CN109342344B - Calibration-free device of mercury analyzer and determination method thereof - Google Patents
Calibration-free device of mercury analyzer and determination method thereof Download PDFInfo
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- CN109342344B CN109342344B CN201811452237.8A CN201811452237A CN109342344B CN 109342344 B CN109342344 B CN 109342344B CN 201811452237 A CN201811452237 A CN 201811452237A CN 109342344 B CN109342344 B CN 109342344B
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000010521 absorption reaction Methods 0.000 claims abstract description 29
- 238000002795 fluorescence method Methods 0.000 claims abstract description 13
- 239000007789 gas Substances 0.000 claims description 45
- 230000003287 optical effect Effects 0.000 claims description 32
- 230000005540 biological transmission Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004809 Teflon Substances 0.000 claims description 4
- 229920006362 Teflon® Polymers 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000005283 ground state Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
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Classifications
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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
- G01N21/17—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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
-
- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
Abstract
The invention discloses a calibration-free device and a measuring method of a mercury analyzer. The invention measures the light intensity of cold atom absorption method and cold atom fluorescence method by using a photomultiplier tube in time-sharing way, and the obtained mercury concentration is irrelevant to the emission power of a light source and is only relevant to the ratio of the light intensity; meanwhile, the current ratio measured by the photomultiplier is combined with the characteristics that the current ratio is irrelevant to the sensitivity of the photomultiplier and only relevant to the light intensity ratio, and the mercury concentration in the gas can be directly obtained through the current ratio measured by the photomultiplier, so that the device does not need to be calibrated again during measurement. In actual use, the workload of testers is reduced, the detection efficiency is greatly improved, meanwhile, the use of raw materials in the calibration process is also saved, and the detection cost is reduced.
Description
Technical Field
The invention belongs to the technical field of mercury gas detection, and particularly relates to a calibration-free device of a mercury analyzer and a measuring method thereof.
Background
Cold atom absorption method and cold atom fluorescence method are the commonly used method for measuring gas mercury concentration at present, but because the performance of the photoelectric device (light source, photoelectric detector, etc.) can change along with the change of time or external conditions, after the photoelectric device is used for a period of time, the photoelectric device in the system needs to be recalibrated, and the whole device needs a set of complete calibration system. The invention provides a calibration-free device and a measuring method thereof by utilizing the internal relation of the two measuring methods.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a calibration-free device of a mercury analyzer and a measuring method thereof.
The invention is realized by the following technical scheme:
a calibration-free device of a mercury analyzer comprises a light source, a cylindrical air chamber, a first plane mirror, a second plane mirror, a first color filter, a second color filter, a third color filter, a rotary platform, a photomultiplier and a data acquisition analyzer; the cylindrical air chamber is of a hollow structure, the two ends of the cylindrical air chamber are respectively a light incident end and a light emergent end, the upper part of the cylindrical air chamber is symmetrically provided with an air inlet and an air outlet for air to enter and exit, and the lower part of the cylindrical air chamber is provided with an optical window; the light source is fixedly arranged at the light incidence end of the cylindrical air chamber, and a first color filter is arranged between the light source and the light incidence end; a first plane mirror is arranged at the light ray outgoing end of the cylindrical air chamber, and a second color filter is arranged between the light ray outgoing end and the first plane mirror; the second plane mirror is vertically arranged below the first plane mirror, and the reflecting surfaces of the first plane mirror and the second plane mirror are arranged oppositely; the rotating platform is vertically arranged right below the optical window and horizontally arranged along the height of the second plane mirror, and a third color filter is arranged between the optical window and the rotating platform; the rotating platform is fixedly connected with a photomultiplier, and when the photomultiplier rotates, a light receiving end of the photomultiplier can respectively correspond to the optical window and the reflecting surface of the second plane mirror and receive measuring light output from the cylindrical gas chamber; the signal output end of the photomultiplier is connected with a data acquisition analyzer, and the data acquisition analyzer is used for outputting the light intensity current measured by the photomultiplier.
The invention further solves the technical problem that the opening direction of the optical window is vertical to the light transmission direction in the cylindrical air chamber.
The technical problem to be further solved by the invention is that the transmission wavelength of the first color filter, the second color filter and the third color filter to the incident light beam is 253.7 nm.
The technical problem to be further solved by the invention is that the cylindrical gas chamber is a silica glass tube, and a Teflon coating is arranged on the inner wall of the glass tube.
The invention further solves the technical problem that the device can adopt a cold atom absorption method or a cold atom fluorescence method to measure the concentration of gas mercury; the optical window is used for outputting measuring light of a cold atom fluorescence method, and the light ray emergent end of the cylindrical gas chamber is used for outputting measuring light of a cold atom absorption method.
The principle of the cold atom absorption method is that mercury vapor selectively absorbs ultraviolet light with the wavelength of 253.7nm, the absorbance is in direct proportion to the mercury concentration in a certain concentration range, and mercury atoms can show selective absorption when mercury-containing vapor receives radiation of a light source.
The cold atom fluorescence method is an emission spectroscopy method based on an atomic absorption method. When the light beam emitted by the light source passes through the mercury vapor cloud converted from the mercury element contained in the water sample, the mercury atom absorbs the energy of the specific resonance wave to excite the mercury atom from a ground state to a high-energy state, and when the excited atom returns to the ground state, the mercury atom emits fluorescence, and the content of the mercury in the water sample can be measured by measuring the intensity of the fluorescence, so that the detector for detecting the intensity of the fluorescence is placed at a position which is at right angle to the light beam emitted by the light source.
The invention also provides a measuring method for protecting the mercury analyzer from a calibration device, which comprises the following steps:
introducing gas to be measured into a cylindrical gas chamber, turning on a light source, enabling light beams emitted by the light source to enter the cylindrical gas chamber from a light incidence end after passing through a first color filter, and outputting the incident light beams by the cylindrical gas chamber in two paths;
step two, closing the optical window, adjusting the rotary platform, outputting light beams from the light emitting end of the cylindrical air chamber, emitting the light beams into the reflecting surface of the first plane mirror through the second color filter, then emitting the light beams into the light receiving end of the photomultiplier after the light beams are reflected by the first plane mirror and the second plane mirror, and recording the light intensity current i output by the data acquisition analyzer1;
Step three, closing the light of the cylindrical air chamberA line outgoing end, an optical window is opened, the rotary platform is adjusted, light beams enter the light receiving end of the photomultiplier from the optical window through a third color filter, and the light intensity current i output by the data acquisition analyzer is recorded2;
Step four, obtaining the mercury concentration C in the gas to be measured according to a formulaHg;
Wherein the content of the first and second substances,is the fluorescence coefficient, εHgIs the absorption coefficient per unit length and per unit concentration of the medium.
step A: introducing pure nitrogen gas into the cylindrical gas chamber, turning on the light source, closing the optical window, and measuring to obtain the absorption light intensity I0;
And B: introducing known mercury gas concentration c into the cylindrical gas chamberHgThe light source is turned on, and the absorption light intensity I is respectively measured by a cold atom absorption method and a cold atom fluorescence method1And the intensity of fluorescence I2;
Mercury concentration C according to the inventionHgThe derivation of the formula is as follows:
the formula for measuring light intensity using the cold atomic absorption method according to beer's law is as follows:
wherein, I1Measured by cold atomic absorption; i is0Is the incident light intensity; epsilonHgAbsorption coefficient of the medium per unit length and unit concentration of mercury; c. CHgIs the concentration of mercury; and L is the length of the cylindrical gas chamber measuring cell.
The formula for measuring light intensity by cold atomic fluorescence is as follows:
wherein the content of the first and second substances,the fluorescence coefficient is related to the structure of the gas chamber to be measured and is unrelated to factors such as mercury concentration, and when the structure of the gas chamber is determined, the value is a constant; epsilonHgAbsorption coefficient of the medium per unit length and unit concentration of mercury; c. CHgIs the concentration of mercury; and L is the length of the cylindrical gas chamber measuring cell.
The invention utilizes a photomultiplier to measure the light intensity of two methods in a time-sharing way, and the light intensity can be obtained by the following formulas 1 and 2:
as can be seen from formula 4, the mercury concentration CHgIndependent of the emission power of the light source, so that variations in the light source do not affect the measurement result, only I1And I2The ratio of (a) to (b) is correlated.
When the same photomultiplier tube is used, since the sensitivity change is the same due to the change in the performance of the photocathode, the ratio of the resulting light intensity current using the measurement is as follows:
wherein k represents the sensitivity of the photomultiplier; from equation 5, it can be seen that the measured current ratio is independent of the sensitivity of the photomultiplier tube and only dependent on the light intensity ratio, so that recalibration due to possible changes in sensitivity is not required during use.
The mercury concentration C can be obtained by combining the formula 4 and the formula 5HgThe formula is as follows:
furthermore, the fluorescence coefficient can be obtained by combining the formula 1 and the formula 2The formula of (1) is:
therefore, only the nitrogen gas needs to be selected to test the initial incident light intensity I during the initial calibration of the system0After standard mercury gas with known concentration is generated by mercury calibrator and its absorption light intensity I is measured1And the intensity of fluorescence I2The fluorescence coefficient can be obtained by the formula
The invention has the beneficial effects that:
the calibration-free device of the mercury analyzer and the determination method thereof provided by the invention have the advantages that the light intensity of a cold atom absorption method and the light intensity of a cold atom fluorescence method are measured in a time-sharing manner by using the photomultiplier, the mercury concentration is obtained through the internal relation of the two methods and is irrelevant to the emission power of a light source and is only relevant to the ratio of the light intensity, and meanwhile, the mercury concentration in gas can be directly obtained through the current ratio measured by the photomultiplier by combining the characteristics that the current ratio measured by the photomultiplier is irrelevant to the sensitivity of the photomultiplier and is only relevant to the ratio of the light intensity, so that the device does not need to be recalibrated during measurement. In actual use, the workload of testers is reduced to a certain extent, the detection efficiency is greatly improved, meanwhile, the use of raw materials in the calibration process is also saved, and the detection cost is reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of the device of the present invention.
FIG. 2 is a schematic view of the structure of the cylindrical air cell of the present invention.
In the figure, the numbers are 1-light source, 2-cylindrical air chamber, 3-first plane mirror, 4-second plane mirror, 5-first color filter, 6-second color filter, 7-third color filter, 8-rotary platform, 9-photomultiplier, 10-data acquisition analyzer, 21-light incident end, 22-light emergent end, 23-air inlet, 24-air outlet, 25-optical window and 26-Teflon coating.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples.
Referring to fig. 1-2, a calibration-free device of a mercury analyzer comprises a light source 1, a cylindrical gas chamber 2, a first plane mirror 3, a second plane mirror 4, a first color filter 5, a second color filter 6, a third color filter 7, a rotating platform 8, a photomultiplier 9 and a data acquisition analyzer 10; the cylindrical air chamber 2 is of a hollow structure, the two ends of the cylindrical air chamber are respectively a light incident end 21 and a light emergent end 22, the upper part of the cylindrical air chamber is symmetrically provided with an air inlet 23 and an air outlet 24 for air to enter and exit, and the lower part of the cylindrical air chamber is provided with an optical window 25; the light source 1 is fixedly arranged at a light incidence end 21 of the cylindrical air chamber, and a first color filter 5 is arranged between the light source 1 and the light incidence end 21; a first plane mirror 3 is arranged at a light ray outgoing end 22 of the cylindrical air chamber, and a second color filter 6 is arranged between the light ray outgoing end 22 and the first plane mirror 3; the second plane mirror 4 is vertically arranged below the first plane mirror 3, and the reflecting surfaces of the first plane mirror 3 and the second plane mirror 4 are oppositely arranged; the rotating platform 8 is vertically arranged right below the optical window 25 and horizontally arranged along the height of the second plane mirror 4, and a third color filter 7 is arranged between the optical window 25 and the rotating platform 8; the rotating platform 8 is fixedly connected with a photomultiplier tube 9, and when the photomultiplier tube 9 rotates, a light receiving end of the photomultiplier tube can respectively correspond to the optical window 25 and the reflecting surface of the second plane mirror 4 and receive measuring light output from the cylindrical gas chamber; the signal output end of the photomultiplier 8 is connected with a data acquisition analyzer 10, and the data acquisition analyzer 10 is used for outputting the light intensity current measured by the photomultiplier.
In this embodiment, the opening direction of the optical window 25 is perpendicular to the light transmission direction in the cylindrical gas chamber 2.
In this embodiment, the first color filter 5, the second color filter 6, and the third color filter 7 all transmit an incident beam at 253.7 nm.
In this embodiment, the cylindrical gas chamber 2 is a silica glass tube, and a teflon plating layer 26 is disposed on an inner wall of the glass tube.
In this embodiment, the device may use a cold atom absorption method or a cold atom fluorescence method to measure the concentration of gas mercury; the optical window 25 is used for outputting the measuring light of the cold atom fluorescence method, and the light ray exit end 22 of the cylindrical gas chamber is used for outputting the measuring light of the cold atom absorption method.
The embodiment is a determination method based on the calibration-free device of the mercury analyzer, and comprises the following steps:
firstly, introducing gas to be detected into a cylindrical gas chamber 2, turning on a light source 1, wherein the light source 1 adopts a hollow cathode lamp, light beams emitted by the light source enter the cylindrical gas chamber 2 from a light incidence end 21 after passing through a first color filter 5, the transmission wavelength of the first color filter 5 to incident light beams is 253.7nm, the wavelength of the incident light beams is 275.7nm, the first color filter is used for selectively absorbing ultraviolet light with the wavelength of 253.7nm by mercury vapor, and the cylindrical gas chamber 2 outputs the incident light beams in two paths;
step two, the optical window 25 is closed, the rotating platform 8 is adjusted to enable the direction of the light receiving end of the photomultiplier tube 9 to point to the second plane mirror 4,the light beam is output from the light emitting end 22 of the cylindrical air chamber, enters the reflecting surface of the first plane mirror 3 through the second color filter 6, then enters the light receiving end of the photomultiplier 9 after being reflected by the first plane mirror 3 and the second plane mirror 4, the photomultiplier 9 converts the received light intensity and transmits the data to the data acquisition analyzer 10, and the light intensity current i obtained at the moment is recorded1;
Step three, closing the light emitting end 22 of the cylindrical air chamber, opening the optical window 25, enabling the opening direction of the optical window 25 to be vertical to the light transmission direction in the cylindrical air chamber 2, meeting the requirement that a detector for detecting fluorescence intensity is placed at a position perpendicular to the position of the light beam emitted by the mercury lamp, adjusting the rotary platform 8 to enable the direction of the light receiving end of the photomultiplier 9 to point to the optical window 25, enabling the light beam to enter the light receiving end of the photomultiplier 9 from the optical window 25 through the third color filter 7, and recording the light intensity current i output by the data acquisition analyzer 102;
Step four, calculating and obtaining the mercury concentration C in the gas to be measured according to the following formulaHg;
Wherein the content of the first and second substances,is the fluorescence coefficient, εHgThe absorption coefficient of the medium is mercury per unit length and per unit concentration.
step A: introducing pure nitrogen gas into the cylindrical gas chamber 2, opening the light source 1, closing the optical window 25, and measuring to obtain the absorption light intensity I0;
And B: introducing known mercury gas concentration c into the cylindrical gas chamber 2HgThe light source 1 is turned on, and the absorption is measured by a cold atom absorption method and a cold atom fluorescence method, respectivelyLight receiving intensity I1And the intensity of fluorescence I2;
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (6)
1. The method for measuring the mercury analyzer without a calibration device uses the mercury analyzer without the calibration device, and is characterized in that: the calibration-free device of the mercury analyzer comprises a light source (1), a cylindrical air chamber (2), a first plane mirror (3), a second plane mirror (4), a first color filter (5), a second color filter (6), a third color filter (7), a rotating platform (8), a photomultiplier (9) and a data acquisition analyzer (10); the cylindrical air chamber (2) is of a hollow structure, a light incident end (21) and a light emergent end (22) are respectively arranged at two ends of the cylindrical air chamber, an air inlet (23) and an air outlet (24) for air to enter and exit are symmetrically arranged at the upper part of the cylindrical air chamber, and an optical window (25) is arranged at the lower part of the cylindrical air chamber; the light source (1) is fixedly arranged at a light incidence end (21) of the cylindrical air chamber, and a first color filter (5) is arranged between the light source (1) and the light incidence end (21); a first plane mirror (3) is arranged at the light ray outgoing end (22) of the cylindrical air chamber, and a second color filter (6) is arranged between the light ray outgoing end (22) and the first plane mirror (3); the second plane mirror (4) is vertically arranged below the first plane mirror (3), and the reflecting surfaces of the first plane mirror (3) and the second plane mirror (4) are arranged oppositely; the rotating platform (8) is vertically arranged right below the optical window (25) and horizontally arranged along the height of the second plane mirror (4), and a third color filter (7) is arranged between the optical window (25) and the rotating platform (8); a photomultiplier (9) is fixedly connected to the rotating platform (8), and when the photomultiplier (9) rotates, a light receiving end of the photomultiplier can respectively correspond to the optical window (25) and the reflecting surface of the second plane mirror (4) and receive measuring light output from the cylindrical gas chamber; the signal output end of the photomultiplier (8) is connected with a data acquisition analyzer (10), and the data acquisition analyzer (10) is used for outputting light intensity current measured by the photomultiplier;
the specific determination method of the mercury analyzer without a calibration device comprises the following steps:
firstly, introducing gas to be detected into a cylindrical gas chamber (2), turning on a light source (1), enabling light beams emitted by the light source to enter the cylindrical gas chamber (2) from a light incidence end (21) after passing through a first color filter (5), and enabling the cylindrical gas chamber (2) to output incident light beams in two paths;
step two, closing the optical window (25), adjusting the rotary platform (8), outputting light beams from a light emitting end (22) of the cylindrical air chamber, emitting the light beams to a reflecting surface of the first plane mirror (3) through the second color filter (6), then emitting the light beams to a light receiving end of the photomultiplier (9) after being reflected by the first plane mirror (3) and the second plane mirror (4), and recording light intensity current i output by the data acquisition analyzer (10)1;
Step three, closing a light ray emitting end (22) of the cylindrical air chamber, opening an optical window (25), adjusting a rotating platform (8), enabling light beams to enter a light ray receiving end of a photomultiplier (9) from the optical window (25) through a third color filter (7), and recording light intensity current i output by a data acquisition analyzer (10)2;
Step four, obtaining the mercury concentration C in the gas to be measured according to a formulaHg;
2. The mercury analyzer calibration-free device determination method according to claim 1, characterized in that: the opening direction of the optical window (25) is vertical to the light transmission direction in the cylindrical air chamber (2).
3. The mercury analyzer calibration-free device determination method according to claim 1, characterized in that: the first color filter (5), the second color filter (6) and the third color filter (7) transmit incident light beams with wavelengths of 253.7 nm.
4. The mercury analyzer calibration-free device determination method according to claim 1, characterized in that: the cylindrical air chamber (2) is a silica glass tube, and a Teflon coating (26) is arranged on the inner wall of the glass tube.
5. The mercury analyzer calibration-free device determination method according to claim 1, characterized in that: the device can adopt a cold atom absorption method or a cold atom fluorescence method to measure the concentration of gas mercury; the optical window (25) is used for outputting measuring light of a cold atom fluorescence method, and the light ray outgoing end (22) of the cylindrical gas chamber is used for outputting measuring light of a cold atom absorption method.
6. The mercury analyzer calibration-free device determination method according to claim 1, characterized in that: the fluorescence coefficientThe obtaining method comprises the following steps:
step A: introducing pure nitrogen gas into the cylindrical gas chamber (2), turning on the light source (1), closing the optical window (25), and measuring to obtain the absorption light intensity I0;
And B: introducing known mercury gas concentration c into the cylindrical gas chamber (2)HgThe light source (1) is turned on, and the absorption light intensity I is respectively measured by a cold atom absorption method and a cold atom fluorescence method1And the intensity of fluorescence I2;
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