CN114088691A - Method for detecting harmful elements in metal orthodontic bracket by plasma emission spectrometry - Google Patents
Method for detecting harmful elements in metal orthodontic bracket by plasma emission spectrometry Download PDFInfo
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- 239000002184 metal Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 title claims abstract description 30
- 239000012086 standard solution Substances 0.000 claims abstract description 33
- 230000029087 digestion Effects 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 31
- 239000000126 substance Substances 0.000 claims abstract description 19
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- 239000012498 ultrapure water Substances 0.000 claims abstract description 9
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 40
- 229910052793 cadmium Inorganic materials 0.000 claims description 38
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 24
- 229910052790 beryllium Inorganic materials 0.000 claims description 24
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 24
- 229910017604 nitric acid Inorganic materials 0.000 claims description 24
- PWOSZCQLSAMRQW-UHFFFAOYSA-N beryllium(2+) Chemical compound [Be+2] PWOSZCQLSAMRQW-UHFFFAOYSA-N 0.000 claims description 20
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- 238000001514 detection method Methods 0.000 abstract description 17
- 238000011084 recovery Methods 0.000 abstract description 6
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- 238000004458 analytical method Methods 0.000 description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000010963 304 stainless steel Substances 0.000 description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
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- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 1
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009616 inductively coupled plasma 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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- 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
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- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to the technical field of detection methods, and particularly relates to a method for detecting harmful elements in a metal orthodontic bracket by using a plasma emission spectroscopy method. Aiming at the problems that the detection method in the prior art is low in detection precision, not simple and convenient enough in operation and incapable of providing technical support for quickly and accurately determining harmful elements in the metal orthodontic bracket, the invention provides a method for detecting the harmful elements in the metal orthodontic bracket by using a plasma emission spectrometry, which comprises the steps of adding a sample to be detected into a digestion device, transferring a digestion solution into a volumetric flask to ensure the volume of ultrapure water to obtain a solution to be determined; preparing a standard solution; establishing a standard curve equation; and measuring the solution to be measured by using a plasma emission spectrometer, and calculating the mass concentration of each metal element in the solution to be measured according to a standard curve equation and the measured chemical signal intensity. The detection method provided by the invention has the characteristics of low detection limit, good precision, high recovery rate, simple operation and the like.
Description
Technical Field
The invention belongs to the technical field of detection methods, and particularly relates to a method for detecting harmful elements in a metal orthodontic bracket by using a plasma emission spectroscopy method.
Background
The metal orthodontic bracket is widely used in the modern orthodontic treatment process, is generally formed by welding precipitation hardening stainless steel, austenitic stainless steel and brazing materials at high temperature, plays roles of correcting teeth, relieving malocclusion and jaw deformity and the like, and achieves the aims of balancing, stabilizing and beautifying the oral and jaw system through treatment. The orthodontic bracket compounded by stainless steel with different brands is generally made of 630 stainless steel to be a main body of the bracket to bear larger stress in orthodontic operation so as to ensure the clinical function of straightening teeth; the 304 stainless steel material is generally used for making the net bottom of the bracket, so that a larger bonding surface is obtained between the bracket and the tooth, and further, a larger bonding force is obtained, and the long-term effect of the orthodontic operation is ensured. The orthodontic period is generally two years, during the period, the metal orthodontic bracket is closely contacted with the oral cavity of a human body, the oral cavity is always in a wet state, the components, concentration and pH value of saliva are frequently changed, and the stable temperature is extremely beneficial to the growth and reproduction of bacteria, so that a special and complex environment is formed. Metallic orthodontic brackets are susceptible to various types of corrosion behavior in such environments, such as galvanic corrosion, intergranular corrosion, fretting corrosion, microbial corrosion, stress corrosion, and the like, resulting in the leaching of metal ions from the metallic orthodontic brackets. For example, beryllium and its compounds are listed as carcinogens in the national toxicology office of the united states, while lead and cadmium are internationally recognized as harmful elements that are easily deposited on the human body and induce diseases. Due to the recognized defects, beryllium-containing alloys are added into oral metal materials by part of enterprises in the medical development history due to good processing properties, and are not forbidden until the existing carcinogenic properties are found, so that the national standard YY/T0915 strictly requires beryllium, cadmium and lead elements in metal orthodontic brackets. This requires that our regulatory authorities must technically implement accurate and fast supervision of such products.
However, the detection method in the prior art has low detection precision and is not simple and convenient enough to operate, and cannot provide technical support for rapidly and accurately measuring the harmful elements in the metal orthodontic bracket.
For example, the chinese patent application discloses a method for detecting heavy metal content [ application No.: 201710988676.X ], the invention patent application comprises the following steps: (1) preparing a solution to be detected: preparing a heavy metal sample to be detected into an aqueous solution, and adding an acid solution and a potassium iodide solution to obtain a liquid to be detected; (2) and (3) detecting a liquid to be detected: transferring the solution to be detected, and dropwise adding the solution to test paper for developing for 50-100 seconds, wherein the test paper contains dye; (3) and (3) judging a detection result: and visually comparing the color test paper with a color comparison card to determine the concentration of the heavy metal.
The traditional method for measuring the stainless steel by adopting the plasma emission spectrometry generally needs to digest the stainless steel at high temperature by using strong acid to prepare a liquid sample, only one type of stainless steel (such as 304 stainless steel) is subjected to test, the content of the component to be tested is generally constant or trace, and only one component can be tested at one time. The components of the metal orthodontic bracket are very complex (generally formed by welding more than 2 stainless steels of different types and brazing materials at high temperature), and the harmful elements to be tested are generally trace or trace components (such as cadmium, lead, beryllium and the like, the content of which is below 0.02 percent), so that the metal orthodontic bracket is greatly influenced by the aspects of matrix effect, interference between spectral lines and the like. A sample preparation method aiming at a complex matrix needs to be developed, and an analysis spectral line suitable for detecting the complex matrix and trace elements is screened out, so that a trace or trace harmful element analysis method suitable for determining the metal orthodontic bracket is established.
The method has the advantages of partially solving the heavy metal detection method and achieving the effect of rapid detection, but the measurement precision is low, and the precision requirement of measuring harmful elements in the metal orthodontic bracket cannot be met. The method provides reference for rapidly and accurately measuring harmful elements in the metal orthodontic bracket and provides technical support for a medical instrument supervision mechanism.
Disclosure of Invention
The invention aims to solve the problems and provides a method for detecting harmful elements in a metal orthodontic bracket by using a plasma emission spectrometry, which has the advantages of high precision and simplicity in operation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for detecting harmful elements in a metal orthodontic bracket by plasma emission spectrometry comprises the following steps:
the method comprises the following steps: adding a sample to be measured into a digestion device, adding mixed acid of nitric acid and hydrochloric acid, digesting by using the digestion device at normal temperature when the sample and the acid fully react until no bubbles are generated, transferring the digestion solution into a volumetric flask to fix the volume by ultrapure water after digestion is finished, and obtaining a solution to be measured;
step two: preparing standard solutions with different concentrations and containing a single metal element for later use;
step three: selecting different characteristic wavelengths aiming at different metal elements, respectively measuring standard solutions containing single metal elements by using a plasma emission spectrometer, and recording the intensity of generated chemical signals;
step four: establishing a standard curve by taking the mass concentration of the metal elements in the standard solution as an abscissa and the corresponding chemical signal intensity measured in the third step as an ordinate to obtain a standard curve equation;
step five: and (4) measuring the solution to be measured in the step one by using the plasma emission spectrometer, and calculating the mass concentration of each metal element in the solution to be measured according to a standard curve equation and the measured chemical signal intensity.
In the method for detecting harmful elements in the metal orthodontic bracket by plasma emission spectrometry, the metal elements comprise beryllium, cadmium and lead.
In the method for detecting harmful elements in the metal orthodontic bracket by plasma emission spectrometry, the characteristic wavelength of the beryllium element is 313.107 nm; the characteristic wavelength of the cadmium element is 214.438 nm; the characteristic wavelength of the lead element is 220.353 nm.
In the method for detecting harmful elements in the metal orthodontic bracket by using the plasma emission spectrometry, the standard curve equation of the beryllium element is as follows: y isBe＝-12.195080+32541.4262XBe；
Wherein,YBeis the mass concentration of beryllium element, XBeThe spectral line intensity of the beryllium element is measured by a plasma emission spectrometer.
In the method for detecting harmful elements in the metal orthodontic bracket by using the plasma emission spectrometry, the standard curve equation of the cadmium element is as follows: y isCd＝-7.302843+3197.73021XCd；
Wherein, YCdIs the mass concentration of cadmium element, XCdThe measured spectral line intensity of cadmium element by the plasma emission spectrometer.
In the method for detecting harmful elements in the metal orthodontic bracket by plasma emission spectrometry, the standard curve equation of the lead element is as follows: y isPb＝5.449474+139.94155XPb；
Wherein, YPbIs the mass concentration of lead element, XPbThe line intensity of the lead element is measured by a plasma emission spectrometer.
In the method for detecting harmful elements in the metal orthodontic bracket by plasma emission spectrometry, the mass concentrations of the metal elements in the standard solution containing the single metal element are respectively 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mug/mL.
In the method for detecting harmful elements in the metal orthodontic bracket by plasma emission spectrometry, the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2O＝1:3:6。
In the method for detecting the harmful elements in the metal orthodontic bracket by the plasma emission spectrometry, the mass of the mixed acid is more than 20 times of that of the sample to be detected.
In the method for detecting harmful elements in the metal orthodontic bracket by plasma emission spectrometry, the linear correlation coefficient of the standard curve established in the fourth step is greater than 0.99.
Compared with the prior art, the invention has the advantages that:
1. compared with the prior art, the method has the advantage that the bracket whole body can be completely digested in a mode of using aqua regia to assist microwave digestion.
2. Compared with the prior art, the method has the advantage that the content of beryllium, cadmium and lead in the bracket product can be detected simultaneously.
3. The method for measuring the content of beryllium, cadmium and lead in the orthodontic bracket provided by the invention adopts a standard curve drawn by a standard solution matched with a matrix, and the linear correlation coefficient Be: 0.9999, Cd: 0.9999, Pb: 0.9995, the linear relationship is better.
4. The method for determining the content of beryllium, cadmium and lead in the orthodontic bracket provided by the invention has the following relevant detection limits Be: 0.00003%, Cd: 0.00002%, Pb: 0.0003%, very sensitive detection limit.
5. The method for measuring the content of beryllium, cadmium and lead in the orthodontic bracket provided by the invention utilizes the inductively coupled plasma transmitting spectrometer for detection, and has short detection time and high working efficiency.
6. According to the method for determining the content of beryllium, cadmium and lead in the orthodontic bracket, the solution of the sample to be determined is prepared by means of aqua regia digestion, microwave digestion instrument digestion and the like, the standard curve drawn by the standard solution matched and configured with the matrix is adopted for determination, the determination repeatability is good, the result is accurate, the reproducibility is good, and effective data can be provided for product quality control.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Example 1
The embodiment provides a method for detecting harmful elements in a metal orthodontic bracket by plasma emission spectrometry, which comprises the following steps:
the method comprises the following steps: removing non-metal markers on the surface of the metal orthodontic bracket by a physical method, cleaning with ether, cleaning in ultrasonic for 15 minutes, removing oil stains on the surface, naturally drying at room temperature to obtain a sample to be detected, accurately weighing 0.1000g of the sample to be detected by a ten-thousandth electronic balance, adding the sample to be detected into a polytetrafluoroethylene microwave digestion tank, adding 10ml of mixed acid, wherein the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2O1: 3:6, and fully reacting the sample with the mixed acid at normal temperature until no product is producedCovering the cover of the digestion tank until the bubbles are generated, installing the outer sleeve of the digestion tank, fully screwing the digestion tank by using a torque wrench, placing the digestion tank in a microwave digestion instrument for microwave digestion, cooling to room temperature after the digestion is finished, taking out the inner tank, transferring the digestion solution into a 100ml volumetric flask, and fixing the volume to the scale by using ultrapure water;
step two: accurately weighing 0.1000g of six parts of pure iron standard substance, respectively placing the six parts in 100ml beakers, respectively adding 10ml of mixed acid, wherein the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2Heating and dissolving on an electric heating plate, cooling, transferring to a 100mL volumetric flask, transferring 0mL, 0.01mL, 0.02mL, 0.03mL, 0.04mL and 0.05mL of beryllium standard stock solutions into the 100mL volumetric flask respectively, wherein the beryllium standard stock solutions are beryllium single element standard solutions GSB 04-1718 (national nonferrous metals and electronic materials analysis and test center), 1000 mug/mL and 1.5mol/L nitric acid as a medium, and then fixing the volume by using ultrapure water, and the mass concentrations of beryllium in the series of standard solutions are 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mug/mL respectively; the steps are repeated to prepare a cadmium element standard solution with mass concentration of 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL and a lead element standard solution with mass concentration of 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL respectively, wherein the cadmium element standard stock solution is a cadmium unit element standard solution GSB 04-1721 (national analysis and test center for nonferrous metals and electronic materials), 1000 mu g/mL, a medium is 1.0mol/L nitric acid, and the lead element standard stock solution is a lead solution standard substance GBW in water (082825 (Beijing Tan ink quality inspection science and technology Limited company), 1000 mg/L;
step three: the beryllium element is selected to have a characteristic wavelength of 313.107nm, and the cadmium element is selected to have a characteristic wavelength of 214.438 nm; selecting 220.353nm characteristic wavelength for lead element, respectively measuring the standard solution containing single metal element prepared in the step two by using a plasma emission spectrometer, and recording the generated spectral line intensity, wherein the working conditions of the plasma emission spectrometer are as follows: the power of a high-frequency generator is 1150W, the atomizer is a quartz atomizer, the flow rate of an argon auxiliary gas is 1.0L/min, the vertical observation height is 15.0mm, the short-wave integration time is 15s, the long-wave integration time is 5s, the rotating speed of a sample injection pump is 50rpm, and the flushing time is 30 s;
step four: establishing a standard curve by taking the mass concentration of the metal element in the standard solution as an abscissa and the corresponding chemical signal intensity measured in the third step as an ordinate, and obtaining a standard curve equation, wherein the standard curve equation of the beryllium element is as follows: y isBe＝-12.195080+32541.4262XBe(ii) a Wherein, YBeIs the mass concentration of beryllium element, XBeThe spectral line intensity of the beryllium element is measured by a plasma emission spectrometer; the standard curve equation of the cadmium element is as follows: y isCd＝-7.302843+3197.73021XCd(ii) a Wherein, YCdIs the mass concentration of cadmium element, XCdThe spectral line intensity of cadmium element measured by a plasma emission spectrometer; the standard curve equation of the lead element is as follows: y isPb＝5.449474+139.94155XPb(ii) a Wherein, YPbIs the mass concentration of lead element, XPbThe spectral line intensity of the lead element measured by a plasma emission spectrometer;
step five: and (4) measuring the solution to be measured in the step one by using the plasma emission spectrometer, and calculating the mass concentration of each metal element in the solution to be measured according to a standard curve equation and the measured chemical signal intensity.
The plasma emission spectrometer is a plasma emission spectrometer produced by the Seimer Feishell technology and having the model of ICAP6300, and the stability (RSD) within 1h less than 2.0% is judged as the stable operation of the instrument.
Example 2
The embodiment provides a method for detecting harmful elements in a metal orthodontic bracket by plasma emission spectrometry, which comprises the following steps:
the method comprises the following steps: removing non-metal markers on the surface of the metal orthodontic bracket by a physical method, cleaning with diethyl ether, cleaning in ultrasonic for 15 minutes, removing oil stains on the surface, naturally drying at room temperature to obtain a sample to be measured, accurately weighing 0.1000g of the sample to be measured by a ten-thousandth electronic balance, adding the sample to be measured into a polytetrafluoroethylene microwave digestion tank, adding 10ml of mixed acid into the mixed acidThe volume ratio of the nitric acid to the hydrochloric acid to the water is HNO3:HCl:H2O is 1:3:6, covering a cover of a digestion tank at normal temperature until the sample and the mixed acid fully react until no bubbles are generated, installing an outer sleeve of the digestion tank, fully screwing the outer sleeve by using a torque wrench, placing the digestion tank in a microwave digestion instrument for microwave digestion, wherein the heating time of the microwave digestion is 15min, the digestion temperature is 150 ℃, the continuous digestion time is 15min, cooling to the room temperature after the digestion is finished, taking out an inner tank, transferring the digestion solution to a 100ml volumetric flask, and fixing the volume to the scale by using ultrapure water;
step two: accurately weighing 0.1000g of six parts of pure iron standard substance, respectively placing the six parts in 100ml beakers, respectively adding 10ml of mixed acid, wherein the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2Heating and dissolving on an electric heating plate, cooling, transferring to a 100mL volumetric flask, transferring 0mL, 0.01mL, 0.02mL, 0.03mL, 0.04mL and 0.05mL of beryllium standard stock solutions into the 100mL volumetric flask respectively, wherein the beryllium standard stock solutions are beryllium single element standard solutions GSB 04-1718 (national nonferrous metals and electronic materials analysis and test center), 1000 mug/mL and 1.5mol/L nitric acid as a medium, and then fixing the volume by using ultrapure water, and the mass concentrations of beryllium in the series of standard solutions are 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mug/mL respectively; the steps are repeated to prepare a cadmium element standard solution with mass concentration of 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL and a lead element standard solution with mass concentration of 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL respectively, wherein the cadmium element standard stock solution is a cadmium unit element standard solution GSB 04-1721 (national analysis and test center for nonferrous metals and electronic materials), 1000 mu g/mL, a medium is 1.0mol/L nitric acid, and the lead element standard stock solution is a lead solution standard substance GBW in water (082825 (Beijing Tan ink quality inspection science and technology Limited company), 1000 mg/L;
step three: the beryllium element is selected to have a characteristic wavelength of 313.107nm, and the cadmium element is selected to have a characteristic wavelength of 214.438 nm; selecting 220.353nm characteristic wavelength for lead element, respectively measuring the standard solution containing single metal element prepared in the step two by using a plasma emission spectrometer, and recording the generated spectral line intensity, wherein the working conditions of the plasma emission spectrometer are as follows: the power of a high-frequency generator is 1150W, the atomizer is a quartz atomizer, the flow rate of an argon auxiliary gas is 1.0L/min, the vertical observation height is 15.0mm, the short-wave integration time is 15s, the long-wave integration time is 5s, the rotating speed of a sample injection pump is 50rpm, and the flushing time is 30 s;
step four: establishing a standard curve by taking the mass concentration of the metal element in the standard solution as an abscissa and the corresponding chemical signal intensity measured in the third step as an ordinate, and obtaining a standard curve equation, wherein the standard curve equation of the beryllium element is as follows: y isBe＝-12.181658+32541.3219XBe(ii) a Wherein, YBeIs the mass concentration of beryllium element, XBeThe spectral line intensity of the beryllium element is measured by a plasma emission spectrometer; the standard curve equation of the cadmium element is as follows: y isCd＝-7.309841+3197.74889XCd(ii) a Wherein, YCdIs the mass concentration of cadmium element, XCdThe spectral line intensity of cadmium element measured by a plasma emission spectrometer; the standard curve equation of the lead element is as follows: y isPb＝5.441568+139.99455XPb(ii) a Wherein, YPbIs the mass concentration of lead element, XPbThe spectral line intensity of the lead element measured by a plasma emission spectrometer;
step five: and (4) measuring the solution to be measured in the step one by using the plasma emission spectrometer, and calculating the mass concentration of each metal element in the solution to be measured according to a standard curve equation and the measured chemical signal intensity.
The plasma emission spectrometer is a plasma emission spectrometer produced by the Seimer Feishell technology and having the model of ICAP6300, and the stability (RSD) within 1h less than 2.0% is judged as the stable operation of the instrument.
Example 3
The embodiment provides a method for detecting harmful elements in a metal orthodontic bracket by plasma emission spectrometry, which comprises the following steps:
the method comprises the following steps: removing nonmetal markers on the surface of the metal orthodontic bracket by a physical method, cleaning with diethyl ether, cleaning in ultrasonic for 15 minutes, removing oil stains on the surface, naturally drying at room temperature to obtain a sample to be measured, and performing electron analysis on ten-thousandth dayAccurately weighing 0.1000g of sample to be detected, adding the sample to be detected into a polytetrafluoroethylene microwave digestion tank, adding 10ml of mixed acid, wherein the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2O is 1:3:6, covering a cover of a digestion tank at normal temperature until the sample and the mixed acid fully react until no bubbles are generated, installing an outer sleeve of the digestion tank, fully screwing the outer sleeve by using a torque wrench, placing the digestion tank in a microwave digestion instrument for microwave digestion, wherein the heating time of the microwave digestion is 15min, the digestion temperature is 180 ℃, the continuous digestion time is 30min, cooling to the room temperature after the digestion is finished, taking out an inner tank, transferring the digestion solution to a 100ml volumetric flask, and fixing the volume to the scale by using ultrapure water;
step two: accurately weighing 0.1000g of six parts of pure iron standard substance, respectively placing the six parts in 100ml beakers, respectively adding 10ml of mixed acid, wherein the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2Heating and dissolving on an electric heating plate, cooling, transferring to a 100mL volumetric flask, transferring 0mL, 0.01mL, 0.02mL, 0.03mL, 0.04mL and 0.05mL of beryllium standard stock solutions into the 100mL volumetric flask respectively, wherein the beryllium standard stock solutions are beryllium single element standard solutions GSB 04-1718 (national nonferrous metals and electronic materials analysis and test center), 1000 mug/mL and 1.5mol/L nitric acid as a medium, and then fixing the volume by using ultrapure water, and the mass concentrations of beryllium in the series of standard solutions are 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mug/mL respectively; the steps are repeated to prepare a cadmium element standard solution with mass concentration of 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL and a lead element standard solution with mass concentration of 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL respectively, wherein the cadmium element standard stock solution is a cadmium unit element standard solution GSB 04-1721 (national analysis and test center for nonferrous metals and electronic materials), 1000 mu g/mL, a medium is 1.0mol/L nitric acid, and the lead element standard stock solution is a lead solution standard substance GBW in water (082825 (Beijing Tan ink quality inspection science and technology Limited company), 1000 mg/L;
step three: the beryllium element is selected to have a characteristic wavelength of 313.107nm, and the cadmium element is selected to have a characteristic wavelength of 214.438 nm; selecting 220.353nm characteristic wavelength for lead element, respectively measuring the standard solution containing single metal element prepared in the step two by using a plasma emission spectrometer, and recording the generated spectral line intensity, wherein the working conditions of the plasma emission spectrometer are as follows: the power of a high-frequency generator is 1150W, the atomizer is a quartz atomizer, the flow rate of an argon auxiliary gas is 1.0L/min, the vertical observation height is 15.0mm, the short-wave integration time is 15s, the long-wave integration time is 5s, the rotating speed of a sample injection pump is 50rpm, and the flushing time is 30 s;
step four: establishing a standard curve by taking the mass concentration of the metal element in the standard solution as an abscissa and the corresponding chemical signal intensity measured in the third step as an ordinate, and obtaining a standard curve equation, wherein the standard curve equation of the beryllium element is as follows: y isBe＝-12.199534+32541.1388XBe(ii) a Wherein, YBeIs the mass concentration of beryllium element, XBeThe spectral line intensity of the beryllium element is measured by a plasma emission spectrometer; the standard curve equation of the cadmium element is as follows: y isCd＝-7.300388+3197.72584XCd(ii) a Wherein, YCdIs the mass concentration of cadmium element, XCdThe spectral line intensity of cadmium element measured by a plasma emission spectrometer; the standard curve equation of the lead element is as follows: y isPb＝5.440357+139.98436XPb(ii) a Wherein, YPbIs the mass concentration of lead element, XPbThe spectral line intensity of the lead element measured by a plasma emission spectrometer;
step five: and (4) measuring the solution to be measured in the step one by using the plasma emission spectrometer, and calculating the mass concentration of each metal element in the solution to be measured according to a standard curve equation and the measured chemical signal intensity.
The plasma emission spectrometer is a plasma emission spectrometer produced by the Seimer Feishell technology and having the model of ICAP6300, and the stability (RSD) within 1h less than 2.0% is judged as the stable operation of the instrument.
Application example 1
The blank solution was continuously measured 10 times in the same manner as described in example 1, and the concentration corresponding to 3 times the standard deviation was taken as the detection limit of each element, and the relevant detection data are shown in the following table:
and (4) analyzing results: therefore, the analysis method provided by the invention has lower detection limit on each metal element.
Application example 2
The solution to be measured was measured 6 times in a short period of time by the method described in example 1, and the average value and standard deviation thereof were determined, and the results are shown in the following table:
and (4) analyzing results: therefore, the relative standard deviation of the analysis method provided by the invention is between 0.3% and 0.8%, which shows that the precision of the method is good.
Application example 3
Standard solutions of various elements to be measured were added to the samples in groups, respectively, and a standard recovery test was performed, and the method for measuring the elements to be measured was the method described in example 1, and the results are shown in the following table:
and (4) analyzing results: therefore, the recovery rate of beryllium is 99.0-101.5%, the standard recovery rate of cadmium is 96.0-100.3%, and the standard recovery rate of lead is 98.0-105.5% in the analysis method provided by the invention, which shows that the recovery rate of the method is good.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. A method for detecting harmful elements in a metal orthodontic bracket by plasma emission spectrometry is characterized by comprising the following steps:
the method comprises the following steps: adding a sample to be measured into a digestion device, adding mixed acid of nitric acid and hydrochloric acid, digesting by using the digestion device at normal temperature when the sample and the acid fully react until no bubbles are generated, transferring the digestion solution into a volumetric flask to fix the volume by ultrapure water after digestion is finished, and obtaining a solution to be measured;
step two: preparing standard solutions with different concentrations and containing a single metal element for later use;
step three: selecting different characteristic wavelengths aiming at different metal elements, respectively measuring standard solutions containing single metal elements by using a plasma emission spectrometer, and recording the intensity of generated chemical signals;
step four: establishing a standard curve by taking the mass concentration of the metal elements in the standard solution as an abscissa and the corresponding chemical signal intensity measured in the third step as an ordinate to obtain a standard curve equation;
step five: and (4) measuring the solution to be measured in the step one by using the plasma emission spectrometer, and calculating the mass concentration of each metal element in the solution to be measured according to a standard curve equation and the measured chemical signal intensity.
2. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 1, wherein: the metal elements include beryllium, cadmium and lead.
3. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectroscopy as claimed in claim 2, wherein: the characteristic wavelength of the beryllium element is 313.107 nm; the characteristic wavelength of the cadmium element is 214.438 nm; the characteristic wavelength of the lead element is 220.353 nm.
4. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 3, wherein: the standard curve equation of the beryllium element is as follows: y isBe＝-12.195080+32541.4262XBe；
Wherein, YBeIs the mass concentration of beryllium element, XBeThe spectral line intensity of the beryllium element is measured by a plasma emission spectrometer.
5. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 3, wherein: the standard curve equation of the cadmium element is as follows: y isCd＝-7.302843+3197.73021XCd；
Wherein, YCdIs the mass concentration of cadmium element, XCdThe measured spectral line intensity of cadmium element by the plasma emission spectrometer.
6. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 3, wherein: the standard curve equation of the lead element is as follows: y isPb＝5.449474+139.94155XPb；
Wherein, YPbIs the mass concentration of lead element, XPbThe line intensity of the lead element is measured by a plasma emission spectrometer.
7. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 1, wherein: the mass concentrations of the metal elements in the standard solution containing the single metal element are respectively 0, 0.10, 0.20, 0.30, 0.40 and 0.50 mu g/mL.
8. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 1, wherein: the volume ratio of nitric acid, hydrochloric acid and water in the mixed acid is HNO3:HCl:H2O＝1:3:6。
9. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectroscopy as claimed in claim 8, wherein: the mass of the mixed acid is more than 20 times of that of the sample to be detected.
10. The method for detecting harmful elements in metal orthodontic brackets by plasma emission spectrometry as claimed in claim 1, wherein: the linear correlation coefficient of the standard curve established in the fourth step is greater than 0.99.
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