CN113189087A - Method for measuring Nb and P contents in ferrocolumbium ball - Google Patents
Method for measuring Nb and P contents in ferrocolumbium ball Download PDFInfo
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- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 49
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910000592 Ferroniobium Inorganic materials 0.000 title claims description 35
- 239000000523 sample Substances 0.000 claims abstract description 46
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000012488 sample solution Substances 0.000 claims abstract description 21
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 12
- 239000012490 blank solution Substances 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012482 calibration solution Substances 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000010813 internal standard method Methods 0.000 claims abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims description 2
- JMAHHHVEVBOCPE-UHFFFAOYSA-N [Fe].[Nb] Chemical compound [Fe].[Nb] JMAHHHVEVBOCPE-UHFFFAOYSA-N 0.000 abstract description 12
- 230000003595 spectral effect Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 2
- 239000010955 niobium Substances 0.000 description 31
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 10
- 239000011574 phosphorus Substances 0.000 description 10
- 230000006872 improvement Effects 0.000 description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000011088 calibration curve Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- GPGMRSSBVJNWRA-UHFFFAOYSA-N hydrochloride hydrofluoride Chemical compound F.Cl GPGMRSSBVJNWRA-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for measuring the content of Nb and P in a niobium-iron ball, which comprises the following steps: preparing a sample solution, a blank solution and a calibration series solution based on an internal standard method, wherein the calibration series solution comprises M calibration solutions containing Nb and P, and the Nb or P concentration in any one calibration solution is different; measuring the calibration series solution by using an inductively coupled plasma emission spectrometer, and drawing a standard curve; and measuring the blank solution and the sample solution by using an inductively coupled plasma emission spectrometer, and calculating the content of Nb and P in the sample solution based on the drawn standard curve. The invention adopts an ICP method for testing, and the calibration series standard sample in the testing process is prepared by niobium-iron standard samples, ferrophosphorus standard samples and spectral pure iron powder with different masses. The sample and the calibration series of standard samples are dissolved in the same way to prepare a solution. The step concentration and the range of the calibration series solution are reasonably configured according to the contents of Nb and P in the niobium-iron ball, so that the contents of Nb and P in the niobium-iron ball can be quickly and accurately measured.
Description
Technical Field
The invention belongs to the field of analysis and determination, and particularly relates to a method for determining the content of Nb and P in a ferrocolumbium ball.
Background
When 400 MPa-grade screw thread steel is smelted, niobium-iron balls (Nb41P5.5) are used for replacing niobium-iron alloy (Nb60P0.3) and are used as niobium element additives in steelmaking production, so that the cost of steel per ton can be obviously reduced. The niobium-iron ball has low niobium content and high phosphorus content, which do not meet the application range of the national standard detection method of niobium-iron alloy, so the niobium-iron ball cannot be detected according to the standard method. In the steel-making production process, the addition amount of the niobium-iron ball needs to be determined by accurate niobium and phosphorus contents so as to control the chemical components of molten steel, so that a method for quickly and accurately determining the contents of Nb and P in the niobium-iron ball needs to be found urgently.
Disclosure of Invention
Aiming at the problem that the prior art cannot accurately measure the contents of Nb and P in the ferrocolumbium ball, the invention provides a quantitative analysis method for measuring the contents of Nb and P in the ferrocolumbium ball by using an inductively coupled plasma emission spectrometer.
The technical purpose is achieved, the technical effect is achieved, and the invention is realized through the following technical scheme:
a method for measuring the content of Nb and P in a ferrocolumbium ball comprises the following steps:
preparing a sample solution, a blank solution and a calibration series solution based on an internal standard method, wherein the calibration series solution comprises M calibration solutions containing Nb and P, and the Nb or P concentration in any standard solution is different;
measuring the calibration series solution by using an inductively coupled plasma emission spectrometer, and drawing a standard curve;
and measuring the blank solution and the sample solution by using an inductively coupled plasma emission spectrometer, and calculating the content of Nb and P in the sample solution based on the drawn standard curve.
As a further improvement of the invention, the same preparation liquid is adopted to dissolve the same mass of the test sample and the calibration standard sample, and the volume is determined to be the same, so as to obtain a sample solution and a calibration series solution.
As a further improvement of the invention, the mass percent of Nb in the calibration standard sample is between 39.0% and 49.0%, the mass percent of P is between 3.0% and 5.5%, and the content of Nb and the content of P are in increasing or decreasing trend changes in M calibration standard samples, and the change trends of the Nb and the P are opposite.
As a further improvement of the invention, the concentration of Nb in the calibration solution is between 0.6 and 0.8mg/mL, and the concentration of P is between 0.04 and 0.09 mg/mL.
As a further improvement of the invention, the calibration standard sample is prepared by selecting a ferrocolumbium standard sample, a ferrophosphorus standard sample and a spectrally pure iron powder.
As a further improvement of the invention, the ferrocolumbium standard sample comprises a plurality of ferrocolumbium standard samples with different Nb contents, the ferrocolumbium standard sample is selected according to the target mass percentage of Nb and P in the calibration standard sample, and the proportion of the ferrocolumbium standard sample, the ferrophosphorus standard sample and the iron powder is adjusted.
As a further improvement of the invention, M is more than or equal to 5.
As a further improvement of the invention, the preparation liquid comprises hydrochloric acid, hydrofluoric acid and nitric acid.
As a further improvement of the invention, molybdenum is used as an internal standard agent.
As a further improvement of the invention, the selected analysis spectral lines comprise:
Nb 313.079nm；
P 178.284nm、214.914nm；
Mo 281.616nm。。
the invention has the beneficial effects that: according to the method, an ICP method is adopted for testing, the sample solution and the calibration series solution are prepared from the same weight of solid in the testing process, and the contents of Nb and P in the ferrocolumbium ball are quickly and accurately determined according to the step concentration and range of the calibration series solution with reasonable contents of Nb and P in the ferrocolumbium ball.
Drawings
FIG. 1 is a standard curve plotted corresponding to the examples: (a) nb (313.079 nm); (b) p (214.914 nm); (c) p (178.284 nm).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
(1) Preparing a sample solution:
crushing the niobium-iron ball to below 1mm by a jaw crusher and a double-roll crusher step by step, mixing and reducing the mixture to about 200g, and grinding the mixture to below 0.125mm by a vibration mill.
Weighing about 0.40g of sample, accurately weighing to 0.0001g, placing in a 100mL polytetrafluoroethylene beaker, wetting with a small amount of water, adding 20mL of hydrochloric acid-hydrofluoric acid mixed solution (the volume ratio of hydrochloric acid to hydrofluoric acid to water is 35: 35: 30) and 3mL of nitric acid, covering a polytetrafluoroethylene watch glass, heating on an electric hot plate for 10min, taking off the watch glass, washing with water, adding 3mL of nitric acid, and continuing to heat for 1 min. After the reaction was complete, the beaker was removed and rinsed with water while the solution temperature was still high. After the solution was cooled to room temperature, the solution was transferred to a 250mL plastic volumetric flask, 15.00mL of molybdenum standard solution (12.00mg/mL) was removed, diluted to the mark with water, mixed well, and dry filtered for future use.
(2) Preparing a blank solution:
along with the preparation of the sample solution, a blank solution having the same hydrochloric acid, hydrofluoric acid and nitric acid as the sample solution was prepared.
(3) Preparation of calibration series solution:
the ferrocolumbium standard, ferrophosphorus standard and pure iron powder (pure spectrum) were weighed out according to table 1, and a calibration series of standards were synthesized. It should be noted here that in order to ensure that the concentration range included in the subsequently plotted calibration curve of the analysis element can cover the concentration range of the analysis element, the finally plotted calibration curve needs to be composed of more than 5 points (including 5 points) of the calibration solution and be suitably graded. And calculating the calibration series standard sample according to the premise, selecting a proper ferroniobium standard sample, and adjusting the corresponding proportion.
Table 1: calibration series standard sample proportion
The contents of niobium and phosphorus in the calibration series of standard samples are calculated according to the following formula.
In the formula: w is a1-niobium content in the ferrocolumbium standard;
w2-the phosphorus content in the ferrocolumbium standard;
w3-the phosphorus content in the ferrophosphorus standard sample;
m1-ferroniobium standard sample weighing, g;
m2-ferrophosphorus standard sample weighing, g;
m3weighing pure iron powder, g;
m-weight of calibration series of standard samples, m ═ m1+m2+m3，g。
The niobium and phosphorus contents of the synthesized calibration series standard samples are shown in table 2:
table 2: calibrating series standard sample niobium and phosphorus content
It should be noted that the method can automatically synthesize calibration series standard samples according to the sample content and the standard samples prepared in the laboratory, table 1 suggests the method for synthesizing calibration series standard samples, and other suitable standard samples can be selected instead if the standard samples are not available.
Preparing a calibration solution from the calibration series of standard samples by the same method as that for dissolving the samples, and calculating the concentration of niobium and phosphorus in the solution according to the content of niobium and phosphorus in the calibration series of standard samples and the mass of the samples.
Table 3: calibrating the concentration of niobium and phosphorus in series of standard samples
| Name (R) | Nb(mg/mL) | P(mg/mL) |
| Calibration series |
0.620160 | 0.087824 |
| Calibration series |
0.648896 | 0.079088 |
| Calibration series standard 3 | 0.707616 | 0.061680 |
| Calibration series standard sample 4 | 0.768384 | 0.053424 |
| Calibration series standard 5 | 0.796080 | 0.044000 |
(4) ICP test
And starting the ICP spectrometer, and preheating for more than 1 h. And installing a hydrofluoric acid-resistant atomizing device, starting an ignition key, confirming that the running parameters of the instrument are in a confirmation range after ignition, and ensuring that the atomizing system and the plasma flame work normally and are stable for more than 30 min.
And after the ICP spectrometer is stabilized, measuring the solution of the calibration system, drawing a calibration curve, analyzing the blank solution and the sample solution, calibrating the measured values of the sample solution and the solution of the calibration system according to the test value of the blank solution, correcting the calibration curve and calculating the content of Nb and P in the sample solution. Note that before and after analyzing the sample, the standard sample is measured and its content is calculated to ensure the accuracy of the curve. The sample injection system was flushed by drawing in deionized water before each sample solution draw, and each sample was analyzed at least 3 times, averaged.
Drawing a standard curve and recommending an analysis spectral line for analyzing the content of the sample: nb (313.079 nm); p (178.284nm, 214.914 nm); mo (281.616 nm). The standard curve is plotted as shown in fig. 1.
And (4) calculating a result: and correspondingly calculating the concentration of Nb and P in the sample solution and the mass fraction of Nb and P in the sample based on the corrected standard curve and the measured spectral line intensity data of the sample solution.
The results prove that:
weighing a ferrocolumbium standard sample [ GBW (E)010414], a ferrophosphorus standard sample [ GBW (E)010420] and pure iron powder (spectral purity), and synthesizing and verifying the ferroniobium/ferrophosphorus composite material by using a standard sample ZKY-1: nb: 43.80%, P: 4.14% for verifying the accuracy of the curve.
And (4) counting the analysis value of the standard sample:
the foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A method for measuring the content of Nb and P in a ferrocolumbium ball is characterized by comprising the following steps:
preparing a sample solution, a blank solution and a calibration series solution based on an internal standard method, wherein the calibration series solution comprises M calibration solutions containing Nb and P, and the Nb or P concentration in any standard solution is different;
measuring the calibration series solution by using an inductively coupled plasma emission spectrometer, and drawing a standard curve;
and measuring the blank solution and the sample solution by using an inductively coupled plasma emission spectrometer, and calculating the content of Nb and P in the sample solution based on the drawn standard curve.
2. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 1, which is characterized in that: dissolving the same mass of test sample and calibration standard sample by using the same preparation solution, and fixing the volume to the same volume to obtain a sample solution and a calibration series solution.
3. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 2, which is characterized in that: the mass percent of Nb in the calibration standard sample is 39.0-49.0%, the mass percent of P is 3.0-5.5%, and the content of Nb and the content of P are changed in an increasing or decreasing trend in M calibration standard samples, and the change trends of the Nb and the P are opposite.
4. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 3, which is characterized in that: in the calibration solution, the concentration of Nb is between 0.6 and 0.8mg/mL, and the concentration of P is between 0.04 and 0.09 mg/mL.
5. The method for measuring the Nb and P contents in the ferrocolumbium ball according to any one of claims 1 to 4, which is characterized in that: the calibration method comprises the steps of selecting a ferrocolumbium standard sample, a ferrophosphorus standard sample and spectrally pure iron powder to prepare the calibration standard sample.
6. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 5, which is characterized in that: the ferrocolumbium standard sample comprises a plurality of ferrocolumbium standard samples with different Nb contents, the ferrocolumbium standard sample is selected according to the target mass percentage of Nb and P in the calibration standard sample, and the proportion of the ferrocolumbium standard sample, the ferrophosphorus standard sample and the iron powder is adjusted.
7. The method for measuring the Nb and P contents in the ferrocolumbium ball according to any one of claims 1 to 3, characterized in that: m is more than or equal to 5.
8. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 2, which is characterized in that: the preparation liquid comprises hydrochloric acid, hydrofluoric acid and nitric acid.
9. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 1, which is characterized in that: molybdenum is used as an internal standard agent.
10. The method for measuring the Nb and P contents in the ferrocolumbium ball according to claim 1, which is characterized in that: the selected analytical lines include:
Nb 313.079nm；
P 178.284 nm、214.914 nm；
Mo 281.616 nm。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609048A (en) * | 2009-07-16 | 2009-12-23 | 武汉钢铁(集团)公司 | A kind of method of measuring niobium element content in the ferro-niobium |
| CN103115916A (en) * | 2013-01-25 | 2013-05-22 | 内蒙古包钢钢联股份有限公司 | Method for testing niobium content in niobium-iron alloy |
| CN103926236A (en) * | 2014-04-04 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Combined method for measuring content of impurity elements and matrix element niobium in niobium-iron alloy |
| CN109916882A (en) * | 2019-03-28 | 2019-06-21 | 武汉钢铁有限公司 | A method of niobium, silicon, phosphorus content in measurement niobium manganese iron |
-
2021
- 2021-04-22 CN CN202110434879.0A patent/CN113189087A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609048A (en) * | 2009-07-16 | 2009-12-23 | 武汉钢铁(集团)公司 | A kind of method of measuring niobium element content in the ferro-niobium |
| CN103115916A (en) * | 2013-01-25 | 2013-05-22 | 内蒙古包钢钢联股份有限公司 | Method for testing niobium content in niobium-iron alloy |
| CN103926236A (en) * | 2014-04-04 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Combined method for measuring content of impurity elements and matrix element niobium in niobium-iron alloy |
| CN109916882A (en) * | 2019-03-28 | 2019-06-21 | 武汉钢铁有限公司 | A method of niobium, silicon, phosphorus content in measurement niobium manganese iron |
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| Title |
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| 苏彬等: "电感耦合等离子体原子发射光谱法测定铌铁中铌钛钽硅铝磷", 《河南冶金》 * |
| 邵海舟等: "电感耦合等离子体原子发射光谱法测定铌铁中铌钛钽硅铝磷", 《冶金分析》 * |
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