CN117092051B - Atomic absorption spectrum measuring device and method - Google Patents
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- 238000000862 absorption spectrum Methods 0.000 title claims abstract description 20
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- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 28
- 238000001479 atomic absorption spectroscopy Methods 0.000 claims description 10
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- 238000005259 measurement Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000004847 absorption spectroscopy Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
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- 230000007613 environmental effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
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Abstract
An atomic absorption spectrum measuring device and method, the device includes gaseous atomic generating module, light path detection module, multi-way pool module, signal processing module, gaseous atomic generating module is used for converting solid sample into gaseous atomic beam distributed in vacuum cavity; the optical path detection module is used for transmitting detection light passing through the gaseous atomic beam to the vacuum cavity and receiving the light beam passing through the gaseous atomic beam to form an electric signal; the multi-pass pool module is used for outputting the detection light after passing through the gaseous atomic beams in the vacuum cavity for a plurality of times; the signal processing module is used for processing the electric signals and analyzing the types and the concentrations of the samples. According to the invention, by arranging the multi-pass cell module, the interaction path length between the gaseous atoms and the detection light is effectively increased, the absorption times of the atoms are effectively increased by the multi-pass cell module, and compared with direct absorption, the spectrum signal intensity is greatly improved, so that the detection sensitivity of the system can be effectively improved.
Description
Technical Field
The invention relates to the technical field of spectrum measurement, in particular to a device and a method for improving the measurement sensitivity of atomic absorption spectroscopy.
Background
The metal isotope analysis has important research significance in archaeological and nuclear forensic analysis, and is widely used in biological, environmental, geological and food detection. The existing isotope analysis method is mainly divided into mass spectrometry and spectrum technology, and the mass spectrometry technology realizes isotope distinction through different nuclear mass ratios among isotopes, obtains isotope ratio information of a sample to be detected and the like, has high detection sensitivity, is limited by huge instrument volume and complex sample pretreatment process, and is difficult to adapt to work in an external field test environment. Spectroscopic techniques exhibit spectral frequency shifts based on the differences in the fine structure of the absorption spectrum between isotopes. Therefore, the target absorption band can be scanned by a tunable absorption spectrum technology to obtain the isotope absorption spectrum with high spectral resolution, so that the isotope ratio information is inverted. The isotope detection method based on the tunable absorption spectrum technology has the advantages of being simple in device, high in spectrum resolution, suitable for on-site rapid deployment and the like. In the current research, isotope abundance information is mainly obtained by a direct absorption spectrum technology, and is only suitable for detecting samples with higher concentration, and accurate isotope ratio information is difficult to obtain for detecting samples with low content (average content is about 1-100 mg per kilogram) such as ores, soil and the like.
Disclosure of Invention
In order to solve the problem that in the detection of a low-concentration sample, the traditional atomic direct absorption spectrum cannot detect a spectrum signal with ideal signal intensity, so that accurate sample information is difficult to obtain. The invention provides a device and a method for improving the measurement sensitivity of atomic absorption spectroscopy, and the specific technical scheme is as follows:
an atomic absorption spectrometry apparatus comprising:
the gaseous atom generating module is used for converting the solid sample into gaseous atom beams distributed in the vacuum cavity;
the optical path detection module is used for transmitting detection light passing through the gaseous atomic beam to the vacuum cavity and receiving the light beam passing through the gaseous atomic beam and forming an electric signal;
the multi-pass pool module is used for outputting the detection light after passing through the gaseous atomic beams in the vacuum cavity for a plurality of times;
and the signal processing module is used for processing the electric signals and analyzing the types and the concentrations of the samples.
Optionally, the position of the multi-pass pool module relative to the multi-pass pool module is adjustable.
Optionally, the multi-way pool module comprises a first spherical mirror and a second spherical mirror which are oppositely arranged at two sides of the vacuum cavity, and a protective film is plated on the surface of the spherical mirror.
Optionally, the gaseous atom generating module includes:
an atomic generator for gasifying a sample to generate an atomic beam;
and a current source connected to the atomic generator such that the atomic generator heats the sample to generate a gaseous atomic beam.
Optionally, the gaseous atom generating module further comprises an infrared thermometer for detecting the temperature of the atom generator.
Optionally, the position of the vacuum chamber is adjustable.
Optionally, the optical path detection module includes:
a detection laser for generating detection light of different frequencies for different samples;
a lens for condensing the probe light;
and the photoelectric detector is used for receiving the detection light passing through the vacuum cavity and generating an electric signal.
Optionally, the optical path detection module further includes an indication laser, and the light beams emitted by the indication laser and the detection laser pass through a lens, and are used for emitting visible laser to assist in optical path adjustment.
Optionally, the signal processing module includes:
the signal acquisition card is used for acquiring the electric signals of the spectrum corresponding to the photoelectric detector;
and the computer is used for processing the electric signals output by the signal acquisition card.
The method for using the atomic absorption spectrometry device comprises the following steps:
placing a sample in the gaseous atom generating module to generate gaseous atom beams, wherein the gaseous atom beams are dispersed in the vacuum cavity;
the optical path detection module is used for selecting and outputting detection light with set wavelength, moving out of the multi-pass pool module, adjusting the positions of the vacuum cavity in the transverse direction and the longitudinal direction, acquiring the absorption spectrum intensity of the gaseous atomic beam at each spatial position of the vacuum cavity, and determining the spatial distribution characteristics of the gaseous atomic beam according to the intensity distribution characteristics;
according to the spatial distribution characteristics of atoms, a multi-pass pool module is placed at a first position, wherein the first position is the position with the largest concentrated distribution intensity of gaseous atomic beams, and the specific positions of all components in the device are determined;
and placing the sample in the atom generating module again, starting the light path detection module, acquiring the isotope spectrum passing through the multi-pass cell module, and acquiring the isotope ratio of the sample according to the difference of the absorption peak intensities of isotopes.
The invention has the advantages that:
(1) According to the invention, by arranging the multi-pass cell module, the interaction path length between the gaseous atoms and the detection light is effectively increased, the absorption times of the atoms are effectively increased by the multi-pass cell module, and compared with direct absorption, the spectrum signal intensity is greatly improved, so that the detection sensitivity of the system can be effectively improved.
(2) The position of the multi-pass pool module is adjustable, and the multi-pass pool module can be supported when moving to the position with the maximum intensity of the gaseous atomic beam.
(3) The arrangement of the first spherical mirror and the second spherical mirror and the plating of the protective film on the surface of the device can enhance the reflectivity and durability of the device in an open environment.
(4) Based on the position adjustable of vacuum cavity, can acquire gaseous atomic beam's absorption spectrum intensity in each spatial position of vacuum cavity under the circumstances that other parts in the device are not removed, confirm gaseous atomic beam's spatial distribution characteristic according to intensity distribution characteristic.
(5) The setting of the indicator laser may be used to assist in the adjustment of the optical path, including placing a spherical mirror in the multipass cell module in place.
(6) The device is simple, the cost is low, the environmental robustness is strong, and the detection of any sample information can be realized by selecting a laser with a proper wave band.
Drawings
FIG. 1 is a diagram of an open type multi-pass cell atomic absorption spectrometry device according to an embodiment of the present invention;
fig. 2 is a schematic diagram of an open type multi-pass cell in an open type multi-pass cell atomic absorption spectrometry device according to an embodiment of the present invention;
FIG. 3 is a graph showing the distribution of the intensity of a gaseous atomic beam longitudinally distributed in the spatial distribution of the gaseous atomic beam obtained by direct absorption spectroscopy according to an embodiment of the present invention;
FIG. 4 is a graph showing the distribution of the intensity of a transverse distribution of gaseous atomic beams in the spatial distribution of gaseous atomic beams obtained by direct absorption spectroscopy according to an embodiment of the present invention;
FIG. 5 is a diagram showing an optimal spot profile of an open-type multi-pass cell module according to the distribution characteristics of atoms according to an embodiment of the present invention;
fig. 6 is a schematic diagram of spectrum measurement results compared with a conventional direct absorption spectroscopy apparatus according to an embodiment of the present invention.
In the figure:
1. a detection laser; 2. an indication laser; 3. a lens; 4. a first mirror; 5. a second mirror; 6. a first spherical mirror; 7. a second spherical mirror; 8. an atom generator; 9. a vacuum chamber; 10. a vacuum pump; 11. a current source; 12. an infrared thermometer; 13. a photodetector; 14. a data acquisition card; 15. and a computer.
Detailed Description
In the research of the metal isotopes at present, the isotope abundance information is mainly obtained by a direct absorption spectrum technology, and is only suitable for the detection of samples with higher concentration, but the technology is difficult to obtain accurate isotope ratio information in the detection of samples with low content (the average content is about 1-100 mg per kilogram) in ores, soil and the like.
The multi-pass cell technology can effectively enhance the signal intensity of a spectrum by increasing the action range of a substance to be detected and detection light, thereby improving the detection sensitivity of the system. The conventional intracavity multipass cell is applied to certain difficulties existing in metal abundance information measurement, such as: the metal vapor can cause the loss of the high-reflectivity reflector of the multi-pass pool, the spatial distribution characteristics of the metal vapor are not clear, and the problems of effective signal amplification and the like are difficult to realize.
In order to be suitable for detection of low-concentration solid metal isotope abundance, concentration information and the like, as shown in fig. 1, the application provides an atomic absorption spectrum measuring device, which comprises a gaseous atom generating module, an optical path detecting module, a multi-pass pool module and a signal processing module, wherein the gaseous atom generating module is used for converting a sample into gaseous atom beams distributed in a vacuum cavity; the optical path detection module is used for emitting detection light passing through the gaseous atomic beam to the vacuum cavity, receiving the light beam passing through the gaseous atomic beam and forming an electric signal; the multi-pass pool module is used for outputting the detection light after passing through the gaseous atomic beam in the vacuum cavity repeatedly; the signal processing module is used for processing the electric signals and analyzing the types and the concentrations of the samples. As shown in fig. 1, the optical path detection module includes a detection laser 1, a lens 3, and a photodetector 13. The gaseous atom generating module comprises an atom generator 8, a vacuum chamber 9, and a current source 11. The multi-pass pool module comprises a first spherical mirror 6 and a second spherical mirror 7, and the signal processing module comprises a data acquisition card 14 and a computer 15.
The detection laser 1 selects proper model and wavelength according to the spectral line characteristics of the absorption spectrum of the detection metal to completely cover the absorption spectrum of the target element.
Optionally, the optical path detecting module further includes a mirror assembly for converting an optical path of the detected light, and in this embodiment, the optical path detecting module includes a first mirror 4 and a second mirror 5 disposed along the optical path. The present application is not limited to mirror assemblies, and other numbers of mirrors may be provided, as the mirror assemblies may be eliminated when the position meets the requirements.
Optionally, the optical path detection module further comprises an indication laser 2, which can be used to assist in the adjustment of the optical path.
The beam emitted by the detection laser 1 is condensed by the lens 3 and then passes through the vacuum cavity 9 after passing through the reflecting mirror component, and the other side of the vacuum cavity 9 is provided with a photoelectric detector 13 for receiving the detection light and generating an electric signal for receiving the detection light passing through the vacuum cavity 9 and outputting the electric signal to the signal processing module for processing.
The atomic generator 8 in the gaseous atomic generation module is connected with the current source 11 and is used for heating the sample to generate stable gaseous atomic beams, the atomic generator 8 is integrated in the vacuum cavity 9, and the gaseous atomic beams are distributed at different spatial positions in the vacuum cavity.
Optionally, the gaseous atomic generating module further includes a vacuum pump 10, which is configured to ensure the vacuum degree of the vacuum cavity 9, and the vacuum pump 10 is configured to make the gaseous atomic beam more dispersed in the vacuum cavity during the process of vacuumizing the vacuum cavity 9. While the vacuum chamber 9 may be maintained in a certain vacuum state, the vacuum pump 10 may not be an essential device in the apparatus, and thus, it is also an embodiment that the apparatus does not include the vacuum pump 10.
Optionally, the position of the vacuum chamber 9 is adjustable, and the vacuum chamber 9 is stepped each time by a set distance in the transverse direction and the longitudinal direction, in this case, 5mm each time;
optionally, the gaseous atom generating module further includes an infrared thermometer 12 for monitoring the temperature of the atom generator 8, and the detection laser 1 and the current source 11 make appropriate adjustments according to the absorption spectrum characteristics and the thermal decomposition temperature of the sample to be detected.
The first spherical mirror 6 and the second spherical mirror 7 of the multi-pass pool module are oppositely arranged on two sides of the vacuum cavity 9, the arrangement of the first spherical mirror 6 and the second spherical mirror 7 can enable the detection light to pass through the vacuum cavity repeatedly, so that the action range of atoms and the detection light is increased, the absorption times of the atoms are effectively increased by the multi-pass pool module, and compared with direct absorption, the spectrum signal intensity of the multi-pass pool module is greatly improved, and the detection sensitivity of the system can be effectively improved.
Preferably, the surface of the spherical mirror is plated with a protective film, specifically, the protective film is a gold film, so that the reflectivity of the first spherical mirror 6 and the second spherical mirror 7 is more than 95%, the thickness range is 0.7-20 micrometers, and the outer layer of the gold film is plated with a silicon dioxide protective film with the thickness of 1-2 micrometers, thereby enhancing the durability of the spherical mirror under an open environment. Wherein the thickness and material of the protective film are optional according to circumstances.
Preferably, the position of the multi-pass cell module is adjustable, in this scheme, the first spherical mirror 6 and the second spherical mirror 7 are fixed on a triaxial precise adjustment frame, so that the position and the light spot of the multi-pass cell module are adjustable, and the multi-pass cell module is placed outside the vacuum cavity 9, and metal vapor pollution (not shown in the figure) is isolated by using a window sheet. Preferably, the first spherical mirror 6 and the second spherical mirror 7 may be fixed on a three-axis precise adjustment frame, and the relative distance may also be adjusted on the three-axis precise adjustment frame, so that the distance between the first spherical mirror 6 and the second spherical mirror 7 is suitable for different measurement scenes. The vacuum chamber 9 in this case has a chamber length of 300mm and the distance between the first spherical mirror 6 and the second spherical mirror 7 is set to 380mm. A schematic diagram of an open multi-pass pool module is shown in fig. 2. The multi-pass pool module firstly determines the spatial distribution of the gaseous atomic beams through direct absorption, and then adjusts the positions of the first spherical mirror 6 and the second spherical mirror 7, so that the signal intensity is enhanced, and the detection sensitivity of the system is effectively improved. The longitudinal and transverse distribution characteristics of the gaseous atomic beam intensity along the atomic generator 8 are shown in fig. 3 and 4, and the optimal light spot distribution condition of the open type multi-pass pool module according to the atomic beam space distribution characteristics is shown in fig. 5.
The signal acquisition card in the signal processing module is used for acquiring the electric signal of the spectrum corresponding to the photoelectric detector 13; the computer is used for processing the electric signals output by the signal acquisition card. And the detection light is output after passing through the vacuum cavity for a plurality of times.
The method for using the atomic absorption spectrometry device comprises the following steps:
s1, placing a sample in a gaseous atom generating module to generate gaseous atom beams, wherein the gaseous atom beams are dispersed in a vacuum cavity; specifically, 10mg of sample is put into an atomic generator, a current source 11 is started to set a proper current required by sample vaporization, and the atomic generator 8 is powered to generate stable gaseous atomic beams;
s2, the optical path detection module selects and outputs detection light with set wavelength, the detection light is moved out of the multi-pass pool module, the positions of the vacuum cavity 9 in the transverse direction and the longitudinal direction are adjusted, the absorption spectrum intensity of the gaseous atomic beam at each spatial position of the vacuum cavity 9 is obtained, and the spatial distribution characteristics of the atomic beam are determined according to the intensity distribution characteristics; according to the spatial distribution absorption intensity characteristics of the particles obtained through direct absorption, the spatial distribution of the gaseous atomic beams is determined, and then the proper light spot distribution is determined, so that the signal intensity is optimal.
The optical path detection module selectively outputs detection light with set wavelength, and specifically comprises: and selecting a proper detection laser 1 according to the characteristic of the absorption spectrum spectral line of the detection metal, and scanning the detection laser 1 to completely cover the absorption spectrum of the target element.
The position of the vacuum chamber 9 in the transverse direction and the longitudinal direction is adjusted, specifically: the vacuum chamber 9 is set for a distance in each step in the transverse and longitudinal directions, in this case 5mm each step.
S3, according to the spatial distribution characteristics of atoms, the multi-pass pool module is placed at a first position by the aid of the indication laser 2, wherein the first position is the position with the largest concentrated distribution intensity of the gaseous atomic beams, and the specific positions of all components in the device are determined;
s4, placing the sample in the atom generating module again, starting the light path detection module, acquiring an isotope spectrum passing through the multi-pass pool module, and acquiring the isotope ratio of the sample according to the difference of absorption peak intensities of isotopes.
Based on the scheme, as shown in fig. 6, the open type multi-channel cell atomic absorption spectrometry device has a larger improvement in signal intensity compared with the metal isotope spectrum information measured by direct absorption spectrometry.
The above embodiments are merely preferred embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for using an atomic absorption spectrometry device, wherein the atomic absorption spectrometry device comprises a gaseous atomic generation module, an optical path detection module, a multi-pass cell module and a signal processing module, and the gaseous atomic generation module is used for converting a solid sample into gaseous atomic beams distributed in a vacuum cavity; the optical path detection module is used for transmitting detection light passing through the gaseous atomic beam to the vacuum cavity and receiving the light beam passing through the gaseous atomic beam to form an electric signal; the multi-pass pool module is used for outputting the detection light after passing through the gaseous atomic beams in the vacuum cavity for a plurality of times; a signal processing module for processing the electrical signal and analyzing the type and concentration of the sample, characterized in that the method comprises:
placing a sample in the gaseous atom generating module to generate gaseous atom beams, wherein the gaseous atom beams are dispersed in the vacuum cavity;
the optical path detection module is used for selecting and outputting detection light with set wavelength, moving out of the multi-pass pool module, adjusting the positions of the vacuum cavity in the transverse direction and the longitudinal direction, acquiring the absorption spectrum intensity of the gaseous atomic beam at each spatial position of the vacuum cavity, and determining the spatial distribution characteristics of the gaseous atomic beam according to the intensity distribution characteristics;
according to the spatial distribution characteristics of atoms, a multi-pass pool module is placed at a first position, wherein the first position is the position with the largest concentrated distribution intensity of gaseous atomic beams, and the specific positions of all components in the device are determined;
and placing the sample in the atom generating module again, starting the light path detection module, acquiring the isotope spectrum passing through the multi-pass cell module, and acquiring the isotope ratio of the sample according to the difference of the absorption peak intensities of isotopes.
2. The method of claim 1, wherein the location of the multi-pass pool module is adjustable.
3. The method of claim 1, wherein the multipass cell module comprises a first spherical mirror and a second spherical mirror disposed opposite each other on both sides of the vacuum chamber, surfaces of the first spherical mirror and the second spherical mirror being coated with a protective film.
4. The method of claim 1, wherein the gaseous atom generating module comprises:
an atomic generator for gasifying a sample to generate an atomic beam;
and a current source connected to the atomic generator such that the atomic generator heats the sample to generate a gaseous atomic beam.
5. The method of claim 4, wherein the gaseous atom generating module further comprises an infrared thermometer for detecting the temperature of the atom generator.
6. The method of claim 1, wherein the position of the vacuum chamber is adjustable.
7. The method of claim 1, wherein the optical path detection module comprises:
a detection laser for generating detection light of different frequencies for different samples;
a lens for condensing the probe light;
and the photoelectric detector is used for receiving the detection light passing through the vacuum cavity and generating an electric signal.
8. The method of claim 7, wherein the optical path detection module further comprises an indication laser, and wherein the light beams emitted by the indication laser and the detection laser are both transmitted through a lens for emitting visible laser light to assist in optical path adjustment.
9. The method according to claim 7 or 8, wherein the signal processing module comprises:
the signal acquisition card is used for acquiring the electric signals of the spectrum corresponding to the photoelectric detector;
and the computer is used for processing the electric signals output by the signal acquisition card.
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