CN104133026B - The oil product pre-treatment degas method of transformer insulated oil gas chromatographic - Google Patents

The oil product pre-treatment degas method of transformer insulated oil gas chromatographic Download PDF

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CN104133026B
CN104133026B CN201410397706.6A CN201410397706A CN104133026B CN 104133026 B CN104133026 B CN 104133026B CN 201410397706 A CN201410397706 A CN 201410397706A CN 104133026 B CN104133026 B CN 104133026B
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gas
wash
cold
oil
sample
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CN104133026A (en
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刘鸿芳
郭军科
卢立秋
于金山
苏展
郝春燕
赵鹏
林琳
路菲
杜涛
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State Grid Corp of China SGCC
State Grid Tianjin Electric Power Co Ltd
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State Grid Corp of China SGCC
State Grid Tianjin Electric Power Co Ltd
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Abstract

The present invention relates to a kind of oil product pre-treatment degas method for transformer insulated oil gas chromatographic, comprising step has: transformer insulated oil samples is fetched in transformer station by (1); (2) sample will be fetched put into constant temperature sales kit (SK) and carry out constant temperature; (3) sample will be fetched again and put into instrument constant temperature sample disc, start sample introduction; (4) sample enters dissolved gas in oil elutriator and carries out sample elution; (5) the potpourri wash-out gas after wash-out is attached by positive pressure-vaccum by cold-trap device bottom, blowback desorb, finally discharges stripping gas by cold-trap device bottom; (6) chromatographic column that the stripping gas of being discharged by cold-trap device bottom enters gas chromatograph carries out being separated rear detection; (7) detecting device detects sample component; (8) component concentration is calculated.Elutriator in the inventive method and cold-trap device improve the degassed rate of oil product, and the accuracy of analysis of experiments result is improved greatly.

Description

The oil product pre-treatment degas method of transformer insulated oil gas chromatographic
Technical field
The invention belongs to insulating oil gas chromatographic analysis technique field, especially a kind of oil product pre-treatment degas method of transformer insulated oil gas chromatographic.
Background technology
At present, the pre-treatment degas method of transformer insulated oil gas chromatographic mostly is the methods such as vibration degassing method, membrane degassing method, vacuum outgas method, be mainly used in the field such as oil, electric power, existing degas method operation link is comparatively complicated, analyst's working strength is larger, and links all easily introduces measuring error and systematic error, the accuracy of easy impact analysis result.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of oil product pre-treatment degas method for transformer insulated oil gas chromatographic is provided.
The present invention solves its technical matters and takes following technical scheme to realize:
For an oil product pre-treatment degas method for transformer insulated oil gas chromatographic, comprise step as follows:
(1) in transformer station, transformer insulated oil samples is fetched;
(2) sample will be fetched put into constant temperature sales kit (SK) and carry out constant temperature;
(3) sample will be fetched again and put into instrument constant temperature sample disc, start sample introduction by instrumentation;
(4) sample enters dissolved gas in oil elutriator by the import of dissolved gas in oil elutriator and carries out sample elution;
Wherein, dissolved gas in oil elutriator, comprise the cylindrical metal wash-out body of upper end open, in wash-out body upper end open, there is sealing cap on wash-out body at place by screw thread spiral cover, filler is filled with in the Lower Half in wash-out body cylindrical inner space, the first half is wash-out headroom, the upper air inlet/outlet be communicated with inner space is shaped with at the upper end face of upper sealing cap, the lower air inlet/outlet be communicated with inner space is shaped with at the bottom surface of wash-out body, heating rod hole is straight down had at the top of wash-out body right side wall, thermometer hole is straight down had at the top of wash-out body left side wall, the top cover of upper sealing cap is shaped with the heating rod corresponding aperture corresponding with heating rod hole site, and the thermometric corresponding aperture corresponding with thermometer hole position,
(5) the potpourri wash-out gas in above-mentioned (4) step after wash-out is attached by positive pressure-vaccum by cold-trap device bottom, the principle of blowback desorb, finally discharges stripping gas by cold-trap device bottom;
Wherein, cold-trap device comprises cylindrical metal cold-trap housing, the enterprising outlet nozzle be connected with enclosure interior is integrally shaped with at the upper end face of housing, the lower turnover valve be connected with enclosure interior is integrally shaped with at the bottom surface of housing, the external refrigeration pipe of metal is wound with in the outside of housing, in the inside of housing, internal refrigeration storage pipe is installed from top to bottom, porous plate is fixed with at the upper and lower side of cold-trap enclosure interior, enclosure interior between upper and lower porous plate is filled with Stationary liquid, the left heat-conducting metal fixture block of tiled configuration symmetry and right heat-conducting metal fixture block, the semi-cylindrical recesses in the middle part of fixture block is utilized outside to be wound with the cold-trap housing of external refrigeration pipe accommodated therein, left and right metal fixture block is all shaped with mounting hole, left and right metal fixture block is fixed by mounting hole by set bolt, left semiconductor refrigerating plate and right semiconductor refrigerating plate is equipped with respectively in the outside of left and right metal fixture block, left and right semiconductor refrigerating plate is bonded in by silica gel cream on the lateral surface of left and right metal fixture block,
(6) chromatographic column that the stripping gas of being discharged by cold-trap device bottom enters gas chromatograph carries out being separated rear detection, and described chromatographic column is existing analysis chromatographic column;
(7) detect sample component by detecting device again, described detecting device is existing analysis detecting device, comprises thermal conductivity detector (TCD) and hydrogen flame detector;
(8) calculated by component concentration by data processing, described data processing is existing data processing software, directly calculates result.
And the sidewall surrounding of the wash-out body in described step (4) is enclosed with heat-insulation layer.
And in described step (4), convex body pipe comprises diameter is 10mm-15mm, and length is the stainless-steel tube of 20mm-30mm, the outer wall of stainless-steel tube is shaped with the hemispherical projections that the even diameter apart from arrangement is 2mm-3mm.
And, in described step (4), the concrete grammar of wash-out is: constant-temperature quantitative transformer insulation oil is headed into elutriator inner space by air inlet/outlet under elutriator, fuel head is identical with packed height, head into wash-out gas by lower air inlet/outlet and wash-out is carried out to transformer insulation oil, by stainless steel convex body pipe fully and biased sample replace, oil soluble gas, wash-out gas reach an equilibrium process repeatedly, and the mixed gas after elution process is carried by wash-out gas and discharged by upper air inlet/outlet.
And, in the cold-trap device of described step (5), the import of the external refrigeration pipe of described metal is on the top of housing, outlet is in the bottom of housing, after the external refrigeration pipe two ends of described metal add HF voltage, produce high frequency variation magnetic field in helical outer refrigerator pipes, high frequency variation magnetic field produces eddy current and heats up on the metal fixture block of described left and right, heating cold-trap.
And in the cold-trap device of described step (5), the porous plate up and down of described cold-trap enclosure interior adopts the cotton plate of porous, and the Stationary liquid that described enclosure interior is filled specifically adopts the TDX-01 Series Molecules sieve of circular 60-80 order particle as Stationary liquid.
And in described step (5), the concrete grammar of being discharged stripping gas by cold-trap device bottom is:
1. the cold-trap of TDX-01 Series Molecules sieve as Stationary liquid of circular 60-80 order particle is filled with in the gas deviate from by wash-out air purge enters, cold-trap is filled with liquid nitrogen by conductor refrigeration and inside and outside refrigerant pipe import and carries out refrigeration, wash-out gas is fully caught in low-temperature solid phasing retain, simultaneously, in the outlet of wash-out gas by Vavle switching blow-back, oil sample after wash-out process is blown into waste oil container;
2. cold-trap stops refrigeration, conductor refrigeration starts heating, outer refrigerant pipe imports and exports two ends energising, carry out high frequency transient heating, high frequency makes the eddy current rapid temperature increases in cold-trap magnetic stainless steel body, make to catch entrap gas and obtain moment desorb, discharge, the sample gas of desorb is discharged by cold-trap device bottom under the purging of carrier gas is worn.
Advantage of the present invention and good effect are:
1, the method has temperature automatically controlled, automatic oil-feed sample, the functions such as automatic deaerating, auto-admission sample, automatic analysis, and filled up the blank of the automatic pre-treating method of oil product of transformer insulated dissolved gas in oil gas chromatographic analysis, automaticity is high;
2, sample is loaded automatic constant-temperature injector device by the method, reaches the object of Multi-example auto injection according to the order of sequence, decreases artificial reading error;
3, the method has invented transformer insulated dissolved gas in oil elutriator, instead of traditional degas method, substantially increases work efficiency;
4, the method has invented the cold-trap device of original creation, for dissolved gas analysis in transformer insulation oil provides enrichment sampling technique, thus improves the degassed rate of oil product, the accuracy of analysis of experiments result is improved greatly.
Accompanying drawing explanation
Fig. 1 is the pre-treatment degas method process flow diagram of transformer insulated oil gas chromatographic in the present invention;
Fig. 2 is that structural representation is partly cutd open in the right side of elutriator device in the present invention;
Fig. 3 is wash-out filling-material structure schematic diagram in the present invention;
Fig. 4 is the assembling schematic diagram of cold-trap device in the present invention;
Fig. 5 is the cold-trap housing interior structure schematic diagram of cold-trap device in the present invention.
Embodiment
Be further described the invention process below in conjunction with accompanying drawing, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
A kind of oil product pre-treatment degas method for transformer insulated oil gas chromatographic, as shown in Figure 1, the equipment that the method uses comprises constant temperature sales kit (SK), instrument constant temperature sample disc, dissolved gas in oil elutriator, cold-trap, chromatographic column, detecting device, the process of manipulation computer data, and the step of the method is as follows:
(1) in transformer station, transformer insulated oil samples is fetched;
(2) will fetch sample to put into constant temperature sales kit (SK) and carry out constant temperature, described constant temperature sales kit (SK) is that the common constant temperature sales kit (SK) that market is sold both can;
(3) will fetch sample again and put into instrument constant temperature sample disc, and start sample introduction by instrumentation, sample can auto injection in order, and described instrument constant temperature sample disc is that the General Instrument constant temperature sample disc that market is sold both can;
(4) sample enters dissolved gas in oil elutriator by the import of dissolved gas in oil elutriator and carries out sample elution;
Wherein, dissolved gas in oil elutriator, as shown in Figure 2, comprise the cylindrical metal wash-out body 4 of upper end open, sealing cap 1 on wash-out body is had by screw thread spiral cover at wash-out body upper end open place, filler 10 is filled with in the Lower Half in wash-out body cylindrical inner space, the first half is wash-out headroom 6, the upper air inlet/outlet 5 be communicated with inner space is shaped with at the upper end face of upper sealing cap, for oil soluble gas, the outlet of wash-out gas and the entrance of blowback air, the lower air inlet/outlet 11 be communicated with inner space is shaped with at the bottom surface of wash-out body, for oil sample, the import of wash-out gas and waste oil, the outlet of blowback air, heating rod hole 8 is straight down had at the top of wash-out body right side wall, for inserting heating rod, thermometer hole 3 is straight down had at the top of wash-out body left side wall, for inserting the temperature of thermometer measure wash-out body sidewall, the top cover of upper sealing cap is shaped with the heating rod corresponding aperture 7 corresponding with heating rod hole site, and the thermometric corresponding aperture 2 corresponding with thermometer hole position.
And, be enclosed with heat-insulation layer 9 in the sidewall surrounding of described cylindrical metal wash-out body.
And described filler is that multiple stainless steel convex body pipe is formed, and as shown in Figure 3, it is 10mm-15mm that convex body pipe comprises diameter, and length is the stainless-steel tube 12 of 20mm-30mm, and the outer wall of stainless-steel tube is shaped with the even jut 13 apart from arrangement.
And, the hemispherical projections of described jut to be diameter be 2mm-3mm.
In specific embodiment of the invention, the concrete grammar of described wash-out is: constant-temperature quantitative transformer insulation oil is headed into elutriator inner space by air inlet/outlet under elutriator, fuel head is identical with packed height, head into wash-out gas by lower air inlet/outlet and wash-out is carried out to transformer insulation oil, by stainless steel convex body pipe fully and biased sample replace, oil soluble gas, wash-out gas reach an equilibrium process repeatedly, and the mixed gas after elution process is carried by wash-out gas and discharged by upper air inlet/outlet.
(5) the potpourri wash-out gas in above-mentioned (4) step after wash-out is attached by positive pressure-vaccum by cold-trap device bottom, the principle of blowback desorb, finally discharges stripping gas by cold-trap device bottom;
Wherein, cold-trap device, as shown in fig. 4 or 5, comprise cylindrical metal cold-trap housing 19, the enterprising outlet nozzle 18 be connected with enclosure interior is integrally shaped with at the upper end face of housing, the lower turnover valve 27 be connected with enclosure interior is integrally shaped with at the bottom surface of housing, the external refrigeration pipe 20 of metal is wound with in the outside of housing, in the inside of housing, internal refrigeration storage pipe 31 is installed from top to bottom, porous plate 32 is fixed with at the upper and lower side of cold-trap enclosure interior, enclosure interior between upper and lower porous plate is filled with Stationary liquid 30, the left heat-conducting metal fixture block 15 of tiled configuration symmetry and right heat-conducting metal fixture block 22, the semi-cylindrical recesses 16 in the middle part of fixture block is utilized outside to be wound with the cold-trap housing of external refrigeration pipe accommodated therein, left and right metal fixture block is all shaped with mounting hole 28, left and right metal fixture block is fixed by mounting hole by set bolt 29, left semiconductor refrigerating plate 14 and right semiconductor refrigerating plate 24 is equipped with respectively in the outside of left and right metal fixture block, left and right semiconductor refrigerating plate is bonded on the lateral surface of left and right metal fixture block by silica gel cream.
And, the import 17 of the external refrigeration pipe of described metal is on the top of housing, outlet 25 is in the bottom of housing, after the external refrigeration pipe two ends of described metal add HF voltage, high frequency variation magnetic field is produced in helical outer refrigerator pipes, high frequency variation magnetic field produces eddy current and heats up on the metal fixture block of described left and right, heating cold-trap.
The induction pipe 21 of described internal refrigeration storage pipe penetrates in housing by the upper portion side wall of housing, and outlet 26 is passed outside housing by the lower sides of housing.
And be shaped with thermometer hole 23 vertically downward on the upper end face of described right heat-conducting metal fixture block, thermometer hole is used for plug-in mounting thermometer thermometric.
And the porous plate up and down of described cold-trap enclosure interior adopts the cotton plate of porous.
And the Stationary liquid that described enclosure interior is filled specifically adopts the TDX-01 Series Molecules sieve of circular 60-80 order particle as Stationary liquid.
And described left and right semiconductor refrigerating plate specifically adopts the semiconductor refrigerating plate purchased in the market.
And described left and right semiconductor refrigerating plate replaces with filling liquid nitrogen cold plate.
And described external refrigeration pipe body adopts liquid nitrogen as the refrigeration modes of cold-producing medium, described internal refrigeration storage pipe body adopts liquid nitrogen as the refrigeration modes of cold-producing medium.
In specific embodiment of the invention, the concrete grammar that stripping gas is discharged in described cold-trap device bottom is:
The cold-trap of TDX-01 Series Molecules sieve as the adsorbent of Stationary liquid of circular 60-80 order particle is filled with in the gas deviate from by wash-out air purge enters, cold-trap is filled with liquid nitrogen by conductor refrigeration and inside and outside refrigerant pipe import to carry out refrigeration, wash-out gas is fully caught in low-temperature solid phasing retain, simultaneously, in the outlet of wash-out gas by Vavle switching blow-back, oil sample after wash-out process is blown into waste oil container; Stop refrigeration at cold-trap simultaneously, conductor refrigeration starts heating (as long as the reversal of poles of power supply just can be reached the object of heating), outer refrigerant pipe imports and exports two ends energising, carry out high frequency transient heating, high frequency makes the eddy current rapid temperature increases in cold-trap magnetic stainless steel body, make to catch entrap gas and obtain moment desorb, discharge, the sample gas of desorb is discharged by cold-trap device bottom under the purging of carrier gas is worn.
(6) chromatographic column that the stripping gas of being discharged by cold-trap device bottom enters gas chromatograph carries out being separated rear detection, and described chromatographic column is existing analysis chromatographic column;
(7) detect sample component by detecting device again, described detecting device is existing analysis detecting device, comprises thermal conductivity detector (TCD) and hydrogen flame detector;
(8) calculated by component concentration by data processing, described data processing is existing data processing software, directly calculates result.

Claims (3)

1., for an oil product pre-treatment degas method for transformer insulated oil gas chromatographic, it is characterized in that comprising step as follows:
(1) in transformer station, transformer insulated oil samples is fetched;
(2) sample will be fetched put into constant temperature sales kit (SK) and carry out constant temperature;
(3) sample will be fetched again and put into instrument constant temperature sample disc, start sample introduction by instrumentation;
(4) sample enters dissolved gas in oil elutriator by the import of dissolved gas in oil elutriator and carries out sample elution;
Wherein, dissolved gas in oil elutriator, comprise the cylindrical metal wash-out body of upper end open, the sidewall surrounding of wash-out body is enclosed with heat-insulation layer, in wash-out body upper end open, there is sealing cap on wash-out body at place by screw thread spiral cover, filler is filled with in the Lower Half in wash-out body cylindrical inner space, described filler is that multiple stainless steel convex body pipe is formed, convex body pipe is diameter 10mm-15mm, the stainless-steel tube of length 20mm-30mm, the outer wall of stainless-steel tube is shaped with the hemispherical projections that the even diameter apart from arrangement is 2mm-3mm, the first half is wash-out headroom, the upper air inlet/outlet be communicated with inner space is shaped with at the upper end face of upper sealing cap, the lower air inlet/outlet be communicated with inner space is shaped with at the bottom surface of wash-out body, heating rod hole is straight down had at the top of wash-out body right side wall, thermometer hole is straight down had at the top of wash-out body left side wall, the top cover of upper sealing cap is shaped with the heating rod corresponding aperture corresponding with heating rod hole site, and the thermometric corresponding aperture corresponding with thermometer hole position,
Wherein, the concrete grammar of sample elution is: constant-temperature quantitative transformer insulation oil is headed into elutriator inner space by air inlet/outlet under elutriator, fuel head is identical with packed height, head into wash-out gas by lower air inlet/outlet and wash-out is carried out to transformer insulation oil, by stainless steel convex body pipe fully and biased sample replace, oil soluble gas, wash-out gas reach an equilibrium process repeatedly, and the mixed gas after elution process is carried by wash-out gas and discharged by upper air inlet/outlet.
(5) the potpourri wash-out gas in above-mentioned (4) step after wash-out is attached by positive pressure-vaccum by cold-trap device bottom, the principle of blowback desorb, finally discharges stripping gas by cold-trap device bottom;
Wherein, cold-trap device comprises cylindrical metal cold-trap housing, the enterprising outlet nozzle be connected with enclosure interior is integrally shaped with at the upper end face of housing, the lower turnover valve be connected with enclosure interior is integrally shaped with at the bottom surface of housing, the external refrigeration pipe of metal is wound with in the outside of housing, the import of the external refrigeration pipe of metal is on the top of housing, outlet is in the bottom of housing, after the external refrigeration pipe two ends of described metal add HF voltage, high frequency variation magnetic field is produced in helical outer refrigerator pipes, high frequency variation magnetic field produces eddy current and heats up on the metal fixture block of described left and right, heating cold-trap, in the inside of housing, internal refrigeration storage pipe is installed from top to bottom, porous plate is fixed with at the upper and lower side of cold-trap enclosure interior, enclosure interior between upper and lower porous plate is filled with Stationary liquid, Stationary liquid is the TDX-01 Series Molecules sieve of 60-80 order particle, the left heat-conducting metal fixture block of tiled configuration symmetry and right heat-conducting metal fixture block, the semi-cylindrical recesses in the middle part of fixture block is utilized outside to be wound with the cold-trap housing of external refrigeration pipe accommodated therein, left and right metal fixture block is all shaped with mounting hole, left and right metal fixture block is fixed by mounting hole by set bolt, left semiconductor refrigerating plate and right semiconductor refrigerating plate is equipped with respectively in the outside of left and right metal fixture block, left and right semiconductor refrigerating plate is bonded in by silica gel cream on the lateral surface of left and right metal fixture block,
(6) chromatographic column that the stripping gas of being discharged by cold-trap device bottom enters gas chromatograph carries out being separated rear detection;
(7) detect sample component by detecting device again, described detecting device is existing analysis detecting device, comprises thermal conductivity detector (TCD) and hydrogen flame detector;
(8) calculated by component concentration by data processing, described data processing is existing data processing software, directly calculates result.
2. the oil product pre-treatment degas method for transformer insulated oil gas chromatographic according to claim 1, is characterized in that: in the cold-trap device of described step (5), and the porous plate up and down of described cold-trap enclosure interior adopts the cotton plate of porous.
3. the oil product pre-treatment degas method for transformer insulated oil gas chromatographic according to claim 1, is characterized in that: in described step (5), and the concrete grammar of being discharged stripping gas by cold-trap device bottom is:
1. the cold-trap of TDX-01 Series Molecules sieve as Stationary liquid of circular 60-80 order particle is filled with in the gas deviate from by wash-out air purge enters, cold-trap is filled with liquid nitrogen by conductor refrigeration and inside and outside refrigerant pipe import and carries out refrigeration, wash-out gas is fully caught in low-temperature solid phasing retain, simultaneously, in the outlet of wash-out gas by Vavle switching blow-back, oil sample after wash-out process is blown into waste oil container;
2. cold-trap stops refrigeration, conductor refrigeration starts heating, outer refrigerant pipe imports and exports two ends energising, carry out high frequency transient heating, high frequency makes the eddy current rapid temperature increases in cold-trap magnetic stainless steel body, make to catch entrap gas and obtain moment desorb, discharge, the sample gas of desorb is discharged by cold-trap device bottom under the purging of carrier gas drives.
CN201410397706.6A 2014-08-13 2014-08-13 The oil product pre-treatment degas method of transformer insulated oil gas chromatographic Active CN104133026B (en)

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