CN217688707U - Dry method inductively coupled plasma mass spectrometry combined analyzer - Google Patents
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Abstract
The utility model discloses a dry process inductively coupled plasma mass spectrometry combination analyzer, combination analyzer includes the primary aerosol conversion device, membrane enrichment device, the secondary aerosol conversion device that connect gradually, primary aerosol conversion device, membrane enrichment device, secondary aerosol conversion device connect the auxiliary gas device respectively, membrane enrichment device connects analysis detector one, secondary aerosol conversion device, auxiliary gas device connect analysis detector two; the utility model discloses need not to use reagent, effectively realize the enrichment, can be applied to impurity element's in complicated base member sample, the high-purity sample detection.
Description
Technical Field
The utility model relates to an inductively coupled plasma mass spectrometry technical field especially relates to a dry process inductively coupled plasma mass spectrometry allies oneself with analysis appearance.
Background
With the development of Inductively Coupled Plasma Mass Spectrometry (ICPMS) technology, it has been widely used in the measurement of inorganic elements in various fields, including food, biomedicine, semiconductor, environment, material, etc. However, ICPMS also faces a number of application challenges facing the complexity of sample analysis. Firstly, in most cases, ICPMS analysis requires sample weighing and then wet digestion, wherein the wet digestion generally requires the use of various acids or bases and other reagents, and the digestion process is also complicated, for example, digestion of some high-temperature alloys often takes more than several hours, wastes time and labor, uses more chemical reagents, generates more waste liquid, and is not green and environment-friendly. Meanwhile, the use of some acids, such as hydrochloric acid, sulfuric acid, etc., may generate a more complex matrix effect, and may also bring inconvenience to the test.
In addition, a large amount of water and reagents are introduced into the ICPMS in a traditional wet atomization sample introduction mode, and a large amount of plasma energy is consumed, so that the ionization efficiency of a sample is reduced. Especially, when a high-salt and high-matrix sample is analyzed, matrix elements or salt components and elements to be detected generate larger ionization competition, so that accurate analysis cannot be completed aiming at the elements to be detected. And the introduction of water and reagents brings about polyatomic ions generated by combination of O, H, N, cl and various elements in the sample, and also brings about a lot of interferences, for example, arO greatly interferes with the analysis of Fe.
Although some pretreatment devices can remove part of water vapor by adopting a condensation or membrane desolventizing mode, the water or the solvent still exists in a larger amount and enters into plasma to consume energy, and the desolventizing mode cannot realize the enrichment of a sample, so that the detection limit and the analysis precision of the ICPMS are not greatly improved.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a dry process inductively coupled plasma mass spectrometry allies oneself with analysis appearance need not to use reagent, effectively realizes the enrichment, can be applied to the detection of impurity element in complicated base member sample, the high-purity sample.
In order to achieve the above object, the utility model provides a following scheme:
a dry inductively coupled plasma mass spectrometry analyzer, comprising: the device comprises a primary aerosol conversion device, a membrane enrichment device and a secondary aerosol conversion device which are sequentially connected, wherein the primary aerosol conversion device, the membrane enrichment device and the secondary aerosol conversion device are respectively connected with an auxiliary gas device, the membrane enrichment device is connected with a first analysis detector, and the secondary aerosol conversion device and the auxiliary gas device are connected with a second analysis detector;
the primary aerosol conversion device is used for realizing primary aerosol of a sample to be analyzed to form aerosol; the membrane enrichment device is provided with a filter membrane and is used for intercepting formed aerosol and carrying out enrichment concentration to form a uniform particulate matter membrane, the secondary aerosol conversion device is used for exciting the particulate matter membrane to generate micro-particle-size particles, and the auxiliary gas device is used for providing high-purity gas and the micro-particle-size particles to be fused to form dried aerosol with a desolventizing agent; the first analysis detector is a nondestructive detection device, and specifically adopts a B-ray analyzer, an X-ray fluorescence spectrometer, a Raman spectrometer or an infrared gas analyzer; and the second analysis detector is a destructive detection device, and specifically adopts an ICP-MS analyzer or an ICP-OES analyzer.
Preferably, the membrane enrichment device further comprises an online weighing device, and the online weighing device is connected with the membrane enrichment device; the online weighing device is an in-situ mass detector.
Preferably, the primary aerosol conversion device is a laser-induced ablation device.
Preferably, the secondary aerosol conversion device is a laser-induced ablation device.
Preferably, the high-purity gas is high-purity argon or helium.
According to the utility model provides a concrete embodiment, the utility model discloses a following technological effect: the utility model provides a dry process inductively coupled plasma mass spectrometry allies oneself with analysis appearance to solid sample, liquid sample or gaseous sample, at first realizes the primary aerosol to the sample that awaits measuring, then through enrichment concentration, and then the secondary arouses to form the secondary aerosol who removes the solvent, forms the allies oneself with analysis appearance with inductively coupled plasma mass spectrograph, realizes the detection of impurity element in complicated base member and the high-purity sample; the utility model can realize the enrichment and concentration of the sample to be measured through the membrane enrichment device, and excite the enriched sample again through the aerosol secondary excitation device, thus improving the detection limit and being applicable to the impurity measurement of semiconductor ultra-pure materials or reagents; the utility model relates to a membrane enrichment device, which can realize in-situ on-line real-time weighing, greatly improve the analysis capability of accurate and quantitative analysis and the stability of data; the utility model relates to a combination analyzer with enrichment function can realize the combination with other various detection methods, including but not limited to X-ray fluorescence analyzer, raman analyzer, infrared analyzer, etc.; the secondary aerosol conversion device can completely degrade the sample, so that the fractionation effect and the matrix effect are completely avoided; the utility model discloses can use standard solution to carry out entire system's calibration, great having broken away from the reliance to the solid standard sample, realized using standard solution calibration for the first time, can realize the test to different base member solid sample, need not to clear up to the solid sample, no liquid waste's production, environment friendly, greatly reduced the pollution problem that the waste liquid brought.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor.
Fig. 1 is a schematic structural diagram of the dry inductively coupled plasma mass spectrometer of the present invention;
fig. 2 is a schematic structural diagram of a dry-process inductively coupled plasma mass spectrometer of an embodiment of the present invention;
description of the reference numerals: 1. a disposable aerosol conversion device; 2. a membrane enrichment device; 3. an on-line weighing device; 4. a secondary aerosol conversion device; 5-1, analyzing and detecting a first detector; 5-2, and a second analysis detector.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
The utility model aims at providing a dry process inductive coupling plasma mass spectrum allies oneself with analysis appearance to solid sample, liquid sample or gas sample, need not to use reagent, effectively realizes the enrichment, can be applied to the detection of impurity element in complicated base member sample, the high-purity sample.
In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description.
As shown in fig. 1, the embodiment of the present invention provides a dry method inductively coupled plasma mass spectrometer, including: the device comprises a primary aerosol conversion device 1, a membrane enrichment device 2 and a secondary aerosol conversion device 4 which are sequentially connected, wherein the primary aerosol conversion device 1, the membrane enrichment device 2 and the secondary aerosol conversion device 4 are respectively connected with an auxiliary gas device 6, the membrane enrichment device 2 is connected with a first analysis detector 5-1, and the secondary aerosol conversion device 4 and the auxiliary gas device 6 are connected with a second analysis detector 5-2;
the primary aerosol conversion device 1 is used for realizing primary aerosol of a sample to be analyzed to form aerosol; the membrane enrichment device 2 is provided with a filter membrane and is used for intercepting formed aerosol and carrying out enrichment concentration to form a uniform particulate matter membrane, the secondary aerosol conversion device 4 is used for exciting the particulate matter membrane to generate particles with tiny particle sizes, and the auxiliary gas device 6 is used for providing high-purity gas and dissolving the particles with tiny particle sizes to form dry aerosol with a solvent removed; the first analysis detector 5-1 is a nondestructive detection device, and specifically adopts a B-ray analyzer, an X-ray fluorescence spectrometer, a Raman spectrometer or an infrared gas analyzer; and the second analysis detector 5-2 is a destructive detection device, and specifically adopts an ICP-MS analyzer or an ICP-OES analyzer.
The dry-method inductively coupled plasma mass spectrometry analyzer also comprises an online weighing device 3, wherein the online weighing device 3 is connected with the membrane enrichment device 2; the online weighing device 3 is an in-situ mass detector.
The primary aerosol conversion device 1 realizes primary aerosol of a sample by adopting various modes according to the form (liquid, solid or gas) of the sample to be analyzed; the membrane enrichment device 2 is responsible for transmitting the primary aerosol containing the element to be detected to the filter membrane and realizing enrichment and concentration on the filter membrane, and mainly extracts the aerosol with large flow through an air pump, the gas diversion enables the substance to be detected to uniformly cover the filter membrane, and meanwhile, the online transmission function of the filter membrane between the position where the filter membrane is not enriched and the position where the secondary aerosol conversion device 4 is located is realized. The rear end of the membrane enrichment device 2 can be provided with an online weighing device 3 and a nondestructive testing device, the mass of the enriched particles can be obtained through online weighing, and the nondestructive testing device can implement in-situ mass detection to obtain the mass information of the main content elements. The secondary aerosol conversion device 4 is a (semi-) continuous measuring analyzer which excites the sample on the film to generate particles with tiny particle size, dissolves and mixes with high-purity gas to form dry aerosol with a desolvation, and forms an ICP-MS analysis method of dry enrichment by matching with the control of an ICP-MS sample injection system.
The utility model also provides an analytical method of dry process inductive coupling plasma mass spectrometry appearance, be applied to foretell dry process inductive coupling plasma mass spectrometry appearance, including following step:
the primary aerosol conversion device 1 is used for realizing primary aerosol of a sample to be analyzed by adopting various modes according to the form of the sample to be analyzed to form aerosol, wherein the form of the sample to be analyzed is liquid, solid or gas;
the membrane enrichment device 2 is responsible for transmitting the aerosol containing the element to be detected to the filter membrane and realizing enrichment and concentration on the filter membrane, the aerosol is mainly extracted at a large flow rate through an air extraction pump, and the aerosol is uniformly covered on the filter membrane through gas diversion to form a uniform particulate matter membrane;
the analysis detector I5-1 carries out in-situ quality detection on the particles on the particle film to obtain quality information of the main content elements;
the secondary aerosol conversion device 4 excites the particulate matter film to generate particles with micro-particle size, and the particles are dissolved with high-purity gas provided by the auxiliary gas device 6 to form dry aerosol with a solvent removed;
and (5) determining inorganic elements of the dry aerosol by using a second analysis detector 5-2 to obtain the content information of the trace elements.
Wherein, the utility model discloses can compatible survey solid, the survey of the inorganic element in the all kinds of samples of liquid, gaseous particulate matter. When the measured sample is solid, digestion is not needed, no liquid waste is generated, the environment is friendly, and the pollution problem caused by waste liquid is greatly reduced. According to the selection of the primary aerosol generation mode, the acquisition of sample element distribution information or sample depth element information can be carried out; when the liquid is measured, the solvent can be separated, the introduction of water and the solvent is greatly reduced, the ionization efficiency of the sample in the plasma is improved, and the salt resistance and the matrix resistance are improved. When the sample is measured to be the particles in the gas, the particles in the air can be directly enriched, and then the online analysis of the particle elements in the ambient air is realized through the secondary aerosol conversion device 4, so that the response speed of minute level can be realized.
The primary aerosol conversion device 1 adopts generation devices of different principles, including but not limited to direct atomization (multiple modes such as venturi principle and ultrasonic atomization) for liquid samples, laser excitation sputtering of solid samples, electrothermal evaporation and the like, so as to cover multiple sample forms. The primary aerosol conversion device 1 forms an aerosol having particles of 100 μm or less.
The on-line weighing device 3 adopts various particulate matter mass detection modes such as a balance, a surface wave, beta rays, light scattering and the like to obtain the total mass of the particulate matter.
The enriched sample is combined with other nondestructive monitoring methods to realize in-situ characterization, such as detection technologies of an X-ray fluorescence analyzer, a Raman analyzer, attenuated total reflection infrared and the like; in the secondary aerosol process, all the excitation of the aerosol is realized through various modes such as laser ablation, electrothermal evaporation, high-temperature heating blowing and the like. The online transmission function of the film enrichment device 2 provides the ICP-MS combined instrument with the hardware function of the dry enrichment ICP-MS (semi-) continuous determination analysis method.
The secondary aerosol conversion device 4 is completely denuded of the sample, and fractionation effect and matrix effect can be avoided.
One embodiment is shown in FIG. 2:
aiming at the test of trace elements in a high-temperature alloy sample, an ICPMS (Integrated micro-tandem System) analyzer enriched by a dry method is adopted for analysis: firstly, fixing a high-temperature alloy sample on a three-dimensional moving sample table of a primary aerosol conversion device 1, namely a laser induced ablation device, adjusting corresponding power, focus, pre-ablation and ablation times, continuously beating ablation and sputtering particles with small particle sizes, extracting the particles by a film enrichment device 2 along with high-purity gas (nitrogen or argon) and uniformly loading the particles on a filter membrane to form a uniformly distributed membrane sample to be tested, directly testing the total mass m (g) of the sample enriched on the filter membrane by using an in-situ mass tester with on-line detection, namely beta-ray in-situ analysis, and simultaneously testing the mass (mu g) of a macroelement in the membrane sample by using an X-ray fluorescence spectrometer in a nondestructive test mode, thereby calculating the mass concentration (mu g/g) of the element; and then, the membrane sample is transmitted to a secondary aerosol conversion device 4, namely a laser induced denudation device, the secondary aerosol conversion device is completely excited to form aerosol along with the purging of high-purity argon, the secondary aerosol conversion device is connected with a sample introduction system of an ICPMS analyzer, the content of the trace elements in the sample is analyzed by a mass spectrum detector, and finally, the total content information of the main content elements and the trace elements in the sample is obtained.
Compared with the traditional wet method, the introduction of digesting agents such as hydrochloric acid and nitric acid and water is avoided, the mass spectrum interference caused by the introduction is greatly reduced, for example, when the wet method is used for dissolving and testing the high-temperature alloy, the mass spectrum interference of the MOO to the Cd covers the isotopes such as 111, 112 and 114 of the Cd, so that the test result of the Cd is higher, and the test is carried out after the dry enrichment, on one hand, the introduction of O is avoided, on the other hand, the Cd with very low content is enriched to a certain extent, the measurement detection limit is reduced, and the analysis precision is improved; meanwhile, complicated steps in the digestion method are saved, and labor and reagent pollution of acid reagents are saved; in addition, the aerosol directly entering the analyzer is a secondary aerosol conversion device for enriching the film sample, so that the entrance of a large number of metal matrixes is avoided, the matrix effect is small in the mass spectrometry process, the excitation efficiency is increased, and the fractionation effect is completely avoided. Wherein, the selection of the standard sample can be carried out by adopting a corresponding standard solution, thereby avoiding the calibration of a solid sample,
example two
The main raw material of the semiconductor gallium arsenide material is high-purity gallium, the requirement on the purity of the high-purity gallium is higher and higher along with the deep research of optoelectronic devices, ultra-high-speed integrated circuits and the like, the requirement on the purity of the high-purity gallium is 99.9999-99.99999%, the detection method for trace elements in the high-purity gallium is ICP-MS, only 99.99-99.999% of the trace elements in the high-purity gallium can be detected by directly using a single-four-level rod ICPMS through a certain pretreatment method (modes such as removing Ga in the digestion process) in a laboratory at present, the requirement on the detection of the trace elements in the high-purity gallium with the purity of more than 6N can not be basically met, and the ICPMS analysis method adopting the dry sampling after enrichment can achieve better experimental effect.
The melting point of high-purity gallium is low, and the high-purity gallium is not beneficial to direct solid aerosol gelation, so that wet dissolution is firstly carried out, a sample liquid to be tested dissolved in hydrochloric acid is used as a solution of primary aerosol, a basic atomizer is adopted for atomization to form aerosol, after enrichment is carried out by a membrane enrichment device, uniform salt is formed on a filter membrane, the volume of membrane enrichment can be set, a membrane sample is subjected to secondary impact by laser-induced ablation to form aerosol, the aerosol is mixed with high-purity argon gas and enters a sample injection system of an ICPMS, and the impurity elements are measured.
Firstly, weighing 1g of high-purity gallium sample, dissolving the high-purity gallium sample, and then fixing the volume in a 100mL volumetric flask to obtain a solution to be measured; then, after a standard solution A (mg/L) of an element to be detected is enriched through a membrane enrichment device and is excited into an ICPMS for the second time, the element mass (g) is taken as a horizontal coordinate, the signal intensity is taken as a vertical coordinate, and a working curve is drawn; in the testing process, the concentration multiple can be determined according to the adjustment of the sample volume of the solution to be tested, then the quality of the element to be tested after concentration is obtained, the requirement of testing pg/g-ng/g-level impurities can be met, and the lower limit of the measurement of the single quadrupole ICPMS is further reduced.
In addition, aiming at the particulate matter sample in the gas phase, the utility model can also directly perform enrichment analysis, and has extremely wide application prospect; and, to solid, liquid, air particle sample, the utility model discloses all can adopt standard solution to calibrate, very big reduction to the reliance of all kinds of standards. In addition, an online weighing device is configured, so that the trace weighing requirement can be met, and the online weighing device can be used together with other various nondestructive testing methods.
The utility model provides a dry process inductively coupled plasma mass spectrometry combined analyzer, to solid sample, liquid sample or gas sample, at first realize the aerosol of one time to the sample that awaits measuring, then through enrichment concentration, and then secondary excitation forms the secondary aerosol who removes the solvent, forms combined analyzer with inductively coupled plasma mass spectrograph, realizes the detection of impurity element in complicated base member and the high-purity sample; the utility model can realize enrichment and concentration of the sample to be detected through the membrane enrichment device, and excite the enriched sample again through the aerosol secondary excitation device, can improve the detection limit, and can be applied to impurity determination of semiconductor ultra-pure materials or reagents; the utility model relates to a membrane enrichment device, which can realize in-situ online real-time weighing, greatly improve the accurate and quantitative analysis capability and the stability of data; the utility model relates to a combination analyzer with enrichment function can realize the combination with other various detection methods, including but not limited to X-ray fluorescence analyzer, raman analyzer, infrared analyzer, etc.; the secondary aerosol conversion device can completely degrade the sample, so that the fractionation effect and the matrix effect are completely avoided; the utility model discloses can use standard solution to carry out entire system's calibration, great having broken away from the reliance to the solid standard sample, realized using standard solution calibration for the first time, can realize the test to different base member solid sample, need not to clear up to the solid sample, no liquid waste's production, environment friendly, greatly reduced the pollution problem that the waste liquid brought.
The principle and the implementation of the present invention are explained herein by using specific examples, and the above description of the embodiments is only used to help understand the method and the core idea of the present invention; meanwhile, for the general technical personnel in the field, according to the idea of the present invention, there are changes in the concrete implementation and the application scope. In summary, the content of the present specification should not be construed as a limitation of the present invention.
Claims (5)
1. The utility model provides a dry process inductively coupled plasma mass spectrometry appearance, its characterized in that includes: the device comprises a primary aerosol conversion device (1), a membrane enrichment device (2) and a secondary aerosol conversion device (4) which are sequentially connected, wherein the primary aerosol conversion device (1), the membrane enrichment device (2) and the secondary aerosol conversion device (4) are respectively connected with an auxiliary gas device (6), the membrane enrichment device (2) is connected with a first analysis detector (5-1), and the secondary aerosol conversion device (4) and the auxiliary gas device (6) are connected with a second analysis detector (5-2);
the primary aerosol conversion device (1) is used for realizing primary aerosol of a sample to be analyzed to form aerosol; the membrane enrichment device (2) is provided with a filter membrane and is used for intercepting formed aerosol and carrying out enrichment concentration to form a uniform particulate matter membrane, the secondary aerosol conversion device (4) is used for exciting the particulate matter membrane to generate particles with tiny particle sizes, and the auxiliary gas device (6) is used for providing high-purity gas and is dissolved with the particles with tiny particle sizes to form dry aerosol with a desolventizing agent; the first analysis detector (5-1) is a nondestructive detection device, and specifically adopts a B-ray analyzer, an X-ray fluorescence spectrometer, a Raman spectrometer or an infrared gas analyzer; and the second analysis detector (5-2) is a destructive detection device, and specifically adopts an ICP-MS analyzer or an ICP-OES analyzer.
2. The dry inductively coupled plasma mass spectrometry of claim 1, further comprising an online weighing device (3), wherein the online weighing device (3) is connected to the membrane enrichment device (2); the online weighing device (3) is an in-situ mass detector.
3. The dry inductively coupled plasma mass spectrometry of claim 1, wherein the primary aerosol conversion device (1) is a laser-induced ablation device.
4. The dry inductively coupled plasma mass spectrometry of claim 1, wherein the secondary aerosol conversion device (4) is a laser-induced ablation device.
5. The dry inductively coupled plasma mass spectrometer of claim 1, wherein the high purity gas is high purity argon or helium.
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