CN111157316A - Preparation method and application of standard sample for verifying gas component content determination capability - Google Patents
Preparation method and application of standard sample for verifying gas component content determination capability Download PDFInfo
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- CN111157316A CN111157316A CN202010053645.7A CN202010053645A CN111157316A CN 111157316 A CN111157316 A CN 111157316A CN 202010053645 A CN202010053645 A CN 202010053645A CN 111157316 A CN111157316 A CN 111157316A
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- 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
Abstract
The invention provides a preparation method and application of a standard sample for verifying the gas component content determination capability, which comprises the following steps: preparing a blank oil sample; preparing characteristic mixed gas according to the preset concentration of the gas components dissolved in the blank oil sample; and introducing the characteristic mixed gas into the blank oil sample, so that the characteristic mixed gas is fully dissolved in the blank oil sample to prepare a standard oil sample in which gas components with preset concentrations are dissolved. The preparation method provided by the invention is simple to operate and high in automation degree, and the obtained standard sample is uniform and stable, so that the accuracy of a verification test can be ensured. The standard sample provided by the invention can effectively evaluate the component content detection capability and level of a transformer oil analysis laboratory, can be used for qualitative and quantitative analysis of components of dissolved gas in transformer oil, verification of an online or offline testing instrument and quality control and assessment of a test result, and can guarantee the detection capability level of the transformer oil analysis laboratory.
Description
Technical Field
The invention relates to the technical field of insulating oil detection and laboratory capacity verification, in particular to a preparation method and application of a standard sample for verifying gas component content determination capacity.
Background
The insulating oil and solid insulation in the oil-immersed power transformer can be gradually aged and decomposed under the action of temperature, electric field, oxygen, moisture and the like to generate various low molecular hydrocarbons and H2、CO、CO2And the like. Most of these gases are dissolved in oil, experience proves that the content of various components of the gases in the oil is directly related to the nature and the degree of faults, and the analysis (DGA) technology of the dissolved gases in the oil is widely used for fault diagnosis and state assessment of oil-immersed power transformers. An oil analysis laboratory of a power enterprise is a main body for monitoring the state of transformer oil, a plurality of indexes of the transformer oil need to be regularly detected, and dissolved gas in the oil is an important index. In addition, the laboratory test result can be compared with an on-line monitoring device and an instrument and meter, and the accuracy of the on-line monitoring device for the dissolved gas in the oil is verified. Therefore, the level of detectability and quality control in the oil analysis laboratory is very important.
The inter-laboratory alignment is the measurement or monitoring of organization, administration and evaluation of the same or similar items by two or more laboratories under predefined conditions. Although the comparison experiment activity is only the inspection and detection of a certain specific parameter or product, the whole quality and level of the mechanism can be reflected, including various aspects such as equipment management, personnel ability, environmental conditions, system operation and the like. Through the statistical analysis to the inspection testing result, evaluate each participating in the organization to the inspection testing capability of specific test, can discern the difference between the problem that the laboratory exists and the laboratory, it is more fair to compare the result between the laboratory to the inside quality supervision of electric wire netting enterprise simultaneously. Therefore, the laboratory-to-laboratory ratio for organizing and implementing the analysis of the dissolved gas in the transformer oil plays an important role in improving the detection capability and ensuring the reliable operation of power equipment. Internationally, the comparison among laboratories for analyzing the dissolved gas in the oil by CIGRE organization is carried out by 25 laboratories from 15 different countries, and the conclusion that the average accuracy of each laboratory is +/-15% under the condition of a medium-concentration oil sample is obtained, but the comparison among laboratories does not analyze data by using a statistical method. In China, the Yunnan institute of Electrical science and technology organizes the comparison among oil analysis laboratories of indexes such as water-soluble acid, acid value, closed flash point, breakdown voltage and the like of the transformer oil in local places, but the preparation and implementation methods of the sample for verifying the content determination capability of the dissolved gas components in the transformer oil are not reported at present.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of a standard sample for verifying the determination capability of the content of gas components, and aims to solve the problem that a verification sample for the determination capability of the content of dissolved gas components in transformer oil is lacked in the prior art.
The invention provides a preparation method of a standard sample for verifying the gas component content determination capability, which comprises the following steps: step 1, preparing a blank oil sample; step 2, preparing characteristic mixed gas according to the preset concentration of the gas components dissolved in the blank oil sample;
and 3, introducing the characteristic mixed gas into the blank oil sample, so that the characteristic mixed gas is fully dissolved in the blank oil sample, and preparing the standard oil sample in which the gas components with preset concentration are dissolved.
Further, in the above preparation method of the standard sample for verifying the gas component content determination capability, in step 1, a certain volume of transformer oil is extracted, the transformer oil is degassed by a vacuum degassing method to be in an undersaturated state, and then the transformer oil is stored in a closed container.
Further, in the above method for preparing a standard sample for verifying the capability of measuring the content of a gas component, the characteristic mixed gas includes at least two of hydrogen, carbon monoxide, carbon dioxide, methane, ethane, ethylene and acetylene; the substrate gas is nitrogen or argon.
Further, in the above method for preparing a standard sample for verifying the capability of measuring the content of the gas component, in step 2, the concentration of each gas component in the characteristic mixed gas oil sample is determined according to the following formula:
in the formula: xiTo dissolve a certain gas component concentration in the oil, p is atmospheric pressure, CiCharacterised by the concentration of the gas component, K, in the gas mixtureiIs the partition coefficient, V ', of the gas component'gTo balance the volume of the characteristic mixture gas under modulation, V'1Is the oil sample volume at equilibrium conditions.
Further, in the above preparation method of the standard sample for verifying the gas component content determination capability, in the step 3, the characteristic mixed gas is introduced into the bottom of the oil tank containing the blank oil sample, so that the characteristic mixed gas contacts and dissolves the blank oil sample in the rising process, the characteristic mixed gas which is not dissolved in the blank oil sample is extracted from the upper layer of the oil tank and then introduced into the bottom of the oil tank, and is mixed with the blank oil sample for the second time, and the above circulation is performed until the characteristic mixed gas is fully dissolved in the oil sample, so that the standard oil sample in which the gas component with the preset concentration is dissolved is prepared.
Further, in the above method for preparing the standard sample for verifying the capability of measuring the content of the gas component, the standard oil sample contains CO and CH4And C2H2(ii) a Wherein the concentration of CO in the blank oil sample is 50-100 μ L/L, CH4The concentration in the blank oil sample is 20-50 μ L/L, C2H2The concentration in the blank oil sample is 10-20. mu.L/L.
Further, in the above method for preparing a standard sample for verifying the capability of measuring the content of a gas component, after the step 3, the method further comprises: and 4, standing for a period of time to enable the undissolved characteristic mixed gas to rise to the oil level and be discharged.
Further, in the above method for preparing a standard sample for verifying the capability of measuring the content of a gas component, after the step 4, the method further includes: and 5, equally distributing the prepared standard oil sample into preset sealed oil tanks, and storing the sealed oil tanks in an environment with a preset temperature.
The preparation method of the standard sample for verifying the gas component content determination capability provided by the invention is simple to operate and high in automation degree, and the obtained standard sample is uniform and stable, so that the accuracy of a verification test can be ensured. The standard sample provided by the invention can effectively evaluate the component content detection capability and level of a transformer oil analysis laboratory, can be used for qualitative and quantitative analysis of components of dissolved gas in transformer oil, verification of an online or offline test instrument and quality control and assessment of test results, guarantees the detection capability level of the transformer oil analysis laboratory, effectively monitors the operation state of a power transformer, warns faults and supports safe and stable operation of the whole power grid.
The invention also provides a standard sample for verifying the gas component content determination capability, which is prepared by adopting the method.
The invention also provides application of the standard sample for verifying the gas component content determination capability in transformer oil analysis laboratory detection capability verification, qualitative and quantitative analysis of dissolved gas components in transformer oil, verification of an online or offline testing instrument and quality control and assessment of a test result.
Drawings
Various other advantages and benefits 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. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic flow chart of a method for preparing a standard sample for verifying the capability of measuring the content of a gas component according to an embodiment of the present invention;
fig. 2 is a closed oil tank for storing a standard oil sample according to an embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure 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 disclosure to those skilled in the art. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Referring to fig. 1, a method for preparing a standard sample for verifying the capability of measuring the content of a gas component according to an embodiment of the present invention includes the steps of:
and step S1, preparing a blank oil sample.
Specifically, the oil sample may be transformer oil or the like, for example, 25 # or 45 # transformer oil. The method comprises the steps of extracting a certain volume of transformer oil, degassing the transformer oil by adopting a vacuum degassing method to enable the transformer oil to be in an undersaturation state, and then storing the transformer oil in a closed container. Wherein, the capacity of the oil sample can be determined according to the actual requirement. In this embodiment, the blank oil sample may be treated by a vacuum oil filter to remove impurities, moisture, and the like in the oil sample.
And step S2, preparing characteristic mixed gas according to the preset concentration of the gas components dissolved in the blank oil sample.
Specifically, the preset concentration of the dissolved gas component in the oil sample can be determined according to the actual application scenario. The characteristic mixed gas comprises at least two of hydrogen, carbon monoxide, carbon dioxide, methane, ethane, ethylene and acetylene; the substrate gas is nitrogen or argon. Determining the concentration of each gas component in the characteristic mixed gas according to the following formula:
in the formula: xiTo dissolve a certain gas component concentration in the oil, p is atmospheric pressure, CiCharacterised by the concentration of the gas component, K, in the gas mixtureiIs the partition coefficient, V ', of the gas component'gTo balance the volume of the characteristic mixture gas under modulation, V'1Is the oil sample volume at equilibrium conditions.
For example, the gas distribution coefficient K of each gasi(50 ℃) the following:
H2：0.06；CO：0.12；CO2：0.92；CH4：0.39；C2H2：1.02；C2H4：1.46；C2H6：2.30。
and step S3, introducing the characteristic mixed gas into the blank oil sample, so that the characteristic mixed gas is fully dissolved in the blank oil sample to prepare a standard oil sample dissolved with gas components with preset concentrations.
Specifically, the characteristic mixed gas is introduced into the bottom of an oil tank filled with the blank oil sample, so that the characteristic mixed gas is contacted with and dissolved in the blank oil sample in the rising process, the characteristic mixed gas which cannot be dissolved in the blank oil sample is extracted from the upper layer of the oil tank and then introduced into the bottom of the oil tank, and is subjected to secondary mixing with the blank oil sample, and the circulation is performed until the characteristic mixed gas is fully dissolved in the oil sample, so that the standard oil sample with the gas components dissolved in the preset concentration is prepared.
Due to CO and CH4And C2H2The gas is representative in the fault characteristic gas of the transformer, and is more stable to be dissolved in oil and is not easy to volatilize and lose. Preferably, the standard oil sample contains CO and CH4And C2H2(ii) a Wherein the concentration of CO in the blank oil sample is 50-100 μ L/L, CH4The concentration in the blank oil sample is 20-50 μ L/L, C2H2The concentration in the blank oil sample is 10-20. mu.L/L. Standard oil sample prepared in this exampleThe method can be used in the verification process of the capacity of measuring the content of the dissolved gas components in the transformer oil.
In this embodiment, after step 3, the method may further include: and 4, standing for a period of time to enable the undissolved characteristic mixed gas to rise to the oil level and be discharged. For example, the sample can be kept still for 30-60 min, so that the characteristic mixed gas is more fully dissolved in the blank oil sample, and the prepared standard oil sample is closer to the preset requirement.
Further, after the step 4, the method further comprises: and 5, equally distributing the prepared standard oil sample into preset sealed oil tanks, and storing the sealed oil tanks in an environment with a preset temperature.
Specifically, the prepared standard oil sample can be divided into a plurality of equal parts, each standard oil sample is numbered and marked, and then the standard oil sample is placed in a normal temperature environment for storage. The preset temperature is 20-30 ℃, preferably (25 +/-2) ℃ so as to avoid the change of the state of the standard oil sample, which is not beneficial to the subsequent application. The structure of the sealed oil tank is shown in fig. 2:
the airtight oil tank includes: the device comprises a tank body 1, a piston device, a bottom oil inlet valve 4 and a top oil outlet valve 5. The inside of the tank body 1 can be cylindrical, the piston device is arranged in the tank body, a through hole communicated with the piston rod 3 is formed in the piston head 2, the piston rod 3 is of a tubular structure, and the top oil outlet valve 5 is arranged at the outlet end of the piston rod 3. Sealing rings are arranged between the tank body 1 and the sealing cover plate 11 on the top surface and between the piston device and the side wall of the tank body 1 to ensure good sealing property. The container is filled with oil through the bottom oil filling port 4 with a certain pressure, air is squeezed out and oil leaks from the top oil outlet after the container is filled with oil, and the top oil outlet valve 5 and the bottom oil inlet valve 4 can be closed. When getting oil, open top and go out oily valve 5, go out oily valve 5 with sampling device interface connection on the top, push down piston 3 and just can extrude oil.
In this embodiment, can use the oil-gas mixing device who possesses functions such as oil feed, admit air, oil extraction, exhaust, oil circulation, gas circulation, keep hydro-cylinder pressure, wireless communication at the in-process of preparing standard sample to improve the degree of automation of preparation process.
In order to verify the stability and uniformity of the prepared standard sample, the standard sample prepared in this example can be tested as follows:
the homogeneity test procedure of the samples follows CNAS-GL003-2018 guide for evaluation of homogeneity and stability of samples for capacity verification, 10 or more samples are randomly extracted from the sample population for homogeneity test, each sample is numbered, each sample is tested at least 2 times under repeated conditions, repeated test samples are respectively sampled and tested in random order, the judgment standard of the homogeneity of the samples is according to the requirement of the F test, if F < the critical value of the degree of freedom (F1, F2) and the given significance level α (usually α is 0.05), the judgment standard of the homogeneity of the samples indicates that no significant difference exists between the samples and the samples, and the samples are homogeneous, and the judgment standard of the degree of freedom F < the critical value of the degree of freedom (F1, F2) and the given significance level α shows that the standard samples prepared in the embodiment are homogeneous.
The stability testing procedure of the samples followed the CNAS-GL003-2018 guide for evaluation of homogeneity and stability of samples for capability verification. 30 samples were randomly taken from the total sample population for stability testing. The first batch tested 10 samples, the second batch 10 samples after 10 days, and the third batch 10 samples after 20 days. The stability time was set to 30 days, covering the entire period from the sample issue to the report expiration date. During the stability test, the samples were kept at (25. + -. 2). degree.C. The judgment standard of the sample stability is according to the requirement of T test, if T<Significance level α (usually α ═ 0.05) with a critical value t of n-1α(n-1), the sample has better stability in the environment, and the result of participating in the capability verification laboratory is not influenced by the stability problem. After verification, T<Significance level α critical value t with degree of freedom n-1α(n-1), which shows that the standard sample prepared in this example is stable.
The method for preparing the standard sample for verifying the gas component content determination capability is simple and reliable, compared with the prior art, the method is higher in preparation accuracy and efficiency, and excellent in uniformity and stability, can meet capability comparison of measurement items of the content of dissolved gas components in transformer oil in a laboratory, verification of a detection method, qualitative and quantitative analysis, verification of an online or offline test instrument, and quality control and assessment of test results, is beneficial to guaranteeing the detection capability level of a transformer oil analysis laboratory, effectively monitors the operation state of a power transformer, warns faults, and supports safe and stable operation of a power grid.
The invention also provides a standard sample for verifying the gas component content determination capability.
The invention also provides application of the standard sample for verifying the gas component content determination capability in transformer oil analysis laboratory detection capability verification, qualitative and quantitative analysis of dissolved gas components in transformer oil, verification of an online or offline testing instrument and quality control and assessment of a test result.
The application of the invention in the verification of the detection capability of the transformer oil analysis laboratory is illustrated by the following specific examples:
by adopting a synchronous capacity verification plan, the capacity verification plan sends 1 part of oil sample to each participating laboratory, wherein the sample is 110mL transformer oil containing H2、CO、CO2、CH4、C2H4、C2H6、C2H2And the like. The test oil sample was enclosed in a sealed metal container (fig. 2) and externally affixed with a sample number, which was associated with a laboratory code and was numbered with a random number.
In order to protect the rights and interests of participating laboratories, the capacity verification plan assigns an independent and unique code to each of the participating laboratories, and the participating laboratories are represented by the codes when the test results, the capacity statuses, and the like related to the laboratories are described in the summary report.
The sample detection method follows GB/T17623 and 2017 gas chromatography determination method for the content of dissolved gas components in insulating oil; a detection instrument: a gas chromatograph; summary of the method: and (3) extracting gas dissolved in the oil sample after collecting the oil sample, separating and detecting each gas component by using a gas chromatograph, and calculating to obtain the content of the gas component dissolved in the oil. The analysis results of the gas dissolved in the oil were expressed in terms of microliter amounts (μ L/L) of the gas component contained per liter of the oil under the conditions of a temperature of 20 ℃ and a pressure of 101.3 kPa.
The determination of the public Value can adopt a Robust statistical mode (Robust statistical), and the Robust statistical average of the reported results of each laboratory is used as an assessed public Value (Assigned Value). The determination of the public affair value can also adopt a collaborative experiment fixed value, and in this example, the average value of the measured values of the Chinese institute of Electrical science and other 2 authoritative laboratories is selected as the public affair value. The evaluation method of the detection result follows the statistical processing and capability evaluation guide of CNAS-GL002 capability verification result and adopts a steady Z ratio score method for evaluation. And calculating the Z ratio score according to a formula.
In the formula, ZiIs a Z ratio score; xiMeasured values for a laboratory; xmedMedian of all laboratory measurements; NIQR is a normalized quartering distance.
Wherein: the result is satisfied when the | Z | is less than or equal to 2;
2 < | Z | < 3 is the result (suspicious value) with problems, and the reason needs to be searched and corrected again;
the result that the | Z | is larger than or equal to 3 is an unsatisfactory result (outlier), which indicates that the test link may have a larger problem and needs to find the reason and take corrective measures.
In conclusion, the preparation method of the standard sample for verifying the gas component content determination capability provided by the invention is simple to operate and high in automation degree, the obtained standard sample is uniform and stable, and the accuracy of a verification test can be ensured. The standard sample provided by the invention can effectively evaluate the component content detection capability and level of a transformer oil analysis laboratory, can be used for qualitative and quantitative analysis of components of dissolved gas in transformer oil, verification of an online or offline test instrument and quality control and assessment of test results, guarantees the detection capability level of the transformer oil analysis laboratory, effectively monitors the operation state of a power transformer, warns faults and supports safe and stable operation of the whole power grid.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A preparation method of a standard sample for verifying the gas component content determination capability is characterized by comprising the following steps:
step 1, preparing a blank oil sample;
step 2, preparing characteristic mixed gas according to the preset concentration of the gas components dissolved in the blank oil sample;
and 3, introducing the characteristic mixed gas into the blank oil sample, so that the characteristic mixed gas is fully dissolved in the blank oil sample, and preparing the standard oil sample in which the gas components with preset concentration are dissolved.
2. The method for preparing a standard sample for verifying the capability of measuring the content of gas components according to claim 1, wherein in the step 1, a certain volume of transformer oil is extracted, the transformer oil is degassed by a vacuum degassing method to be in an undersaturated state, and then the transformer oil is stored in a closed container.
3. The method for preparing a standard sample for verifying the capability of measuring the content of a gas component according to claim 1, wherein the characteristic mixed gas comprises at least two of hydrogen, carbon monoxide, carbon dioxide, methane, ethane, ethylene and acetylene; the substrate gas is nitrogen or argon.
4. The method for preparing a standard sample for verifying the capability of measuring the content of the gas component in the oil sample according to claim 1, wherein in the step 2, the concentration of each gas component in the characteristic mixed gas oil sample is determined according to the following formula:
in the formula: xiTo dissolve a certain gas component concentration in the oil, p is atmospheric pressure, CiCharacterised by the concentration of the gas component, K, in the gas mixtureiIs the partition coefficient, V ', of the gas component'gTo balance the volume of the characteristic mixture gas under modulation, V'1Is the oil sample volume at equilibrium conditions.
5. The method according to claim 1, wherein in the step 3, the characteristic mixed gas is introduced into the bottom of the oil tank containing the blank oil sample, so that the characteristic mixed gas contacts and dissolves the blank oil sample during the rising process, the characteristic mixed gas which is not dissolved in the blank oil sample is extracted from the upper layer of the oil tank and then introduced into the bottom of the oil tank, and the characteristic mixed gas is mixed with the blank oil sample for the second time, and the circulation is performed until the characteristic mixed gas is sufficiently dissolved in the oil sample, so that the standard oil sample in which the gas component with the preset concentration is dissolved is prepared.
6. The method for preparing a standard sample for verifying the capability of measuring the content of a gas component according to claim 1, wherein the standard oil sample contains CO and CH4And C2H2(ii) a Wherein the concentration of CO in the blank oil sample is 50-100 μ L/L, CH4The concentration in the blank oil sample is 20-50 μ L/L, C2H2The concentration in the blank oil sample is 10-20. mu.L/L.
7. The method for preparing a standard sample for verifying the capability of measuring the content of a gas component according to claim 1, further comprising, after the step 3: and 4, standing for a period of time to enable the undissolved characteristic mixed gas to rise to the oil level and be discharged.
8. The method for preparing a standard sample for verifying the capability of measuring the content of a gas component according to claim 7, further comprising, after the step 4: and 5, equally distributing the prepared standard oil sample into preset sealed oil tanks, and storing the sealed oil tanks in an environment with a preset temperature.
9. A standard sample for verifying the capability of assaying the content of a gas component prepared by the method according to any one of claims 1 to 8.
10. The use of the standard sample for verifying the capability of measuring the content of the gas component according to claim 9 in verification of the detection capability of a transformer oil analysis laboratory, qualitative and quantitative analysis of the component of the gas dissolved in the transformer oil, verification of an online or offline test instrument, and quality control and assessment of test results.
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