CN117538103A - Inclination angle sampling device and method for detecting furfural Raman spectrum in transformer oil - Google Patents
Inclination angle sampling device and method for detecting furfural Raman spectrum in transformer oil Download PDFInfo
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- CN117538103A CN117538103A CN202311501855.8A CN202311501855A CN117538103A CN 117538103 A CN117538103 A CN 117538103A CN 202311501855 A CN202311501855 A CN 202311501855A CN 117538103 A CN117538103 A CN 117538103A
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims description 58
- 238000005070 sampling Methods 0.000 title claims description 40
- 238000001237 Raman spectrum Methods 0.000 title claims description 18
- 238000000034 method Methods 0.000 title description 25
- 238000002347 injection Methods 0.000 claims abstract description 152
- 239000007924 injection Substances 0.000 claims abstract description 152
- 239000000758 substrate Substances 0.000 claims abstract description 91
- 239000007788 liquid Substances 0.000 claims abstract description 77
- 239000002699 waste material Substances 0.000 claims abstract description 43
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 11
- 238000001069 Raman spectroscopy Methods 0.000 claims description 20
- 238000007789 sealing Methods 0.000 claims description 9
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims description 7
- 230000005284 excitation Effects 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002042 Silver nanowire Substances 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims 1
- 239000000523 sample Substances 0.000 description 101
- 239000003921 oil Substances 0.000 description 50
- 238000001514 detection method Methods 0.000 description 23
- 230000008901 benefit Effects 0.000 description 8
- 230000032683 aging Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000520 microinjection Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
-
- 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
- G01N21/65—Raman scattering
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- Health & Medical Sciences (AREA)
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- Biochemistry (AREA)
- Physics & Mathematics (AREA)
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- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Hydrology & Water Resources (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The device comprises an injection needle cylinder for accommodating a sample to be detected, wherein the injection needle cylinder comprises an injection end for outputting the sample to be detected, and a pair of guide rails and a waste liquid slit perpendicular to the guide rails and used for flowing in waste liquid are arranged on the upper surface of a waste liquid collector; the quartz glass cover is arranged on the waste liquid collector, the inclination bearing device is supported on the waste liquid collector and is accommodated in the quartz glass cover, the drawing type clamping groove is connected with a pair of guide rails in a sliding manner, the ceramic heating plate is obliquely arranged in the drawing type clamping groove at a preset angle, the heat conducting copper sheet is paved on the top surface of the ceramic heating plate and is provided with a substrate clamping groove for accommodating a substrate, the substrate is detachably connected with the substrate clamping groove and is opposite to the sample injection groove, the surface of the substrate is coupled with oil 4-ATP molecules, a sample from the injection syringe enters the sample injection port through the sample injection hose, flows through the bottom end from the top end of the substrate through the sample injection groove, and then enters the waste liquid collector through the waste liquid slit.
Description
Technical Field
The invention relates to the technical field of Raman detection, in particular to an inclination angle sampling device and method for detecting a furfural Raman spectrum in transformer oil.
Background
The safe and reliable operation of the electrical equipment is a first defense line for avoiding major accidents of the power system; oil paper insulating electrical equipment such as transformers, converter transformers, bushings, reactors and the like are important components of an electric power system. The method can accurately grasp the insulating aging state of the oil paper of the electrical equipment, can prevent the oil paper from happening, and is one of the keys for ensuring the safe production of the power grid and realizing the efficient overhaul of the electrical equipment. Under the action of electricity, heat and the like, the oil paper insulating material of the operating electrical equipment can be decomposed to generate various substances reflecting the insulating property, and the substances are dissolved in oil, and the most common ageing characteristic is furfural. The accurate detection of the dissolved trace furfural in the oil is a key for realizing the insulation aging diagnosis of the oil paper of the electrical equipment, and is an important technical support for ensuring the safe and reliable operation of the large-scale oil paper insulation electrical equipment.
The surface enhanced Raman scattering technology is a spectrum analysis method for directly measuring Raman scattered light generated by laser irradiation of a substance based on Raman scattering effect, so as to infer the property and content of the substance, and can simultaneously and qualitatively and quantitatively analyze liquid and solid objects to be detected according to the Raman frequency shift position and the intensity molecular concentration thereof. The raman detection device of the prior art is only suitable for laboratory detection. The intelligent field detection for the aging state of the transformer does not realize the field on-line detection of the transformer oil at present. The traditional Raman spectrometer is large in size, high in price and inconvenient to detach and carry in the use process. Meanwhile, the traditional liquid detection method generally adopts a long-time soaking method, and is placed in a quartz cuvette for sampling, so that the operation is complex, time and labor are consumed, the mode is limited by the operation level of an operator, and a large error exists in repeated sample injection.
The information disclosed in the background section is only for enhancement of understanding of the background of the invention and therefore may contain information that does not form the prior art that is already known to a person of ordinary skill in the art.
Disclosure of Invention
Aiming at the defects or drawbacks existing in the prior art, the inclination angle sampling device and the inclination angle sampling method for detecting the Raman spectrum of the furfural in the transformer oil are provided, the sample preparation and the sample detection are integrated, the detection of the transformer oil sample can be completed in a short time by combining a portable Raman spectrometer, and the inclination angle sampling device and the inclination angle sampling method are suitable for detecting the liquid sample. By combining a portable Raman spectrometer, the on-site monitoring of the concentration of the dissolved furfural in the transformer oil can be realized rapidly and accurately with high sensitivity, and the purpose of high-sensitivity and rapid detection of the dissolved ageing characteristic of the oil-immersed electrical equipment is achieved.
The aim of the invention is achieved by the following technical scheme.
An inclination angle sample injection device for detecting the Raman spectrum of furfural in transformer oil comprises a sample injection device,
an injection syringe containing a sample to be tested, the injection syringe including an injection end for outputting the sample to be tested,
an injection needle which is connected with the injection end of the injection syringe in a sealing way,
a sample injection hose which is connected with the injection needle in a sealing way,
an injection needle push-pull rod which is connected with the injection needle cylinder in a sliding and sealing way;
a needle tube holder nested in the syringe to hold the syringe,
a fixing clamp of the injection needle push-pull rod, which is fixed at the end part of the injection needle push-pull rod,
a driving motor which controllably pushes and pulls the injection needle push-pull rod,
a power supply connected to the driving motor,
an injection button connected with the power supply to control the driving motor to push and pull the injection needle push-pull rod;
a waste liquid collector, the upper surface of which is provided with a pair of guide rails and a waste liquid slit perpendicular to the guide rails for flowing in waste liquid;
a quartz glass cover which is covered on the waste liquid collector and comprises,
a sample inlet which is arranged above the quartz glass cover and is connected with the sample inlet hose,
the sample injection groove penetrates through the quartz glass cover and is positioned below the sample injection port;
an inclination bearing device supported on the waste liquid collector and accommodated in the quartz glass cover, the inclination bearing device comprising,
a pull-out type clamping groove which is connected with the pair of guide rails in a sliding way,
a ceramic heating plate which is obliquely arranged in the drawing clamping groove at a preset angle,
a heat conducting copper sheet laid on the top surface of the ceramic heating plate, the heat conducting copper sheet is provided with a substrate clamping groove for accommodating a substrate,
the substrate is detachably connected with the substrate clamping groove and is just opposite to the sample introduction groove, the surface of the substrate is coupled with oil 4-ATP molecules, a sample from a syringe enters the sample introduction port through a sample introduction hose, flows through the bottom end from the top end of the substrate through the sample introduction groove, and then enters the waste liquid collector through the waste liquid slit.
In the dip angle sampling device, the injection needle cylinder comprises an injection end for outputting a sample to be detected and a driving end opposite to the injection end, and the injection needle push-pull rod is connected with the injection needle cylinder in a sliding and sealing manner through the driving end.
In the dip angle sampling device, the fixing clamp at the front end of the injection needle is nested outside the injection end to fix the injection needle.
In the dip angle sampling device, the drawing clamping groove can adjust the preset inclination angle of the ceramic heating plate.
In the inclination sampling device, the preset angle is 30 degrees.
In the dip angle sample injection device, the syringe needle cylinder adopts a capacity of 5 ml.
In the dip angle sample injection device, the substrate is a silver nanowire SERS substrate.
The inclination sampling device further comprises a Raman spectrometer facing the substrate.
In the dip angle sample injection device, the wavelength of excitation light emitted by the Raman spectrometer is 785nm.
The detection method of the inclination angle sample injection device for detecting the furfural Raman spectrum in the transformer oil comprises the following steps,
the injection syringe sucks the liquid of the furfural-transformer oil as a sample to be detected, one end of the injection hose is connected with an injection needle on the injection syringe, the other end is connected with the injection port,
opening a drawing type clamping groove along a guide rail, placing a substrate on the surface of the clamping groove of the substrate, and placing the substrate in a quartz glass cover, wherein the inclination angle of the surface of the substrate is 30 degrees, so that liquid to be measured can flow from the top end to the bottom end of the substrate conveniently;
the ceramic heating plate is heated so that the temperature of the surface of the substrate reaches a predetermined temperature,
the injection button is connected with the power supply to control the driving motor to push and pull the injection needle push-pull rod, a sample to be detected is dripped into the sample inlet at a preset speed, the liquid sample enters the sample inlet through the sample inlet, so that the sample flows through the bottom end along the width direction of the top end of the surface of the substrate, the liquid to be detected can realize specific adsorption on furfural in transformer oil when flowing through the surface of the substrate, and the liquid which participates in the reaction on the surface of the substrate can pass through the waste liquid slit due to the action of gravity and enter the lower waste liquid collector;
and (3) aligning the Raman spectrum to the surface of the substrate, acquiring a Raman spectrum graph to acquire data, opening a pull-type clamping groove after the test is finished, taking down the substrate, opening a waste liquid collector switch, and carrying out centralized treatment on the waste liquid after the test.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the surface of the SERS substrate for detection is coupled with 4-ATP molecules, so that the specific capture of furfural in transformer oil can be realized under the catalysis of acid and heat, the SERS substrate is easier to enrich target molecules, meanwhile, the designed portable inclination sampling device adopts a liquid flow rule, the liquid to be detected can be fully contacted with the surface of the substrate, the detection sensitivity is higher, and the low-concentration detection of furfural in the transformer oil is realized, and the actual requirements of on-site detection are met. The portable dip angle sample injection device can be reused, and is suitable for multi-parameter detection of various liquid objects to be detected.
The device has the advantages of exquisite design, flexible use, convenient carrying and wide universality, and can be suitable for Raman spectrometers of different models. The method is accurate, convenient and high in universality, and can rapidly and accurately realize online monitoring of the dissolved furfural in the transformer oil, so that the purpose of high-sensitivity and high-consistency detection of the dissolved ageing characteristic of the oil-immersed electrical equipment is achieved.
The description is merely an overview of the technical solutions of the present invention, in order to make the technical means of the present invention more clearly apparent to those skilled in the art, and in order to make the description of the present invention and other objects, features and advantages of the present invention more obvious, the following description of the specific embodiments of the present invention will be exemplified.
Drawings
Various other advantages and benefits of the present invention will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. It is evident that the figures described below are only some embodiments of the invention, from which other figures can be obtained without inventive effort for a person skilled in the art. Also, like reference numerals are used to designate like parts throughout the figures.
In the drawings:
fig. 1 is a block diagram of a tilt angle sampling device for detecting raman spectra of furfural in transformer oil according to an embodiment of the present invention;
fig. 2 is an exploded schematic diagram of an inclination sampling device for detecting raman spectrum of furfural in transformer oil according to an embodiment of the present invention;
fig. 3 is a schematic diagram of raman spectra of furfural in mineral oil with different concentrations of an inclination angle sample injection device for detecting the raman spectra of furfural in transformer oil according to an embodiment of the present invention.
The invention is further explained below with reference to the drawings and examples.
Detailed Description
Specific embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While specific embodiments of the invention are shown in the drawings, it should be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. Those of skill in the art will understand that a person may refer to the same component by different names. The description and claims do not identify differences in terms of components, but rather differences in terms of the functionality of the components. As used throughout the specification and claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description hereinafter sets forth a preferred embodiment for practicing the invention, but is not intended to limit the scope of the invention, as the description proceeds with reference to the general principles of the description. The scope of the invention is defined by the appended claims.
For the purpose of facilitating an understanding of the embodiments of the invention, reference will now be made to the drawings of several embodiments illustrated in the drawings, and the accompanying drawings are not to be taken as limiting the embodiments of the invention.
For better understanding, as shown in fig. 1 to 2, an inclination sampling device for raman spectrum detection of furfural in transformer oil comprises,
a syringe 1 containing a sample to be tested, the syringe 1 including an injection end for outputting the sample to be tested,
an injection needle 2, which is connected with the injection end of the injection needle cylinder 1 in a sealing way,
a sample injection hose 6 which is connected with the injection needle 2 in a sealing way,
a needle push-pull rod 4 slidably and sealingly connected to the syringe 1;
a needle tube holder 3 which is nested in the syringe 1 to hold the syringe 1,
a fixing clamp of the injection needle push-pull rod 4, which is fixed at the end part of the injection needle push-pull rod 4,
a driving motor which controllably pushes and pulls the injection needle push-pull rod 4,
a power supply connected to the driving motor,
an injection button 5 connected to the power supply to control the driving motor to push and pull the injection needle push-pull rod 4;
a waste liquid collector 12 having a pair of rails on an upper surface thereof and a waste liquid slit 16 perpendicular to the rails for inflow of waste liquid;
a quartz glass cover 10 provided to cover the waste liquid collector 12, the quartz glass cover 10 including,
a sample inlet 7 which is arranged above the quartz glass cover 10 and is connected with the sample inlet hose 6,
a sample introduction groove 8 penetrating through the quartz glass cover 10 and positioned below the sample introduction port 7;
an inclination bearing device supported on the waste liquid collector 12 and accommodated in the quartz glass cover 10, the inclination bearing device comprising,
a pull-out type card slot 14 which is slidably connected to the pair of guide rails,
a ceramic heating plate 15 provided in the drawing type clamping groove 14 so as to be inclined at a predetermined angle,
a heat conducting copper sheet 11 laid on the top surface of the ceramic heating plate 15, the heat conducting copper sheet 11 having a substrate clamping groove 9 for accommodating a substrate 17,
a substrate 17 detachably connected to the substrate clamping groove 9 and facing the sample introduction groove 8, wherein the surface of the substrate 17 is coupled with oil 4-ATP molecules, and a sample from the syringe 1 enters the sample introduction port 7 through the sample introduction hose 6, flows from the top end to the bottom end of the substrate 17 through the sample introduction groove 8, and then enters the waste liquid collector 12 through the waste liquid slit 16.
In the preferred embodiment of the tilt sampling apparatus, the syringe 1 includes an injection end for outputting a sample to be tested and a driving end opposite to the injection end, and the injection needle push-pull rod 4 is slidably and sealingly connected to the syringe 1 via the driving end.
In the preferred embodiment of the tilt sampling device, the fixing clip at the front end of the injection needle is nested outside the injection end to fix the injection needle 2.
In the preferred embodiment of the tilt sampling device, the pull-out clamping groove 14 can adjust the predetermined tilt angle of the ceramic heating plate 15.
In a preferred embodiment of the tilt sampling apparatus, the predetermined angle is 30 degrees.
In the preferred embodiment of the dip angle sampling device, the syringe needle cylinder adopts a capacity of 5 ml.
In the preferred embodiment of the tilt sampling apparatus, the substrate 17 is a silver nanowire SERS substrate 17.
In a preferred embodiment of the tilt sampling apparatus, the apparatus further comprises a raman spectrometer facing the substrate 17.
In the preferred embodiment of the tilt sampling device, the wavelength of excitation light emitted by the raman spectrometer is 785nm.
In one embodiment, the dip angle sample injection device comprises an external device, an internal component and an operating system; the internal assembly comprises an injection assembly and a portable dip angle liquid filtering device, the injection assembly comprises an injection needle assembly, an injection needle driving assembly and an injection assembly fixing device, and the injection needle assembly comprises an injection needle cylinder 1, an injection needle push-pull rod 4, an injection needle head 2 and an injection sample injection hose 6. The external device comprises a sample injection device external component; the sample injection device external component comprises a quartz glass cover 10, an inclination bearing device arranged in the quartz glass cover 10, a ceramic heating plate 15 arranged on the surface of the inclination bearing device, a heat conduction copper sheet 11 arranged on the surface of the inclination bearing device, and the sample injection device operation component comprises a device switch button, an indicator lamp, a waste liquid collector 12 and a drawing clamping groove 14. The external device further comprises a sample inlet 7 connected with the sample injection hose 6, wherein the sample inlet 7 is arranged above the surface of the quartz glass, and the sample inlet 7 is aligned with the sample injection groove 8 and the substrate 17 to be tested is aligned with the sample injection groove 7. The injection assembly fixture includes: the injection needle front end fixing clamp is arranged outside the front end of the injection needle cylinder 1 in a nested manner and used for fixing the injection needle cylinder 1, the injection needle cylinder 1 fixing clamp is arranged outside the injection needle cylinder 1 in a nested manner and used for fixing the injection needle push-pull rod 4 outside the injection needle push-pull rod 4, and the injection needle push-pull rod 4 fixing clamp is arranged outside the injection needle push-pull rod 4 in a nested manner; a mechanical assembly is arranged between the injection needle assembly and the injection driving assembly. The needle drive assembly includes: the injection needle push-pull rod 4 drives a motor, a power supply, a controller and a control switch, so that semi-automatic control of the injection process is realized.
In one embodiment, the needle is a 6 gauge needle. The operation system comprises: a processor for executing the following procedures, an injection needle sampling procedure, a ceramic heating plate 15 procedure, a drawing type clamping groove 14 procedure, a substrate 17 placed in the drawing type clamping groove 14 procedure, a heating plate preheating procedure, a sample injection procedure, a sample flowing through the surface of the substrate 17 procedure and a waste liquid collecting procedure; the program is that the injection needle push-pull rod 4 is controlled by the device operation key-assembling command controller, and the ceramic heating plate 15 realizes strict time sequence, logic control and displacement control of the process.
In one embodiment, the main function of the quartz glass cover 10 is to effectively protect a liquid sample in the device, when the sample injection device is used, due to the fact that furfural-transformer oil solution of the sample is unstable and easy to volatilize, the quartz glass cover 10 can slow down volatilization of furfural, compared with other transparent glass, the laser transmittance is large, the loss is small, the quartz glass cover 10 enables internal components of the sample injection device to be in a relatively sealed state, interference of the outside on the operation process of the sample injection device can be effectively prevented, and normal operation of each function of an instrument is guaranteed; the operation group key is an execution key for starting to run the system program by the sample injection device, and different keys execute corresponding operation programs. When the switch key of the pull type clamping groove 14 is pressed, the pull type clamping groove 14 of the device pops up, a prepared SERS substrate can be placed on the surface of the substrate clamping groove 9, a heating switch 13 button is started, when an indicator light displays a green signal and the signal is stable and does not flicker, the instrument is indicated to be in a normal running state after self-inspection, at the moment, an injection button 5 is started, liquid to be detected flows into the sample inlet 7 along a needle and flows into the sample injection groove 8, and the liquid is dripped into the surface of the substrate 17 in a proper way; further, the external device further comprises an injection needle support, wherein the injection needle support is fixedly arranged outside the needle cylinder, and the injection needle is kept in a constant-speed injection state in the injection process.
The detection method of the inclination angle sample injection device for detecting the furfural Raman spectrum in the transformer oil comprises the following steps,
the injection needle cylinder 1 sucks the liquid of the furfural-transformer oil as a sample to be detected, one end of the injection hose 6 is connected with the injection needle head 2 on the injection needle cylinder 1, the other end is connected with the injection port 7,
opening the drawing type clamping groove 14 along the guide rail, placing the substrate 17 on the surface of the substrate clamping groove 9, placing the substrate 17 in the quartz glass cover 10, wherein the inclination angle of the surface of the substrate 17 is 30 degrees, so that the liquid to be measured can conveniently flow from the top end to the bottom end of the substrate 17;
the ceramic heating plate 15 is heated so that the temperature of the surface of the substrate 17 reaches a predetermined temperature,
the injection button 5 is connected with the power supply to control the driving motor to push and pull the injection needle push-pull rod 4, a sample to be detected is dripped into the sample inlet 7 at a preset speed, and a liquid sample enters the sample inlet 8 through the sample inlet 7, so that the sample flows through the bottom end along the width direction of the top end of the surface of the substrate 17, the furfural in the transformer oil is specifically adsorbed when the liquid to be detected flows through the surface of the substrate 17, and the liquid which participates in the reaction on the surface of the substrate 17 can enter the lower waste liquid collector 12 through the waste liquid slit 16 under the action of gravity;
and (3) acquiring data by aligning a Raman spectrum with the surface of the substrate 17, acquiring a Raman spectrum chart, opening the drawing type clamping groove 14 after the test is finished, removing the substrate 17, opening a switch of the waste liquid collector 12, and carrying out centralized treatment on the waste liquid after the test.
In one embodiment, detecting comprises:
(1) The liquid sample is injected, the furfural-transformer oil liquid is sucked into the syringe by adopting a needle tube, the needle tube is fixed on a microinjection pump, an injection hose 6 matched with the needle is sleeved on the needle, and the other end of the hose is connected with an injection port 7 of the portable injector.
(2) The drawing type clamping groove 14 is opened, the developed substrate 17 is placed on the surface of the substrate clamping groove 9, the substrate 17 is pushed into the portable dip angle sample injection cavity, the drawing type clamping groove is placed on the surface of the substrate clamping groove 9, the angle between the surface of the substrate 17 and the bottom of the portable dip angle sample injector is 30 degrees, and liquid to be measured conveniently flows from the top end to the bottom end of the substrate 17.
(3) The MCH alumina ceramic heating plate 15 is started to heat the green button, and the temperature is controlled at about 60 ℃, so that the temperature of the surface of the substrate 17 can reach about 60 ℃.
(4) The power supply of the needle push-pull rod 4 was started, and the liquid sample was dropped into the sample inlet 7 at a rate of 100. Mu.L/s. The liquid sample enters the cuboid sample injection groove 8 through the sample injection port 7, so that the liquid sample can be contacted with the surface of the substrate 17 as simultaneously as possible.
(5) When the liquid to be detected flows through the surface of the substrate 17, the liquid can realize specific adsorption on the furfural in the transformer oil, 2mL of the liquid is completely dripped into the portable dip angle sampler, and the liquid which participates in the reaction on the surface of the substrate 17 can pass through the bottom slit according to the liquid flow rule and enter the lower waste liquid collector 12.
(6) And (3) aligning the ATR3000 probe of the portable Raman spectrometer with the quartz glass surface of the portable tilt angle sampler, performing automatic focusing, and acquiring a Raman spectrogram to acquire data.
(7) After the test is completed, the pull type clamping groove 14 is opened, the substrate 17 is taken down, and the inclined plane is cleaned. And opening a switch of the waste liquid collector 12 to intensively treat the tested waste liquid.
In one embodiment, the method of detection includes,
(1) the injection needle sampling procedure is that 2ml of liquid sample is moved into the injection needle, for the on-site oil sample of transformer oil, the transformer should be sampled from the lower valve, the throttle is cleaned with clean rag before sampling, then the oil is discharged and washed clean, and the oil sample bottle is washed at least twice, then the oil is directly injected into the sample bottle (the middle of the oil sample bottle is not in transition with rubber tube, filter paper or other containers, tools, etc.), the sample bottle must be filled, space must not be reserved, then the oil sample bottle is covered with bottle stopper, and the oil sample bottle is cleaned and then labeled. Then the needle is pulled out from the disposable needle tube with 5mL, the oil sample is sucked, no bubbles are remained, and after the oil sample with 2mL is sucked, the needle is rapidly assembled and locked.
(2) The sampling needle is fixed on the needle tube fixer 3, and a sampling hose 6 with matched caliber is arranged at the top of the needle head, the length of the sampling hose 6 is 50mm, and the other end of the injection hose is connected with the sampling port 7.
(3) The heating switch 13 is started to enable the sample bearing surface of the portable inclination angle sampler to enter a preheating mode in advance, and after 1min, the average temperature of the inclined plane reaches about 60 ℃.
(4) The drawing type clamping groove 14 is opened, the prepared substrate 17 is placed in the center of the substrate clamping groove 9, the position above the substrate 17 is completely parallel to the sample injection groove 8 and is positioned on the same horizontal line, and the purpose of doing so is to enable oil drops to completely contact with the substrate 17, so that the enrichment effect of furfural molecules is realized.
(5) The bottom of the substrate clamping groove 9 is provided with the heat conducting copper sheet 11, which not only can play a role in quick heat transfer, but also can prevent the lower MCH alumina ceramic heating plate 15 from being polluted as a partition.
(6) The MCH alumina ceramic heater plate 15 is mounted under the thermally conductive copper sheet 11, 1x1cm in size, the same as the substrate card slot 9 in size, in order to enable the substrate 17 to be heated uniformly.
(7) The inclination angle between the inner bearing plane and the horizontal plane of the portable inclination angle sample injection device is 30 degrees, and according to the liquid flow rule, the oil sample can flow from the upper part to the lower part of the substrate 17 and fully contact with the surface of the substrate 17.
(8) A slit of 1mm of oil is reserved between the heat conducting copper sheet 11 and the waste liquid collector 12, so that liquid flowing through the substrate 17 can be recovered in the waste liquid collector 12, and environmental pollution is avoided.
(9) When the furfural-transformer oil sample flows through the surface of the substrate 17, as the surface of the substrate 17 is coupled with oil 4-ATP molecules and the substrate 17 is soaked in 65% sulfuric acid solution in advance, the substrate 17 can specifically capture furfural in the transformer oil under the conditions of acid and heat, so that the furfural molecules completely occupy 'hot spots', and the detection sensitivity is higher.
The portable raman spectrometer in the step (9) is an ATR8800 auto-focusing auto-scanning raman spectrometer of the osbeck zenda company, and the wavelength of the excitation light corresponding to the detection is 785nm.
Preparing furfural-transformer oil solutions (100-0.01 mg/L) with different concentration gradients by adopting a pipetting gun, soaking a substrate in the solutions with different concentrations for 360min, and transferring the substrate into a portable dip angle sample injection device for Raman spectrum acquisition (laser power: 30mW, integration time: 1s, and integration times: 10 times). As can be seen from FIG. 3, at 1080cm -1 As the external standard peak, along with the reduction of the concentration of the furfural, the furfural is positioned at 1658cm -1 The characteristic raman peak at the concentration was gradually decreased until the characteristic furfural peak at the concentration of 0.01mg/L was submerged, so that the lowest detection limit was 0.025mg/L.
The basic principles of the present application have been described above in connection with specific embodiments, however, it should be noted that the advantages, benefits, effects, etc. mentioned in the present application are merely examples and not limiting, and these advantages, benefits, effects, etc. are not to be considered as necessarily possessed by the various embodiments of the present application. Furthermore, the specific details disclosed herein are for purposes of illustration and understanding only, and are not intended to be limiting, as the application is not intended to be limited to the details disclosed herein as such.
The foregoing description has been presented for purposes of illustration and description. Furthermore, this description is not intended to limit the embodiments of the application to the form disclosed herein. Although a number of example aspects and embodiments have been discussed above, a person of ordinary skill in the art will recognize certain variations, modifications, alterations, additions, and subcombinations thereof.
Claims (9)
1. An inclination angle sample injection device for detecting the Raman spectrum of furfural in transformer oil is characterized by comprising,
an injection syringe containing a sample to be tested, the injection syringe including an injection end for outputting the sample to be tested,
an injection needle which is connected with the injection end of the injection syringe in a sealing way,
a sample injection hose which is connected with the injection needle in a sealing way,
an injection needle push-pull rod which is connected with the injection needle cylinder in a sliding and sealing way;
a needle tube holder nested in the syringe to hold the syringe,
a fixing clamp of the injection needle push-pull rod, which is fixed at the end part of the injection needle push-pull rod,
a driving motor which controllably pushes and pulls the injection needle push-pull rod,
a power supply connected to the driving motor,
an injection button connected with the power supply to control the driving motor to push and pull the injection needle push-pull rod;
a waste liquid collector, the upper surface of which is provided with a pair of guide rails and a waste liquid slit perpendicular to the guide rails for flowing in waste liquid;
a quartz glass cover which is covered on the waste liquid collector and comprises,
a sample inlet which is arranged above the quartz glass cover and is connected with the sample inlet hose,
the sample injection groove penetrates through the quartz glass cover and is positioned below the sample injection port;
an inclination bearing device supported on the waste liquid collector and accommodated in the quartz glass cover, the inclination bearing device comprising,
a pull-out type clamping groove which is connected with the pair of guide rails in a sliding way,
a ceramic heating plate which is obliquely arranged in the drawing clamping groove at a preset angle,
a heat conducting copper sheet laid on the top surface of the ceramic heating plate, the heat conducting copper sheet is provided with a substrate clamping groove for accommodating a substrate,
the substrate is detachably connected with the substrate clamping groove and is just opposite to the sample introduction groove, the surface of the substrate is coupled with oil 4-ATP molecules, a sample from a syringe enters the sample introduction port through a sample introduction hose, flows through the bottom end from the top end of the substrate through the sample introduction groove, and then enters the waste liquid collector through the waste liquid slit.
2. The tilt angle sampling apparatus of claim 1, wherein the syringe preferably comprises an injection end for outputting a sample to be tested and a drive end opposite the injection end, the needle push-pull rod being slidably and sealingly connected to the syringe via the drive end.
3. The tilt angle sampling apparatus of claim 1, wherein the needle front end retention clip is nested outside the injection end to retain the needle.
4. The tilt angle sampling apparatus of claim 1, wherein the draw-in type clamping groove is configured to adjust a predetermined angle of tilt of the ceramic heating plate.
5. The tilt angle sampling apparatus of claim 1, wherein the predetermined angle is 30 degrees.
6. The tilt angle sampling apparatus of claim 1, wherein the needle cartridge employs a 5ml capacity.
7. The tilt angle sampling apparatus of claim 1, wherein the substrate is a silver nanowire SERS substrate.
8. The tilt angle sampling apparatus of claim 1, further comprising a raman spectrometer oriented toward the substrate.
9. The tilt angle sampling apparatus of claim 1, wherein the wavelength of excitation light from the raman spectrometer is 785nm.
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| CN202311501855.8A CN117538103A (en) | 2023-11-10 | 2023-11-10 | Inclination angle sampling device and method for detecting furfural Raman spectrum in transformer oil |
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| CN202311501855.8A CN117538103A (en) | 2023-11-10 | 2023-11-10 | Inclination angle sampling device and method for detecting furfural Raman spectrum in transformer oil |
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| CN219532602U (en) * | 2023-02-23 | 2023-08-15 | 陕西送变电工程有限公司 | Transformer oil syringe fixing device |
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