CN105259159A - Analysis method for measuring content of phosphorus in ferro-molybdenum - Google Patents
Analysis method for measuring content of phosphorus in ferro-molybdenum Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of phosphorus in ferro-molybdenum. The method comprises steps as follows: preparation of a sample solution, preparation of a standard solution, drawing of a standard curve and calculation of the content of phosphorus in a sample according to the standard curve. Ferric hydroxide is adopted for phosphorus coprecipitation in a sample solution preparation process, phosphorus and molybdenum matrixes are separated, spectral interference to the measurement of the phosphorus content due to a large quantity of molybdenum matrixes is avoided, the lower limit of detection is lowered, the accuracy of a detection result is guaranteed, measurement errors are effectively reduced, and the repeatability is good. According to the method, the use of an organic solvent is avoided, so that harm to the human body and the environment due to the use of the organic solvent is effectively eliminated; the operation is simple and convenient, the measurement is rapid, the analysis time is greatly shortened, the analysis efficiency is improved, and a large quantity of manpower and material resources is saved.
Description
Technical field
The invention belongs to alloy medium trace element analytical technology, be specifically related to a kind of method measuring phosphorus content in ferro-molybdenum.
Background technology
Ferro-molybdenum is alloy addition important in steelmaking process, and it adds can make steel have uniform fine grained texture, improves the quenching degree of steel, is conducive to eliminating temper brittleness.The content of the P elements in ferro-molybdenum, affects steel products quality and smelting cost very large, needs to carry out Accurate Determining to it.But phosphorus element content in ferro-molybdenum is very low, usual employing colourimetry detects, concrete steps are as follows: sample is after nitric acid-sulfuric acid acid mixture decomposes, with normal butyl alcohol-methenyl choloride hybrid extraction liquid extraction in sulfuric acid medium, P-Mo blue is become to carry out colorimetric with Reduction with Stannous Chloride, the method long flow path, the organic reagent of use not only to environment, and is detrimental to health.In recent years, along with the widespread use of instrumental analysis, also some report application inductively coupled plasma atomic emissions are had to measure the phosphorus element content in ferro-molybdenum, the analysis spectral line mainly selected has P178.221nm and P213.618nm, because the phosphorus element content in ferro-molybdenum is very low, P178.221nm cause because its emissive porwer is low measure precision and detection limit undesirable; In ferro-molybdenum, molybdenum element mass percentage is up to 60%, the analysis spectral line 213.618nm of analysis spectral line 213.606nm to P of Mo disturbs, and then have considerable influence to the mensuration of phosphorus element content, only adopt Matrix phase, for the P elements of low content, cannot its content of Accurate Determining.New by looking into, be not also particularly suitable for the analytical approach fast and accurately of phosphorus detection in ferro-molybdenum at present both at home and abroad.
Summary of the invention
Object of the present invention will overcome an above-mentioned difficult problem exactly, provides a kind of simple to operation, method of measuring phosphorus element content in ferro-molybdenum fast and accurately.
For achieving the above object, the technical solution adopted in the present invention is as follows:
Measure an analytical approach for phosphorus element content in ferro-molybdenum, adopt inductive coupling plasma emission spectrograph to measure.
One, the reagent used in mensuration process is as follows:
1, nitric acid, ρ 1.42g/ml, top grade is pure;
2, sulfuric acid, ρ 1.84g/ml, top grade is pure;
3, hydrochloric acid, ρ 1.19g/ml, top grade is pure;
4, nitric acid-sulfuric acid acid mixture: measure 50ml nitric acid and 5ml sulfuric acid in beaker, add in 45ml water, mix;
5, ammoniacal liquor, ρ 0.91g/ml, top grade is pure;
6, hartshorn salt, solid, top grade is pure;
7, iron reference solution: 5mg/ml; Take 1.0000g high purity iron and be placed in 200ml volumetric flask, add hydrochloric acid 20ml, be then diluted with water to scale, shake up;
8, hot washing liquid: 20mg/ml; Take 10.0000g hartshorn salt and be placed in 500ml volumetric flask, be dissolved in water, add the mixing of 20ml ammoniacal liquor, be then diluted with water to scale, shake up;
9, phosphorus standard solution: 100 μ g/ml; Take 0.4394g and be dried to constant and the potassium dihydrogen phosphate standard reagent being cooled to room temperature is placed in 1000ml volumetric flask through 105 DEG C ± 5 DEG C in advance, be dissolved in water, be then diluted with water to scale, shake up;
Two, sampling and sample preparation: the sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
Three, analytical procedure is as follows:
1, sample solution is prepared
Sample: take 0.50g sample, be accurate to 0.0001g;
Sample dissolves: sample is placed in 500ml beaker, add 20ml nitric acid-sulfuric acid acid mixture, cover surface plate, after vigorous reaction stops, moving to electric hot plate heating makes sample dissolve completely, adds deionized water, boils removing oxides of nitrogen, with deionized water rinsing surface plate and wall of cup, cool to be measured;
Precipitation: i.e. ferric hydroxide co-precipitation phosphorus, adds iron reference solution, adds deionized water 150ml and dilutes, under agitation slowly add ammoniacal liquor to precipitate completely to ferric hydroxide, and add excessive ammonia 20ml, add hartshorn salt 10g, solution is heated to micro-5min that boils, places 1h.
Sedimentation and filtration: by precipitation Filter paper filtering at a slow speed, washes beaker and filter paper 8-10 time with hot washing liquid, discards filtrate.Wash in former beaker with deionized water by precipitation, dissolve retained sediments on filter paper with hot hydrochloric acid 10ml, with hot deionized water washing filter paper until filter paper is colourless, washing lotion is incorporated in former beaker, and low-temperature heat concentrates, and cooling moves into constant volume in 50mL volumetric flask.
2, preparation standard solution
Take 0.18g high purity iron and replace sample, according to the step operation preparing sample solution, before being finally settled to volumetric flask, add 0.5ml, 1.0ml, 2.0ml, 5.0ml, 8.0ml, 10.0ml phosphorus standard solution respectively, the standard solution of preparation different phosphate content.
3, drawing standard curve
Use Inductively coupled plasma optical emission spectrometer to measure phosphorescence spectrum intensity in calibration solution in 213.618nm place, with spectral intensity values, calibration curve is drawn to the respective concentration of its element.
4, the content of P elements in sample is calculated
Use Inductively coupled plasma optical emission spectrometer to measure phosphorescence spectrum intensity in sample solution in 213.618nm place, according to the spectral intensity values of testing liquid, contrast calibration curve, calculates the content of P elements.
In technique scheme, the running parameter of inductive coupling plasma emission spectrograph is as follows: power: 1.10-1.20Kw; Nebulizer pressure: 25-35psi; Plasma flow speed: 0.25-0.5L/min; Cooling gas flow: 15-20L/Min; Peristaltic pump rotating speed: 100-150r; Integral time: 10-20s.
In technique scheme, when bioassay standard solution, according to solution concentration order from low to high, the standard solution to be measured of typical curve each point is sucked instrument successively, and repeated test 3-5 time, improve the sensitivity level of instrument, reduce test error.
In technique scheme, the linear coefficient of P elements typical curve will more than 0.995.
Beneficial effect of the present invention:
1) compare conventional colorimetric method to detect, we are bright to be decreased with the extraction of normal butyl alcohol-methenyl choloride hybrid extraction liquid, becomes P-Mo blue to carry out the step of colorimetric with Reduction with Stannous Chloride, avoids organic reagent and uses harm to human body and environment.
2) ferric hydroxide co-precipitation phosphorus is adopted, after co-precipitation, phosphorus is separated with matrix molybdenum, avoid a large amount of Mo substrate and phosphorus element content is measured to the spectra1 interfer-caused, under the wavelength of the higher P213.618nm of sensitivity, measure the phosphorus element content in ferro-molybdenum, reduce Monitoring lower-cut, ensure that the accuracy of testing result, effectively reduce test error, reproducible.
3) the method applied in the present invention is easy and simple to handle, measures fast, substantially reduces analysis time, improve analysis efficiency, saved a large amount of manpower and materials.
Accompanying drawing explanation
Fig. 1 is the calibration curve that inductive coupling plasma emission spectrograph measures phosphorus element content in ferro-molybdenum.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Adopt inductive coupling plasma emission spectrograph to measure the content of P elements in ferro-molybdenum, spectrometer running parameter is as follows: power: 1.10-1.20Kw; Nebulizer pressure: 25-35psi; Plasma flow speed: 0.25-0.5L/min; Cooling gas flow: 15-20L/Min; Peristaltic pump rotating speed: 100-150r; Integral time: 10-20s.
(1) reagent used in mensuration process is as follows:
(1.1) nitric acid, ρ 1.42g/ml, top grade is pure;
(1.2) sulfuric acid, ρ 1.84g/ml, top grade is pure;
(1.3) hydrochloric acid, ρ 1.19g/ml, top grade is pure;
(1.4) nitric acid-sulfuric acid acid mixture: measure 50ml nitric acid and 5ml sulfuric acid in beaker, add in 45ml water, mix;
(1.5) ammoniacal liquor, ρ 0.91g/ml, top grade is pure;
(1.6) hartshorn salt, solid, top grade is pure;
(1.7) iron reference solution: 5mg/ml; Take 1.0000g high purity iron and be placed in 200ml volumetric flask, add hydrochloric acid 20ml, be then diluted with water to scale, shake up;
(1.8) hot washing liquid: 20mg/ml; Take 10.0000g hartshorn salt and be placed in 500ml volumetric flask, be dissolved in water, add the mixing of 20ml ammoniacal liquor, be then diluted with water to scale, shake up;
(1.9) phosphorus standard solution: 100 μ g/ml; Take 0.4394g and be dried to constant and the potassium dihydrogen phosphate standard reagent being cooled to room temperature is placed in 1000ml volumetric flask through 105 DEG C ± 5 DEG C in advance, be dissolved in water, be then diluted with water to scale, shake up;
(2) sampling and sample preparation: the sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
(3) analytical procedure is as follows:
(3.1) sample solution is prepared
(3.1.1) sample: take 0.50g sample, be accurate to 0.0001g;
(3.1.2) sample dissolves: sample is placed in 500ml beaker, add 20ml nitric acid-sulfuric acid acid mixture, cover surface plate, after vigorous reaction stops, moving to electric hot plate heating makes sample dissolve completely, adds deionized water, boils removing oxides of nitrogen, with deionized water rinsing surface plate and wall of cup, cool to be measured;
(3.1.3) precipitation: i.e. ferric hydroxide co-precipitation phosphorus, adds iron reference solution, adds deionized water 150ml and dilutes, under agitation slowly add ammoniacal liquor to precipitate completely to ferric hydroxide, and add excessive ammonia 20ml, add hartshorn salt 10g, solution is heated to micro-5min that boils, places 1h.
(3.1.4) sedimentation and filtration: by precipitation Filter paper filtering at a slow speed, washes beaker and filter paper 8-10 time with hot washing liquid, discards filtrate.Wash in former beaker with deionized water by precipitation, dissolve retained sediments on filter paper with hot hydrochloric acid 10ml, with hot deionized water washing filter paper until filter paper is colourless, washing lotion is incorporated in former beaker, and low-temperature heat concentrates, and cooling moves into constant volume in 50ml volumetric flask.
(3.2) preparation standard solution
Take 0.18g high purity iron and replace sample, according to the step operation preparing sample solution, before being finally settled to volumetric flask, add 0.5ml, 1.0ml, 2.0ml, 5.0ml, 8.0ml, 10.0ml phosphorus standard solution respectively, the standard solution of preparation different phosphate content.
(3.3) drawing standard curve
Use Inductively coupled plasma optical emission spectrometer in 213.618nm place, according to solution concentration order from low to high, phosphorescence spectrum intensity 5 times in the variant phosphorus content standard solution of replication, average, with spectral intensity mean value, calibration curve is drawn to the respective concentration of its element, as shown in Figure 1, calculate the linear coefficient of typical curve, its linear coefficient is 0.997.
(3.4) content of P elements in sample is calculated
Use Inductively coupled plasma optical emission spectrometer to measure phosphorescence spectrum intensity in sample solution in 213.618nm place, according to the spectral intensity values of testing liquid, contrast calibration curve, calculates the content of P elements.
Table 1 is that the standard model of three kinds of different phosphate content is measured by Inductively coupled plasma optical emission spectrometer by this method, contrast calibration curve, the phosphorus content result calculated.
Table 1 standard model measured value
| Sample ID | Phosphorus content asserting value | Spectral intensity | Phosphorus detection value |
| GBW01423 | 0.025％ | 30.87 | 0.024％ |
| YSBC28632-2012 | 0.046％ | 62.03 | 0.046％ |
| YSBC18605-08 | 0.154％ | 225.35 | 0.157％ |
Table 1 result shows, measured value and the asserting value anastomose property of phosphorus content are good, and good stability, the precision of this method measurement result are high, and measurement result is accurate.
Claims (4)
1. measure an analytical approach for phosphorus element content in ferro-molybdenum, it is characterized in that: adopt inductive coupling plasma emission spectrograph to measure;
(1) reagent used in mensuration process is as follows:
(1.1) nitric acid, ρ 1.42g/ml, top grade is pure;
(1.2) sulfuric acid, ρ 1.84g/ml, top grade is pure;
(1.3) hydrochloric acid, ρ 1.19g/ml, top grade is pure;
(1.4) nitric acid-sulfuric acid acid mixture: measure 50ml nitric acid and 5ml sulfuric acid in beaker, add in 45ml water, mix;
(1.5) ammoniacal liquor, ρ 0.91g/ml, top grade is pure;
(1.6) hartshorn salt, solid, top grade is pure;
(1.7) iron reference solution: 5mg/ml; Take 1.0000g high purity iron and be placed in 200ml volumetric flask, add hydrochloric acid 20ml, be then diluted with water to scale, shake up;
(1.8) hot washing liquid: 20mg/ml; Take 10.0000g hartshorn salt and be placed in 500ml volumetric flask, be dissolved in water, add the mixing of 20ml ammoniacal liquor, be then diluted with water to scale, shake up;
(1.9) phosphorus standard solution: 100 μ g/ml; Take 0.4394g and be dried to constant and the potassium dihydrogen phosphate standard reagent being cooled to room temperature is placed in 1000ml volumetric flask through 105 DEG C ± 5 DEG C in advance, be dissolved in water, be then diluted with water to scale, shake up;
(2) sampling and sample preparation: the sample analyzed carries out sampling and sample preparation according to the requirement of HB/Z205;
(3) analytical procedure is as follows:
(3.1) sample solution is prepared
(3.1.1) sample: take 0.50g sample, be accurate to 0.0001g;
(3.1.2) sample dissolves: sample is placed in 500ml beaker, add 20ml nitric acid-sulfuric acid acid mixture, cover surface plate, after vigorous reaction stops, moving to electric hot plate heating makes sample dissolve completely, adds deionized water, boils removing oxides of nitrogen, with deionized water rinsing surface plate and wall of cup, cool to be measured;
(3.1.3) precipitation: i.e. ferric hydroxide co-precipitation phosphorus, add iron reference solution, add deionized water 150ml to dilute, under agitation slowly add ammoniacal liquor (1.5) to precipitate completely to ferric hydroxide, and add excessive ammonia 20ml, add hartshorn salt 10g, solution is heated to micro-5min that boils, place 1h.
(3.1.4) sedimentation and filtration: by precipitation Filter paper filtering at a slow speed, washes beaker and filter paper 8-10 time with hot washing liquid, discards filtrate.Wash in former beaker with deionized water by precipitation, dissolve retained sediments on filter paper with hot hydrochloric acid 10ml, with hot deionized water washing filter paper until filter paper is colourless, washing lotion is incorporated in former beaker, and low-temperature heat concentrates, and cooling moves into constant volume in 50ml volumetric flask.
(3.2) preparation standard solution
Take 0.18g high purity iron and replace sample, according to the step operation preparing sample solution, before being finally settled to volumetric flask, add 0.5ml, 1.0ml, 2.0ml, 5.0ml, 8.0ml, 10.0ml phosphorus standard solution respectively, the standard solution of preparation different phosphate content.
(3.3) drawing standard curve
Use Inductively coupled plasma optical emission spectrometer to measure phosphorescence spectrum intensity in calibration solution in 213.618nm place, with spectral intensity values, calibration curve is drawn to the respective concentration of its element.
(3.4) content of P elements in sample is calculated
Use Inductively coupled plasma optical emission spectrometer to measure phosphorescence spectrum intensity in sample solution in 213.618nm place, according to the spectral intensity values of testing liquid, contrast calibration curve, calculates the content of P elements.
2. the analytical approach of phosphorus element content in mensuration ferro-molybdenum according to claim 1, is characterized in that: the running parameter of inductive coupling plasma emission spectrograph is as follows: power: 1.10-1.20Kw; Nebulizer pressure: 25-35psi; Plasma flow speed: 0.25-0.5L/min; Cooling gas flow: 15-20L/Min; Peristaltic pump rotating speed: 100-150r; Integral time: 10-20s.
3. the analytical approach of phosphorus element content in mensuration ferro-molybdenum according to claim 1, it is characterized in that: when bioassay standard solution, according to solution concentration order from low to high, the standard solution to be measured of typical curve each point is sucked instrument successively, and repeated test 3-5 time, improve the sensitivity level of instrument, reduce test error.
4. the analytical approach of phosphorus element content in mensuration ferro-molybdenum according to claim 3, is characterized in that: the linear coefficient of P elements typical curve will more than 0.995.
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| CN107024557A (en) * | 2016-01-29 | 2017-08-08 | 深圳市虹彩检测技术有限公司 | The assay method of red phosphorus content and application |
| CN107389662A (en) * | 2017-06-06 | 2017-11-24 | 舞阳钢铁有限责任公司 | In a kind of quick measure, in low-carbon ferrochromium alloy vanadium analysis method |
| CN108318476A (en) * | 2018-05-09 | 2018-07-24 | 郭秀娟 | The ICP-AES measurement methods of micro- antimony content in a kind of ferro-molybdenum |
| CN108507858A (en) * | 2018-03-01 | 2018-09-07 | 白银有色集团股份有限公司 | A kind of method of impurity element aluminium, phosphorus, titanium in measurement nickel ore concentrate |
| CN108872223A (en) * | 2018-07-12 | 2018-11-23 | 攀钢集团江油长城特殊钢有限公司 | A kind of method of phosphorus content in measurement molybdenum compound |
| CN109030471A (en) * | 2018-06-04 | 2018-12-18 | 金堆城钼业股份有限公司 | The improved method of phosphorus detection standard curve in a kind of molybdenum-iron |
| CN110161016A (en) * | 2019-05-30 | 2019-08-23 | 中航金属材料理化检测科技有限公司 | A kind of method of phosphorus content in measurement Fe Ni matrix high temperature alloy |
| CN110927144A (en) * | 2019-12-10 | 2020-03-27 | 辽宁科技大学 | ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for content of impurity phosphorus in steel |
| CN113466211A (en) * | 2021-06-11 | 2021-10-01 | 福建中凯检测技术有限公司 | Coprecipitation method for measuring various heavy metal elements in seawater |
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| CN107024557A (en) * | 2016-01-29 | 2017-08-08 | 深圳市虹彩检测技术有限公司 | The assay method of red phosphorus content and application |
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| CN107389662A (en) * | 2017-06-06 | 2017-11-24 | 舞阳钢铁有限责任公司 | In a kind of quick measure, in low-carbon ferrochromium alloy vanadium analysis method |
| CN108507858A (en) * | 2018-03-01 | 2018-09-07 | 白银有色集团股份有限公司 | A kind of method of impurity element aluminium, phosphorus, titanium in measurement nickel ore concentrate |
| CN108318476A (en) * | 2018-05-09 | 2018-07-24 | 郭秀娟 | The ICP-AES measurement methods of micro- antimony content in a kind of ferro-molybdenum |
| CN109030471A (en) * | 2018-06-04 | 2018-12-18 | 金堆城钼业股份有限公司 | The improved method of phosphorus detection standard curve in a kind of molybdenum-iron |
| CN108872223A (en) * | 2018-07-12 | 2018-11-23 | 攀钢集团江油长城特殊钢有限公司 | A kind of method of phosphorus content in measurement molybdenum compound |
| CN110161016A (en) * | 2019-05-30 | 2019-08-23 | 中航金属材料理化检测科技有限公司 | A kind of method of phosphorus content in measurement Fe Ni matrix high temperature alloy |
| CN110927144A (en) * | 2019-12-10 | 2020-03-27 | 辽宁科技大学 | ICP-AES (inductively coupled plasma-atomic emission Spectrometry) measuring method for content of impurity phosphorus in steel |
| CN113466211A (en) * | 2021-06-11 | 2021-10-01 | 福建中凯检测技术有限公司 | Coprecipitation method for measuring various heavy metal elements in seawater |
| CN113466211B (en) * | 2021-06-11 | 2023-12-15 | 福建中凯检测技术有限公司 | Coprecipitation method for measuring multiple heavy metal elements in seawater |
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