted with water to scale and shake up, obtain standard solution b;
2) working curve is drawn: pipette 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.00ml, 8.00ml phosphorus standard solution b, be placed in 100ml volumetric flask respectively, add water to 20.0ml, add 5ml hydrochloric acid, develop the color by step C, respectively gained nitrite ion is moved in 1cm cuvette, with the nitrite ion corresponding to 0.00ml phosphorus standard solution b for reference, adopt spectrophotometer, in wavelength 700nm place, measure the absorbance of nitrite ion, absorbance is respectively 0.164, 0.367, 0.563, 0.762, 0.863, take absorbance as horizontal ordinate, phosphorus quality is ordinate, drawing curve.
Measurement range of the present invention is 0.05-1.5%, solve the mensuration that phosphorus content is greater than 0.8%, and the present invention is once measuring the mensuration just completed from low content to high-load, eliminate simultaneously vanadium interference simple to operate, easily grasp, therefore to setting up the phosphorus content that this method measures in vanadium slag, smelting production is of great practical significance.
The sample of the method for the invention to phosphorus content 0.05-1.5% is adopted to detect, compared with traditional detection method: measurement range is larger, in the accuracy of testing result, the analytical procedure that the method for the invention adopts and setting parameter, being conducive to sample dissolves completely, noresidue, and the interference reducing substances of vanadium and chromium is reduced to colourless low price form, decrease experimental error, testing result has good stability, reappearance and accuracy.In detection speed, it is fast that the method for the invention has analysis speed, and sense cycle is short, the feature that analysis efficiency is high, has not only saved detection time, alleviates the labour intensity of test analysis personnel, also reduces energy consumption, is conducive to enterprise's cost efficiency.In testing process, the method for the invention is simple to operate, easily learns well and understands, to test analysis personnel without excessive demand, has good popularizing application prospect.
Accompanying drawing explanation
Fig. 1 is working curve diagram of the present invention;
Wherein: horizontal ordinate is absorbance, ordinate is phosphorus quality.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The detection method of phosphorus content in vanadium slag of the present invention, comprises pre-treatment, determination step, specifically comprises:
A, pre-treatment:
1) sample is pulverized, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h, be sealed in exsiccator and be cooled to 20 ~ 25 DEG C;
2) precision takes 1) sample 0.1000 ~ 0.5000g after step process, add 5.0 ~ 6.0g sodium carbonate-boric acid mixed solvent, mixing, be placed in graphite crucible, after 890 ~ 910 DEG C of melting 20 ~ 25min, be cooled to 20 ~ 25 DEG C, add 70 ~ 80ml dissolve with hydrochloric acid solution frit, dissolve completely until frit and be cooled to 20 ~ 25 DEG C, move in 250ml volumetric flask, be diluted with water to scale, shake up rear filtration and obtain test solution a;
3) pipette in 20.00ml test solution a to 100ml volumetric flask, add 2 ~ 4 paranitrophenol solution, drip sodium hydroxide solution to solution in yellow, dropping hydrochloric acid solution is decorporated to yellow, adds 4 ~ 6ml hydrochloric acid solution, 4 ~ 6ml ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor successively again, place 3 ~ 5min, then add 4 ~ 6ml ammonium molybdate-potassium antimony tartrate mixed liquor, be diluted with water to scale after shaking up, shake up, place 15 ~ 25min, obtain nitrite ion b;
B, mensuration:
1) nitrite ion b is moved in 1cm cuvette, with blank test solution for reference, adopt spectrophotometer, in wavelength 700nm place, measure the absorbance of nitrite ion b;
2) compound concentration is the phosphorus standard specimen of 20 μ g/ml, pipette the phosphorus standard specimen of 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.00ml, 8.00ml, be placed in 100ml volumetric flask respectively, add water to 20.0ml, in with 1 after adding the colour developing of 5ml hydrochloric acid) in measure absorbance drawing curve under spectrophotometer similarity condition, in sample, phosphorus content is calculated as follows:
In formula:
M
1---according to the phosphorus quality that sample absorbance checks in from working curve, μ g;
M---sample mass, g;
V
1---the volume that test solution a pipettes, ml;
V---the cumulative volume of test solution a, ml.
Step A 1) described in pulverize granularity be≤0.125mm.
Step A 2) described in sodium carbonate-boric acid mixed solvent be mixed by the sodium carbonate of mass ratio 2:1 and boric acid.
Step A 2) described in hydrochloric acid solution be mixed by mass percentage concentration 37% hydrochloric acid of volume ratio 1:2 and water.
Step A 3) described in paranitrophenol solution be the ethanolic solution of concentration 10g/L.
Step A 3) described in the concentration of sodium hydroxide solution be 200g/L.
Step A 3) described in hydrochloric acid solution be mixed by mass percentage concentration 37% hydrochloric acid of volume ratio 4:96 and water.
Step A 3) described in ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor be dissolved in the 1+1 hydrochloric acid of 20ml by 2g bismuth nitrate, separately get 25g ascorbic acid and 25g oxammonium hydrochloride is dissolved in the 1+47 hydrochloric acid of 480ml, merged by above-mentioned two kinds of solution, mixing obtains.
Step A 3) described in ammonium molybdate-potassium antimony tartrate mixed liquor be dissolved in 500ml water mixing by 10g ammonium molybdate and 20g potassium antimony tartrate obtaining.
Described detection method is applicable to the mensuration of the sample of phosphorus content 0.05 ~ 1.5% in vanadium slag.
Detection method concrete operation method of the present invention is as follows:
A, sample pretreatment: sample is crushed to granularity≤0.125mm, at 105-110 DEG C of dry 1.5-2.5h, be sealed in exsiccator, be cooled to room temperature;
B, sample dissolve: take sample size by table 1, after mixing with the mixed flux of 5.0-6.0g sodium carbonate-boric acid, be placed in the high alumina crucible at the bottom of graphite pads, room temperature is cooled to after 900 ± 10 DEG C of melting 20-25min, gained frit is dissolved in 75ml hydrochloric acid solution, after frit dissolving completely, is cooled to room temperature, then move in 250ml volumetric flask, be diluted with water to scale, shake up rear dry filtration, obtain test solution;
C, colour developing: pipette 20.00ml step B gained test solution in 100ml volumetric flask, add 3 paranitrophenol solution, drip sodium hydroxide solution to solution in yellow, dropping hydrochloric acid is decorporated to yellow, add 5ml hydrochloric acid, add 5ml ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor, place 3-5min, add 5ml amine molybdate-potassium antimony tartrate mixed liquor, scale is diluted with water to after shaking up, shake up, place 20min, obtain nitrite ion;
D, absorbance measurement: moved into by step C gained nitrite ion in 1cm cuvette, with blank test solution for reference, adopt spectrophotometer, in wavelength 700nm place, measures the absorbance of nitrite ion;
E, standard specimen are prepared: take 4.3937g in advance at 105-110 DEG C of dry 2h and the potassium dihydrogen phosphate (standard reagent) being cooled to room temperature in exsiccator in 300ml beaker, be dissolved in water, move in 1000 volumetric flasks, be diluted with water to scale and shake up, obtain standard solution a;
Pipette 20.00ml standard solution a in 1000ml volumetric flask, be diluted with water to scale, shake up, obtain standard solution b;
F, working curve is drawn: pipette 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.00ml, 8.00ml phosphorus standard solution b, be placed in 100ml volumetric flask respectively, add water to 20.0ml, add 5ml hydrochloric acid, develop the color by step C, respectively gained nitrite ion is moved in 1cm cuvette, with the nitrite ion corresponding to 0.00ml phosphorus standard solution b for reference, adopt spectrophotometer, in wavelength 700nm place, measure the absorbance of nitrite ion, absorbance is respectively 0.164, 0.367, 0.563, 0.762, 0.863, take absorbance as horizontal ordinate, phosphorus quality is ordinate, drawing curve,
G, cubage: in sample, phosphorus content calculates according to the following formula:
In formula:
M
1---according to the phosphorus quality that sample absorbance checks in from working curve, ug;
M---the sample mass in step B, g;
V
---the test solution volume pipetted in step C, ml;
V---the test solution cumulative volume in step B, ml.
In described steps A, dried sample is sealed in exsiccator, is cooled to room temperature.
In described step B, taking of sample size takes sample size by table 1, hydrochloric acid solution by volume ratio 1:2 37% hydrochloric acid and water mix.
In described step B, the mixed flux of sodium carbonate-boric acid is mixed by the sodium carbonate of mass ratio 2:1 and boric acid.
In described step C, the concentration of paranitrophenol solution is the ethanolic solution of 10g/L, the concentration of sodium hydroxide solution is 200g/L, hydrochloric acid solution by volume ratio 4:96 37% hydrochloric acid and water mix, ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor is dissolved in the hydrochloric acid of 20ml1+1 by 2g bismuth nitrate, separately get 25g ascorbic acid and 25g oxammonium hydrochloride is dissolved in the hydrochloric acid of 480ml1+47, above-mentioned two kinds of solution are merged, mixing, amine molybdate-potassium antimony tartrate mixed liquor is dissolved in 500ml water by 10g amine molybdate and 20g potassium antimony tartrate, mixing.
In described step e, the phosphorus content of standard solution a is 1mg/ml, and the phosphorus content of standard solution b is 20ug/ml.
In described steps A, step B and step e, be cooled to room temperature and refer to and be cooled to 20-25 DEG C.
In described step D and step F, spectrophotometric counts ultraviolet spectrophotometer, and model is UV-2000.
Table 1 takes sample size
| Phosphorus content (%) | Sample size (%) |
| >0.05-0.30 | 0.5000 |
| >0.30-0.80 | 0.2000 |
| >0.80-1.50 | 0.1000 |
With concrete case study on implementation, the present invention will be further described below:
Embodiment 1
---the detection of phosphorus content in vanadium slag sample
Detection reagent:
The mixed flux of sodium carbonate-boric acid: mixed with boric acid by the sodium carbonate of mass ratio 2:1, porphyrize is made.
Hydrochloric acid solution: by volume ratio 1:2 37% hydrochloric acid and water mix, volume ratio 4:96 37% hydrochloric acid and water mix.
Paranitrophenol solution: concentration is the ethanolic solution of 10g/L.
Sodium hydroxide solution: concentration is 200g/L.
Ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor: be dissolved in the hydrochloric acid of 20ml1+1 by 2g bismuth nitrate, separately gets 25g ascorbic acid and 25g oxammonium hydrochloride is dissolved in the hydrochloric acid of 480ml1+47, is merged by above-mentioned two kinds of solution, mixing.
Amine molybdate-potassium antimony tartrate mixed liquor: be dissolved in 500ml water by 10g amine molybdate and 20g potassium antimony tartrate, mixing.
Potassium dihydrogen phosphate standard specimen: purity is 99.99%.
Sample detection:
A, sample pretreatment: sample is crushed to granularity≤0.125mm, at 105-110 DEG C of dry 1.5-2.5h, be sealed in exsiccator, be cooled to room temperature;
B, sample dissolve: take 0.5000g sample, after mixing with the mixed flux of 5.0-6.0g sodium carbonate-boric acid, be placed in the high alumina crucible at the bottom of graphite pads, room temperature is cooled to after 900 ± 10 DEG C of melting 20-25min, gained frit is dissolved in 75ml hydrochloric acid solution, after frit dissolving completely, is cooled to room temperature, then move in 250ml volumetric flask, be diluted with water to scale, shake up rear dry filtration, obtain test solution;
C, colour developing: pipette 20.00ml step B gained test solution in 100ml volumetric flask, add 3 paranitrophenol solution, drip sodium hydroxide solution to solution in yellow, dropping hydrochloric acid is decorporated to yellow, add 5ml hydrochloric acid, add 5ml ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor, place 3-5min, add 5ml amine molybdate-potassium antimony tartrate mixed liquor, scale is diluted with water to after shaking up, shake up, place 20min, obtain nitrite ion;
D, absorbance measurement: moved into by step C gained nitrite ion in 1cm cuvette, with blank test solution for reference, adopt spectrophotometer, in wavelength 700nm place, measures the absorbance of nitrite ion;
E, standard specimen are prepared: take 4.3937g in advance at 105-110 DEG C of dry 2h and the potassium dihydrogen phosphate (standard reagent) being cooled to room temperature in exsiccator in 300ml beaker, be dissolved in water, move in 1000 volumetric flasks, be diluted with water to scale and shake up, obtain standard solution a;
Pipette 20.00ml standard solution a in 1000ml volumetric flask, be diluted with water to scale and shake up, obtain standard solution b;
F, working curve is drawn: pipette 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.00ml, 8.00ml phosphorus standard solution b, be placed in 100ml volumetric flask respectively, add water to 20.0ml, add 5ml hydrochloric acid, develop the color by step C, respectively gained nitrite ion is moved in 1cm cuvette, with the nitrite ion corresponding to 0.00ml phosphorus standard solution b for reference, adopt spectrophotometer, in wavelength 700nm place, measure the absorbance of nitrite ion, absorbance is respectively 0.164, 0.367, 0.563, 0.762, 0.863, take absorbance as horizontal ordinate, phosphorus quality is ordinate, drawing curve,
G, cubage: being calculated as follows of phosphorus content in vanadium slag sample:
M
1---be 32.39ug according to vanadium slag sample absorbance 0.227 from the phosphorus quality that working curve checks in;
M---the sample mass in step B is 0.5000g;
V
1---the test solution volume pipetted in step C is 20.00ml;
V---the test solution cumulative volume in step B is 250ml.
Embodiment 2
---the detection of phosphorus content in vanadium slag sample
Detection reagent: with embodiment 1
Sample detection:
A, sample pretreatment: sample is crushed to granularity≤0.125mm, at 105-110 DEG C of dry 1.5-2.5h, be sealed in exsiccator, be cooled to room temperature;
B, C, D, E, F step is with embodiment 1.
G, cubage: being calculated as follows of phosphorus content in vanadium slag sample:
M
1---be 67.33ug according to vanadium slag sample absorbance 0.401 from the phosphorus quality that working curve checks in;
M---the sample mass in step B is 0.2000g;
V
1---the test solution volume pipetted in step C is 20.00ml;
V---the test solution cumulative volume in step B is 250ml.
Embodiment 3
---the detection of phosphorus content in vanadium slag sample
Detection reagent: with embodiment 1
Sample detection:
A, sample pretreatment: sample is crushed to granularity≤0.125mm, at 105-110 DEG C of dry 1.5-2.5h, be sealed in exsiccator, be cooled to room temperature;
B, C, D, E, F step is with embodiment 1.
G, cubage: being calculated as follows of vanadium slag content in sample:
M
1---be 125.36ug according to vanadium slag sample absorbance 0.690 from the phosphorus quality that working curve checks in;
M---the sample mass in step B is 0.2000g;
V
1---the test solution volume pipetted in step C is 20.00ml;
V---the test solution cumulative volume in step B is 250ml.
Embodiment 4
---the detection of phosphorus content in vanadium slag sample
Detection reagent: with embodiment 1
Sample detection:
A, sample pretreatment: sample is crushed to granularity≤0.125mm, at 105-110 DEG C of dry 1.5-2.5h, be sealed in exsiccator, be cooled to room temperature;
B, C, D, E, F step is with embodiment 1.
G, cubage: being calculated as follows of phosphorus content in sample:
M
1---be 118.13ug according to vanadium slag sample absorbance 0.654 from the phosphorus quality that working curve checks in;
M---the sample mass in step B is 0.1000g;
V
1---the test solution volume pipetted in step C is 20.00ml;
V---the test solution cumulative volume in step B is 250ml.
The precision of test example 1---detection method of the present invention, accuracy, recovery experiment
(1) Precision Experiment
Select 5 vanadium slag samples, carry out phosphorus mensuration by test method respectively, calculate relative standard deviation, the results are shown in Table 2.
The Precision test result of table 2 detection method of the present invention
| Sample | Measured value (%) | Mean value | Relative standard deviation RSD |
| Sample 1 | 0.128，0.129, 0.131, 0.133, 0.127 | 0.130 | 1.88 |
| Sample 2 | 0.254, 0.252, 0.248, 0.258, 0.256 | 0.254 | 1.52 |
| Sample 3 | 0.308, 0.300, 0.314, 0.319, 0.304 | 0.309 | 1.62 |
| Sample 4 | 0.397, 0.407, 0.401, 0.392, 0.393 | 0.398 | 1.55 |
| Sample 5 | 0.435, 0.432, 0.426, 0.431, 0.442 | 0.433 | 1.36 |
(2) accuracy test
Select 4 vanadium slag standard models, carry out phosphorus mensuration by test method respectively, each sample parallel analyzes 5 times, the results are shown in Table 3.
The accuracy test result of table 3 detection method of the present invention
| Standard model | Standard (P%) | Measured value (%) | Mean value | Relative standard deviation RSD |
| YSBC19811-2000 | 0.064 | 0.065,0.064,0.066,0.067,0.066 | 0.066 | 1.86 |
| YSBC19808-86 | 0.0807 | 0.081,0.080,0.082,0.083,0.080 | 0.081 | 1.51 |
| YSBC19810-2000 | 0.097 | 0.097,0.099,0.099,0.098,0.096 | 0.098 | 1.35 |
| YSBC19808-2000 | 0.297 | 0.300,0.295,0.290,0.285,0.295 | 0.293 | 1.95 |
(3) recovery experiment
Select 1 vanadium slag standard model, add the phosphorus amount of different amount respectively, measure by detection method of the present invention, each sample parallel analyzes 4 times, averages, and trying to achieve the recovery is 98.3%-101.7%, and experimental result is in table 4.
The recovery experimental result of table 4 detection method of the present invention
| Standard model | Standard value (P%) | Addition (ug) | Record total value (ug) | The recovery (%) |
| BH0106 | 0.0807 | 100 | 505.19 | 101.7 |
| BH0106 | 0.0807 | 300 | 698.33 | 98.3 |
| BH0106 | 0.0807 | 500 | 906.52 | 100.60 |
| BH0106 | 0.0807 | 700 | 1097.16 | 99.09 |
Oxide reduction coefficient:
P
2O
5（%）=2.2914P%
From above-mentioned experimental result, the analysis result deviation of detection method of the present invention is little, and precision, accuracy all can meet analyzes requirement, and analysis speed is fast, simple to operate, easily grasps, has higher application value.
Claims (10)
1. the detection method of phosphorus content in vanadium slag, is characterized in that comprising pre-treatment, determination step, specifically comprises:
A, pre-treatment:
1) sample is pulverized, at 105 ~ 110 DEG C of drying 1.5 ~ 2.5h, be sealed in exsiccator and be cooled to 20 ~ 25 DEG C;
2) precision takes 1) sample 0.1000 ~ 0.5000g after step process, add 5.0 ~ 6.0g sodium carbonate-boric acid mixed solvent, mixing, be placed in graphite crucible, after 890 ~ 910 DEG C of melting 20 ~ 25min, be cooled to 20 ~ 25 DEG C, add 70 ~ 80ml dissolve with hydrochloric acid solution frit, dissolve completely until frit and be cooled to 20 ~ 25 DEG C, move in 250ml volumetric flask, be diluted with water to scale, shake up rear filtration and obtain test solution a;
3) pipette in 20.00ml test solution a to 100ml volumetric flask, add 2 ~ 4 paranitrophenol solution, drip sodium hydroxide solution to solution in yellow, dropping hydrochloric acid solution is decorporated to yellow, adds 4 ~ 6ml hydrochloric acid solution, 4 ~ 6ml ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor successively again, place 3 ~ 5min, then add 4 ~ 6ml ammonium molybdate-potassium antimony tartrate mixed liquor, be diluted with water to scale after shaking up, shake up, place 15 ~ 25min, obtain nitrite ion b;
B, mensuration:
1) nitrite ion b is moved in 1cm cuvette, with blank test solution for reference, adopt spectrophotometer, in wavelength 700nm place, measure the absorbance of nitrite ion b;
2) compound concentration is the phosphorus standard specimen of 20 μ g/ml, pipette the phosphorus standard specimen of 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.00ml, 8.00ml, be placed in 100ml volumetric flask respectively, add water to 20.0ml, in with 1 after adding the colour developing of 5ml hydrochloric acid) in measure absorbance drawing curve under spectrophotometer similarity condition, in sample, phosphorus content is calculated as follows:
In formula:
M
1---according to the phosphorus quality that sample absorbance checks in from working curve, μ g;
M---sample mass, g;
V
1---the volume that test solution a pipettes, ml;
V---the cumulative volume of test solution a, ml.
2. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 1) described in the granularity pulverized be≤0.125mm.
3. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 2) described in sodium carbonate-boric acid mixed solvent be mixed by the sodium carbonate of mass ratio 2:1 and boric acid.
4. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 2) described in hydrochloric acid solution be mixed by mass percentage concentration 37% hydrochloric acid of volume ratio 1:2 and water.
5. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 3) described in paranitrophenol solution be the ethanolic solution of concentration 10g/L.
6. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 3) described in the concentration of sodium hydroxide solution be 200g/L.
7. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 3) described in hydrochloric acid solution be mixed by mass percentage concentration 37% hydrochloric acid of volume ratio 4:96 and water.
8. the detection method of phosphorus content in vanadium slag according to claim 1, it is characterized in that step A 3) described in ascorbic acid-oxammonium hydrochloride-bismuth nitrate mixed liquor be dissolved in the 1+1 hydrochloric acid of 20ml by 2g bismuth nitrate, separately get 25g ascorbic acid and 25g oxammonium hydrochloride is dissolved in the 1+47 hydrochloric acid of 480ml, merged by above-mentioned two kinds of solution, mixing obtains.
9. the detection method of phosphorus content in vanadium slag according to claim 1, is characterized in that step A 3) described in ammonium molybdate-potassium antimony tartrate mixed liquor be dissolved in 500ml water mixing by 10g ammonium molybdate and 20g potassium antimony tartrate obtaining.
10., according to the detection method of phosphorus content in the arbitrary described vanadium slag of claim 1 ~ 9, it is characterized in that described detection method is applicable to the mensuration of the sample of phosphorus content 0.05 ~ 1.5% in vanadium slag.
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| CN111812045A (en) * | 2020-06-30 | 2020-10-23 | 新兴铸管股份有限公司 | Method for measuring phosphorus content in high-carbon ferrochrome |
| CN112051230A (en) * | 2020-09-17 | 2020-12-08 | 攀枝花学院 | Analytical method for determining content of phosphorus in vanadium carbide by spectrophotometry |
| CN112683818A (en) * | 2020-12-08 | 2021-04-20 | 山东祥通橡塑科技有限公司 | Method for measuring total phosphorus content in ammonium polyphosphate |
| CN112858199A (en) * | 2021-03-31 | 2021-05-28 | 江苏永林油脂科技有限公司 | Method for detecting content of phosphorus in dimer acid |
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| CN112858199A (en) * | 2021-03-31 | 2021-05-28 | 江苏永林油脂科技有限公司 | Method for detecting content of phosphorus in dimer acid |
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