CN202748285U - Device for measuring oil and/or water content in samples - Google Patents
Device for measuring oil and/or water content in samples Download PDFInfo
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- CN202748285U CN202748285U CN 201220262780 CN201220262780U CN202748285U CN 202748285 U CN202748285 U CN 202748285U CN 201220262780 CN201220262780 CN 201220262780 CN 201220262780 U CN201220262780 U CN 201220262780U CN 202748285 U CN202748285 U CN 202748285U
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Abstract
The utility model provides an improved device for measuring the oil and/or water content in samples. The device comprises an extraction device, wherein the extraction device is used for carrying out sample extraction through solvents, so that steam of water and the solvents enters a dean-stark water separator for separating moisture to measure the water content, and the extraction device comprises an extraction bottle, an extraction tube and a steam and liquid flow dividing head, the extraction bottle is used for accommodating and extracting the solvents, the extraction tube is arranged in the extraction bottle and is used for accommodating samples to be measured, the upper end of the extraction tube is open, the middle upper part of the tube wall is provided with an overflowing hole, the steam and liquid flow dividing head is used for connecting the water separator and the extraction bottle, is provided with a steam ascending tube and a liquid descending pipe, the steam ascending tube is used for enabling the steam to upwards flow from the extraction bottle to enter the water separator through the steam and liquid flow dividing head, and the liquid descending pipe is used for enabling the liquid to downwards flow from the water separator to enter the extraction tube through the seam and liquid flow dividing head. When the device is utilized for measuring the oil and/or water content of the samples, the accuracy and the stability are good, in addition, the manufacturing cost is low, and the device is suitable for being popularized and applied in large areas.
Description
Technical field
The utility model relates to a kind of device for working sample oil and/or liquid water content, specifically, refers to a kind of improvement Dean-Stark device that is applicable to measure oil in solid-state in oil, petrochemical industry or the food industry, the semisolid sample and/or liquid water content.
Background technology
In some scientific researches of oil, petrochemical industry or food industry, usually need to measure the content of oil in the sample and/or water.Dean-Stark device (being called again Dean-Stark receiver or Dean-Stark distiller) is a kind of glass apparatus by liquid water content in the distillating method working sample of commonly using.
For example, what oil/Water content determination adopted in the oily sludge at present is " the Dean-Stark modifying device " that the fuel-efficient sand of Canadian Alberta management board is recommended, its structure as shown in Figure 1, this device mainly comprises extraction element part and Dean-Stark separator portion.Extraction element part mainly be utilize solvent that sample is carried out extracting so that the steam of solvent and water enters that Separation of Water in the Dean-Stark separation vessel divides so the liquid water content of working sample, the core of being somebody's turn to do " Dean-Stark modifying device " is Dean-Stark separation vessel (or claiming water trap) 10, it is a device that is similar to " h " type structure, its main body is a vertical column glass tube, the top links to each other with the bottom of reflux condenser 20, the below connects can measure the water trap 101 of liquid volume (with metering scale, this water trap 101 also can change the glass that is similar to buret gathering-device processed into to collect the liquid of more volume), tiltedly stretch out an arm (or claiming recirculatory pipe) in the middle and upper part of water trap 10 main body glass tubes, arm and column glass tube below tube wall acutangulate, arm is stretched over to be rolled over when closing on end for vertically, in order to insert in the crossover sub 50 that connects extraction flask.Extraction element part mainly comprises extraction flask 30 and is set in extraction tube 40 in the extraction flask 30, and extraction tube 40 is suspended from the extraction flask 30 (certain distance is arranged at extraction tube 40 bottoms and extraction flask 30 bottoms), and extraction tube 40 bottoms are provided with the aperture 401 of perforation.Inside and outside ground by crossover sub 50 between extraction element part and the Dean-Stark water trap 10 is connected, with being tightly connected between assurance extraction element and the water trap.When utilizing this device to measure in oily sludge oil and/or liquid water content, solvent (such as toluene) is housed in the extraction flask 30, oily sludge sample to be measured is placed in the extraction tube 40 with the filter paper parcel, install water trap 10, condenser 20, utilize 60 pairs of extraction flasks 30 of heating arrangement to heat (middle and lower part and bottom-heated).Rising along with temperature, toluene solvant in the extraction flask 30 and the water in the sample evaporate in extraction element, form the arm that steam enters water trap 10, and enter the reflux condenser that skin is connected with chilled water along arm, be condensed into liquid, splash into the water trap 101 of Dean-Stark water trap 10 supervisor belows.In water trap 101, solvent toluene that can not be miscible and steeping in water for reconstitution layer estranged, lower floor is water, the upper strata is the less toluene of density.Carrying out along with evaporation, liquid in the water trap increases gradually, when highly reaching the arm junction, will be back to (all being the upper strata solvent) in the extraction element along arm, the tested oily sludge with the filter paper parcel directly carries out shower in the extraction tube 40 to being contained in, and flows in the extraction flask 30 through the aperture 401 of extraction tube 40 bottoms.The water of water trap lower floor is then stayed in the water trap and is measured (if the moisture in the testing sample is higher, can change bottom the water trap and be made as the buret gathering-device that is similar to knob, treat that water collects certain volume, can open the knob of gathering-device bottom and emit the water that part is collected, too much enter extraction element along the arm backflow to prevent the water amount).After extracting is complete, can tested oily sludge sample is dry under 115 ℃ of temperature conditions, make the toluene solvant volatilization and to the sample constant weight, be scaled the liquid water content of sample according to the volume number that from water trap water trap, reads water, utilize the decrement method can calculate the oil content of sample.
Above-mentioned " Dean-Stark modifying device ", simple in structure, easy operating, not only can be used for oil in the oily sludge and/or liquid water content are measured, also can be used for measuring other petroleum products, oil and/or liquid water content such as tar, emulsified asphalt and other asphalt material, also can be used in addition in the food industry, such as the oil of bread, biscuit, fries etc. and/or the mensuration of liquid water content.
Yet, owing to always following resistance minimum principle (following the shortest flow principle of point-to-point transmission straight line) during downward liquid flow, therefore contain oil samples, such as oily sludge, in oil can not be complete by extracting; In addition for guaranteeing that rapid outflow of solvent that flows into extraction tube is suspended from the extraction flask extraction tube so that carry out next time extracting, this complete extracting for oil also is disadvantageous (relying on shower fully), and the direct result of these problems is that accuracy and the collimation of oil content determination data is relatively poor.
The utility model content
Fundamental purpose of the present utility model is the problem for the device existence of oil and/or liquid water content in the above-mentioned existing method working sample, measurement mechanism is improved, provide the device of oil in a kind of new working sample and/or liquid water content, to improve accuracy and the collimation of determination data.
For reaching above-mentioned purpose, the utility model provides a kind of device for working sample oil and/or liquid water content, this device has mainly partly carried out further improvement to the extraction element of above-mentioned prior art " Dean-Stark modifying device ", and then can make the oil content extracting in the sample more complete, improve accuracy and the collimation measured.Specifically, the device that is used for working sample oil and/or liquid water content that the utility model provides mainly comprises:
Utilize solvent that sample is carried out extracting so that the steam of solvent and water enters Separation of Water in the Dean-Stark water trap, and then measured the extraction element of moisture, this extraction element mainly comprises:
The extraction flask that is used for accommodating extraction solvent;
Place the extraction tube that described extraction flask is interior, be used for accommodating testing sample, this extraction tube upper end is uncovered, and the tube wall middle and upper part is provided with liquid overflow hole;
The vapour-liquid shunt head that be used for to connect Dean-Stark water trap and extraction flask, this vapour-liquid shunt head are provided with the downspout that makes progress and enter the Steam Pipe of Dean-Stark water trap and enter for liquid extraction tube from the Dean-Stark water trap downwards by this vapour-liquid shunt head by this vapour-liquid shunt head in the extraction flask for steam.
According to specific embodiments of the present utility model, the device that the utility model is used for working sample oil and/or liquid water content also comprises:
The Dean-Stark water trap: this water trap can adopt the Dean-Stark water trap of prior art, its structure as mentioned above, this water trap main body is a vertical column glass tube, and the top links to each other with the bottom of condenser, and the below connects the water trap with metering scale; An arm is tiltedly stretched out as the solvent refluxing pipe in vertical column glass tube middle and upper part in the water trap main body, and this arm and column glass tube below tube wall acutangulate, and arm lower end folding is for vertically also being connected with extraction flask by described vapour-liquid shunt head.
According to the preferred specific embodiments of the utility model, the utility model is used in the device of working sample oil and/or liquid water content, described vapour-liquid shunt head arranges upper grinding port and lower ground, and upper grinding port and water trap arm lower end form and be tightly connected, and lower ground and extraction flask bottleneck form and be tightly connected.
According to the preferred specific embodiments of the utility model, the device that the utility model is used for working sample oil and/or liquid water content also comprises: the condenser that is used for condensation Dean-Stark water trap solvent vapo(u)r and water vapour, this condenser can be reflux condenser commonly used in the prior art, and its concrete structure the utility model repeats no more.
According to the preferred specific embodiments of the utility model, the utility model is used in the device of working sample oil and/or liquid water content, described extraction tube is positioned at the center of extraction flask, and the bottom connection of bottom and extraction flask touches, when heating extracting, the solvent that can keep reaching in the extraction tube in the extraction flask is in fluidized state all the time.
According to the preferred specific embodiments of the utility model, the utility model is used in the device of working sample oil and/or liquid water content, and the downspout of described vapour-liquid shunt head is positioned at the eccentric position of vapour-liquid shunt head, and the downspout lower end extends to the bottom of extraction tube.
According to the preferred specific embodiments of the utility model, the utility model is used in the device of working sample oil and/or liquid water content, the Steam Pipe top of described vapour-liquid shunt head is higher than the place, liquid inlet of downspout, preferably, the Steam Pipe top of described vapour-liquid shunt head is higher than the 1.5cm of place, liquid inlet of downspout at least, that is, the discrepancy in elevation can effectively prevent like this that at least greater than 1.5cm the reflux solvent in the water trap from flowing into extraction flask from Steam Pipe.
When utilizing the device for working sample oil and/or liquid water content described in the utility model that sample is carried out extracting, carry out in accordance with the following methods: extraction solvent is placed extraction flask, testing sample is placed in the extraction tube with the filter paper parcel, utilize heating arrangement that the solvent in the extraction flask is heated, make that the water in the sample forms steam in solvent in the extraction flask and the extraction tube, these steam enter in the Dean-Stark water trap through the Steam Pipe rising of vapour-liquid shunt head, after being condensed into liquid, again through solvent with the layering of water so that the moisture in the sample is separated and then the liquid water content of working sample.
After extracting is complete, sample is dry, solvent evaporates is weighed to the sample constant weight, and according to the quality of separating water outlet from water trap, utilize the decrement method to calculate the oil content of sample.
According to the preferred experimental program of the utility model, in the described extractive process, the solvent that reaches in the extraction tube in the extraction flask is in fluidized state all the time.
Device of the present utility model, can be widely used in oil and/or liquid water content in solid-state or semi-solid petroleum products, petroleum chemicals, mineral or the food are measured, can be oily sludge, oil-sand, pitch, resinous shale, bread, biscuit, fries etc. such as testing sample.Preferably, described extraction solvent be good to oily dissolubility and density less than the organic solvent of water, such as toluene, hexane and sherwood oil etc.
The beneficial effects of the utility model:
Compare with " the Dean-Stark modifying device " of prior art, the utility model, to change to the shower extractive process of sample continuous dynamic leaching process into, enter the bottom of extraction tube from the liquid toluene of vapour-liquid shunt head downspout outflow, when liquid level rises to the liquid overflow hole of extraction tube middle and upper part in the pipe to be extracted, flowed out continuously by liquid overflow hole, flow in the extraction flask.Solvent in the extraction tube overflows and the violent disturbance of solvent steam bubble continuously, can guarantee that solvent is to the complete extracting of solvable oil content in the sample, also can make simultaneously the water in the sample steam and after condenser condenses, enter into the water trap bottom of water trap fully with the form of water-solvent azeotropic mixture, thereby make measurement result more accurately and reliably.Experimental result shows, " Dean-Stark modifying device " than prior art utilizes the utility model device, and the oil in the testing sample and/or liquid water content are measured, accuracy and the collimation of determination data increase substantially, and extraction efficiency also increases substantially simultaneously; And the utility model apparatus cost is cheap, is suitable for large scale application.
Description of drawings
Fig. 1 is prior art " Dean-Stark modifying device " structural representation.
Fig. 2 is the structural representation that the utility model is used for working sample oil and/or liquid water content device.
Fig. 3 is the plan structure schematic diagram that the utility model is used for extraction tube in working sample oil and/or the liquid water content device.
Fig. 4 is the structural representation of facing that the utility model is used for extraction tube in working sample oil and/or the liquid water content device.
Fig. 5 is the plan structure schematic diagram that the utility model is used for vapour-liquid shunt head in working sample oil and/or the liquid water content device.
Fig. 6 is the structural representation of facing that the utility model is used for vapour-liquid shunt head in working sample oil and/or the liquid water content device.
Fig. 7 is that oil content is measured " the Dean-Stark modifying device " of speed and prior art to the correlation curve figure of oil content mensuration speed in the oily sludge in specific embodiment 2 oily sludges.
Fig. 8 is that " the Dean-Stark modifying device " of Water content determination speed and prior art in specific embodiment 2 oily sludges is to the correlation curve figure of Water content determination speed in the oily sludge.
Embodiment
Also further describe by reference to the accompanying drawings apparatus structure characteristics of the present utility model and result of use below by specific embodiment, but therefore the utility model is not subject to any restriction.
As shown in Figure 2, the device that is used for working sample oil and/or liquid water content that the present embodiment provides mainly comprises:
Dean-Stark water trap 1, this water trap main body are a vertical column glass tube, and the top links to each other with the bottom of reflux condenser 2, and the below connects the water trap 11 with metering scale; Tiltedly stretch out an arm as the solvent refluxing pipe in the vertical column glass tube middle and upper part of water trap main body, arm and column glass tube below tube wall acutangulate, folding was for vertically, in order to insert in the top ground of extraction element vapour-liquid shunt head 5 when arm was stretched over end.
Described extraction element part mainly is to utilize solvent that sample is carried out extracting and make solvent and the steam of water enters Separation of Water in the Dean-Stark water trap, and then is able to the liquid water content of working sample, and this extraction element mainly comprises:
The extraction flask 3 that is used for accommodating extraction solvent;
Place in the described extraction flask 3, be used for the extraction tube 4 (seeing Fig. 3, extraction tube structural representation illustrated in Figure 4 for details) of accommodating testing sample, this extraction tube 4 be glass test tube, and is uncovered on it, and the tube wall middle and upper part is provided with liquid overflow hole 41:
The vapour-liquid shunt head 5 (seeing Fig. 5, vapour-liquid shunt head structural representation shown in Figure 6 for details) that be used for to connect Dean-Stark water trap and extraction flask, this vapour-liquid shunt head 5 are provided with to make progress in the extraction flask to enter the Steam Pipe 51 of Dean-Stark water trap and flow downward from the Dean-Stark water trap for liquid by this vapour-liquid shunt head for steam and enter the downspout 52 of extraction tube by this vapour-liquid shunt head; Steam Pipe 51 tops are higher than the place, liquid inlet of downspout 52, and preferred heights is poor at least greater than 1.5cm; Downspout 52 is positioned at the eccentric position of vapour-liquid shunt head, and the downspout lower end extends to the bottom of extraction tube; And, vapour-liquid shunt head 5 arranges upper and lower ground, and (upper grinding port shown in the figure is interior ground, lower ground is outer grinding port), upper grinding port and water trap 1 arm lower end are tightly connected, be tightly connected between lower ground and extraction flask 3 bottlenecks, for guaranteeing airtight nothing gas leakage between mensuration process ground, to smear vaseline between ground during mensuration, guaranteed the sealing that connects.
In utilizing this device working sample when oil and/or liquid water content, solvent (the organic solvent good and less than water-mass density to oily dissolubility of packing in the extraction flask 3, such as toluene, hexane, sherwood oil etc.), testing sample places extraction tube 4 (at random in extractive process for preventing testing sample, as can to wrap sample with filter paper or filter screen in advance).Utilize heating arrangement 6 that the solvent in the extraction flask 3 is heated to boiling, the steam of solvent and water enters the arm of water trap 1 by Steam Pipe 51 risings of vapour-liquid shunt head 5, and rise to condenser 2 along arm, be condensed in the water trap 11 of the backward lower inflow water trap 1 of liquid through condenser 2, the layering in the water trap of solvent and water, lower floor is water, the upper strata is solvent, when treating that the solvent of condensation in the water trap 1 water trap and water increase to the arm junction gradually, flow downward and flow into extraction tubes 4 bottoms through the downspout 52 of vapour-liquid shunt head 5 along arm, testing sample at extraction tube 4 in-built useful filter paper parcels, the solvent of extraction tube 4 interior excessive buildup is flowed in the extraction flask 3 by liquid overflow hole 41, repeats said process through heating.In the extractive process, the addition of extraction flask internal solvent should ensure enough liquid and overflow from the extraction tube liquid overflow hole; The loading height of sample should be lower than liquid overflow hole in the extraction tube; Also can suitably control heating power, flow out continuously to guarantee the condensed fluid in the condenser pipe, etc., these for a person skilled in the art can be according to its operating experience and definite voluntarily after reading the utility model, and the utility model repeats no more.
After the extracting complete (usually increase in half an hour with the volume of water in the water trap and be no more than 0.1mL to be considered as extracting complete), the sample oven dry that extracting is complete (usually dry under 100-120 ℃ of condition), make solvent evaporates, from the water trap of water trap, read the volume number of water, then be translated into the liquid water content of sample, utilize the oil content of decrement method calculation sample, circular can be with reference to following computing formula:
The computing formula that the water volume that reads from described water trap water trap is converted into quality the sample is:
m
w=V
w×ρ
w
The computing formula that the water volume that reads from described water trap water trap is converted into sample water content is:
Utilize the computing formula of decrement method calculation sample oil content to be:
Above-mentioned various in:
S
wLiquid water content in the-sample, g (water)/g;
S
oOil content in the-sample, g (oil)/g;
V
wThe volume of water in the-water trap water trap, mL;
ρ
wThe density of water under the-mensuration temperature conditions, g/mL;
m
wThe quality of water in the-water trap water trap, g;
m
S0The initial mass of-sample, g;
m
SeThe solids quality of sample after-extracting and the dry constant weight, g.
The utility model is used in the device of working sample oil and/or liquid water content, described extraction tube is positioned at the extraction flask center, its bottom contacts with the extraction flask bottom, can heat sample in the extraction tube and solvent better like this, in extractive process, extraction tube 4 inside and outside solvents are in fluidized state all the time.Overflowing continuously of the violent disturbance of extraction tube 4 interior steam bubbles and solvent can guarantee that not only solvent is with the complete extracting of soluble oil content in the testing sample, the water that contains in the oil samples is steamed fully with the form of water-solvent azeotropic mixture, thereby make measurement result more accurately and reliably.
Take oily sludge A as testing sample, the device and method that utilizes embodiment 1 carries out extracting to the oil of oily sludge and liquid water content and measures, the tested oily sludge sample that extracting is complete is dry under 115 ℃ of conditions, makes the toluene volatilization and weigh the content of calculating oil and water to the sample constant weight.And compare with " Dean-Stark modifying device " measurement result of utilizing prior art shown in Figure 1, measurement result is listed in the table below.
The collimation analysis of oily sludge A oil content (wet basis massfraction) measurement result
The collimation analysis of oily sludge A liquid water content (wet basis massfraction) measurement result
In the present embodiment, also the extracting speed of oil in the oily sludge and water has been carried out record, the result is referring to Fig. 7 and Fig. 8, can be found out by Fig. 7 and Fig. 8, " Dean-Stark modifying device " than prior art, utilize oil of the present utility model and/or Water content determination method and device, oil and the extracting speed of water in the oily sludge are also had by a relatively large margin lifting.
Take oil-sand B as testing sample, to utilize the device and method of embodiment 1 that sample is carried out extracting mensuration, and compare with " Dean-Stark modifying device " measurement result of utilizing prior art shown in Figure 1, measurement result is listed in the table below.
The collimation analysis of the oil content of oil-sand B (wet basis massfraction) measurement result
The collimation analysis of the liquid water content of oil-sand B (wet basis massfraction) measurement result
Take resinous shale C as testing sample, to utilize the device and method of embodiment 1 that sample is carried out extracting mensuration, and compare with " Dean-Stark modifying device " measurement result of utilizing prior art shown in Figure 1, measurement result is listed in the table below.
The collimation analysis of the oil content of resinous shale C (wet basis massfraction) measurement result
The liquid water content of resinous shale C: liquid water content is vestige in the resinous shale.
Take chips D as testing sample, utilize the device and method of embodiment 1 that sample is carried out extracting mensuration, and compare with " Dean-Stark modifying device " measurement result of utilizing prior art shown in Figure 1.
The transversal section of chips is square, is of a size of 1.0 ± 0.1cm (the section length of side) * 5 ± 0.1cm (potato slices length);
Fried medium: commodity eat salad oil;
Frying temperature: 160 ℃;
The fried time: t=5min;
After fried the finishing, potato slices are taken out, control oily 2min surperficial oil slick is flowed away, cool off under the room temperature condition.
Cooled sample is carried out the mensuration of oil and liquid water content.
Measurement result is listed in the table below.
The collimation analysis of the oil content of chips D (wet basis massfraction) measurement result
The collimation analysis of the liquid water content of chips D (wet basis massfraction) measurement result
Upper table is the collimation analytical table of liquid water content (wet basis massfraction) measurement result of chips D.
Claims (8)
1. a device that is used for working sample oil and/or liquid water content is characterized in that, this device comprises:
Utilize solvent that sample is carried out extracting and separate moisture so that the steam of solvent and water enters in the Dean-Stark water trap, and then measured the extraction element of moisture, this extraction element comprises:
The extraction flask that is used for accommodating extraction solvent;
Place the extraction tube that described extraction flask is interior, be used for accommodating testing sample, this extraction tube upper end is uncovered, and the tube wall middle and upper part is provided with liquid overflow hole;
The vapour-liquid shunt head that be used for to connect Dean-Stark water trap and extraction flask, this vapour-liquid shunt head are provided with the downspout that makes progress and enter the Steam Pipe of Dean-Stark water trap and enter for liquid extraction tube from the Dean-Stark water trap downwards by this vapour-liquid shunt head by this vapour-liquid shunt head in the extraction flask for steam.
2. the device for working sample oil and/or liquid water content according to claim 1 is characterized in that, this device also comprises:
Dean-Stark water trap, this water trap main body are a vertical column glass tube, and the top links to each other with the bottom of condenser, and the below connects the water trap with metering scale; Tiltedly stretch out an arm as the solvent refluxing pipe in the vertical column glass tube middle and upper part of water trap main body, this arm and column glass tube below tube wall acutangulate, and arm lower end folding is for vertically also being connected with extraction flask by described vapour-liquid shunt head.
3. the device for working sample oil and/or liquid water content according to claim 2, it is characterized in that, described vapour-liquid shunt head arranges upper grinding port and lower ground, and upper grinding port and water trap arm lower end form and be tightly connected, and lower ground and extraction flask bottleneck form and be tightly connected.
4. the device for working sample oil and/or liquid water content according to claim 1 is characterized in that, this device also comprises:
The reflux condenser that is used for condensation Dean-Stark water trap solvent vapo(u)r and water vapour.
5. the device for working sample oil and/or liquid water content according to claim 1 is characterized in that, described extraction tube is positioned at the center of extraction flask, and the bottom connection of bottom and extraction flask touches.
6. the device for working sample oil and/or liquid water content according to claim 1 is characterized in that, the downspout of described vapour-liquid shunt head is positioned at the eccentric position of vapour-liquid shunt head, and the downspout lower end extends to the bottom of extraction tube.
7. be used for according to claim 1 or 5 the device of working sample oil and/or liquid water content, it is characterized in that, the Steam Pipe top of described vapour-liquid shunt head is higher than the place, liquid inlet of downspout.
8. be used for according to claim 1 or 5 the device of working sample oil and/or liquid water content, it is characterized in that, the Steam Pipe top of described vapour-liquid shunt head is higher than the 1.5cm of place, liquid inlet of downspout at least.
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CN102778409A (en) * | 2012-06-05 | 2012-11-14 | 中国石油大学(北京) | Device and method used for measuring content of oil and/ or liquid water in sample |
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CN102778409A (en) * | 2012-06-05 | 2012-11-14 | 中国石油大学(北京) | Device and method used for measuring content of oil and/ or liquid water in sample |
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Granted publication date: 20130220 |