CN110749577A - Automatic alignment method for optical path of hollow cathode spectrometer - Google Patents

Automatic alignment method for optical path of hollow cathode spectrometer Download PDF

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Publication number
CN110749577A
CN110749577A CN201910618479.8A CN201910618479A CN110749577A CN 110749577 A CN110749577 A CN 110749577A CN 201910618479 A CN201910618479 A CN 201910618479A CN 110749577 A CN110749577 A CN 110749577A
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intensity
hollow cathode
light
spectrometer
value
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李帆
丁妍
刘颖韬
杨党纲
王东升
王强
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AECC Beijing Institute of Aeronautical Materials
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/0205Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28Investigating the spectrum
    • G01J3/443Emission spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/12Circuits of general importance; Signal processing
    • G01N2201/127Calibration; base line adjustment; drift compensation

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention relates to an automatic alignment method for an optical path of a hollow cathode spectrometer, which comprises the steps of exciting a hollow cathode graphite electrode inserted on a cathode tungsten filament of a hollow cathode lamp to emit light, detecting the light intensity emitted by the graphite electrode by a spectrometer while moving a translation system for clamping the hollow cathode lamp, and judging the optimal position for the alignment of the optical path and the light emission of a sample by calculating and processing light intensity signals. The method can automatically align the light path of the hollow cathode spectrometer with the light emitting position of the sample, and has the advantages of convenient operation, high efficiency and accurate alignment of the light path.

Description

Automatic alignment method for optical path of hollow cathode spectrometer
Technical Field
The invention discloses an automatic alignment method for an optical path of a hollow cathode spectrometer, and belongs to the technical field of spectral analysis.
Background
The hollow cathode spectrometer is a quantitative detection device for trace and ultra-trace elements by directly injecting solid samples, has high sensitivity, high accuracy and simple operation, the solid samples do not need any chemical pretreatment, the chip-shaped samples are directly injected and placed in a graphite electrode and inserted into a cathode tungsten filament of a hollow cathode lamp, a light source system is introduced with current, argon and water to realize low-voltage glow discharge luminescence, and the spectrometer performs light splitting and detection on light emitted by the samples, thereby detecting the types and the content of the elements in the samples.
In the detection process, in order to achieve stability of analysis data, the light emission of the sample and the light path of the spectrometer need to be kept at the optimal position, namely the light collected by the spectrometer is always the strongest light of the light emitted by the sample, so that the light path of the spectrometer and the light emitted by the sample are required to be completely aligned. However, due to assembling of the spectrometer, processing of the graphite electrode and assembling and processing deviation of the glass hollow cathode lamp, a focusing position of a sample after light emission slightly deviates from a light path, so that the stability of an analysis result is poor.
Disclosure of Invention
The invention provides an automatic alignment method for the optical path of a hollow cathode spectrometer, which is designed aiming at the prior art, and aims to automatically perform optical path fine adjustment to realize automatic optical path alignment when an electrode and a sample are changed every time, so that the analysis stability is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the automatic alignment method for the optical path of the hollow cathode spectrometer is characterized by comprising the following steps: the method comprises the following steps:
exciting the hollow cathode graphite electrode 16 to emit light and irradiating the light on the light splitting system 8 of the emission spectrometer 10;
the intensity of the light split by the light splitting system 8 is detected by the spectrometer detection system 9 of the emission spectrometer 10 and the position of the hollow cathode graphite electrode 16 is adjusted to maximize the detected intensity of the light.
In one implementation, the hollow bore of the hollow cathode graphite electrode 16 contains a test sample in the form of powder or chips. When no sample exists in the hollow cathode graphite electrode 16, the hollow cathode light source 11 is excited, the graphite electrode 16 emits light, and the light emitted by the graphite electrode 16 is detected by the photomultiplier at the moment; when a sample exists in the hollow cathode graphite electrode 16, the hollow cathode light source 11 is excited, the graphite electrode 16 and the sample in the hollow cathode light, and the photomultiplier detects the light emitted by the graphite electrode and the sample.
In one implementation, the detected light intensity is the zero-order light intensity directly reflected by the grating, the light intensity emitted by the test sample substrate, the background light intensity emitted by the hollow cathode light source 11, or the C element line intensity emitted by the graphite electrode 16.
In one implementation, the detector installed in the spectrometer detection system 9 is a photomultiplier tube or a CCD.
In one implementation, the negative high voltage of a photomultiplier tube for collecting zero-order light directly reflected by the grating is-300V to-460V; the photomultiplier for collecting zero-order light has too low negative high voltage, the collected signal is unstable, and the signal fluctuation influences the judgment of the optimal position; the negative high voltage is too high, the signal of the photomultiplier is saturated, the judgment of the optimal position cannot be carried out, and the negative high voltage is-300V to-460V according to the experimental result, so that the judgment of the optimal range of zero-order light is most sensitive and accurate;
in one implementation, the negative high voltage of the photomultiplier tube for collecting the light intensity emitted by the test sample substrate is-300V to-760V;
in one implementation, the negative high voltage of the photomultiplier tube, which collects the intensity of the background light emitted by the hollow cathode light source 11, is-500V to-900V in one implementation; the negative high voltage of the photomultiplier for collecting the C element spectral line intensity emitted by the graphite electrode 16 is-300V to-700V.
In one embodiment, the hollow cathode graphite electrode 16 is positioned in a plane perpendicular to the light axis 7 of the hollow cathode light source by moving in a direction perpendicular to each other and simultaneously measuring the light intensity.
Further, the movement in the mutually perpendicular direction is a movement in a horizontal or vertical direction.
In the above embodiment, the moving pitch is 0.05mm to 0.3mm, and the moving speed is 5 steps/s to 20 steps/s. The principle of moving step distance adjustment is to ensure the efficiency and accuracy of automatic alignment of the light path. The step pitch is too high, the cost is high, and the speed is slow; if the step pitch is too low, the focusing effect is poor, and the optimum range is likely to be not found. According to the experimental result, the effect that the moving step distance is selected to be 0.05 mm-0.3 mm is optimal;
the moving speed is related to the analysis efficiency and the analysis accuracy, the moving speed is too low, the automatic alignment speed of the light path is low, the analysis speed of the hollow cathode is low, the pre-excitation time of the sample is easy to be too long, and the intensity of the analysis element spectral line is not detected in time and lost when the analysis element spectral line is measured formally; the moving speed is too high, the detection speed of the photomultiplier of the emission spectrometer 10 cannot follow the moving speed, so that the detection cannot be performed in a certain translation position, the automatic alignment of the optical path is inaccurate, and even the automatic alignment of the optical path fails;
in the above embodiment, the maximum moving distance of the movement is set to be 10 seconds after the measured light intensity change has four intensity value mutations, or the movement has only one intensity value mutation within 1 minute, or no intensity value mutation position within 1 minute.
In the above embodiment, the maximum moving distance of the movement is set to be an optimum position at the middle position of the positions corresponding to the second intensity numerical mutation 2 and the third intensity numerical mutation 3 after four intensity numerical mutations appear in the measured light intensity change;
and if the intensity numerical mutation only occurs once within 1 minute or does not occur within 1 minute, prompting the light path automatic alignment failure information.
In the above implementation, the mutation of the intensity value is judged in the following manner:
in the continuous moving process, synchronously acquiring light intensity signals, and judging that the intensity value mutation begins to occur when the difference value between the maximum value or the minimum value of the measured intensity value within 5-10 seconds and the average value of the measured intensity value within 5-10 seconds is more than or equal to 5% -15% of the average value; in the subsequent moving process, when the difference between the maximum value and the minimum value of the measured intensity values within 5-10 seconds and the average value of the measured intensity values within 5-10 seconds is less than 5% -15% of the average value, the intensity value mutation is ended, and the middle position of the moving distance in the time from the beginning of the intensity value mutation to the end of the intensity value mutation is set as the position of the intensity value mutation.
The detected light may be zero order light. When the sample is nickel-based, a spectral line of Ni can be used, when the sample is iron-based, a spectral line of Fe is used, and so on, and an insensitive spectral line of a matrix is generally selected; a background position in the spectrum emitted by the hollow cathode light source 11 can also be selected, and the background position should not overlap with or interfere with the wavelength of the emitted spectral line of the matrix and other alloy elements in the sample; or the C element line intensity emitted by the graphite electrode 16. In the moving process, the measured light intensity can be increased along with the gradual alignment with the positive center of the light path and then reduced along with the deviation from the positive center of the light path, so that the optimal position aligned with the light path is obtained, and after the light path is moved to the optimal position, the light path is aligned, so that the aim of aligning the light path is fulfilled.
Drawings
FIG. 1 is a graph of intensity signals collected by a spectrometer moving in a single direction
FIG. 2 is a schematic diagram of a combination structure of a hollow cathode light source and an emission spectrometer
In the figure: 1-first numerical mutation, 2-second numerical mutation, 3-third numerical mutation, 4-fourth numerical mutation; 5-hollow cathode lamp; 6-a clamping translation system; 7-the direction of the axis of the light of the hollow cathode light source; 8-a light splitting system; 9-spectrometer detection system; 10-an emission spectrometer; 11-a hollow cathode light source; 12-a waterway system; 13-a gas path system; 14-circuitry; 15-computer and control system; 16-a graphite electrode; 17-tungsten filament.
Detailed Description
The technical scheme of the invention is further detailed in the following by combining the drawings and the embodiment:
referring to fig. 2, the hollow cathode light source and spectrometer combined structure for implementing the method of the present invention comprises a lens system, a collimating lens system, and an entrance slit, an emission spectrometer 10 comprises a light splitting system 8 and a spectrometer detection system 9, the light splitting system 8 is a plane grating or a concave grating or a echelle grating system, and the spectrometer detection system 9 is a photomultiplier tube or a CCD detector or a CID detector. The hollow cathode light source 11 comprises a hollow cathode lamp 5, and the hollow cathode lamp 5 comprises a graphite electrode 16 and a tungsten filament 17. In addition, the hollow cathode light source 11 further comprises a water path system 12, an air path system 13 and an electric circuit system 14; the clamping translation system 6 clamps the hollow cathode lamp 5 for adjusting the position of the hollow cathode graphite electrode 16 by moving in mutually perpendicular directions on a plane perpendicular to the light axis direction 7 of the hollow cathode light source and simultaneously measuring the light intensity.
The operation steps of automatically aligning the optical path of the hollow cathode spectrometer are as follows:
the method comprises the following steps: weighing 0.05g of nickel-based alloy sample chips, placing the nickel-based alloy sample chips in a hollow hole of a hollow cathode graphite electrode 16, inserting the graphite electrode 16 on a cathode tungsten wire 17 of a hollow cathode lamp 5, starting a hollow cathode light source 11 under the control of a light source circuit system 14, an air circuit system 13, a water circuit system 12 and a control system 15, exciting the graphite electrode 16, and then exciting the graphite electrode 16 to emit light;
step two: the light emitted by the graphite electrode 16 irradiates the light splitting system 8 of the emission spectrometer 16 through the optical path of the spectrometer 10;
step three: a photomultiplier detector in the spectrometer detection system 9 detects the intensity of light split by the light splitting system at the C193.0nm, and the negative high voltage of the photomultiplier is-600V;
step four: the control system 15 controls the clamping translation system 6 for clamping the hollow cathode lamp 5 to horizontally move in the direction 7 vertical to the axis of the hollow cathode light source, the translation system moves to the translation initial position according to the set translation initial position, then moves at 8 steps/s according to the translation step pitch of the translation system 6, the light intensity at the position of C193.0nm is measured, the difference value between the maximum value and the minimum value of the intensity values in every 6 seconds and the average value of the intensity values measured in the 6 seconds is calculated in real time, and the ratio of the maximum value and the minimum value of the intensity values in the 6 seconds to the average value in the 6 seconds is calculated;
step five: calculating the translation distance by using the translation step distance, the translation speed and the translation time of the translation system 6, drawing a graph as shown in fig. 1 by using the translation distance as an abscissa and the acquired light intensity as an ordinate, judging that an intensity value abrupt change starts to occur when the difference between the maximum value or the minimum value of the intensity values measured in 6 seconds and the average value of the intensity values measured in the 6 seconds is more than or equal to 10% of the average value during the continuous movement of the translation system for clamping the hollow cathode lamp, setting the intensity value abrupt change to end when the difference between the maximum value and the minimum value of the intensity values measured in the 6 seconds and the average value of the intensity values measured in the 6 seconds is less than 10% of the average value during the subsequent movement of the translation system and the measurement of the light intensity, and setting the middle position of the distance moved by the translation system in the time change from the intensity value abrupt change starting to occur to the end of the intensity value abrupt change as the position of the intensity value abrupt change. Figure 1 shows four intensity value mutations. The second intensity value mutation 2 and the third intensity value mutation 3 are centered at the optimal positions. The translation system 6 moves horizontally to this optimal position.
Then the control system controls the translation system for clamping the hollow cathode lamp to move up and down in the direction vertical to the axis of the hollow cathode light source, the translation system moves to the translation initial position according to the set translation initial position, then the translation system moves according to the step pitch of 0.08mm and the translation speed of 8 steps/s, and simultaneously the third step is carried out, the light intensity at the position of C193.0nm is measured, the difference value between the maximum value and the minimum value of the intensity value in every 6 seconds and the average value of the measured intensity values in the 6 seconds is calculated in real time and is divided by the average value in the 6 seconds, and whether the ratio is more than or equal to 5% -15% of the average value is judged;
step five: calculating the translation distance by using the translation system step distance, the translation speed and the translation time, drawing a graph as shown in figure 1 by using the translation distance as an abscissa and the acquired light intensity as an ordinate, judging that sudden intensity value change begins to occur when the difference between the maximum value or the minimum value of the intensity value measured in 6 seconds and the average value of the intensity values measured in the 6 seconds is more than or equal to 5% -15% of the average value in the continuous moving process of the translation system for clamping the hollow cathode lamp, finishing the sudden intensity value change when the difference between the maximum value and the minimum value of the intensity value measured in the 6 seconds and the average value of the intensity values measured in the 6 seconds is less than 5% -15% of the average value in the subsequent moving and light intensity measuring processes of the translation system, and setting the middle position of the moving distance of the translation system in the time change from the sudden intensity value change beginning to the end of the sudden intensity value change as the sudden intensity value change Location. Figure 1 shows four intensity value mutations. The second intensity value mutation and the third intensity value mutation center at the optimal position. The translation system 6 moves up and down to this optimal position.
By the mode, the light emission of the hollow cathode lamp of the hollow cathode spectrometer is automatically, simply and accurately aligned with the light path of the spectrometer.

Claims (11)

1. A method for automatically aligning the optical path of a hollow cathode spectrometer is characterized by comprising the following steps: the method comprises the following steps:
exciting the hollow cathode graphite electrode (16) to emit light and irradiating the light on a light splitting system (8) of the emission spectrometer (10);
the intensity of the light split by the light splitting system (8) is detected by a spectrometer detection system (9) of the emission spectrometer (10), and the position of the hollow cathode graphite electrode (16) is adjusted to maximize the intensity of the detected light.
2. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 1, wherein: the hollow hole of the hollow cathode graphite electrode (16) is filled with a test sample in the form of powder or chips.
3. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 1, wherein: the detected light intensity is zero-order light intensity directly reflected by the grating, light intensity emitted by a test sample substrate, background light intensity emitted by the hollow cathode light source (11) or C element spectral line intensity emitted by the graphite electrode (16).
4. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 1, wherein: the detector arranged in the spectrometer detection system (9) is a photomultiplier or a CCD.
5. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 3, wherein:
the negative high voltage of a photomultiplier for collecting zero-order light directly reflected by the grating is-300V to-460V;
the negative high voltage of a photomultiplier for collecting the light intensity emitted by a test sample matrix is-300V to-760V;
the negative high voltage of a photomultiplier for collecting the background light intensity emitted by the hollow cathode light source (11) is-500V to-900V; the negative high voltage of the photomultiplier for collecting the C element spectral line intensity emitted by the graphite electrode (16) is-300V-700V.
6. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 1, wherein: the position of the hollow cathode graphite electrode (16) is adjusted on a plane vertical to the axial direction (7) of the hollow cathode light source, and the position is moved in the mutually vertical directions to synchronously measure the light intensity.
7. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 6, wherein: the movement in the mutually perpendicular direction is a movement in a horizontal or vertical direction.
8. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 6 or 7, wherein: the moving step pitch is 0.05 mm-0.3 mm, and the moving speed is 5 steps/s-20 steps/s.
9. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 6 or 7, wherein: the maximum moving distance of the movement is set to be that the movement is continued for 10 seconds after four intensity value mutations occur in the measured light intensity change, or the intensity value mutations occur only once within 1 minute, or the intensity value mutation position does not occur within 1 minute.
10. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 9, wherein: the maximum moving distance of the movement is set to be the optimal position of the middle position of the positions corresponding to the second intensity numerical mutation (2) and the third intensity numerical mutation (3) after the measured light intensity change has four intensity numerical mutations;
and if the intensity numerical mutation only occurs once within 1 minute or does not occur within 1 minute, prompting the light path automatic alignment failure information.
11. The method for automatically aligning the optical path of the hollow cathode spectrometer as claimed in claim 9, wherein: the mutation of the intensity value is judged in the following way:
in the continuous moving process, synchronously acquiring light intensity signals, and judging that the intensity value mutation begins to occur when the difference value between the maximum value or the minimum value of the measured intensity value within 5-10 seconds and the average value of the measured intensity value within 5-10 seconds is more than or equal to 5% -15% of the average value; in the subsequent moving process, when the difference between the maximum value and the minimum value of the measured intensity values within 5-10 seconds and the average value of the measured intensity values within 5-10 seconds is less than 5% -15% of the average value, the intensity value mutation is ended, and the middle position of the moving distance in the time from the beginning of the intensity value mutation to the end of the intensity value mutation is set as the position of the intensity value mutation.
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Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2327752A1 (en) * 1973-05-30 1974-12-05 Beckman Instruments Gmbh LIGHTING SYSTEM FOR AN ATOMIC ABSORPTION SPECTRALPHOTOMETER
CN102866138A (en) * 2012-09-13 2013-01-09 北京瑞利分析仪器有限公司 Four-quadrant detector-based auxiliary system and method for atomic fluorescence hollow cathode lamp
CN106678007A (en) * 2016-11-17 2017-05-17 上海空间推进研究所 Intelligent cathode moving device
CN106783519A (en) * 2016-12-06 2017-05-31 中国航空工业集团公司北京航空材料研究院 A kind of excitation light source device

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Application publication date: 20200204