CN102778409A - Device and method used for measuring content of oil and/ or liquid water in sample - Google Patents
Device and method used for measuring content of oil and/ or liquid water in sample Download PDFInfo
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- CN102778409A CN102778409A CN2012101832716A CN201210183271A CN102778409A CN 102778409 A CN102778409 A CN 102778409A CN 2012101832716 A CN2012101832716 A CN 2012101832716A CN 201210183271 A CN201210183271 A CN 201210183271A CN 102778409 A CN102778409 A CN 102778409A
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Abstract
The invention provides to a device and a method used for measuring the content of oil and/ or liquid water in a sample. The device comprises an extraction device which is used for measuring the content of water by utilizing a solvent to carry out extraction on the sample so that the steams of the solvent and water enter into a Dean-Stark water separator to isolate water; the extraction device comprises an extraction bottle used for placing an extraction solvent, an extraction pipe which is placed in the extraction bottle and is used for placing samples to be tested and a vapor-liquid split-flow head which is used for connecting the water separator with the extraction bottle, wherein the upper end of the extraction pipe is opened, and the upper part of the pipe wall is provided with a discharge hole; the vapor-liquid split-flow head is provided with a steam raising pipe in which steam upward passes through the vapor-liquid split-flow head from the extraction bottle to enter a water separator and a downtake pipe in which liquid downward passes through the vapor-liquid split-flow head so as to enter the extraction pipe. The device provided by the invention is utilized to measure the content of the oil and/ or water in the sample, the accuracy and the stability are good, the manufacturing cost is cheap, and the device is suitable for large-area popularization and application.
Description
Technical field
The present invention relates to the device and method of oil in a kind of working sample and/or liquid water content; More particularly, be meant a kind of improved Dean-Stark device and utilize this device to measure the method for oil in solid-state in petroleum industry or the food industry, the semisolid sample and/or liquid water content.
Background technology
In some scientific researches of petroleum industry or food industry, need usually oil in the sample and/or liquid water content are measured.Dean-Stark device (being called Dean-Stark receiver or Dean-Stark distiller again) is a kind of glass apparatus through liquid water content in the distillating method working sample of using always.
For example; What oil/liquid water content was measured employing in the oily sludge at present is " the Dean-Stark modifying device " that the fuel-efficient management of sand of Canadian Alberta office is recommended; Its structure sees for details shown in Figure 1; This device mainly comprises extraction element part and Dean-Stark separation vessel, and the extraction element part mainly is to utilize solvent that sample is carried out extracting so that separate moisture and then must measure moisture in solvent vapo(u)r and the water vapour entering Dean-Stark separation vessel, utilizes the decrement method to calculate oil content again.The core of being somebody's turn to do " Dean-Stark modifying device " is a 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, below connection can measure liquid volume water trap 101 (have metering scale, this water trap 101 also can change into be similar to buret the glass gathering-device to collect the liquid of more volume); An arm (or claiming recirculatory pipe) is tiltedly stretched out in the middle and upper part of these water trap 10 main body glass tubes; Arm and column glass tube below tube wall acutangulate, and arm is stretched over to be rolled over when closing on end for vertically, so that insert in the crossover sub 50 that connects extraction flask.The extraction element part mainly comprises extraction flask 30 and is set in the extraction tube 40 in the extraction flask 30 that 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.Be connected through crossover sub 50 grounds between extraction element part and the Dean-Stark water trap 10, be connected sealing between assurance extraction element and the water trap.When utilizing this device to measure oil in oily sludge/liquid water content; Solvent (like 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 heating).Rising along with temperature; Water in extraction flask 30 internal solvent toluene and the sample evaporates in extraction element; Form steam and get into water trap 10 arms; And, be condensed into liquid along the outer reflux condenser that is connected with chilled water of arm entering, splash into the water trap 101 that Dean-Stark water trap 10 is responsible for the below.In water trap 101, solvent toluene that can not be miscible and water generation layering, lower floor is a water, the upper strata is the less toluene solvant of density.Carrying out along with evaporation; When water trap when solvent increases to the arm junction gradually at the middle and upper levels; Will be back in the extraction element along arm, the tested oily sludge with the filter paper parcel directly dashes pouring 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 has then been stayed in the water trap and has been able to measure (if the moisture in the testing sample is higher; Water trap part can change the gathering-device that is made as the band knob that is similar to buret; By the time water is collected certain volume; Can open the knob of gathering-device bottom and emit the water that part is collected, too much get into extraction element) along the arm backflow to prevent the water amount.After extracting finishes, can tested oily sludge sample is dry under 115 ℃ of temperature conditions, make toluene and to constant weight, be scaled the liquid water content of sample according to the volume number that from water trap water trap, reads water, further utilize the decrement method to calculate the oil content of sample.
Above-mentioned " Dean-Stark modifying device "; Simple in structure, easy operating; Not only can be used in oil, the petrochemical industry mensuration of oily sludge oil and/or liquid water content also can be used for measuring other petroleum products, like the liquid water content of tar, emulsified asphalt and other asphalt material; Also can be used in addition in the food industry to some food samples, like the oil of bread, biscuit, fries etc. and/or the mensuration of liquid water content.
Yet, owing to always follow the minimum principle (following the shortest flow principle of point-to-point transmission straight line) of resistance during downward liquid flow, therefore contain oil samples, like oily sludge, in oil can not be complete by extracting; Carry out extracting next time and make extraction tube be suspended from that the complete extracting for oil also is disadvantageous (relies on fully to dash and drench) in the extraction flask for the solvent that guarantees to flow in the extraction tube flows out rapidly in addition, the direct result of these problems is that the accuracy and the collimation of oil content determination data is relatively poor.
Summary of the invention
One object of the present invention is the existing problem of device to oil in the above-mentioned existing method working sample and/or liquid water content; Measurement mechanism is improved; The device of oil in a kind of new working sample and/or liquid water content is provided, to improve the accuracy and the collimation of determination data.
Another object of the present invention is to provide a kind of method of utilizing oil in the said device working sample and/or liquid water content, accurately and rapidly the content of oil and/or water in the working sample.
For achieving the above object; On the one hand; The invention provides the device of oil in a kind of working sample and/or liquid water content; This device has mainly partly been done 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, improves accuracy and the collimation measured.Specifically, the device of oil and/or liquid water content mainly comprises in the working sample provided by the invention:
Utilize solvent that sample is carried out extracting so that the steam of solvent and water gets into and divides dried up in the Dean-Stark water trap and be able to the extraction element of working sample liquid water content, this extraction element mainly comprises:
The extraction flask that is used for ccontaining extraction solvent;
Place the extraction tube that said extraction flask is interior, be used for ccontaining testing sample, this extraction tube upper end is uncovered, and the tube wall middle and upper part is provided with liquid overflow hole;
Be used to connect the vapour-liquid shunt head of Dean-Stark water trap and extraction flask, this vapour-liquid shunt head is provided with and supplies steam in extraction flask, upwards to get into the Steam Pipe of Dean-Stark water trap and pass through the downspout that this vapour-liquid shunt head gets into the extraction tube bottom downwards from the Dean-Stark water trap for liquid through this vapour-liquid shunt head.
According to specific embodiments of the present invention, the device of oil and/or liquid water content also comprises in the working sample of the present invention:
The Dean-Stark water trap: this water trap can adopt the Dean-Stark water trap of prior art; Its structure can be with reference to as previously mentioned; 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 that has metering scale; Tiltedly stretch out an arm as the solvent refluxing pipe in the middle and upper part of the vertical column glass tube 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 through said vapour-liquid shunt head.
The preferred specific embodiments according to the present invention; The device of oil and/or liquid water content also comprises in the working sample of the present invention: the condenser that is used for condensation Dean-Stark water trap steam; This condenser can be reflux condenser commonly used in the prior art, and its concrete structure the present invention repeat no more.
The preferred specific embodiments according to the present invention; In the working sample of the present invention in the device of oil and/or liquid water content; Said vapour-liquid shunt head is provided with upper and lower ground, and upper grinding port and water trap arm lower end form and be tightly connected, and forms between following ground and the extraction flask bottleneck to be tightly connected.
The preferred specific embodiments according to the present invention; In the working sample of the present invention in the device of oil and/or liquid water content; Said extraction tube is positioned at the extraction flask center; Its bottom contacts with the extraction flask bottom, and when heating extracting, the solvent that can keep reaching in the extraction tube in the extraction flask is in fluidized state all the time.
The preferred specific embodiments according to the present invention, in the device of oil and/or liquid water content, the downspout of said vapour-liquid shunt head is positioned at the eccentric position of vapour-liquid shunt head in the working sample of the present invention, and the downspout lower end extends to the bottom of extraction tube.
The preferred specific embodiments according to the present invention; In the working sample of the present invention in the device of oil and/or liquid water content; The Steam Pipe top of said vapour-liquid shunt head is higher than the place, liquid inlet of downspout; Preferably potential difference 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.
On the other hand, the present invention also provides the method for oil in a kind of working sample and/or liquid water content, and this method comprises:
Utilize the device of oil in the working sample of the present invention and/or liquid water content that sample is carried out extracting: extraction solvent is placed extraction flask; Testing sample is placed extraction tube; Utilize heating arrangement that the solvent in the extraction flask is heated; Make that the water in the sample forms steam in solvent and the extraction tube in the extraction flask; These steam rise and get in the Dean-Stark water trap, after being condensed into liquid, make the moisture in the sample be able to separate through the layering of solvent and water again, and then the liquid water content of working sample.
The preferred specific embodiments according to the present invention, the method for oil and/or liquid water content also comprises in the working sample of the present invention:
After extracting finishes, sample is dry, weigh after making solvent evaporates to sample constant weight, and, utilize the decrement method to calculate the oil content of sample according to the quality of separating water outlet from water trap.
The preferred specific embodiments according to the present invention, the method for oil and/or liquid water content in the working sample of the present invention, in the said extractive process, the solvent that keeps reaching in the extraction tube in the extraction flask is in fluidized state always.
The preferred specific embodiments according to the present invention, in the working sample of the present invention in the method for oil and/or liquid water content, said extraction solvent preferably to oily dissolubility good and density less than the organic solvent of water, like toluene, hexane, sherwood oil etc.
Device and method of the present invention; Can be adaptable across water and/or oil in solid-state or semi-solid petroleum products or mineral or the food are measured; As, testing sample can be oily sludge, oil-sand, pitch, resinous shale, bread, biscuit, fries etc.
Compare with " the Dean-Stark modifying device " of prior art; Among the present invention; To drench extractive process to dashing of sample and change the continuous dynamic leaching process into, the liquid toluene that flows out from vapour-liquid shunt head downspout gets into the bottom of extraction tube, when treating that liquid level rises to the liquid spill-way of extraction tube middle and upper part in the extraction tube; Flow out continuously by liquid spill-way, enter into extraction flask.Solvent in the extraction tube overflows and the violent disturbance of solvent steam bubble continuously; Can guarantee the complete extracting of solvent to 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, thereby make the mensuration result more accurately and reliably with the form of water-solvent azeotropic mixture.Experimental result shows; " Dean-Stark modifying device " than prior art utilizes device and method of the present invention, and oil in the testing sample and/or liquid water content are measured; The accuracy and the collimation of determination data increase substantially, and extraction efficiency also increases substantially simultaneously.And apparatus cost of the present invention is cheap, so be suitable for large scale application.
Description of drawings
Fig. 1 is prior art " Dean-Stark modifying device " structural representation.
Fig. 2 is the apparatus structure synoptic diagram of oil and/or liquid water content in the working sample of the present invention.
Fig. 3 is the plan structure synoptic diagram of extraction tube in oil and/or the liquid water content device in the working sample of the present invention.
Fig. 4 is the structural representation of facing of extraction tube in oil in the working sample of the present invention and/or the liquid water content device.
Fig. 5 is the plan structure synoptic diagram of vapour-liquid shunt head in oil and/or the liquid water content device in the working sample of the present invention.
Fig. 6 is the structural representation of facing of vapour-liquid shunt head in oil in the working sample of the present invention 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 comparative graph to oil content mensuration speed in the oily sludge in specific embodiment 2 oily sludges.
Fig. 8 is that liquid water content is measured " the Dean-Stark modifying device " of speed and prior art comparative graph to liquid water content mensuration speed in the oily sludge in specific embodiment 2 oily sludges.
Embodiment
Below through specific embodiment and combine accompanying drawing further explain apparatus and method characteristics of the present invention and result of use, but therefore the present invention does not receive any restriction.
As shown in Figure 2, the device of oil and/or liquid water content mainly comprises in the working sample that present embodiment provides:
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 that has 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 vertical, so that in the top ground of the vapour-liquid shunt head 5 of insertion extraction element when arm was stretched over end.
Said extraction element part mainly is to utilize solvent that sample is carried out extracting and make solvent and the steam of water gets into and divides dried uply 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 ccontaining extraction solvent;
Place in the said extraction flask 3, be used for the extraction tube 4 of ccontaining testing sample; See Fig. 3, extraction tube structural representation shown in Figure 4 for details, this extraction tube 4 is a glass test tube, and its upper end is uncovered, and the tube wall middle and upper part is provided with liquid overflow hole 41;
Be used to connect the vapour-liquid shunt head 5 of Dean-Stark water trap and extraction flask; See Fig. 5, vapour-liquid shunt head structural representation shown in Figure 6 for details, this vapour-liquid shunt head 5 is provided with the downspout 52 that supplies steam upwards to get into the Steam Pipe 51 of Dean-Stark water trap and get into extraction tube for liquid from the Dean-Stark water trap downwards through this vapour-liquid shunt head through this vapour-liquid shunt head in the extraction flask; Steam Pipe 51 tops are higher than the place, liquid inlet of downspout 52, and preferred potential difference is 1.5cm at least; 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 is provided with upper and lower ground, and (upper grinding port shown in the figure is interior ground; Following ground is an outer grinding port), upper grinding port and water trap 1 arm lower end form and are tightly connected, and form between following ground and extraction flask 3 bottlenecks to be tightly connected; Guaranteed the sealing that connects (, will smear vaseline between ground during experiment) for guaranteeing airtight nothing gas leakage between mensuration process ground.
In utilizing this device working sample when oil and/or liquid water content; Solvent (the organic solvent good and littler of packing in the extraction flask 3 than water-mass density to oily dissolubility; Like toluene, hexane, sherwood oil etc.); Testing sample places extraction tube 4 (at random in extractive process for preventing testing sample, as can to have wrapped up 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; Solvent vapo(u)r and water vapour pass through the arm of the Steam Pipe 51 rising entering water traps 1 of vapour-liquid shunt head 5, and rise to condenser 2 along arm, after condenser 2 is condensed into liquid, flow in the water trap 11 of water trap 1 downwards; The layering in the water trap of solvent and water; Lower floor is a water, and the upper strata is a solvent, when the solvent of treating condensation in the water trap 1 water trap increases to the arm junction gradually; Flow downward and flow into extraction tubes 4 bottoms along arm through the downspout of vapour-liquid shunt head 5 52; Testing sample with the filter paper parcel is housed in extraction tube 4, and the solvent of excessive buildup will be flowed in the extraction flask 3 by liquid overflow hole 41 in the extraction tube 4, through heating repetition said process.In the extractive process, the addition of extraction flask internal solvent should guarantee that enough liquid overflows 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, or the like, these can confirm that voluntarily the present invention repeats no more according to its operating experience for a person skilled in the art after reading the present invention.
Extracting finishes after (usually increase in half an hour with the volume of water trap water and be no more than 0.1ml and be regarded as extracting and finish); The sample that extracting finishes is dried (dry under 100-120 ℃ of condition usually); Make solvent evaporates; From the water trap of water trap, read the volume number of water, be translated into the liquid water content of sample then, utilize the decrement method to calculate the oil content of sample.Concrete computing method can be with reference to following computing formula:
The computing formula that the water volume that reads from said 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 said 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
wWater volume in the-water trap water trap, mL;
ρ
wThe density of water under the-mensuration temperature conditions, g/mL;
m
wThe quality of-water, g;
m
S0The initial mass of-sample, g;
m
SeSample solids quality after-extracting and the dry constant weight, g.
In the working sample of the present invention in the device of oil and/or liquid water content; Said extraction tube bottom is positioned at the extraction flask center and 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 always.The violent disturbance and the overflowing continuously of solvent of bubble can guarantee that not only solvent is with the complete extracting of soluble oil content in the testing sample in the extraction tube 4; The water that contains in the oil samples is steamed with the form of water-solvent azeotropic mixture fully, measure the result more accurately and reliably thereby make.
With oily sludge A is testing sample; Utilize the device and method of embodiment 1 that oily sludge oil, liquid water content are carried out extracting mensuration; The tested oily sludge sample that extracting finishes is dry under 115 ℃ of conditions, make toluene and to the sample constant weight, weigh the content of calculating oil, water.And measure the result with " the Dean-Stark modifying device " that utilize prior art shown in Figure 1 and compare, measure the result and be listed in the table below.
Oily sludge A oil content (wet basis massfraction) is measured collimation analysis as a result
Oily sludge A liquid water content (wet basis massfraction) is measured collimation analysis as a result
In the present embodiment; Also the extracting speed of oil, water in the oily sludge has been carried out record; The result can find out referring to Fig. 7 and Fig. 8, than " the Dean-Stark modifying device " of prior art; Utilize oil of the present invention and/or liquid water content assay method and device, the extracting speed of oil and water also has greatly improved.
With oil-sand B is testing sample, utilizes the device and method of embodiment 1 that sample is carried out extracting mensuration, and compares with " Dean-Stark modifying device " mensuration result who utilizes prior art shown in Figure 1, measures the result and is listed in the table below.
The oil content of oil-sand B (wet basis massfraction) is measured collimation analysis as a result
The liquid water content of oil-sand B (wet basis massfraction) is measured collimation analysis as a result
With resinous shale C is testing sample, utilizes the device and method of embodiment 1 that sample is carried out extracting mensuration, and compares with " Dean-Stark modifying device " mensuration result who utilizes prior art shown in Figure 1, measures the result and is listed in the table below.
The oil content of resinous shale C (wet basis massfraction) is measured collimation analysis as a result
The liquid water content of resinous shale C: liquid water content is a vestige in the resinous shale.
With chips D is testing sample, utilizes the device and method of embodiment 1 that sample is carried out extracting mensuration, and compares with " Dean-Stark modifying device " mensuration result who utilizes prior art shown in Figure 1.
Chips: the transversal section is square dimensions: 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 the fried completion, potato slices are taken out, control oily 2min surface oil is flowed away, room temperature condition cooling down.
Cooled product is carried out the mensuration of oil/liquid water content.
Mensuration result is listed in the table below.
The oil content of chips D (wet basis massfraction) is measured collimation analysis as a result
The liquid water content of chips D (wet basis massfraction) is measured collimation analysis as a result
Claims (10)
1. the device of oil and/or liquid water content in the working sample, this device comprises:
Utilize solvent that sample is carried out extracting and separate moisture so that the steam of solvent and water gets in the Dean-Stark water trap, and then be able to measure the extraction element of moisture, this extraction element comprises:
The extraction flask that is used for ccontaining extraction solvent;
Place the extraction tube that said extraction flask is interior, be used for ccontaining testing sample, this extraction tube upper end is uncovered, and the tube wall middle and upper part is provided with liquid overflow hole;
Be used to connect the vapour-liquid shunt head of Dean-Stark water trap and extraction flask, this vapour-liquid shunt head is provided with and supplies steam in extraction flask, upwards to get into the Steam Pipe of Dean-Stark water trap and pass through the downspout that this vapour-liquid shunt head gets into extraction tube downwards from the Dean-Stark water trap for liquid through this vapour-liquid shunt head.
2. the device of oil and/or liquid water content in the working sample according to claim 1, 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 that has metering scale; Tiltedly stretch out an arm as the solvent refluxing pipe in the middle and upper part of the vertical column glass tube 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 through said vapour-liquid shunt head;
Preferably, this device also comprises: the reflux condenser that is used for condensation Dean-Stark water trap steam.
3. the device of oil and/or liquid water content in the working sample according to claim 2; Wherein, Said vapour-liquid shunt head is provided with upper grinding port and reaches ground down, and upper grinding port and water trap arm lower end form and be tightly connected, and forms between following ground and the extraction flask bottleneck to be tightly connected.
4. the device of oil and/or liquid water content in the working sample according to claim 1, wherein, said extraction tube is positioned at the center of extraction flask, the pig of bottom and extraction flask.
5. the device of oil and/or liquid water content in the working sample according to claim 1, wherein, the downspout of said 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.
6. according to the device of oil and/or liquid water content in claim 1 or the 5 described working samples, wherein, the Steam Pipe top of said vapour-liquid shunt head is higher than the liquid inlet height of downspout, and preferred potential difference is at least greater than 1.5cm.
7. the method for oil and/or liquid water content in the working sample, this method comprises:
Utilize the device of oil in each described working sample of claim 1～6 and/or liquid water content sample to be carried out the extracting of oil and/or water: solvent is placed extraction flask; Testing sample is placed extraction tube; Utilize heating arrangement that the solvent in the extraction flask is heated, make that the water in the sample forms steam in solvent and the extraction tube in the extraction flask, these steam rise and get in the Dean-Stark water trap; And the water in condensation makes sample is able to separate, and then measures liquid water content.
8. method according to claim 7, this method also comprises:
After extracting finishes, sample is dry, weigh after making solvent evaporates to constant weight, and, utilize the oil content of decrement method calculation sample according to from the isolated water yield of water trap.
9. according to claim 7 or 8 described methods, wherein, in the said extractive process, keep the solvent in extraction flask and the extraction tube to be in fluidized state all the time.
10. method according to claim 7, wherein, said testing sample is solid-state or semi-solid petroleum products or mineral or food, for example oily sludge, oil-sand, pitch, resinous shale, bread, biscuit, fries etc.; Preferably, said extraction solvent be to oily dissolubility good and density less than the organic solvent of water, for example toluene, hexane, sherwood oil etc.
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