CN111537494A - Analysis method for furfural extraction effect in transformer oil - Google Patents

Analysis method for furfural extraction effect in transformer oil Download PDF

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CN111537494A
CN111537494A CN202010387973.0A CN202010387973A CN111537494A CN 111537494 A CN111537494 A CN 111537494A CN 202010387973 A CN202010387973 A CN 202010387973A CN 111537494 A CN111537494 A CN 111537494A
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unextracted
furfural
stock solution
raffinate
extraction
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李光茂
乔胜亚
朱晨
莫文雄
王勇
熊俊
杨森
陈莎莎
邓剑平
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Guangzhou Power Supply Bureau of Guangdong Power Grid Co Ltd
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Guangzhou Power Supply Bureau of Guangdong Power Grid Co Ltd
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering

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Abstract

The invention relates to the technical field of insulation online monitoring and fault diagnosis of electrical equipment, and discloses an analysis method for a furfural extraction effect in transformer oil. The analysis method disclosed by the invention is used for respectively carrying out Raman detection on the unextracted stock solution and the raffinate, and calculating the extraction rate according to a quantitative analysis model of the unextracted stock solution obtained by the Raman detection and the Raman characteristic peak area of the raffinate so as to analyze the extraction effect. The extraction effect analysis method has the advantages of high accuracy of extraction rate calculation, simple operation, high efficiency, low cost and environmental friendliness. The method provided by the invention indirectly measures the extraction rate by respectively performing Raman detection on the unextracted stock solution and the raffinate, and does not need to calculate the extraction rate by using methods such as a high performance liquid chromatography method, an electrochemical analysis method and the like in the traditional analysis method, so that the reagent and time can be effectively saved, and the method is an environment-friendly high-efficiency extraction effect analysis method.

Description

Analysis method for furfural extraction effect in transformer oil
Technical Field
The invention relates to the technical field of insulation online monitoring and fault diagnosis of electrical equipment, in particular to an analysis method for a furfural extraction effect in transformer oil.
Background
The power transformer is a core device in a power system, and the insulation operation condition and the health level of the power transformer are directly related to the safety and stability of a power grid. As with most electrical equipment, power transformers suffer from degradation under the action of electricity and heat, resulting in reduced insulation performance. Of these, furfural, which is produced only from the cracking of cellulose in paper insulation, is one of the most common indicators currently used to assess the degree of aging of oil-paper insulation. Therefore, the method can accurately detect the content of the dissolved furfural in the transformer oil, further judge the aging degree of the oil paper insulating material, and is an important technical support for ensuring the safe and reliable operation of the large-scale power transformer. Furfural is an important feature for evaluating the aging state of the oiled paper insulation equipment and needs to be accurately detected. When the extraction effect is analyzed, the furfural concentration of the extraction liquid is directly measured by using the traditional methods such as high performance liquid chromatography, electrochemical analysis and the like, and the problems of complex detection procedure, high requirement on operators, high cost, low efficiency and the like are faced.
Disclosure of Invention
Based on this, it is necessary to provide an analysis method for the furfural extraction effect in transformer oil, aiming at the problems that the furfural concentration of the extraction liquid is measured by using the traditional method, the detection procedure is complex, the requirement on operators is high, the cost is high and the efficiency is low.
A method for analyzing the furfural extraction effect in transformer oil comprises the steps of extracting furfural dissolved in the transformer oil, and reserving unextracted stock solution and raffinate; respectively carrying out Raman detection on the unextracted stock solution and the raffinate, and establishing a quantitative analysis model of the unextracted stock solution; and calculating the extraction rate according to the Raman characteristic peak areas of the quantitative analysis model and the raffinate, and drawing an extraction effect analysis curve.
In one embodiment, deionized water is used to extract furfural dissolved in transformer oil.
In one of the examples, equal amounts of unextracted dope and raffinate were retained.
In one embodiment, deionized water and unextracted stock solution are mixed, mixed by ultrasonic oscillation for 10-15 min, and then centrifuged by a centrifuge at 7500-8500 r/min for 5-10 min.
In one embodiment, when the unextracted stock solution and the raffinate are subjected to Raman detection respectively, the same Raman characteristic peak is selected, and the Raman characteristic peak is 1702cm-1
In one embodiment, the establishing of the quantitative analysis model of the unextracted stock solution comprises taking the concentration of the furfural dissolved in the transformer oil as an abscissa and taking the unextracted stock solution at 1702cm-1Taking the Raman characteristic peak area as a vertical coordinate, and establishing a quantitative analysis model of the unextracted stock solution.
In one embodiment, the unextracted stock solution is treated at 1702cm using least squares-1And carrying out unitary linear regression on the Raman characteristic peak area and the concentration of furfural dissolved in the transformer oil to obtain a quantitative analysis model of the unextracted stock solution.
In one embodiment, the raman characteristic peak area of the raffinate obtained after raman detection is taken into a quantitative analysis model of the unextracted stock solution to obtain the furfural concentration in the raffinate.
In one embodiment, the extraction rate is calculated by the formula of extraction rate ═ (furfural concentration of unextracted stock solution — furfural concentration of raffinate obtained by raman spectroscopy calculation)/furfural concentration of unextracted stock solution.
In one embodiment, the drawing of the extraction effect analysis curve comprises drawing of an extraction effect analysis curve by taking the extraction rate as an abscissa and the concentration of the furfural dissolved in the transformer oil as an ordinate; and analyzing the extraction effect of the Raman detection of the furfural in the transformer oil extracted by the deionized water according to the extraction effect analysis curve.
According to the analysis method for the furfural extraction effect in the transformer oil, the extraction effect is analyzed by respectively carrying out Raman detection on the unextracted stock solution and the raffinate and calculating the extraction rate according to a quantitative analysis model of the unextracted stock solution obtained by the Raman detection and the Raman characteristic peak area of the raffinate. The extraction effect analysis method has the advantages of high accuracy of extraction rate calculation, simple operation, high efficiency, low cost and environmental friendliness. The method provided by the invention indirectly measures the extraction rate by respectively performing Raman detection on the unextracted stock solution and the raffinate, and does not need to calculate the extraction rate by using methods such as a high performance liquid chromatography method, an electrochemical analysis method and the like in the traditional analysis method, so that the reagent and time can be effectively saved, and the method is an environment-friendly high-efficiency extraction effect analysis method.
Drawings
FIG. 1 is a flow chart of a method for analyzing the extraction effect of furfural in transformer oil according to an embodiment of the present invention;
FIG. 2 is a flowchart of a method for plotting an analysis curve of extraction effect according to an embodiment of the present invention;
FIG. 3 is a model curve of the Raman characteristic peak area of the unextracted stock solution and the quantitative analysis of the furfural concentration in the transformer oil according to one embodiment of the present invention;
fig. 4 is an extraction efficiency and an extraction effect analysis curve of furfural concentration in transformer oil according to an embodiment of the invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," "upper," "lower," "front," "rear," "circumferential," and the like are based on the orientation or positional relationship shown in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Furfural is an important feature for evaluating the aging state of the oiled paper insulation equipment and needs to be accurately detected. The Raman spectroscopy based on the Raman effect can quickly and accurately detect the dissolved aging characteristics in the oil. The key is to improve the Raman detection sensitivity of the dissolved furfural in the oil. Based on the fact that furfural is dissolved in deionized water extracted transformer oil, the Raman detection sensitivity can be improved. When the extraction effect is analyzed, the furfural concentration of the extraction liquid is directly measured by using the traditional methods such as high performance liquid chromatography, electrochemical analysis and the like, the problems of complex detection procedure, high requirement on operators, high cost, low efficiency and the like are faced, the extraction rate cannot be quickly and accurately judged, and the indirect measurement of the extraction rate can be realized by combining Raman spectroscopy.
Fig. 1 is a flowchart illustrating an analysis method for an extraction effect of furfural in transformer oil according to an embodiment of the present invention, where the analysis method for the extraction effect of furfural in transformer oil includes the following steps S100 to S300.
S100: and extracting furfural dissolved in the transformer oil, and reserving unextracted stock solution and raffinate.
S200: and respectively carrying out Raman detection on the unextracted stock solution and the raffinate, and establishing a quantitative analysis model of the unextracted stock solution.
S300: and calculating the extraction rate according to the Raman characteristic peak areas of the quantitative analysis model and the raffinate, and drawing an extraction effect analysis curve.
According to the analysis method for the furfural extraction effect in the transformer oil, provided by the invention, the unextracted stock solution and the raffinate before extraction of furfural dissolved in the transformer oil are respectively subjected to Raman detection. And establishing a quantitative analysis model of the unextracted stock solution according to the detection result, comparing the Raman characteristic peak area of the raffinate with the quantitative analysis model, obtaining the extraction rate of extracting the furfural in the transformer oil, and drawing an extraction effect analysis curve to analyze the extraction effect. The analysis method provided by the invention indirectly measures the extraction rate of Raman detection of the dissolved furfural in the transformer oil extracted by the deionized water, does not need to use the traditional high performance liquid chromatography, electrochemical analysis method and the like, saves reagents and time, can realize the analysis and measurement of the Raman detection extraction effect of the dissolved furfural in the transformer oil extracted by the deionized water, and has the advantages of high calculation accuracy of the extraction rate, simple operation, high efficiency, low cost and environmental friendliness.
In one of the examples, equal amounts of unextracted dope and raffinate were retained. Before extraction, a certain amount of unextracted stock solution was retained. After extraction, an equal amount of raffinate was retained as the unextracted dope. When the non-extracted stock solution and the raffinate are respectively subjected to Raman detection, the extraction rate of furfural can be obtained according to the comparison of the furfural content in the non-extracted stock solution and the raffinate, so that the extraction effect of furfural dissolved in the transformer oil is judged.
In one embodiment, deionized water is used to extract furfural dissolved in transformer oil. The components in the transformer oil are complex, the furfural content is low, and therefore separation and enrichment are needed before a sample is analyzed, so that the detection sensitivity is effectively improved. During extraction, deionized water is added into the transformer oil to extract furfural dissolved in the transformer oil. Compared with the conventional analysis method in which methanol is used as an extracting agent for Raman detection, the analysis method provided by the invention uses deionized water as the extracting agent for furfural and is used for Raman detection, so that the lower detection limit of a test is effectively reduced, and the Raman detection sensitivity of furfural in transformer oil is further improved.
In one embodiment, after mixing deionized water and unextracted stock solution, ultrasonic oscillation is used for 10-15 min to fully mix the deionized water and the transformer oil, and then a centrifuge is used for centrifuging for 5-10 min at the speed of 7500-8500 r/min. The ultrasonic oscillation is generated by utilizing high-frequency sound waves of ultrasonic waves and is used for extracting furfural. The ultrasonic wave can generate sound wave cavitation between the solvent and the furfural, so that bubbles in the solution are formed, grown and exploded and compressed, and the contact area between the furfural and the extraction solvent is increased. Compared with the conventional extraction technology, the ultrasonic-assisted extraction technology has the advantages of few operation steps, simple extraction process and difficult pollution to the extract. And putting the mixed solution of the deionized water and the unextracted stock solution subjected to ultrasonic extraction into a centrifuge, and centrifuging for 5-10 min at the speed of 7500-8500 r/min to enable the extract and the extraction solution to be layered. In this example, the centrifuge speed of the centrifuge was 8000 r/min. The sedimentation velocity of particles in the mixed solution can be accelerated by utilizing the strong centrifugal force generated by the high-speed rotation of the centrifugal machine, and the substances with different sedimentation coefficients and buoyancy densities in the mixed solution are separated.
In one embodiment, when the unextracted stock solution and the raffinate are subjected to Raman detection respectively, the same Raman characteristic peak is selected, and the Raman characteristic peak is 1702cm-1. According to the Raman detection result, the furfural molecules are 1702cm in unextracted stock solution and raffinate respectively-1There is a strong raman characteristic peak. Thus, for unextracted raw liquor and raffinateWhen the concentration of furfural in the liquid is analyzed for extraction effect, 1702cm is selected-1The Raman characteristic peak data is used as evaluation basis.
In one embodiment, the establishing of the quantitative analysis model of the unextracted stock solution comprises taking the concentration of the furfural dissolved in the transformer oil as an abscissa and taking the unextracted stock solution at 1702cm-1Taking the Raman characteristic peak area as a vertical coordinate, and establishing a quantitative analysis model of the unextracted stock solution. Taking the concentration of furfural dissolved in the transformer oil as the abscissa of the quantitative analysis model, and placing the unextracted stock solution at 1702cm-1The Raman characteristic peak area is used as a vertical coordinate, the quantitative relation between the concentration of furfural dissolved in the transformer oil and the Raman characteristic peak area can be effectively and visually observed, and the extraction rate can be obtained by combining the Raman characteristic peak area in the raffinate, so that the extraction effect can be analyzed.
In one embodiment, the unextracted stock solution is treated at 1702cm using least squares-1And carrying out unitary linear regression on the Raman characteristic peak area and the concentration of furfural dissolved in the transformer oil to obtain a quantitative analysis model of the unextracted stock solution. The quantitative analysis model of the unextracted stock solution is established by applying a least square method, and the goodness of fit of the quantitative relation between the concentration of furfural dissolved in the transformer oil and the Raman characteristic peak area is high, and the detection error is small.
In one embodiment, the raman characteristic peak area of the raffinate obtained after raman detection is taken into a quantitative analysis model of the unextracted stock solution to obtain the furfural concentration in the raffinate. Because the quantitative analysis model is that the unextracted stock solution is at 1702cm-1And the relation model between the Raman characteristic peak area and the concentration of the furfural dissolved in the transformer oil is obtained, so that the concentration of the furfural corresponding to the Raman characteristic peak area of the raffinate can be obtained by substituting the Raman characteristic peak area of the raffinate into the quantitative analysis model. The concentration of the furfural in the raffinate is indirectly obtained and compared with the concentration of the furfural in the unextracted stock solution, so that the extraction rate of the extraction operation can be obtained.
In one embodiment, the extraction rate is calculated by the formula of extraction rate ═ (furfural concentration of unextracted stock solution — furfural concentration of raffinate obtained by raman spectroscopy calculation)/furfural concentration of unextracted stock solution. By substituting the furfural concentration in the unextracted stock solution and the furfural concentration of the raffinate obtained by raman spectroscopy calculation into the above formula, the extraction rate based on raman detection of dissolved furfural in the deionized water-extracted transformer oil can be indirectly measured.
Fig. 2 is a flowchart illustrating a method for drawing an extraction effect analysis curve according to an embodiment of the present invention, wherein the drawing of the extraction effect analysis curve includes the following steps S310 and S320.
S310: and drawing an extraction effect analysis curve by taking the extraction rate as a horizontal coordinate and the concentration of the furfural dissolved in the transformer oil as a vertical coordinate.
S320: and analyzing the extraction effect of the Raman detection of the furfural in the transformer oil extracted by the deionized water according to the extraction effect analysis curve.
Specifically, when an extraction effect analysis curve is drawn, the extraction rate obtained in the above step is taken as an abscissa, the concentration of furfural dissolved in the transformer oil is taken as an ordinate, a coordinate system is constructed, and an extraction effect analysis curve graph is drawn. And according to the extraction effect analysis curve graph, the extraction effect of the converter oil can be analyzed based on the change relation between the extraction rate of the deionized water to the furfural in the converter oil and the concentration of the dissolved furfural in the converter oil. According to the analysis method provided by the invention, the traditional high performance liquid chromatography, electrochemical analysis and the like are not needed, the reagent and time are saved, the analysis and measurement of the Raman detection extraction effect of the dissolved furfural in the deionized water extracted transformer oil can be realized, and the method has the advantages of high calculation accuracy of the extraction rate, simplicity in operation, high efficiency, low cost and environmental friendliness.
The invention is described in detail below with reference to specific examples, which are intended to further illustrate the invention, but not to limit it. The instruments and reagents used in the examples are all commercially available.
Combined laboratory liquid Raman spectrum detection planeThe platform is used for carrying out Raman spectrum detection on unextracted stock solution and raffinate, and comprises main devices such as a laser, an Andor iDus-416 type CCD, a Leica DM2700 type upright microscope, an Andor SR-500i dispersion type Raman spectrometer and the like, wherein the laser wavelength of the laser is 532nm, the output power is 100mW, the line width is less than 0.001pm, the noise is less than 0.25% rms, the output laser mode is TEM00, in a microscope light path, a 50 × long-focus objective lens is selected, a 100 mu m slit width and a 1200l/mm type grating are adopted, and the spectrum detection range is 545cm-1To 570cm-1The Raman detection integration times are 2, the exposure time is 30s, the read noise of a CCD detector is less than 5e/pixel, the refrigeration temperature can reach-75 ℃, the monitoring wavelength range is 200-1100 nm, the pixel is 2000 × 256, the dark current is less than 0.0006e/s/pixel, and the Raman scattering wavelength monitoring of the trace furfural dissolved in the transformer oil can be met.
In order to help better understand the technical scheme of the application, the following analysis method test of the furfural extraction effect in the transformer oil is performed by taking pure furfural as a material.
Test step 1: preparing the unextracted stock solution
Excess pure furfural was dissolved in the test oil to prepare a 353mg/L furfural saturated oil solution. And carrying out ultrasonic oscillation on the furfural saturated oil solution for 15min so as to uniformly mix the pure furfural in the test oil. And then diluting the furfural saturated oil solution to different degrees to prepare several unextracted stock solutions with different furfural concentrations, wherein the unextracted stock solutions with different furfural concentrations are 100mL respectively, and light shielding is required in the whole process of preparing the unextracted stock solutions. The concentrations of the unextracted stock solution of the prepared furfural with nine concentration gradients are 176mg/L, 88mg/L, 44mg/L, 22mg/L, 11mg/L, 5.5mg/L, 2.75mg/L, 1.38mg/L and 0.69mg/L respectively.
Test step 2: preparation of raffinate
Respectively extracting 70mL of unextracted stock solutions of the nine furfural with concentration gradients, and mixing the unextracted stock solutions with deionized water according to a ratio of 10: 1. And placing the prepared nine different mixed solutions into nine centrifuge tubes with the capacity of 100mL, and respectively carrying out ultrasonic oscillation for 15min to fully mix the unextracted stock solution and the deionized water. Nine centrifuge tubes containing the mixed solution after ultrasonic oscillation were centrifuged at 8000r/min using a centrifuge. After 10min, nine centrifuge tubes were removed and the centrifuged supernatant raffinate was extracted separately for further assay.
Test step 3: determination of Raman characteristic peaks of furfural
Before Raman spectrum detection, detection parameters of a laboratory liquid Raman spectrum detection platform are set to be 1200l/mm type grating, the width of a slit is selected to be 100 mu m, the integration time is set to be 30s, and the integration times is set to be 2 times. Respectively carrying out Raman detection on nine unextracted stock solutions and raffinate of furfural with certain concentration gradients, and determining Raman characteristic peaks of furfural in the unextracted stock solutions and the raffinate according to Raman spectrograms obtained by detection. Wherein, the furfural in the unextracted stock solution and the raffinate is 1702cm-1Has stronger Raman characteristic peak, therefore, 1702cm is selected-1The Raman characteristic peak data is used as evaluation basis.
Test step 4: determination of furfural concentration in raffinate
The unextracted stock solution measured in test step 3 was measured at 1702cm using the least squares method-1And carrying out unitary linear regression on the Raman characteristic peak area and the concentration of furfural dissolved in the transformer oil to obtain a quantitative analysis model of the unextracted stock solution. Wherein the quantitative analysis model takes the concentration of furfural dissolved in the transformer oil as a horizontal coordinate x, and the unextracted stock solution is 1702cm-1The area of the raman characteristic peak at (a) is taken as the ordinate y. Fig. 3 is a raman characteristic peak area of the unextracted raw liquid and a quantitative analysis model curve of furfural concentration in transformer oil according to an embodiment of the present invention, and a relational expression of the quantitative analysis model of the unextracted raw liquid calculated by a least square method is: y is 2179.7034+1080.87179x and goodness of fit is R20.99541. The raffinate obtained in test step 3 was found to be 1702cm-1Substituting the Raman characteristic peak area into the quantitative analysis model of the unextracted stock solution for calculationAnd obtaining the concentration of furfural in the raffinate.
Test step 5: drawing of extraction effect curve
And (4) calculating the extraction rate of furfural in the raffinate after extracting the transformer oil by deionized water according to the extraction rate (the concentration of furfural in the unextracted stock solution-the concentration of furfural in the raffinate calculated by Raman spectroscopy)/the concentration of furfural in the unextracted stock solution in combination with the concentration of furfural in the raffinate obtained in the test step 4. Fig. 4 is an extraction efficiency analysis curve of the extraction rate and the concentration of furfural in the transformer oil according to an embodiment of the present invention, where the extraction efficiency analysis curve is a curve drawn by taking the extraction rate as an abscissa and the concentration of furfural dissolved in the transformer oil as an ordinate. And analyzing the extraction effect of extracting furfural in the transformer oil by using deionized water according to the drawn extraction effect analysis curve. As can be seen from fig. 4, the change trend of the extraction rate of furfural in the transformer oil based on deionized water extraction and the concentration of furfural dissolved in the transformer oil is as follows: along with the continuous reduction of the concentration of the furfural dissolved in the transformer oil, the extraction rate shows a rule of increasing and then decreasing. Therefore, for a furfural solution with lower concentration, the extraction effect of extracting furfural from transformer oil based on deionized water has certain limitation.
Although a few exemplary embodiments of the present invention have been shown and described, it would be appreciated by those skilled in the art that changes may be made in these exemplary embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. An analysis method for furfural extraction effect in transformer oil is characterized by comprising the following steps:
extracting furfural dissolved in the transformer oil, and reserving unextracted stock solution and raffinate;
respectively carrying out Raman detection on the unextracted stock solution and the raffinate, and establishing a quantitative analysis model of the unextracted stock solution;
and calculating the extraction rate according to the Raman characteristic peak areas of the quantitative analysis model and the raffinate, and drawing an extraction effect analysis curve.
2. The method of claim 1, wherein the extraction of furfural dissolved in transformer oil is performed using deionized water.
3. The process of claim 1 wherein equal amounts of unextracted liquor and raffinate are retained.
4. The method as claimed in claim 3, wherein the deionized water and the unextracted stock solution are mixed, mixed by ultrasonic oscillation for 10-15 min, and then centrifuged by a centrifuge at 7500-8500 r/min for 5-10 min.
5. The method of claim 1The method is characterized in that when the unextracted stock solution and the raffinate are respectively subjected to Raman detection, the same Raman characteristic peak is selected, and the Raman characteristic peak is 1702cm-1
6. The method of claim 5, wherein said modeling the quantitative analysis of the unextracted liquor comprises:
taking the concentration of furfural dissolved in the transformer oil as a horizontal coordinate, and taking unextracted stock solution at 1702cm-1Taking the Raman characteristic peak area as a vertical coordinate, and establishing a quantitative analysis model of the unextracted stock solution.
7. The method of claim 6, wherein the unextracted liquor is treated at 1702cm using least squares-1And carrying out unitary linear regression on the Raman characteristic peak area and the concentration of furfural dissolved in the transformer oil to obtain a quantitative analysis model of the unextracted stock solution.
8. The method according to claim 7, wherein the concentration of furfural in the raffinate is obtained by substituting the Raman characteristic peak area of the raffinate obtained by Raman detection into a quantitative analysis model of the unextracted stock solution.
9. The method of claim 1, wherein the extraction rate is calculated by the formula:
the extraction rate (furfural concentration of the unextracted stock solution-furfural concentration of the raffinate obtained by raman spectroscopy calculation)/furfural concentration of the unextracted stock solution.
10. The method of claim 1, wherein said plotting an extraction effect analysis curve comprises:
drawing an extraction effect analysis curve by taking the extraction rate as a horizontal coordinate and the concentration of furfural dissolved in the transformer oil as a vertical coordinate;
and analyzing the extraction effect of the Raman detection of the furfural in the transformer oil extracted by the deionized water according to the extraction effect analysis curve.
CN202010387973.0A 2020-05-09 2020-05-09 Analysis method for furfural extraction effect in transformer oil Pending CN111537494A (en)

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