CN112304927A - Method for measuring Nb and P contents in high-phosphorus ferrocolumbium - Google Patents
Method for measuring Nb and P contents in high-phosphorus ferrocolumbium Download PDFInfo
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- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 80
- 239000011574 phosphorus Substances 0.000 title claims abstract description 60
- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 55
- 229910000592 Ferroniobium Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000010955 niobium Substances 0.000 claims abstract description 57
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 38
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 37
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012086 standard solution Substances 0.000 claims abstract description 22
- 230000003595 spectral effect Effects 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims abstract description 6
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012452 mother liquor Substances 0.000 claims abstract description 5
- 238000002386 leaching Methods 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 32
- 239000000523 sample Substances 0.000 claims description 28
- 238000004458 analytical method Methods 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000001228 spectrum Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012490 blank solution Substances 0.000 claims description 6
- 238000000295 emission spectrum Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000035945 sensitivity Effects 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 4
- 239000010413 mother solution Substances 0.000 claims description 4
- 239000012488 sample solution Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 230000010354 integration Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000002572 peristaltic effect Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 27
- 230000007547 defect Effects 0.000 abstract description 8
- 229910052729 chemical element Inorganic materials 0.000 abstract description 2
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910000640 Fe alloy Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000012496 blank sample Substances 0.000 description 3
- 238000011088 calibration curve Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 239000013582 standard series solution Substances 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 229910000922 High-strength low-alloy steel Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to the technical field of chemical element detection, and relates to a method for determining the content of Nb and P in high-phosphorus ferrocolumbium; the detection method comprises the following steps: firstly, preparing a niobium standard solution and a phosphorus standard solution; adding a ferrocolumbium sample into a ceramic crucible with an inner layer coated with zirconia, firstly melting with sodium peroxide, leaching with nitric acid, then dissolving with hydrofluoric acid, carrying out constant volume after dissolving in a water bath, and taking the constant volume as mother liquor; after spectral lines are determined, establishing a standard curve according to standard values and spectral intensities of the contents of niobium and phosphorus in the ferrocolumbium standard sample; then calculating the contents of Nb and P in the sample according to the standard curve; the method overcomes the defects of the traditional detection method, is simple and convenient to operate, has the same pretreatment method for the detection samples of niobium and phosphorus, reduces the steps of repeatedly weighing and pretreating the samples, and realizes the rapid and accurate simultaneous determination of Nb and P in the high-phosphorus ferrocolumbium.
Description
Technical Field
The invention belongs to the technical field of chemical element detection, and particularly relates to a method for determining the content of Nb and P in high-phosphorus ferrocolumbium.
Background
The ferroniobium comprises an iron alloy of niobium and iron as a main component. It also contains impurities such as aluminum, silicon, carbon, sulfur, phosphorus, etc. Ferrocolumbium is an alloy material mainly used for smelting high-temperature (heat-resistant) alloy, stainless steel, high-strength low-alloy steel and the like; niobium has a strong inhibiting effect on the austenite recrystallization of steel, so that the rolling of the steel is effectively controlled at a higher temperature, and the strengthening and toughening effects of the controlled rolling are very obvious. The niobium is added to prevent the growth of steel grains at high temperature, refine the steel structure, improve the strength, toughness, creep property and the like of the steel
Therefore, the consumption of niobium as a microalloy element in the carbon steel is greatly increased, and the detection of the content of niobium and other elements in the ferrocolumbium has great significance for production. The chemical components of the ferrocolumbium are detected by the conventional national standard chemical analysis method at present, and niobium, titanium, silicon, aluminum, phosphorus and the like in the ferrocolumbium are analyzed, but the method consumes more reagents, is complicated in operation process and long in period, and is difficult to meet the steel-making requirement.
In the conventional niobium and phosphorus detection method, the samples need to be treated separately and detected separately. In the detection of niobium, such as a chromatographic gravimetric method, toxic reagents are involved in the detection process, so that the detection is not beneficial to the health of detection personnel and environment-friendly treatment; meanwhile, the analysis method is complex in operation flow, long in analysis period and low in detection efficiency. In the detection of the phosphorus content, if a precipitation method is used for separating phosphorus from other elements, the defects of complex operation flow, long analysis period and low detection efficiency of an analysis method are also faced. Other element analysis and detection methods, such as the gravimetric method for measuring tantalum, the EDTA volumetric method for measuring aluminum, the molybdenum blue spectrophotometry for measuring phosphorus and other traditional chemical analysis methods for measuring single elements of impurity elements contained in ferrocolumbium have the defects of complex operation, long detection period, toxic and much reagent consumption, high labor intensity, low efficiency and the like.
Therefore, a method which is simple and convenient to operate, can quickly, quickly and effectively analyze the content of elements in the ferrocolumbium is urgently needed, and has a certain guiding significance for steelmaking production.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to overcome the technical defects of the prior art; in order to solve the defects of the traditional detection method, the method for determining the content of Nb and P in the high-phosphorus ferrocolumbium is provided.
The present invention achieves the above-described object by the following technical means.
A method for measuring the Nb and P contents in high-phosphorus ferrocolumbium comprises the following steps:
(1) preparing a standard solution: preparing a niobium standard solution and a phosphorus standard solution;
(2) preparation of a sample mother solution: adding a ferrocolumbium sample into a ceramic crucible with an inner layer coated with zirconia, firstly melting with sodium peroxide, then leaching with nitric acid, then dissolving with hydrofluoric acid, carrying out water bath at a certain temperature, carrying out constant volume after complete dissolution, using the solution as mother liquor after constant volume, dividing two solutions from the mother liquor, and respectively marking as solution A and solution B after constant volume and uniform mixing; the solution A is used for measuring niobium in the high-phosphorus ferrocolumbium, and the solution B is used for measuring phosphorus in the high-phosphorus ferrocolumbium.
(3) Selecting a spectral line;
respectively scanning the background signal intensity value of the element to be detected at the wavelength of the analysis line of the coexistent element to be detected by using a plasma atomic emission spectrometer for the phosphorus and niobium single element standard solution, and selecting a spectral line with high sensitivity from the spectral lines of the phosphorus and niobium elements as the analysis line;
(4) preparing a standard curve;
s1, preparing a blank solution, wherein the preparation method is the same as the preparation of the sample treatment solution in the step (2), and the difference is that no ferrocolumbium sample is added;
s2, taking n parts of blank solution, respectively adding n parts of niobium and phosphorus standard solutions with gradient volumes, fixing the volume, and uniformly mixing; sequentially introducing the uniformly mixed solution into an instrument, setting working conditions, measuring the emission spectrum intensity of each solution, and establishing a standard curve according to the standard value and the spectrum intensity of the content of the niobium and phosphorus elements in the ferrocolumbium standard sample;
(5) measuring the contents of niobium and phosphorus;
and (3) respectively introducing the solution A and the solution B of the sample prepared in the step (2) into an instrument, measuring the intensity of an emission spectrum, and calculating according to the standard curve established in the step (4) to obtain the content of niobium and phosphorus in the sample solution.
Preferably, in the step (1), the concentration of the niobium standard solution and the concentration of the phosphorus standard solution are both 1000. mu.g/mL.
Preferably, the consumption ratio of the ferrocolumbium sample, the sodium peroxide, the concentrated nitric acid and the hydrofluoric acid in the step (2) is 1 g: 10-15 g: 60-80 mL: 40-50 mL.
Preferably, the concentration of the nitric acid in the step (2) is 1.42g/mL, and the concentration of the hydrofluoric acid is 1.15 g/mL.
Preferably, the certain temperature in the step (2) is 40-50 ℃.
Preferably, the wavelength of the niobium element spectral line in the step (3) is 309.418 nm; the wavelength of the phosphorus element spectral line is 213.617 nm.
Preferably, the instrument in the step (4) is a Thermo iCAP7400 full-spectrum direct-reading plasma atomic emission spectrometer and a hydrofluoric acid resistant sample injection system; the working conditions are as follows: the high-frequency emission power is 1300-1400W, the auxiliary gas is argon, and the flow rate is 0.2-0.5 L.min-1The gas flow rate of the atomizer is 0.70-0.80 L.min-1The rotating speed of the peristaltic pump is 50 r.min-1The observation height is 12.0-15 mm, the measurement integration time is 30s, and the sample injection amount is 1-2 mL/min.
The invention has the advantages and technical effects that:
(1) the method overcomes the defects of the traditional detection method, is simple and convenient to operate, has the same pretreatment method for the detection samples of niobium and phosphorus, reduces the steps of repeatedly weighing and pretreating the samples, and realizes the rapid and accurate simultaneous determination of Nb and P in the high-phosphorus ferrocolumbium; and the linear range is wide, the detection limit and the detection lower limit are greatly improved, the sensitivity is high, and the method is suitable for mass production analysis.
(2) The sample preparation method can effectively overcome the mineral effect and the particle effect of the iron alloy by adopting the ceramic crucible with the inner layer coated with the zirconium oxide, and avoids the pollution of the ceramic crucible material to the measured components; the standard series solution of the calibration curve is prepared by adopting a method of backing a ferrocolumbium standard sample and adding the standard series solution of the element to be detected, the linear relation of the standard curve is good, and the linear range of the curve can be flexibly adjusted according to the content change of the element to be detected in the sample.
(3) The detection process of the invention does not need toxic reagents, and is safe and environment-friendly; and simultaneously, the defects of high labor intensity and low efficiency of the traditional detection are overcome.
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
(1) preparing a standard solution: the concentration of the niobium standard solution and the phosphorus standard solution was 1000. mu.g/mL.
(2) Preparation of sample treatment solution: adding 0.1g of ferrocolumbium sample into a ceramic crucible with an inner layer coated with zirconia, firstly melting by using 2g of sodium peroxide, then leaching by using 8mL of nitric acid, then dissolving by using 5mL of hydrofluoric acid, carrying out water bath at 50 ℃, carrying out constant volume of 250mL after complete dissolution, taking the solution as mother solution after constant volume, respectively taking 10mL of two solutions from the mother solution, carrying out constant volume of 100mL, uniformly mixing, and respectively marking as solution A and solution B; the solution A is used for measuring niobium in the high-phosphorus ferrocolumbium, and the solution B is used for measuring phosphorus in the high-phosphorus ferrocolumbium;
(3) selecting a spectral line;
respectively scanning the background signal intensity value of the element to be detected at the wavelength of the analysis line of the coexistent element to be detected by using a plasma atomic emission spectrometer for the phosphorus and niobium single element standard solution, and selecting a spectral line with high sensitivity from the spectral lines of the phosphorus and niobium elements as the analysis line; the wavelength of the niobium element spectral line is 309.418 nm; the wavelength of the phosphorus element spectral line is 213.617 nm;
(4) preparing a standard curve;
s1, preparing a blank solution, wherein the preparation method is the same as the preparation of the sample treatment solution in the step (2), and the difference is that no sample is added;
s2, dividing 5 parts of 50mL of blank solution into 100mL volumetric flasks, adding 0mL, 1mL, 2mL, 4mL and 6mL of phosphorus and niobium standard solution with the concentration of 1000ug/mL, fixing the volume and uniformly mixing; the mixed solution is sequentially introduced into a Thermo iCAP7400 full-spectrum direct-reading plasma atomic emission spectrometer and a hydrofluoric acid-resistant sample injection system; the working conditions are as follows: the high-frequency emission power is 1300W, the auxiliary gas is argon, and the flow rate is 0.5 L.min-1The gas flow of the atomizer is 0.80 L.min-1The rotating speed of the peristaltic pump is 50 r.min-1The observation height is 15mm, the measurement integration time is 30s, and the sample injection amount is 2 mL/min;
measuring the emission spectrum intensity of each solution, and establishing a standard curve according to the standard value (x) and the spectrum intensity (y) of the Nb and P element content in the solution, wherein the specific structure is shown in Table 2; the blank samples were analyzed 12 times in parallel and the standard deviation of the assay results calculated.
And (3) calculating and analyzing according to the formula (1) to determine the detection limit of a component to be detected.
CL＝KSb/b(1)
In the formula: cLThe detection limit of the component to be detected, mg/L;
Sb-measuring the standard deviation, mg/L, of the blank sample;
b-slope of the calibration curve in the low concentration region, which indicates the change in the analytical signal when the component to be measured changes by one unit
Amount, i.e. sensitivity;
k-a confidence related constant, IUPAC recommended k 3.95%.
(5) Measuring the content of Nb and P;
and (3) introducing the sample treatment solution prepared in the step (2) into an instrument, measuring the intensity of an emission spectrum, and calculating according to the standard curve established in the step (3) to obtain the contents of Nb and P in the sample solution.
Analysis and test:
(1) the detection limit was calculated by measuring 12 blank samples and calculating 3 times the standard deviation of the measured values, and the results are shown in Table 1.
| Element(s) | Analysis line/nm | Detection limit/(mg.L)-1) |
| Nb | 309.418 | 0.005 |
| P | 213.617 | 0.002 |
(2) TABLE 2 Linear equation, correlation coefficient and Linear Range of calibration curves
| Element(s) | Linear equation of equations | Linear range/%) | Correlation coefficient |
| Nb | Y＝2138.6x+339.4 | 41.61～70.03 | 0.9998 |
| P | Y＝1021.4x+0.030 | 0.034～0.127 | 0.9993 |
(3) The high phosphorus ferrocolumbium samples were measured 6 times, and the standard deviation and the relative standard deviation were counted, and the results are shown in table 3.
TABLE 4 results of measurement by the national standard method (chemical analysis of ferrocolumbium: determination of carbon content by gravimetric combustion method (GB 3654.4-1983))
As can be seen from the results in tables 3 and 4, the relative standard deviation of Nb is 4.01%, and the relative standard deviation of P is 2.32%, which are substantially identical to the results measured by the national standard method, indicating that the method has better precision.
(4) Recovery rate test: adding a quantitative standard solution of the element to be detected into the high-phosphorus ferrocolumbium sample solution before the constant volume according to a test method, and carrying out a standard adding recovery test, wherein the result is shown in table 5.
As can be seen from Table 5, the recovery rate of the spiked sample in the method is between 99.3% and 102.5%, and the result has higher accuracy.
Description of the drawings: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; thus, while the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention and protected by the following claims.
Claims (8)
1. A method for measuring the Nb and P contents in high-phosphorus ferrocolumbium is characterized by comprising the following steps:
(1) preparing a standard solution: preparing a niobium standard solution and a phosphorus standard solution;
(2) preparation of a sample mother solution: adding a ferrocolumbium sample into a ceramic crucible with an inner layer coated with zirconia, firstly melting with sodium peroxide, then leaching with nitric acid, then dissolving with hydrofluoric acid, carrying out water bath at a certain temperature, carrying out constant volume after complete dissolution, using the solution as mother liquor after constant volume, dividing two solutions from the mother liquor, and respectively marking as solution A and solution B after constant volume and uniform mixing; the solution A is used for measuring niobium in the high-phosphorus ferrocolumbium, and the solution B is used for measuring phosphorus in the high-phosphorus ferrocolumbium.
(3) Selecting a spectral line;
respectively scanning the background signal intensity value of the element to be detected at the wavelength of the analysis line of the coexistent element to be detected by using a plasma atomic emission spectrometer for the phosphorus and niobium single element standard solution, and selecting a spectral line with high sensitivity from the spectral lines of the phosphorus and niobium elements as the analysis line;
(4) preparing a standard curve;
s1, preparing a blank solution, wherein the preparation method is the same as the preparation of the sample treatment solution in the step (2), and the difference is that no ferrocolumbium sample is added;
s2, taking n parts of blank solution, respectively adding n parts of niobium and phosphorus standard solutions with gradient volumes, fixing the volume, and uniformly mixing; sequentially introducing the uniformly mixed solution into an instrument, setting working conditions, measuring the emission spectrum intensity of each solution, and establishing a standard curve according to the standard value and the spectrum intensity of the content of the niobium and phosphorus elements in the ferrocolumbium standard sample;
(5) measuring the contents of niobium and phosphorus;
and (3) respectively introducing the solution A and the solution B of the sample prepared in the step (2) into an instrument, measuring the intensity of an emission spectrum, and calculating according to the standard curve established in the step (4) to obtain the content of niobium and phosphorus in the sample solution.
2. The method for determining the Nb and P contents in high-phosphorus ferrocolumbium according to claim 1, wherein in the step (1), the concentrations of the niobium standard solution and the phosphorus standard solution are both 1000 μ g/mL.
3. The method for determining the Nb and P contents in high-phosphorus ferrocolumbium according to claim 1, wherein the ratio of the consumption of the ferrocolumbium sample, the sodium peroxide, the concentrated nitric acid and the hydrofluoric acid in the step (2) is 1 g: 10-15 g: 60-80 mL: 40-50 mL.
4. The method for measuring the Nb and P contents in high-phosphorus ferrocolumbium according to claim 1, wherein the concentration of the nitric acid in the step (2) is 1.42g/mL, and the concentration of the hydrofluoric acid is 1.15 g/mL.
5. The method for measuring the Nb and P contents in the high-phosphorus ferrocolumbium according to claim 1, wherein the predetermined temperature in the step (2) is 40 to 50 ℃.
6. The method for measuring the Nb and P contents in high-phosphorus ferrocolumbium according to claim 1, wherein the wavelength of the spectrum line of the niobium element in the step (3) is 309.418 nm; the wavelength of the phosphorus element spectral line is 213.617 nm.
7. The method for measuring the Nb and P contents in a high-phosphorus ferrocolumbium according to claim 1, wherein in S2 in the step (4), n is a positive integer of 3 or more.
8. The method for determining the Nb and P contents in the high-phosphorus ferrocolumbium according to claim 1, wherein the instrument in the step (4) is a Thermo iCAP7400 type full-spectrum direct-reading plasma atomic emission spectrometer and a hydrofluoric acid-resistant sample injection system; the working conditions are as follows: the high-frequency emission power is 1300-1400W, the auxiliary gas is argon, and the flow rate is 0.2-0.5 L.min-1The gas flow rate of the atomizer is 0.70-0.80 L.min-1The rotating speed of the peristaltic pump is 50 r.min-1The observation height is 12.0-15 mm, the measurement integration time is 30s, and the sample injection amount is 1-2 mL/min.
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