CN106198153B - A kind of degreasing method - Google Patents

A kind of degreasing method Download PDF

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Publication number
CN106198153B
CN106198153B CN201610492877.6A CN201610492877A CN106198153B CN 106198153 B CN106198153 B CN 106198153B CN 201610492877 A CN201610492877 A CN 201610492877A CN 106198153 B CN106198153 B CN 106198153B
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cylinder
sample
immersion
centrifugation
degreasing
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CN106198153A (en
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石建州
赵金兵
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Nanyang Normal University
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Nanyang Normal University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/30Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

The present invention relates to a kind of degreasing methods, belong to fat content the field of test technology.The degreasing method includes the following steps: to carry out sample to be processed into following degreasing operation unit primary or more than twice: being centrifugated using impregnating after solvent is impregnated;Up to degreasing sample.Degreasing method of the invention can increase substantially the efficiency that fat dissolves out in soak.

Description

A kind of degreasing method
Technical field
The present invention relates to a kind of degreasing methods, belong to fat content the field of test technology.
Background technique
Measurement feed and the device of the crude fat content in food are Soxhlet extractors at present, using lipolyse in organic The characteristic of solvent extracts the fat in sample in such a way that sample is distilled and flowed back repeatedly, then removes organic Solvent can measure the fat content in sample.Due to also containing free fatty acid, phosphatide, sterol in the fat that extracts Equal liposoluble substances, so referred to as crude fat.
Soxhlet extractor when in use, first grinds sample material, to increase the area of solid-liquid contact, then puts sample It in filter paper packet, is placed in extractor, the lower end of extractor is connected with the round-bottomed flask for filling leaching solvent, connects returned cold above Solidifying pipe, heats round-bottomed flask, solvent is made to boil, and steam is risen by connecting tube, enters in condenser pipe, instills and mentions after being condensed It takes in device, solvent and solid contact are extracted, and when solvent liquid level reaches the highest point of siphon pipe in extractor, contain extraction The solvent siphon of object returns to flask, thus extracts a part of substance.Then the leaching solvent in round-bottomed flask continue evaporation, it is cold Solidifying, leaching, reflux, so repeat, extract solid matter constantly by pure leaching solvent, the material collection extracted is existed In flask.
Soxhlet extractor extracts the fat in sample using the evaporation of solvent, condensation, leaching, reflux, to sample Degreasing is carried out, is instilled in extractor by then passing through condensed pure solvent, sample is leached, when most of in extractor It is interior to be constantly filled with the higher solvent of fatty consistency, and the higher solvent of fatty consistency is then filled in sample particle gap, Influence is caused on the dissolution efficiency of fat remaining in sample, causes the fat in sample to be fully dissolved out and needs to spend very long Time needs to spend 8 hours or more in general, Soxhlet extractor extracts fat.And the whole needs of Soxhlet extractor work are special People's nurse, so as to avoid an accident.
Summary of the invention
The purpose of the present invention is to provide the degreasing methods that one kind can carry out quick degreasing to sample.
To achieve the above object, the technical solution of degreasing method of the invention is:
A kind of degreasing method includes the following steps: to carry out sample to be processed into following degreasing primary or more than twice Operating unit: it is centrifugated using impregnating after solvent is impregnated;Up to degreasing sample.
The time of the immersion is greater than 10min.
The time that method of the invention is impregnated each time should be greater than 10min, which can make the fat in sample It dissolves as far as possible in the solution.The upper limit time of immersion does not require, when arranging with can making staff's maneuverability in this way Between, for example can stay overnight, continue next step within second day, does not influence experimental result, it is more convenient to the time of detection artificial Control.In general, soaking time control is 10-20min if needing to complete test as early as possible in the short time.
When being tested for most of sample, impregnate and the number of repetition of centrifugation can according to the type of sample to be tested into Row adjustment determines that the number of repetition of the sample high for fat content can be more.
The sample to be processed dries 60-90min at 80-90 DEG C before impregnating.
The immersion solvent is ether or petroleum ether.
The sample that last time is centrifugally separating to obtain is dried.To constant weight, the difference of the weight stressed twice is less than for drying 0.001g is considered as constant weight.
The drying can naturally dry at normal temperature, can also dry at relatively high temperatures, accelerate drying efficiency, high temperature Temperature when dry is 105 ± 2 DEG C.For organic solvents such as ether, since its is inflammable and explosive and low boiling point, volatile, generally It takes and is placed on ventilation after wrapping sample with filter paper and dries, so that ether is fully volatilized completely, avoid ether in high temperature It explodes in closed container baking oven, then the sample packet (filter paper packet) dried is put into 105 DEG C ± 2 DEG C of baking oven and is dried to perseverance Amount, is accurate to 0.001g.The purpose to dry to constant weight is to keep away remaining in sample packet (filter paper packet) and the moisture removal absorbed Exempt from influence of the moisture to measurement result, reduces evaluated error.
After obtaining degreasing sample, obtained in sample to be processed according to the Mass Calculation of degreasing sample and sample to be processed Crude fat content.
The pre- degreasing sample is washed using immersion solvent before it is dried.Washing times are 1-2 times.
It impregnates and the duplicate number of centrifugation can determine as follows: after centrifugation, pre- degreasing sample being connected It reinstates fresh immersion solvent with filter paper packet one to be washed, after the immersion solvent on paper bag to be filtered volatilizees completely, filter paper is wrapped Visual grease spot is not left, can be entered next step, otherwise be continued immersion and centrifugally operated.
The sample to be processed includes various samples.Each sample is wrapped respectively in different filter paper packets.
Revolving speed and centrifugation time when centrifugation are provided to get rid of de- soak as far as possible, reduce filter paper packet and dry in ventilation When aerial volatile quantity;And shortening the time that soak volatilizees in filter paper packet, the soak that filter paper includes is more, then filtering The time that paper bag needs sufficiently volatilization to be completely soaked liquid is longer.Specifically, 200 revs/min of revolving speed of the present invention, centrifugation time 2min ?.
Crude fat content in sample to be processed is calculated according to following formula: crude fat content (%)=(m1-m2)/ M × 100%, wherein m is the quality of sample to be processed, and m1 packs into quality of the sample packet before immersion, m2 with filter paper for sample For the quality of pre- degreasing samples packet, mass unit gram.
The immersion and centrifuge separation carry out in same separation vessel.
Be provided with the cylinder for holding sample to be processed in the separation vessel, it is described in be provided with for separation Cylinder be supported and be immersed in cylinder partly or entirely in soak immersion support construction, for propping up cylinder The centrifugation support construction for supportting and making cylinder completely disengage soak and being rotatably assorted with cylinder.
The immersion support construction and centrifugation support construction between be provided with for make cylinder impregnate support construction and It is centrifuged the guide rail of guiding movement between support construction.
The guide rail is the long hole for being arranged on separation vessel side wall and cooperating with cylinder guiding movement.
The cylinder is rotatably assorted with support construction is impregnated.
The cylinder includes the cylinder for holding test sample, and being provided on the cylinder can be such that soak flows into Or the immersion fluid through-hole of outflow tube.In filter paper packet, filter paper packet is placed in the cylinder sample packet to be processed.
The cylinder is arranged in separate tank, and the separation bottom of pond portion has the space for holding and impregnating solvent.Described point Cylinder at least one end is provided with the rotary shaft being rotatably assorted with the separate tank.
The cylinder has reticular structure.
It is detachably provided with rotating handle in the rotary shaft of described cylinder one end or is used to connect with driving motor belt The belt pulley connect when cylinder rotates, rotates rotating handle or drives cylinder rotation by driving motor.
The rotary shaft, which is pierced by the end of soaking container, is arranged with sealing element, which includes being used for sealing blocking phase The occluding body in gap between axis and axis hole is answered, occluding body has the mounting hole installed for the sealing, which is characterized in that blocks At least two elastic valves for being used to block the mounting hole along occluding body circumferentially is provided on body, the elasticity valve can edge The elastomeric radial of mounting hole by the axis can be opened.
The occluding body has the sealed end for being used to cooperate with the face seal for offering axis hole far from one end of elastic valve Face offers mounting hole opening on the seal face.
The sealing element is seal cap, and the seal cap includes the cap body made of elastic material, and the cap body includes cap Top and the cap tail portion being fixed in crown portion, the cap tail portion far from the one end in crown portion be provided with for separate Container outer wall sealing cooperation seal face, the cap body be internally provided with it is axially extending along cap body, be used to and corresponding rotation Axis outer peripheral surface seals the sealing hole of cooperation, sealing hole opening is provided on the seal face, the crown portion is far from cap tail portion One end be provided with the sealing for capableing of sealing open at one end by sealing hole far from seal face, on crown portion outer peripheral surface It is provided in the axis hole being pierced by with corresponding rotary shaft along the sealing surface of sealing cooperation.
It is provided in the crown portion and is stitched with the coplanar opening and closing of cap body axis, the opening and closing seam cuts crown portion to be formed More than two sealing lips, the sealing lip constitutes the sealing, when the sealing lip can be inserted into shaft in cap body It opens so that rotary shaft is pierced by from crown portion and is mutually closed when can be not inserted into rotary shaft in cap body with will be far from sealing hole One end of cap tail portion seals.
The cap tail portion is provided with ring cap edge far from the one end in crown portion, and the ring cap is along the side for deviating from crown portion It is provided with the seal face.
The beneficial effects of the present invention are:
Degreasing method of the invention be by sample impregnate solvent in impregnate, after the completion of immersion, be centrifuged with Separate the soak in sample with sample, after centrifugation, if reaching degreasing requirement, degreasing method is completed;If Do not reach degreasing requirement, sample can be placed again into impregnate and be impregnated in solvent, be then centrifuged, repeat more again Secondary immersion, centrifugally operated can increase substantially the efficiency that fat dissolves out in soak, the survey particularly suitable for a large amount of samples Amount.
Measure cage gu-shi chicken egg egg white and yolk in crude fat content when, egg white crude fat content is about 10.75% ± 1.04%, 10min is impregnated every time, is impregnated 10 times, is centrifuged 2min every time, and the time of operation is 2min, each sample The total time of immersion and the centrifugation of product is 140min.Yolk crude fat content is about 61.66% ± 1.02%, is impregnated every time 10min impregnates 30 times, is centrifuged 2min, 2min is operated, then being to the total time of immersion and the centrifugation of each sample 420min。
Further, since method of the invention can wrap each sample in different filter paper packets respectively, to more Kind sample is tested simultaneously, further improves the efficiency of measurement.Method of the invention being capable of 1-50 sample packet of single-time measurement.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the embodiment of crude fat content measuring device of the invention;
Fig. 2 is the structural schematic diagram of the cylinder in Fig. 1;
Fig. 3 is the structural schematic diagram of the rotating handle in Fig. 2;
Fig. 4 is the structural schematic diagram of seal cap in Fig. 1.
Specific embodiment
Embodiments of the present invention are described further with reference to the accompanying drawing.
Embodiment 1
The degreasing method of the present embodiment includes the following steps:
1) crude fat content sample to be processed is ground, then weighs 6g, example weight is denoted as m, uses fat-free filter paper Sample packet is made in packaging, and the wrapping of sample packet external application degreasing cotton thread wraps mark sample ID or label information in filter paper with pencil;
2) above-mentioned sample packet is put into baking oven, 80 DEG C of drying 90min, weighs, is accurate to 0.001g, weight is denoted as m1; Sample packet after weighing is put into cylinder;
3) cylinder is put into separate tank, separate tank is sealed, the rotary shaft of cylinder is fixed in separate tank In the support construction for impregnating position, keep cylinder axis horizontally disposed, is added into separate tank and impregnates solvent ether, make to soak The liquid level for steeping solvent is higher than the top of the sample packet in cylinder, impregnates 10min;
4) cylinder is moved upward in the support construction of separation position, so that cylinder is completely disengaged immersion solvent, passes through Fixed rotating handle rotation cylinder in cylinder rotary shaft, the centrifugally operated for being separated by solid-liquid separation the sample in cylinder, The revolving speed of cylinder is 200 revs/min, and the time of centrifugally operated is 2min;
5) the sample packet after centrifugation is taken out from cylinder with tweezers, with fresh washed with ether, band ether is evaporated completely Quan Hou carries out step 6) if filter paper is wrapped without obvious visual fatty spot;If filter paper is wrapped obvious visual Fatty spot repeats step 3) and step 4), until filter paper is wrapped without obvious visual fatty spot, carries out step 6);
6) the sample packet in cylinder is washed 2 times with fresh ether, cleaning solution pours into fermentation vat;Sample after washing Product first hang 10min in the open dish of ventilation makes the ether in sample packet volatilize, and is then placed in baking oven, at 105 DEG C Drying is no longer changed to weight, is cooled to room temperature in drier, is weighed, is denoted as m2;The movement of sample packet uses tweezer Son is clamped;
7) crude fat content in sample to be processed is calculated according to following formula:
Crude fat content (%)=(m1-m2)/m × 100%,
Wherein, m is the quality of sample to be processed, and m1 packs into quality of the sample packet before immersion, m2 with filter paper for sample For the quality of pre- degreasing samples packet, mass unit gram.
The crude fat content measuring device for implementing the above method is as shown in Figures 1 to 4, the crude fat content measuring device packet The cylinder for including separate tank and being arranged in separate tank, the cylinder include cylinder 1 and the cylinder that cylinder both ends are arranged in Body support frame 2, cylinder are reticular structure, specifically, cylinder is columnar net cylinder made of stainless steel wire braiding, width of mesh For 1cm × 1cm or 1.5cm × 1.5cm, barrel support frame includes annular support 201, support bar 202 and rotary shaft 203, Annular support 201 is stainless steel coil, and internal diameter is roughly the same with cylinder internal diameter, and two stainless steel coils are welded with cylinder both ends respectively Connection, rotary shaft and cylinder are coaxially disposed and extend along 1 axial direction of cylinder, and support bar 202 is stainless steel strip, and one end is welded in The inner wall of stainless steel coil, the other end and rotary shaft 203 are welded, and the support bar on each barrel support frame is three, each Root support bar extends along 1 radial direction of cylinder, and three support bars are uniformly distributed in cylinder circumferential direction in radioactivity.1 both ends of cylinder Rotary shaft in an axial rotary outside one end on be threaded with rotating handle 3, which includes interconnecting piece 301, diameter To portion 302, handle portion 303, interconnecting piece 301, radial part 302 and handle portion 303 are made of stainless steel tube, 301 edge of interconnecting piece Rotary shaft 203 is axially extending, and one end is threadedly coupled with rotary shaft, and the inner end of the other end and radial part is welded to connect, radial part edge Cylinder radial direction is extended, and outer end and handle portion are welded to connect, and handle portion is extended along cylinder axial direction.
Separate tank includes the pond body 5 of upper opening and the pond lid 4 for the sealing cooperation that is open with pond body, and pond body and Chi Gai are used Stainless steel is made, and pond body is rectangular parallelepiped structure, and Chi Gai is rectangle, and pond cap upper surface is fixedly installed handle 401, in order to incite somebody to action Chi Gai takes away from pond body.Cylinder supporting mechanism is fixedly installed in pond body, cylinder supporting mechanism includes impregnating support knot Structure and centrifugation support construction, impregnating support construction is to impregnate support frame, and centrifugation support construction is centrifugation support frame, impregnates support frame Including be respectively fixedly disposed on two opposite inner sidewalls of pond body first impregnate support frame and second impregnate support frame, first Support frame is impregnated to include the first immersion support ring 501 and be fixedly connected in the first immersion support ring 501 to the first immersion branch Pushing out ring 501 provides the first immersion support column 502 of upward support force, and first impregnates support ring 501 for stainless steel annulus, and first soaks Bubble support column 502 is two stainless steel strips, and stainless steel strip extends along pond body side wall inner surfaces and is welded on table in pond body side wall On face, the lower end of each stainless steel strip is weldingly fixed on pool bottom, and upper end is welded on 501 outer wall of the first immersion support ring On, two stainless steel strips impregnate 501 place vertical line of support ring about first and are symmetrical arranged, the angle between two stainless steel strips It is 60 °.Second immersion support frame is identical as the first immersion support frame structure, is symmetricly set on the opposite another side wall of pond body. The axis of first immersion support ring 501 and the second immersion support ring 503 in the same horizontal line, and is each perpendicular to pond body side wall, Guarantee that two are impregnated support ring apart from the vertical highly identical of pool bottom.It is corresponding with each immersion support ring on pond body side wall Position be coaxially arranged with internal diameter immersion through-hole 504 identical with stainless steel internal radius, which is round hole.
Being centrifuged support frame includes the first centrifugation support frame and the second centrifugation support frame, and the first centrifugation support frame and first impregnates The same side of pond body inner wall is arranged in support frame, and the same of pond body inner wall is arranged in the first immersion support frame in the second centrifugation support frame Side.First centrifugation support frame includes the first centrifugation support ring 505 and the first centrifugation support being fixedly connected in support ring Column 506, the first centrifugation support ring 505 are stainless steel annulus, and the first centrifugation support column 506 is two stainless steel strips, stainless steel strip Extend along pond body side wall inner surfaces and be welded in pond body side wall inner surfaces, the lower end of each stainless steel strip is weldingly fixed on Pool bottom, upper end are welded on 505 outer wall of the first centrifugation support ring, and two stainless steel strips are about the first centrifugation support ring 505 Place vertical line is symmetrical arranged, and the angle between two stainless steel strips is 60 °.Second centrifugation support frame and the first centrifugation support frame Structure is identical, is symmetricly set on the opposite another side wall of pond body.First centrifugation support ring 505 and the second centrifugation support ring 507 Axis in the same horizontal line, and be each perpendicular to pond body side wall, guarantee two centrifugation support rings apart from the vertical of pool bottom It is highly identical.Position corresponding with each centrifugation support ring is coaxially arranged in internal diameter and stainless steel annulus on pond body side wall The identical centrifugation through-hole 508 of diameter, the centrifugation through-hole are round hole.
First centrifugation support frame and the first immersion support frame are successively set in the lateral direction on a side wall of pond body, Second centrifugation support frame and the second immersion support frame are successively set in the lateral direction on another opposite side wall of pond body, The lower end of the Right side support column of first immersion support frame and the Left-side support column of the first centrifugation support frame welds together and welds It is fixed on pool bottom, the lower end of the Right side support column of the first centrifugation support frame is welded on the lower right corner of corresponding pond body side wall. Correspondingly, the Right side support column of the second immersion support frame and the lower end of the Left-side support column of the second centrifugation support frame weld together And it is weldingly fixed on pool bottom, the lower end of the Right side support column of the second centrifugation support frame is welded on the right side of corresponding pond body side wall Inferior horn.
It impregnates support ring and the line being centrifuged between support ring and vertical direction is in a certain angle, such as 45 °, support centrifugation Ring is in the diagonal upward direction for impregnating support ring, and the vertical height for impregnating the centre distance pool bottom of support ring is greater than cylinder Radius, vertical height of the centrifugation support ring apart from pool bottom be greater than the vertical height for impregnating support ring apart from pool bottom, Difference in height between the two is wanted after capable of guaranteeing that cylinder is moved on centrifugation support frame from immersion support frame, can make to separate Cylinder completely disengages soak in pond body, in general, height difference setting between the two be it is close with the diameter of cylinder, So when in use, cylinder can be made when impregnating on support frame, the soak of addition can be such that cylinder is fully immersed in In soak, and soak can be completely disengaged after cylinder is moved on centrifugation support frame.
The internal diameter for being centrifuged support ring is identical as the internal diameter of support ring is impregnated, and is all larger than the outer of the rotary shaft at cylinder both ends Diameter so that the rotary shaft of cylinder is inserted into being pierced by support ring and from the circular hole on pond body side wall, centrifugation support ring and It impregnates the opposite side of support ring and is provided with open slots, the width of slit and the diameter of rotary shaft are identical so that rotary shaft energy It is enough therefrom to deviate from.The inner wall of support ring is set as smooth surface, so that the rotary shaft of cylinder is rotated with support ring inner wall and matches It closes.
Length is offered between immersion support ring two circular holes corresponding with centrifugation support ring on the same side wall of pond body Hole forms rotary shaft sliding channel, is respectively provided between the immersion support ring and the corresponding annulus of centrifugation support ring of pond body two sides There is long hole, the rotary shaft of cylinder can be enable to impregnate the corresponding circular hole of support ring and centrifugation support ring along the sliding channel Guiding movement between corresponding circular hole realizes that cylinder impregnates the transfer of position and eccentric position in pond body.Rotary shaft sliding channel with One end of the corresponding circular hole connection of centrifugation support ring is slightly above the circular hole, and the rotary shaft of cylinder is enable firmly to be placed on centrifugation In the corresponding circular hole of support ring.
Sealing strip is provided in the long hole of pond body two sides, sealing strip is made of flexible material such as rubber, sealing strip Section is equilateral triangle, and the side length of triangle is greater than the width of corresponding long hole, will when cylinder does not need to move in long hole Sealing strip fills in long hole to realize sealing.
It is provided with hole shaft-assembling structure sealing element in the corresponding circular hole of the support ring of pond body two sides, is sealed in the present embodiment Part is seal cap, and seal cap is made of elastic material such as rubber, and seal cap includes occluding body and the sealing that is arranged in occluding body Valve, seal cap include cap body, and cap body 6 includes being wholely set the crown portion 601 and cap tail portion 602 to link together, cap tail portion 602 For cylinder-like structure, it is internally provided with the sealing hole 605 coaxial with cap tail portion 602, which is round hole and its internal diameter etc. In or be slightly less than cylinder rotary shaft outer diameter, keep the inner wall of sealing hole 605 and cylinder rotary shaft outer peripheral surface close Envelope cooperation, the sealing hole also constitute the mounting hole of rotary shaft, and cap tail portion 602 has been wholely set far from the one end in crown portion 601 Cap is along 604, and for cap along for circular ring shape, the side that cap edge deviates from crown portion 601 has the plane perpendicular to 602 axis of cap tail portion, should The end face of the one end of plane with cap tail portion 602 far from crown portion 601 is coplanar, and constitutes to seal with pond body outer wall and cooperate Seal face, sealing hole 605 on the end face be equipped with opening.The cap tail portion constitutes the occluding body of sealing element.
Crown portion 601 is arc cylinder, and outer diameter gradually subtracts on the direction extended from cap tail portion 602 to crown portion 601 Small, crown portion 601 is provided with two opening and closing seams 603 on one end far from cap tail portion 602, opening and closing seam 603 is with cap body axis same In one plane, crown portion 601 is divided into pintongs sealing lip far from one end of cap tail portion 602 by opening and closing seam, is not had in sealing hole 605 When having insertion rotary shaft, sealing lip can be opened sealing hole close to one end of cap tail portion 602 in Natural closure under elastic reaction Mouth sealing.After being inserted into rotary shaft in sealing hole 605, sealing lip 605 can be strutted by rotary shaft, and make rotary shaft from cap body It is pierced by.The maximum outside diameter in crown portion 601 be more than or equal to above-mentioned circular hole internal diameter, make on the outer peripheral surface in crown portion have can The sealing surface of cooperation is sealed with above-mentioned round hole inner wall, it, can be by circle after filling in the crown portion of cap body in round hole The sealing of shape hole.Above-mentioned sealing lip constitutes the elastic valve of sealing element.
Embodiment 2
The degreasing method of the present embodiment includes the following steps:
1) 10 kinds of crude fat content samples to be processed are ground respectively, then weighs 1g respectively, with fat-free filter paper point Sample packet Bao Zhuan not be made, wrapped up with degreasing cotton thread outside sample packet, wrap mark sample ID or label in filter paper with pencil Information;
2) above-mentioned sample Bao Jun being put into baking oven, 90 DEG C of drying 60min respectively weigh to each sample packet, It is accurate to 0.001g;Sample packet dispersion after weighing is put into cylinder;
3) cylinder is put into separate tank, separate tank is sealed, the rotary shaft of cylinder is fixed in separate tank In the support construction for impregnating position, keep cylinder axis horizontally disposed, is added into separate tank and impregnates solvent ether, make to soak The liquid level for steeping solvent is higher than the top of the sample packet in cylinder, impregnates 20min;
4) cylinder is moved upward in the support construction of separation position, so that cylinder is completely disengaged immersion solvent, passes through Fixed rotating handle rotation cylinder in cylinder rotary shaft, the centrifugally operated for being separated by solid-liquid separation the sample in cylinder, The revolving speed of cylinder is 200 revs/min, and the time of centrifugally operated is 2min;
5) one in the sample packet after centrifugation is taken out from cylinder with tweezers, with fresh washed with ether, band second After ether volatilization completely, if filter paper is wrapped without obvious visual fatty spot, step 6) is carried out;If filter paper has been wrapped bright Visual fatty spot is shown, step 3) and step 4) are repeated, until filter paper is wrapped without obvious visual fatty spot, is walked It is rapid 6);
6) the sample packet in cylinder is all taken out, is washed 1 time with fresh ether, cleaning solution pours into fermentation vat; Sample after washing first hangs 10min in the open dish of ventilation makes the ether in sample packet volatilize, and is then placed in baking oven, Drying is no longer changed to weight at 105 DEG C, is cooled to room temperature in drier, is weighed;The movement of sample packet uses Tweezers are clamped;
7) calculation method of the crude fat content in sample to be processed is the same as embodiment 1.
Implement the crude fat content measuring device of the above method with embodiment 1.
Embodiment 3
The degreasing method of the present embodiment includes the following steps:
1) 30 kinds of crude fat content samples to be processed are ground respectively, then weighs 4g respectively, with fat-free filter paper point Sample packet Bao Zhuan not be made, wrapped up with degreasing cotton thread outside sample packet, wrap mark sample ID or label in filter paper with pencil Information;
2) above-mentioned sample Bao Jun being put into baking oven, 85 DEG C of drying 70min respectively weigh to each sample packet, It is accurate to 0.001g;Sample packet dispersion after weighing is put into cylinder;
3) cylinder is put into separate tank, separate tank is sealed, the rotary shaft of cylinder is fixed in separate tank In the support construction for impregnating position, keep cylinder axis horizontally disposed, is added into separate tank and impregnates solvent ether, make to soak The liquid level for steeping solvent is higher than the top of the sample packet in cylinder, impregnates 15min;
4) cylinder is moved upward in the support construction of separation position, so that cylinder is completely disengaged immersion solvent, passes through Fixed rotating handle rotation cylinder in cylinder rotary shaft, the centrifugally operated for being separated by solid-liquid separation the sample in cylinder, The revolving speed of cylinder is 200 revs/min, and the time of centrifugally operated is 2min;
5) one in the sample packet after centrifugation is taken out from cylinder with tweezers, with fresh washed with ether, band second After ether volatilization completely, if filter paper is wrapped without obvious visual fatty spot, step 6) is carried out;If filter paper has been wrapped bright Visual fatty spot is shown, step 3) and step 4) are repeated, until filter paper is wrapped without obvious visual fatty spot, is walked It is rapid 6);
6) the sample packet in cylinder is all taken out, is washed 1 time with fresh ether, cleaning solution pours into fermentation vat; Sample after washing first hangs 10min in the open dish of ventilation makes the ether in sample packet volatilize, and is then placed in baking oven, Drying is no longer changed to weight at 105 DEG C, is cooled to room temperature in drier, is weighed;The movement of sample packet uses Tweezers are clamped;
7) calculation method of the crude fat content in sample to be processed is the same as embodiment 1.
Implement the crude fat content measuring device of the above method with embodiment 1.
Embodiment 4
Degreasing method and embodiment 1 the difference is that only in the present embodiment, and step 5) is no longer to the sample after centrifugation Fatty spot of testing is wrapped, but directly repeats step 3) and step 4) 5 times, it is other identical as in embodiment 1.
In other embodiments, immersion and centrifuge separation can carry out in two containers respectively.
In other embodiments, belt is fixedly connected in the rotary shaft of rotating cylinder one end of crude fat content measuring device Wheel, and be connected by belt with driving motor, drive cylinder rotation to be centrifuged by motor.
In other embodiments, position corresponding with position is impregnated is not provided with impregnating through-hole on pond body side wall, only leans on support frame It is supported.Blind hole corresponding with rotary shaft can also be set on the inner wall of pond body side wall, and rotary shaft can be fixed on blind hole In.
In other embodiments, guide rail can be the elongated slot being provided on pond body inner wall, and rotary shaft is not pierced by from pond body. In other embodiments, it is not provided with guide rail.
In other embodiments, cylinder is not rotatably assorted with immersion support construction.
In other embodiments, be not provided in separation vessel impregnate support construction and be centrifuged support construction in one or Two.In other embodiments, be not provided with impregnating support frame and be centrifuged support frame, only rely on immersion through-hole on pond body side wall and Centrifugation through-hole is supported cylinder.The wall thickness of pond body is answered sufficiently thick can support cylinder at this time.In this case, The surface that also can be set in the oblique upper for impregnating through-hole impregnating through-hole can be set in centrifugation through-hole, to reduce separate tank Volume.
In other embodiments, it is not provided with impregnating through-hole and is centrifuged through-hole, cylinder is only supported by support ring, is being needed When moving cylinder, the rotary shaft at cylinder both ends is pulled to be moved inside separate tank.
In other embodiments, it impregnates in through-hole and the long hole being centrifuged between through-hole and other kinds of sealing strip is set, such as Section is the sealing strip of rectangle, can also be not provided with sealing strip.Or impregnate and be not provided with long hole between through-hole and centrifugation through-hole, point When moving rotary shaft is perhaps centrifuged in through-hole to take out from immersion through-hole from cylinder and is inserted into centrifugation through-hole or immersion through-hole In.
In other embodiments, support bar is substituted using circular end plate in the barrel support frame of cylinder, in circular end plate Setting sample-adding sample wells.
In other embodiments, be not provided in crown portion opening and closing seam, crown portion directly by sealing hole far from cap tail portion one End sealing, rotary shaft are not required to be pierced by from cap body.
In other embodiments, crown portion is circular cylinder body.
In other embodiments, it is not provided with ring cap edge.
In other embodiments, it is not provided with seal cap in pond body, impregnates through-hole and centrifugation through-hole without sealing.Or it adopts The immersion through-hole for being not inserted into rotary shaft or centrifugation through-hole are filled in into sealing with rubber stopper, and the centrifugation for insertion rotary shaft Through-hole or immersion through-hole are sealed using band.
Experimental example
By taking the crude fat content in the egg white and yolk for measuring cage gu-shi chicken egg as an example.
1) egg white crude fat content is about 10.75% ± 1.04%, impregnates 10min every time, and impregnating 10 times (can also be more again It impregnates several times, the time of immersion and number are subject to and the crude fat in sample are substantially dissolved in soak, the standard of detection It is after centrifugation, pre- degreasing sample to be reinstated into fresh immersion solvent together with filter paper packet one and is washed, the leaching on paper bag to be filtered After bubble solvent volatilizees completely, filter paper, which is wrapped, does not leave visual grease spot, that is, can determine that the crude fat in sample has eluted and fill Point), being centrifuged 2min every time, (purpose of centrifugation is to get rid of soak as much as possible, can be reduced when ventilation is dried in air In volatilization, and the time that soak in filter paper packet volatilizees can be shortened, i.e. time for drying of shortening filter paper packet, so centrifugation Time can be longer than 2min), time of operation is 2min, then being to the total time of immersion and the centrifugation of each sample 140min。
2) yolk crude fat content is about 61.66% ± 1.02%, impregnates 10min every time, is impregnated 30 times, and 2min is centrifuged, 2min is operated, then being 420min to the total time of immersion and the centrifugation of each sample.

Claims (6)

1. a kind of degreasing method, which comprises the steps of: carry out once or more than twice sample to be processed Following degreasing operation unit: it is centrifugated using impregnating after solvent is impregnated;Up to degreasing sample;The immersion and centrifugation point From being carried out in same separation vessel;The cylinder for holding sample to be processed is provided in the separation vessel, it is described It is provided in separation vessel for being supported to cylinder and cylinder being made partly or entirely to be immersed in the immersion in soak Support construction, the centrifugation for being supported to cylinder and making cylinder completely disengage soak and be rotatably assorted with cylinder Support construction;The immersion support construction and centrifugation support construction between be provided with for make cylinder impregnate support construction and It is centrifuged the guide rail of guiding movement between support construction;After immersion, cylinder is moved upward in the support construction of separation position, is made Cylinder completely disengages immersion solvent, the centrifugally operated for being separated by solid-liquid separation the sample in cylinder.
2. degreasing method according to claim 1, which is characterized in that the time of the immersion is greater than 10min.
3. degreasing method according to claim 1, which is characterized in that the sample to be processed impregnates preceding at 80-90 DEG C Dry 60-90min.
4. degreasing method according to claim 1, which is characterized in that the sample being centrifugally separating to obtain for the last time is 105 It is dried at DEG C.
5. degreasing method according to claim 1, which is characterized in that the guide rail is to be arranged on separation vessel side wall simultaneously With the long hole (509) of cylinder guiding movement cooperation.
6. degreasing method according to claim 1, which is characterized in that the cylinder is matched with support construction rotation is impregnated It closes.
CN201610492877.6A 2016-06-23 2016-06-23 A kind of degreasing method Expired - Fee Related CN106198153B (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
GB1398459A (en) * 1972-11-14 1975-06-25 Pfeifer & Langen Method for degreasing crushed starchy fatty vegetable material
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CN102174094A (en) * 2011-01-26 2011-09-07 南昌大学 Method for extracting protein from akebia trifoliata var. varaustralis seeds by adopting water extraction process and alkali dissolution and acid precipitation process
CN203253536U (en) * 2013-04-25 2013-10-30 杨洁 Cold headed nut degreaser

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GB1398459A (en) * 1972-11-14 1975-06-25 Pfeifer & Langen Method for degreasing crushed starchy fatty vegetable material
CN2481323Y (en) * 2000-12-08 2002-03-13 天津理工学院 Chinese medicine pill-dropping defatting centrifugal
CN102174094A (en) * 2011-01-26 2011-09-07 南昌大学 Method for extracting protein from akebia trifoliata var. varaustralis seeds by adopting water extraction process and alkali dissolution and acid precipitation process
CN203253536U (en) * 2013-04-25 2013-10-30 杨洁 Cold headed nut degreaser

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