CN117483215A - Method for coating inner part of measuring cavity by ultraviolet fluorescence method - Google Patents

Method for coating inner part of measuring cavity by ultraviolet fluorescence method Download PDF

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Publication number
CN117483215A
CN117483215A CN202311424523.4A CN202311424523A CN117483215A CN 117483215 A CN117483215 A CN 117483215A CN 202311424523 A CN202311424523 A CN 202311424523A CN 117483215 A CN117483215 A CN 117483215A
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CN
China
Prior art keywords
coating
measuring cavity
inner part
cavity
wavelength
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202311424523.4A
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Chinese (zh)
Inventor
彭志敏
董月红
周凯
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tsinghua University
CHN Energy Group Science and Technology Research Institute Co Ltd
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Tsinghua University
CHN Energy Group Science and Technology Research Institute Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Tsinghua University, CHN Energy Group Science and Technology Research Institute Co Ltd filed Critical Tsinghua University
Priority to CN202311424523.4A priority Critical patent/CN117483215A/en
Publication of CN117483215A publication Critical patent/CN117483215A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/002Pretreatement
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • B05D3/0254After-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/22Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2506/00Halogenated polymers
    • B05D2506/10Fluorinated polymers
    • B05D2506/15Polytetrafluoroethylene [PTFE]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2602/00Organic fillers

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses a method for coating an inner part of a measuring cavity for ultraviolet fluorescence detection, which comprises the following steps: the first step: preparing a measuring cavity; and a second step of: cleaning the measuring cavity; and a third step of: preparing a coating, and adding an organic solvent for absorbing wavelength into polytetrafluoroethylene emulsion; fourth step: spraying or brushing the mixed emulsion on the inner surface of the measuring cavity, putting the sprayed or brushed measuring cavity into a baking oven for baking until the solvent is completely volatilized, and forming a coating; fifth step: sintering at high temperature, sintering in a baking oven at 380-420 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent; sixth step: and (5) rough surface treatment. The invention is used for inhibiting and absorbing stray light in the cavity, absorbing light with specific wavelength by using chemical substances in the coating, reducing the intensity of non-signal light, thereby reducing background signals, improving the detection limit and detection sensitivity of the whole instrument, and simultaneously the coating film has high temperature resistance, corrosion resistance and adsorption resistance.

Description

Method for coating inner part of measuring cavity by ultraviolet fluorescence method
Technical Field
The invention particularly relates to a method for coating an inner part of a measuring cavity by ultraviolet fluorescence.
Background
Typically SO 2 The measuring cavity used by the instrument can be plated with a layer of black substance in the cavity, so that the effect of inhibiting and absorbing stray light to a certain extent is achieved. The technical scheme is that a layer of black Teflon material is plated on an aluminum alloy, the inner surface of a measuring cavity sprayed by Teflon coating is relatively smooth, specular reflection is easy to generate, light source signal light can enter a detector, the surface of the blackened aluminum alloy has certain roughness, light entering the cavity generates diffuse reflection, and stray light can also be generated.
The other is that the aluminum alloy material is oxidized and blackened, and the specific treatment method is as follows: the anodic oxidation is carried out on aluminum in sulfuric acid electrolyte under the action of current, so that a thin layer of about 10 microns of oxide film is formed on the surface of the aluminum, and then dyeing treatment is carried out by using dyeing liquid prepared from black organic dye.
Use of Teflon coating treated cavities and oxidized blackening treated measurement cavities in SO 2 On an analyzer, SO is detected 2 Signal intensity at zero gas concentration, i.e. background signal of stray light.
When the light source emits 214nm excitation light to irradiate the interior of the measuring cavity, the photodetector detects the light signal reflected by the inner surface of the measuring cavity irradiated by the light source, and the signal is called as a background noise signal, and is free of SO 2 When the gas enters the measuring cavity, the detected background noise signal intensity is equivalent to the fluorescence signal intensity radiated by excited SO2 gas with the concentration of 200-300 ppb, and the fluctuation range of the background noise signal amplitude is about 10 percent (20 ppb-30 ppb) of the signal intensity, thereby the signal intensity is measured in SO 2 The measurement of the concentration of the gas interferes with the measurement of the emitted fluorescent signal. In advanceTrace or ultra trace SO 2 When the concentration is measured, the real fluorescent signal is often submerged in the background noise signal, SO that SO of 10ppb or less can not be stably measured 2 Fluorescence signal of gas concentration. Cavities treated with teflon coating alone or with oxidative blackening do not meet SO on the ppb level 2 And detecting a gas concentration signal.
Disclosure of Invention
The invention aims to provide a method for coating an inner part of a measuring cavity by ultraviolet fluorescence.
The aim of the invention is achieved by the following technical scheme:
a method for coating an inner part of a measuring cavity for ultraviolet fluorescence detection, comprising the following steps:
the first step: preparing a measuring cavity;
and a second step of: cleaning the measuring cavity;
and a third step of: preparing a coating, and adding an organic solvent for absorbing wavelength into polytetrafluoroethylene emulsion;
fourth step: spraying or brushing the mixed emulsion on the inner surface of the measuring cavity, repeatedly coating and drying according to the requirement until the required thickness is reached, putting the sprayed or brushed measuring cavity into a drying oven for drying until the solvent is completely volatilized, and forming a coating;
fifth step: sintering at high temperature, sintering in a baking oven at 380-420 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent;
sixth step: rough surface treatment reduces specular reflection.
Further, in a first step, a measuring cavity of the aluminum alloy is manufactured by machining.
Further, in the second step, the grease in the measuring cavity is dissolved by using an organic solvent, then the temperature is increased by 400 ℃ to volatilize the grease, and the bonding capability of the coating and the surface layer of the measuring cavity is improved by using an adhesive additive.
Preferably, in the third step, 0.5 to 1.5% of yellow powder of 2-hydroxy-4-n-octoxybenzophenone is added into the polytetrafluoroethylene emulsion, so that the ultraviolet rays with the wavelength of 240 to 340nm can be absorbed strongly.
Preferably, in the third step, 0.5 to 1.5% of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole is added to the polytetrafluoroethylene emulsion, so that light with a wavelength of 270 to 380nm can be strongly absorbed.
Preferably, in the third step, 0.5 to 1.5% of 2, 4-dihydroxybenzophenone is added to the polytetrafluoroethylene emulsion, so that the light with the wavelength of 280 to 340nm can be strongly absorbed.
Preferably, in the third step, 0.5 to 1.5% of 2-hydroxy-4-methoxybenzophenone is added into polytetrafluoroethylene emulsion, so that light with the wavelength of 280 to 340nm can be absorbed strongly.
Preferably, in the third step, 0.5 to 1.5% of 2- (2 ' -hydroxy-3 ',5' -di-t-phenyl) -5-chlorobenzotriazole is added to the polytetrafluoroethylene emulsion, so that light with the wavelength of 270 to 380nm can be absorbed strongly.
Preferably, in the fourth step, the drying temperature is 75-85 ℃.
Further, in the fifth step, sintering is carried out in an oven at 350-450 ℃, and after the coating material is melted, a net structure is formed by the coating material and the bonding auxiliary agent.
The beneficial technical effects are as follows:
the invention is used for inhibiting and absorbing stray light in the cavity, absorbing light with specific wavelength by using chemical substances in the coating, reducing the intensity of non-signal light, thereby reducing background signal, improving the detection limit and detection sensitivity of the whole instrument, and simultaneously, the coating has the characteristics of high temperature resistance, corrosion resistance, adsorption resistance and the like, is favorable for being used under various severe working conditions.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a graph showing the effect of the coating layer of the measuring cavity according to example 1 of the present invention.
FIG. 2 is a graph showing the detection result of the background signal in example 1 of the present invention.
FIG. 3 is the SO in example 1 of the present invention 2 And (3) a graph of the detection result of the gas low concentration condition.
FIG. 4 is a flow chart of a method of the present invention for coating the interior of a measurement chamber for UV fluorescence detection.
Detailed Description
The ultraviolet fluorescence method is a fluorescence measurement technology which uses the fact that certain substances are in an excited state after being irradiated by ultraviolet light, excited state molecules undergo a collision and emission de-excitation process, the characteristics of the substances can be reflected, and the detection sensitivity is limited by the stray light intensity in a fluorescence measurement cavity. Stray light is generated by reflection of light from the light source through the optical element and the inner surface of the measurement cavity.
The film coating of the invention is mainly applied to ultraviolet fluorescence SO 2 An analyzer using a zinc lamp light source with a center wavelength of 214nm as excitation light, SO 2 The fluorescence wavelength generated by the molecules under the laser is around 330 nm. The film coating in the cavity mainly inhibits and reduces the stray light formed by the light source, and the wavelength range of the stray light to be inhibited in the process is 210 nm-300 nm. Fig. 1 shows the effect of the invention after coating the film.
Then, SO is used as 2 The analyzer illustrates the invention.
Example 1
Referring to fig. 4, a method for coating the interior of a measurement chamber for ultraviolet fluorescence detection, comprising the steps of:
the first step: manufacturing a reaction cavity of the aluminum alloy through machining;
and a second step of: cleaning a reaction cavity, dissolving grease in an organic solvent, volatilizing the grease at a high temperature of 400 ℃, and improving the bonding capability of a coating and the surface layer of the measurement cavity by using an adhesive auxiliary agent;
and a third step of: preparing a coating, namely adding 1% of 2-hydroxy-4-n-octoxybenzophenone yellow powder into polytetrafluoroethylene emulsion, and strongly absorbing ultraviolet rays with the wavelength of 240-340 nm;
fourth step: spraying the mixed emulsion on the inner surface of a measuring cavity, putting the sprayed measuring cavity into a baking oven for baking until the solvent is completely volatilized to form a coating, wherein the baking temperature is 80 ℃;
fifth step: sintering at high temperature, sintering in a baking oven at 400 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent;
sixth step: rough surface treatment reduces specular reflection.
Referring to FIG. 2, S1 is a reaction chamber for oxidizing and blackening an aluminum alloy material in the background art, S2 is a reaction chamber subjected to the treatment of the embodiment, and SO with the same concentration is introduced into the reaction chamber 2 The indication of the instrument after the gas, the concentration on the graph is that of the introduced SO 2 From the graph, the curve of S2 represents the detection of SO 2 The meter reading, i.e., the background signal at zero gas concentration, is less than 10ppb with a noise of about 2ppb.
Referring to FIG. 3, in SO 2 Under the condition of low concentration of gas, [ SO ] 2 ]The x-axis represents time of operation under this condition, which is still clearly distinguishable =5 ppb.
Therefore, after the film coating provided by the invention is used, stray light is obviously reduced, the background signal of the instrument is obviously reduced, and a signal with lower concentration can be detected.
Meanwhile, the working temperature of the reaction cavity is set to be 45 ℃, and the observation shows that the coating of the reaction cavity has no influence, thus the invention has the advantages of applicability to the temperature and SO resistance 2 And (3) corroding.
Example 2
A method for coating an inner part of a measuring cavity for ultraviolet fluorescence detection, comprising the following steps:
the first step: preparing a measuring cavity, and manufacturing the measuring cavity of the aluminum alloy through machining;
and a second step of: cleaning a measuring cavity, dissolving grease in an organic solvent, volatilizing the grease at a high temperature of 380 ℃, and improving the bonding capability of a coating and the surface layer of the measuring cavity by using an adhesive additive;
and a third step of: preparing a coating, namely adding 0.5% of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole into polytetrafluoroethylene emulsion, so that light with the wavelength of 270-380 nm can be strongly absorbed;
fourth step: spraying the mixed emulsion on the inner surface of a measuring cavity, putting the sprayed measuring cavity into a baking oven for baking until the solvent is completely volatilized to form a coating, wherein the baking temperature is 75 ℃;
fifth step: sintering at high temperature, sintering in a baking oven at 350 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent;
sixth step: rough surface treatment reduces specular reflection.
Example 3
The first step: preparing a measuring cavity, and manufacturing the measuring cavity of the aluminum alloy through machining;
and a second step of: cleaning a measuring cavity, dissolving grease in an organic solvent, volatilizing the grease at a high temperature of 420 ℃, and improving the bonding capability of a coating and the surface layer of the measuring cavity by using an adhesive additive;
and a third step of: preparing a coating, namely adding 1.5% of 2, 4-dihydroxybenzophenone into polytetrafluoroethylene emulsion, and strongly absorbing light with the wavelength of 280-340 nm;
fourth step: spraying the mixed emulsion on the inner surface of a measuring cavity, putting the sprayed measuring cavity into a baking oven for baking until the solvent is completely volatilized to form a coating, wherein the baking temperature is 85 ℃;
fifth step: sintering at high temperature, sintering in an oven at 450 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent;
sixth step: rough surface treatment reduces specular reflection.
Example 4
A method for coating an inner part of a measuring cavity for ultraviolet fluorescence detection, comprising the following steps:
the first step: preparing a measuring cavity, and manufacturing the measuring cavity of the aluminum alloy through machining;
and a second step of: cleaning a measuring cavity, dissolving grease in an organic solvent, volatilizing the grease at a high temperature of 400 ℃, and improving the bonding capability of a coating and the surface layer of the measuring cavity by using an adhesive additive;
and a third step of: preparing a coating, namely adding 1% of 2-hydroxy-4-methoxybenzophenone into polytetrafluoroethylene emulsion, and strongly absorbing light with the wavelength of 280-340 nm;
fourth step: spraying the mixed emulsion on the inner surface of a measuring cavity, putting the sprayed measuring cavity into a baking oven for baking until the solvent is completely volatilized to form a coating, wherein the baking temperature is 80 ℃;
fifth step: sintering at high temperature, sintering in a baking oven at 400 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent;
sixth step: rough surface treatment reduces specular reflection.
Example 5
A method for coating an inner part of a measuring cavity for ultraviolet fluorescence detection, comprising the following steps:
the first step: preparing a measuring cavity, and manufacturing the measuring cavity of the aluminum alloy through machining;
and a second step of: cleaning a measuring cavity, dissolving grease in an organic solvent, volatilizing the grease at a high temperature of 400 ℃, and improving the bonding capability of a coating and the surface layer of the measuring cavity by using an adhesive additive;
and a third step of: preparing a coating, namely adding 1% of 2- (2 ' -hydroxy-3 ',5' -di-tertiary phenyl) -5-chloridized benzotriazole into polytetrafluoroethylene emulsion, so as to strongly absorb light with the wavelength of 270-380 nm;
fourth step: spraying the mixed emulsion on the inner surface of a measuring cavity, putting the sprayed measuring cavity into a baking oven for baking until the solvent is completely volatilized to form a coating, wherein the baking temperature is 80 ℃;
fifth step: sintering at high temperature, sintering in a baking oven at 400 ℃, melting the coating material, and forming a net structure with the bonding auxiliary agent;
sixth step: rough surface treatment reduces specular reflection.
While the fundamental and principal features of the invention and advantages of the invention have been shown and described, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (10)

1. A method for coating an inner part of a measuring cavity for ultraviolet fluorescence detection, comprising the following steps:
the first step: preparing a measuring cavity;
and a second step of: cleaning the measuring cavity;
and a third step of: preparing a coating, and adding an organic solvent for absorbing wavelength into polytetrafluoroethylene emulsion;
fourth step: spraying or brushing the mixed emulsion on the inner surface of the measuring cavity, putting the sprayed or brushed measuring cavity into a baking oven for baking until the solvent is completely volatilized, and forming a coating;
fifth step: sintering at high temperature;
sixth step: and (5) rough surface treatment.
2. The method of claim 1, wherein in the first step, the measuring chamber of the aluminum alloy is produced by machining.
3. The method for coating the inner part of a measuring cavity for ultraviolet fluorescence detection according to claim 1, wherein in the second step, the grease of the measuring cavity is dissolved by using an organic solvent, then the grease is volatilized by increasing the temperature to 380-420 ℃, and the bonding capability of the coating to the surface layer of the measuring cavity is improved by using an adhesive auxiliary agent.
4. The method for coating the inner part of a measuring cavity for ultraviolet fluorescence detection according to claim 1, wherein in the third step, 0.5-1.5% of 2-hydroxy-4-n-octoxybenzophenone yellow powder is added into polytetrafluoroethylene emulsion to absorb ultraviolet rays with the wavelength of 240-340 nm.
5. The method for coating the inner part of a measuring cavity for ultraviolet fluorescence detection according to claim 1, wherein in the third step, 0.5-1.5% of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole is added into polytetrafluoroethylene emulsion to absorb light with a wavelength of 270-380 nm.
6. The method for coating the inner part of a measuring cavity for ultraviolet fluorescence detection according to claim 1, wherein in the third step, 0.5-1.5% of 2, 4-dihydroxybenzophenone is added into polytetrafluoroethylene emulsion to absorb light with a wavelength of 280-340 nm.
7. The method for coating the inner part of a measuring cavity for ultraviolet fluorescence detection according to claim 1, wherein in the third step, 0.5-1.5% of 2-hydroxy-4-methoxybenzophenone is added into polytetrafluoroethylene emulsion to absorb light with a wavelength of 280-340 nm.
8. The method for coating the inner part of a measuring cavity for ultraviolet fluorescence detection according to claim 1, wherein in the third step, 0.5-1.5% of 2- (2 ' -hydroxy-3 ',5' -di-tertiary phenyl) -5-chlorinated benzotriazole is added into polytetrafluoroethylene emulsion to absorb light with a wavelength of 270-380 nm.
9. The method for coating the inner part of a measuring chamber for ultraviolet fluorescence detection according to claim 1, wherein in the fourth step, the drying temperature is 75-85 ℃.
10. The method of claim 1, wherein in the fifth step, the coating is sintered in an oven at 350-450 ℃ and after the coating material is melted, the coating and the bonding aid form a network structure.
CN202311424523.4A 2023-10-30 2023-10-30 Method for coating inner part of measuring cavity by ultraviolet fluorescence method Pending CN117483215A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311424523.4A CN117483215A (en) 2023-10-30 2023-10-30 Method for coating inner part of measuring cavity by ultraviolet fluorescence method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311424523.4A CN117483215A (en) 2023-10-30 2023-10-30 Method for coating inner part of measuring cavity by ultraviolet fluorescence method

Publications (1)

Publication Number Publication Date
CN117483215A true CN117483215A (en) 2024-02-02

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311424523.4A Pending CN117483215A (en) 2023-10-30 2023-10-30 Method for coating inner part of measuring cavity by ultraviolet fluorescence method

Country Status (1)

Country Link
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