CN1654952A - Apparatus and method for measuring distribution constant of dissolved gas in transformer oil - Google Patents
Apparatus and method for measuring distribution constant of dissolved gas in transformer oil Download PDFInfo
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Abstract
A device for on-line testing solved gas distribution constant in transformer oil by gas-phase chromatography includes a constant temperature water-bath, a magnetic mixer, an oil-gas balance bottle, a six-way valve and an on-line gas-phase chromatograph to accurately test solved gas distribution constant in transformer oil under different temperatures.
Description
Technical field
The present invention relates to a kind of gaseous sample be dissolved in the liquid quantitative device for formulating and with gas chromatography coupling quantitative analysis tech, particularly gas Chromatographic Determination transformer oil dissolved gas distribution constant technology relates in particular to direct injected device and sample injection method that a kind of transformer oil dissolved gas online acquisition and single injected sampling are finished the normalization quantitative test.
Background technology
For a long time, (dissolved gas analysis, DGA) be known as by countries in the world is to monitor and diagnose oil-filled power transformer initial failure, prevention catastrophic failure the best way to the transformer dissolved gas analysis.Standard method to the transformer oil dissolved gas analysis in the laboratory mainly contains vacuum outgas method, gas extraction method and dissolution equilibrium method.Owing to need arrive spot sampling at lab analysis transformer oil dissolved gas, sampling is wasted time and energy and is had to leak and adopts and the omission problem, is difficult to sampling test every day, and the drawback that analysis result can not in time be provided is arranged.Therefore the research of on-line analysis method and device is very necessary.
ASTM3612 adopts vacuum method to measure transformer oil dissolved gas content, is characterized in gas extraction efficient height, but owing to adopted mercury as sealing medium in its method, complicated operation, poor stability, and on-line analysis device complexity.What China GB7252 adopted is the dissolution equilibrium method, adopt the machinery concussion to shorten equilibration time, be characterized in that with static head space be principle, easy and simple to handle, Repeatability and Reproducibility poor (requiring the parallel laboratory test result between the different experiments chamber to be not more than 30%), its precision of test result depends primarily on the accuracy of Ostwald (Ostwald) values of factor K that is adopted.Simultaneously, make on-line analysis be restricted because GB GB7252 has only provided Ostwald (Ostwald) coefficient under 50 ℃ of conditions.Head space method on-line analysis device is simple, but the dissolved gas distribution constant under the necessary known site environment temperature, the distribution constant of therefore measuring under the different temperatures is very necessary.
Ostwald coefficient is defined as:
That is: when gas, when the liquid two-phase reaches balance, concerning certain specific gas:
C
0i＝K
iC
gi (2)
In the formula:
C
0i-under equilibrium condition, be dissolved in the concentration of component i in the oil, ppm;
C
Gi-under equilibrium condition, the concentration of component i in the gas phase, ppm;
K
iThe ostwald coefficient of-component i, i.e. distribution constant.
According to the mass balance equation of closed system component, can obtain following formula:
X
i＝C
g(K
i+β) (3)
In the formula:
X
i-be dissolved in the original concentration of component i in the oil, ppm;
C
Gi-under equilibrium condition, the concentration of component i in the gas phase, ppm;
K
iThe ostwald coefficient of-component i;
Gas-liquid under β-equilibrium condition is compared, i.e. V
g/ V
l
Formula (3) is the computing formula that GB GB7252-2001 adopts, the method comparing under must known equilibrium condition.
Work as V
gDuring much smaller than Vl, compare β=V
g/ V
l∝ 0, and then (3) formula can be reduced to:
X
i＝K
iC
g (4)
Summary of the invention
The object of the present invention is to provide a kind of device of gas Chromatographic Determination transformer oil dissolved gas gas-liquid distribution constant, and sample injection method.The present invention is suitable for the mensuration that electric system is used for the dissolved gas analysis underlying parameter.
Device provided by the invention is simple, and method is reliable, and quantitatively accurately, personal error is little.
Specifically, device provided by the invention mainly is made up of water bath with thermostatic control, magnetic stirring apparatus, gas and oil equilibration bottle, balance syringe, six-way valve, cubing bottle, is connected by transfer capillary between its each several part.Water bath with thermostatic control control experimental temperature, its temperature-controlled precision is ± 0.1 ℃, magnetic stirring apparatus stirs transformer oil, shorten equilibration time, gas and oil equilibration bottle and balance syringe are realized operations such as the oily preparation of mark, gas and oil equilibration, equalized pressure and sample introduction, six-way valve connects gas and oil equilibration bottle and gas chromatograph, is implemented in line analysis.Non-magnetic material is adopted in the design of water bath, guarantees that magnetic stirring apparatus normally uses, and temperature control system adopts Artificial intelligence industry regulator, and temperature-controlled precision is ± 0.1 ℃.Water circulating pump guarantees that bath temperature is even.
The present invention adopts six-way valve, directly links to each other with the gas and oil equilibration bottle, connects a volume at the sample drain simultaneously and measures bottle.By pushing syringe gas is introduced in the six-way valve quantity tube, and measured the volume of eluting gas, thereby realized the gatherer process of balanced gas by the stereometry bottle of drain; Rotate six-way valve then to the sample introduction position, carrier gas is carried sample and is directly entered the disposable quantitative test of gas chromatography.
Assay method provided by the invention, be that gas and oil equilibration and gas chromatographic analysis are organically combined, can reach vapor liquid equilibrium in the short time, and directly carry out gas chromatographic analysis by valve injection, quantitatively accurately, simple to operate, be specially adapted to the mensuration of transformer oil dissolved gas distribution constant.Described gas and oil equilibration method is to adopt the gas and oil equilibration bottle, links to each other with the volumetric balance syringe, places water bath with thermostatic control, adopts magnetic agitation to shorten equilibration time.Overflowing of gas avoided in the design of gas and oil equilibration bottle, and being free to slide of syringe can keep normal pressure by guarantee system pressure.
The design of this method makes V
gMuch smaller than V
l, compare β=V
g/ V
l=0.0125.If ignore and compare, the methane less (K=0.39,50 ℃) to distribution constant, relative error only is 3.2%, the error of other component is littler.Therefore adopt the gaseous component concentration under the gas Chromatographic Determination different temperatures equilibrium condition, ostwald coefficient under this temperature that can calculate according to (4) formula, and owing to adopt the micro-packed column analysis, sampling amount only is 20～80 μ L, prepares a standard oil sample and can measure 20～90 ℃ of distribution constants under some temperature simultaneously.
Apparatus of the present invention synoptic diagram is seen Fig. 1.Fig. 1 is the process flow diagram of transformer oil dissolved gas gas-liquid distribution constant determinator, the transformer oil dissolved gas of concentration known reaches vapor liquid equilibrium in equilibration flask, then pushing syringe makes balanced gas enter in the six-way valve quantity tube by quartz capillary, and the valve switching enters quantitative test in the gas chromatography.
Description of drawings
Below by embodiment and accompanying drawing the present invention is done detailed narration, the present invention and classic method difference relatively is described simultaneously.
Fig. 1 is the process flow diagram of transformer oil dissolved gas distribution constant determinator.The transformer oil dissolved gas of concentration known reaches vapor liquid equilibrium in equilibration flask, then pushing syringe makes balanced gas enter in the six-way valve quantity tube by quartz capillary, and the valve switching enters quantitative test in the gas chromatography.
Fig. 2 is a hydro carbons dissolved gas gas chromatogram in the transformer oil;
Embodiment
Embodiment:
Device of the present invention sees also Fig. 1.One gas and oil equilibration bottle 3, integral body places water bath with thermostatic control 1, and the bottle bottom is equipped with a magnetic stirring apparatus 2, is placed with magnetic stir bar in the gas and oil equilibration bottle 3, so that gas and oil equilibration bottle 3 is carried out constant temperature and stirring simultaneously.Water bath with thermostatic control 1 is made up of water bath, heating rod, thermopair (platinum resistance), temperature regulator and water circulating pump, and water bath wherein is to make with non-magnetic material, for example but do not limit materials such as ground available stainless steel, aluminium alloy, glass.About water bath with thermostatic control is that those skilled in the art are familiar with, and is readily appreciated that and imagines according to one section top description.Therefore the present invention does not do too much introduction to this water bath with thermostatic control.
Place in the gas and oil equilibration bottle 3 of water bath the siphunculus 7 of vertically planting from bottleneck to a bottle end, this siphunculus 7 for example but do not limit ground useable glass pipe or quartz capillary.The other end of this siphunculus 7 is connected with a piston syringe 4.
The side pipe of gas and oil equilibration bottle 3 is connected with six-way valve 5 by a pipeline 8 (for example quartz capillary), and this six-way valve 5 also is connected with cubing bottle 6 and gas chromatograph (not shown) respectively.
Its internal diameter of quartz capillary that the present invention adopts can be 0.25mm, 0.32mm or 0.53mm.
The 25# transformer oil is placed the 3L flask, vacuumized under the condition of magnetic agitation 2 hours, vacuum tightness is less than 10Pa, and to remove dissolved gas wherein, the blank oil of handling keeps certain vacuum stand-by.The oily vacuum of blank is sucked in the gas and oil equilibration bottle 3 of certain volume until all being full of, the volume of this gas and oil equilibration bottle 3 is 4L, place the piston syringe 4 balance volume change of water bath with thermostatic control by being free to slide, with the 100mL gastight syringe 50mL normal mixture body is injected the gas and oil equilibration bottle, magnetic agitation all is dissolved in the oil until gas.Calculate concentration of dissolved gas.
Get the blank nitrogen (also can be helium or argon gas) of certain volume with the 100mL gastight syringe, inject the gas and oil equilibration bottle, the mark oil of equal volume is spilled in the piston syringe 4, owing to syringe piston 4 can be free to slide, thereby guarantees that pressure of the inside of a bottle is a normal pressure.Water bath with thermostatic control, magnetic agitation stop magnetic agitation to gas and oil equilibration; after static 10 minutes; promote piston syringe 4, balanced gas is introduced in six-way valve 5 quantity tubes by the fused quartz kapillary 8 of an outer stopping off, rotate six-way valve 5 and realize gas chromatography sample introduction and quantitative test.
Chromatographic column is micro-packed column 2m * 1mmI.D., and stationary phase is 100-120 order GDX502, and carrier gas is N
2, flow velocity 3mL/min, 60 ℃ of column temperatures, detecting device are FID, 250 ℃ of temperature.Valve injection, quantity tube are 80 μ L.According to above chromatographic condition, each component degree of separation satisfies chromatographic resolution and requires (see figure 2) all greater than 1.5.
Measured the distribution constant of 20 ℃～90 ℃ of hydrocarbon gas according to above method, and (20 ℃ and the 50 ℃) distribution constant that provides with GB7252-2001 relatively, and the accuracy of this method is described, the results are shown in Table 1.
The mensuration of distribution constant under table 1 different temperatures
Equilibrium temperature method methane ethylene-ethane acetylene propane
20 0.47 1.72 2.68 1.20 8.60
50 experiments 0.46 1.45 2.09 1.06 5.96
90 0.46 1.15 1.55 0.91 3.66
20 0.43 1.70 2.40 1.20 -
IEC567
50 0.40 1.40 1.80 0.90 -
50 GB7252 0.39 1.46 2.30 1.02 -
Claims (10)
1, a kind of device of gas Chromatographic Determination transformer oil dissolved gas distribution constant mainly comprises: constant temperature water bath, gas and oil equilibration bottle, six-way valve and on-line gas chromatography;
Wherein:
One gas and oil equilibration bottle, integral body places water bath with thermostatic control, and the bottle bottom is equipped with a magnetic stirring apparatus, is placed with magnetic stir bar in the gas and oil equilibration bottle, so that the gas and oil equilibration bottle is carried out constant temperature and stirring simultaneously;
Water bath with thermostatic control is made up of water bath, heating rod, thermopair, temperature regulator and water circulating pump, and water bath wherein is to make with non-magnetic material;
The interior siphunculus of vertically planting from bottleneck to a bottle end of gas and oil equilibration bottle, the other end of this siphunculus is connected with a piston syringe;
The side mouth of gas and oil equilibration bottle is connected with six-way valve;
This six-way valve drain connects a volume and measures bottle and gas chromatograph.Gas volume is measured bottle and is linked to each other with the six-way valve drain by connecting pipe, and seal fluid adopts saturated aqueous common salt.
2. device as claimed in claim 1 is characterized in that, described constant temperature water bath is the non-magnetic material manufacturing, and this material is stainless steel, aluminium alloy or glass.
3. device as claimed in claim 1 or 2 is characterized in that, described constant temperature water bath outer wall is incubated with heat-barrier material.
4. device as claimed in claim 1 is characterized in that, gas and oil equilibration bottle side mouth adopts the silicagel pad sealing.
5. device as claimed in claim 1 is characterized in that, links to each other with quartz capillary between gas and oil equilibration bottle and the six-way valve.
6. device as claimed in claim 5 is characterized in that, described quartz capillary internal diameter is 0.25mm, 0.32mm or 0.53mm.
7. method of measuring transformer oil dissolved gas distribution constant, its key step is:
A) transformer oil is removed dissolved gas under the condition of vacuum tightness less than 10Pa;
B) transformer oil that will remove dissolved gas is full of equilibration flask;
C) equilibration flask is placed water bath with thermostatic control, and link to each other with the piston syringe;
D) the normal mixture body with certain volume injects equilibration flask from equilibration flask side mouth, and the bottom tube of unnecessary transformer oil in the gas and oil equilibration bottle is spilled over to the continuous piston syringe, is stirred to gas and is dissolved in fully in the oil, calculates oil dissolved gas concentration;
E) with gastight syringe the blank gas of certain volume is injected equilibration flask from gas and oil equilibration bottle side mouth, the bottom tube of unnecessary transformer oil in the gas and oil equilibration bottle is spilled over to the continuous piston syringe, is stirred to gas and oil equilibration;
F) gas and oil equilibration bottle side mouth is linked to each other with six-way valve, promote the piston syringe, the gas in the gas and oil equilibration bottle enters in the six-way valve quantity tube, and gas volume is measured by the cubing bottle of six-way valve outlet, rotate six-way valve, carrier gas is brought gaseous sample in gas chromatography quantitative test.
8. method as claimed in claim 7 is characterized in that, described blank gas is helium, argon gas or nitrogen.
9. method as claimed in claim 7 is characterized in that little chromatography column is adopted in described gas chromatographic analysis, and the gas sampling amount is 20～80 μ L.
10. method as claimed in claim 7 is characterized in that, can measure the distribution constant under the arbitrary temp in 20～90 ℃ of temperature ranges simultaneously.
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| CNB2004100049550A CN100387989C (en) | 2004-02-13 | 2004-02-13 | Apparatus and method for measuring distribution constant of dissolved gas in transformer oil |
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| CNB2004100049550A CN100387989C (en) | 2004-02-13 | 2004-02-13 | Apparatus and method for measuring distribution constant of dissolved gas in transformer oil |
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| CN100387989C CN100387989C (en) | 2008-05-14 |
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