CN116380877A - Method for measuring medium-low silicon content - Google Patents
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- CN116380877A CN116380877A CN202310135705.3A CN202310135705A CN116380877A CN 116380877 A CN116380877 A CN 116380877A CN 202310135705 A CN202310135705 A CN 202310135705A CN 116380877 A CN116380877 A CN 116380877A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 72
- 239000010703 silicon Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000012086 standard solution Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000003595 spectral effect Effects 0.000 claims abstract description 14
- LXPCOISGJFXEJE-UHFFFAOYSA-N oxifentorex Chemical compound C=1C=CC=CC=1C[N+](C)([O-])C(C)CC1=CC=CC=C1 LXPCOISGJFXEJE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 46
- 239000004033 plastic Substances 0.000 claims description 22
- -1 polytetrafluoroethylene Polymers 0.000 claims description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 18
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- 238000011088 calibration curve Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000012488 sample solution Substances 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 238000009616 inductively coupled plasma Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000013068 control sample Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000012085 test solution Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 229910001297 Zn alloy Inorganic materials 0.000 abstract description 11
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000009614 chemical analysis method Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000003908 quality control method Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 239000004809 Teflon Substances 0.000 abstract 1
- 229920006362 Teflon® Polymers 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 238000004512 die casting Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- LGERWORIZMAZTA-UHFFFAOYSA-N silicon zinc Chemical compound [Si].[Zn] LGERWORIZMAZTA-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000012795 verification 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
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Plasma & Fusion (AREA)
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Abstract
The invention provides a method for measuring the content of medium and low silicon, which relates to the technical field of spectrochemical analysis and test, and comprises the following steps: s1, preparing a silicon standard solution with the concentration of 100ug/mL, firstly weighing 0.3171g of ammonium hexafluorosilicate (NH) 4 ) 2 SiF 6 The solution was then heated to complete dissolution with 50ml of hydrochloric acid solution (1+10) in a teflon beaker. The invention adopts standard addition method to prepare series standard solution, which can reduce matrix interference and inter-element spectral line interference, the quantitative range can cover detection requirement of 0.0010% -0.10%, the Relative Standard Deviation (RSD) of repeated determination is not more than 1.5%, and the standard recovery rate is 95% -110%, the accuracy of the method meets the requirement of ISO-17025 on nonstandard chemical analysis method, and the method can rapidly and accurately determine low silicon in cast zinc alloyThe content provides reliable guarantee for production, scientific research, application and quality control of the cast low-silicon zinc alloy, and the method has high practicality and outstanding creativity.
Description
Technical Field
The invention relates to the technical field of spectrochemical analysis and test, in particular to a method for measuring the content of medium and low silicon.
Background
Compared with other die casting modes, the zinc alloy die casting has smoother surface and higher dimensional consistency, and is widely applicable to pressure casting or gravity casting, such as various instrument shell castings, and the bearings of various lifting equipment, machine tools, water pumps and the like are cast. However, because of excessive impurities of raw materials, particularly zinc alloy has poor die casting corrosion resistance due to silicon, the air tightness of a workpiece is reduced, and die castings are easy to crack, so that the wide application of the alloy is greatly hindered.
The standard for measuring the silicon content of the existing domestic chemical analysis method for casting zinc alloy is GB/T12689.8 molybdenum blue spectrophotometry, the measuring range is 0.010% -0.050%, an instrument is a spectrophotometer, silicon dioxide and sodium carbonate are used for preparing a silicon standard solution and are melted in a platinum crucible, so that the problem that the analysis range cannot meet the requirement exists, meanwhile, the interference factors are large, the analysis speed is low, the requirement for preparing the silicon standard solution by using a noble metal platinum crucible is high, and the method has application limitation.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a method for measuring low silicon content (0.0010% -0.10%) in a cast zinc alloy.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the method for measuring the content of the medium and low silicon comprises the following steps:
s1, preparing a silicon standard solution with the concentration of 100ug/mL, firstly weighing 0.3171g of ammonium hexafluorosilicate
【(NH 4 ) 2 SiF 6 Adding the solution into a polytetrafluoroethylene beaker, then heating the solution to be completely dissolved by 50mL of hydrochloric acid solution (1+10) at low temperature, then cooling the solution to room temperature, then transferring the solution into a 500mL plastic volumetric flask, filling the 500mL plastic volumetric flask with water to a scale, and uniformly mixing the solution to obtain a silicon standard solution A;
s2, preparing a silicon standard solution with the concentration of 10ug/mL, transferring 10.00mL of the silicon standard solution A, placing the silicon standard solution A in a 100mL plastic volumetric flask, filling the 100mL plastic volumetric flask with water to a scale, and uniformly mixing to obtain a silicon standard solution B;
s3, dissolving the sample, namely weighing 4 parts of 1.0000g of sample into a group of 150mL polytetrafluoroethylene beakers, adding 5mL of water and 10mL of nitric acid (1+1) into the polytetrafluoroethylene beakers, dissolving for 10 minutes at low temperature, taking down and cooling. Adding 3 drops of hydrofluoric acid into the polytetrafluoroethylene beaker at the temperature of not higher than 60 ℃, standing for 5-10 minutes until the sample is completely dissolved, adding 3mL of saturated boric acid solution into the polytetrafluoroethylene beaker, cooling to room temperature, respectively transferring into 100mL plastic volumetric flasks, sequentially adding 0, 1, 2 and 3 times of silicon standard solution B into the plastic volumetric flasks, adding water into the 100mL plastic volumetric flasks to scale, and uniformly mixing to obtain a sample test solution;
s4, establishing a calibration curve of a standard addition method, preparing 4 parts of sample solution through the step S3, then opening an inductively coupled plasma emission spectrometer, selecting 288.1nm, 212.4nm and 184.7nm of three silicon analysis spectral lines after the instrument is stable, and selecting the standard addition method in equipment analysis software, and sucking 4 parts of sample solution one by one to establish a concentration and intensity calibration curve equation and a spectrogram, wherein the linear correlation coefficient of the curve equation is not lower than 0.999;
s5, measuring a sample, inputting the mass of the sample into an inductively coupled plasma emission spectrometer, and measuring the strength of the element to be measured in the sample solution. And opening a calibration curve to be overlapped with the sample spectrogram, selecting a spectral peak position and a background deduction position, storing information and completing the method establishment. The silicon content in the sample was automatically calculated by a computer by means of a regression curve. After the sample is measured, a standard sample with the content close to that of the element to be measured of the sample is selected as a control sample, and the accuracy of the result is verified.
In order to facilitate the preparation of the silicon standard solution, the invention is improved in that in the step S1, 100ug/mL of the silicon standard solution is prepared from the ammonium hexafluorosilicate (NH 4 ) 2 SiF 6 Dissolving with hydrochloric acid solution (1+10), diluting with water to scale, and mixing.
In order to improve the measurement accuracy, the invention is improved in that in the steps S2 and S3, 100ug/mL of silicon standard solution is diluted to 10ug/mL step by step, a working curve is manufactured, the concentration of the added silicon solution is 0, 1 time, 2 times and 3 times of the concentration of a sample to be measured, and the linearity of the working curve is better.
In order to completely dissolve the low silicon of the cast zinc alloy, the improvement of the invention is that 3 drops of hydrofluoric acid are dissolved in the solution at the temperature of lower than 60 ℃ in the step S3.
In order to reduce the influence of the cast zinc matrix, the improvement of the invention is that the standard addition method is adopted to replace the conventional working curve method in the steps S4 and S5, and three spectral lines of silicon are selected to have more choices on possible interference. And by spectrogram superposition, the positions of the spectral peaks and the positions of the background are confirmed, and the signal-to-background ratio is improved.
In order to reduce the pollution introduced by silicon during the operation, the improvement of the invention is that in the steps S1 and S3, the dissolving and holding vessel is a 150mL polytetrafluoroethylene beaker or a plastic volumetric flask. 3mL of saturated boric acid solution eliminates excess hydrofluoric acid.
Compared with the prior art, the method adopts the standard addition method to prepare the series of standard solutions, can reduce matrix interference and inter-element spectral line interference, can cover detection requirements of 0.001% -0.1% in a quantitative range, has a Relative Standard Deviation (RSD) of repeated measurement of not more than 1.5%, and has a labeling recovery rate of 95% -110%, the accuracy of the method meets the requirements of ISO-17025 on a nonstandard chemical analysis method, can rapidly and accurately measure the low silicon content in the cast zinc alloy, and provides reliable guarantee for production, scientific research, application and quality control of the low silicon cast zinc alloy.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof as well as the appended drawings.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a step diagram of a method for measuring the content of medium and low silicon according to the present invention;
FIG. 2 is a table diagram showing the results of sample measurement and sample control verification of a method for measuring the content of medium and low silicon in the invention;
FIG. 3 is a table diagram showing the linear correlation coefficient of the calibration curve in the method for measuring the content of medium and low silicon;
FIG. 4 is a table diagram of the detection limits of the method in the method for measuring the content of medium and low silicon;
FIG. 5 is a chart showing a precision test table in the method for measuring the content of medium and low silicon according to the present invention;
fig. 6 is a table diagram of the test result of the standard recovery rate in the method for measuring the content of medium and low silicon.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-6, a method for measuring the content of medium and low silicon comprises the following steps:
s1, preparing a silicon standard solution with the concentration of 100 ug/mL: 0.3171g of ammonium hexafluorosilicate (NH) are first weighed out 4 ) 2 SiF 6 In a polytetrafluoroethylene beaker, heated to complete dissolution with 50mL of hydrochloric acid solution (1+10) at low temperature, cooled to room temperature, and then transferred into a 500mL plastic containerIn the measuring flask, diluting with water until the plastic volumetric flask is uniformly mixed to the scale, and obtaining a silicon standard solution A;
s2, preparing a 10ug/mL silicon standard solution: transferring 10.00mL of silicon standard solution A, placing the silicon standard solution A in a 100mL plastic volumetric flask, diluting the plastic volumetric flask with water until the scale is uniformly mixed to obtain silicon standard solution B;
s3, dissolving the sample, namely weighing 4 parts of 1.0000g of sample respectively, placing the sample in 4 150mL polytetrafluoroethylene beakers, then adding 5mL of water and 10mL of nitric acid (1+1) into the polytetrafluoroethylene beakers, dissolving the sample at a low temperature for 10 minutes, taking down and cooling the sample. Adding 3 drops of hydrofluoric acid into the polytetrafluoroethylene beaker at the temperature of not higher than 60 ℃, standing for 5-10 minutes until the sample is completely dissolved, then adding 3mL of saturated boric acid solution into the polytetrafluoroethylene beaker, cooling to room temperature, transferring into 100mL plastic volumetric flasks respectively, sequentially adding 0, 1, 2 and 3 times of silicon standard solution B into the sample silicon, and then adding water into the 100mL plastic volumetric flasks until the scales are uniformly mixed to obtain a sample test solution;
s4, establishing a calibration curve, preparing 4 parts of sample solution through the step S3, then opening an inductively coupled plasma emission spectrometer, selecting three analysis spectral lines 288.1nm, 212.4nm and 184.7nm of silicon after the instrument is stable, and selecting a standard addition method in equipment analysis software, and sucking 4 parts of sample solution one by one to establish a concentration and intensity calibration curve equation and a spectrogram, wherein the linear correlation coefficient of the curve equation is not lower than 0.999, and the linear correlation coefficient of the calibration curve is shown in figure 3;
s5, measuring a sample, inputting the mass of the sample into an inductively coupled plasma emission spectrometer, and measuring the strength of the element to be measured in the sample solution. And opening a calibration curve to be overlapped with the sample spectrogram, selecting a spectral peak position and a background deduction position, storing information and completing the method establishment. The silicon content in the sample was automatically calculated by a computer by means of a regression curve. After the sample is measured, a standard sample with the content close to that of the element to be measured of the sample is selected as a control sample, and the accuracy of the result is verified, wherein the result is shown in figure 2.
In this example, in step S1, the silicon standard solution is prepared from the hexafluoroAmmonium silicate [ NH ] 4 ) 2 SiF 6 Dissolving with hydrochloric acid solution (1+10), diluting with water, and mixing.
In the embodiment, in the steps S2 and S3, 100ug/mL of silicon standard solution is diluted stepwise to 10ug/mL, and the concentration of the silicon solution added in the working curve is 0, 1, 2 and 3 times of the concentration of the sample to be measured.
In this example, in step S3, 3 drops of hydrofluoric acid are present in the solution at less than 60 ℃.
In the embodiment, in the step S4 and the step S5, a standard addition method is adopted to replace a conventional working curve method, three spectral lines of silicon are selected, and the spectral peak position and the background buckling position are selected according to the characteristics of a sample.
In this example, in steps S1 and S3, the dissolution and holding vessel is a 150mL polytetrafluoroethylene beaker, a plastic volumetric flask, and 3mL saturated boric acid solution.
And after a calibration curve is established, the measured value of the blank standard solution is the blank value of the method, and the method is carried out for 10 times in parallel. The standard deviation of the blank value is 3 times the detection limit of the method, and the result is shown in fig. 4.
Precision test:
the sample of the cast zinc alloy, SYD1101, was subjected to 6 determinations, and the relative standard deviation RSD was the precision, and the results are shown in FIG. 5.
And (3) standard adding recovery rate test:
3 samples of the solution were treated in parallel, a certain amount of silicon standard solution was added in a concentration gradient, the addition amount was measured, and the addition recovery rate was calculated, and the result was shown in FIG. 6.
According to the embodiment, the standard solution is prepared by adopting the standard addition method, so that the matrix interference and the inter-element spectral line interference can be reduced, the quantitative range can cover the detection requirement of 0.0010% -0.10%, the Relative Standard Deviation (RSD) of repeated measurement is not more than 1.5%, the standard recovery rate is 95% -110%, the accuracy of the method meets the requirement of ISO-17025 on a nonstandard chemical analysis method, the low silicon content in the zinc alloy can be rapidly and accurately measured, the reliable guarantee is provided for the production, scientific research, application and quality control of the low silicon zinc alloy, the practicability is higher, and the method has outstanding creativity.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (6)
1. The method for measuring the content of the medium and low silicon is characterized by comprising the following steps of:
s1, preparing a silicon standard solution with the concentration of 100ug/mL, firstly weighing 0.3171g of ammonium hexafluorosilicate
【(NH 4 ) 2 SiF 6 Adding the solution into a polytetrafluoroethylene beaker, then heating the solution to be completely dissolved by 50mL of hydrochloric acid solution (1+10) at low temperature, then cooling the solution to room temperature, then transferring the solution into a 500mL plastic volumetric flask, adding water into the plastic volumetric flask to scale, and uniformly mixing the solution to obtain a silicon standard solution A;
s2, preparing a 10ug/mL concentration silicon standard solution, transferring 10.00mL of the silicon standard solution A, placing the silicon standard solution A in a 100mL plastic volumetric flask, adding water into the plastic volumetric flask to scale, and uniformly mixing to obtain a silicon standard solution B;
s3, dissolving the sample, namely weighing 4 parts of 1.0000g of sample into a group of 150mL polytetrafluoroethylene beakers, adding 5mL of water and 10mL of nitric acid (1+1) into the polytetrafluoroethylene beakers to dissolve the sample at low temperature for 10 minutes, taking down and cooling. Adding 3 drops of hydrofluoric acid into the polytetrafluoroethylene beaker at the temperature of not higher than 60 ℃ to assist dissolution, then standing for 5-10 minutes until the sample is completely dissolved, then adding 3mL of saturated boric acid solution into the polytetrafluoroethylene beaker to eliminate the influence of fluorine ions, then cooling to room temperature, respectively transferring into 100mL plastic volumetric flasks, sequentially adding silicon standard solution B with the amount of 0, 1, 2 and 3 times of the silicon amount of the sample, and then adding water into the 100mL plastic volumetric flasks to scale and uniformly mixing to obtain a sample test solution;
s4, establishing a calibration curve, opening an inductively coupled plasma emission spectrometer, selecting a silicon analysis spectral line after the instrument is stable, selecting a standard addition method in equipment analysis software, sucking 4 parts of sample solution prepared in the step S3 one by one, and establishing a calibration curve equation, wherein the linear correlation coefficient is not lower than 0.999;
s5, measuring a sample, inputting the mass of the sample into an inductively coupled plasma emission spectrometer, measuring the strength of an element to be measured in a sample solution, automatically calculating the element content in the sample by the instrument, and selecting a standard sample close to the element content to be measured of the sample as a control sample after the sample is measured, so as to verify the accuracy of the result.
2. The method for measuring the content of medium and low silicon according to claim 1, wherein the method comprises the following steps: in step S1, 100ug/mL of silicon standard solution is prepared from the ammonium hexafluorosilicate (NH 4 ) 2 SiF 6 Dissolving with hydrochloric acid solution (1+10), diluting with water to scale, and mixing.
3. The method for measuring the content of medium and low silicon according to claim 1, wherein the method comprises the following steps: in the steps S2 and S3, 100ug/mL of silicon standard solution is diluted to 10ug/mL step by step, a working curve is made, and the concentration of the added silicon solution is 0, 1, 2 and 3 times that of the sample to be tested.
4. The method for measuring the content of medium and low silicon according to claim 1, wherein the method comprises the following steps: in the step S3, 3 drops of hydrofluoric acid are dissolved in the solution at the temperature lower than 60 ℃.
5. The method for measuring the content of medium and low silicon according to claim 1, wherein the method comprises the following steps: in the S4 and S5 steps, a standard addition method is adopted to replace a conventional working curve method, three spectral lines of silicon are selected, and the spectral peak position and the background buckling position are selected according to the characteristics of the sample.
6. The method for measuring the content of medium and low silicon according to claim 1, wherein the method comprises the following steps: in the steps S1 and S3, the dissolution and holding vessel is a 150mL polytetrafluoroethylene beaker, a plastic volumetric flask, and 3mL of saturated boric acid solution.
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