CN106198153B - A kind of degreasing method - Google Patents
A kind of degreasing method Download PDFInfo
- 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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- degreasing
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- 238000005238 degreasing Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 31
- 238000005119 centrifugation Methods 0.000 claims description 68
- 238000007654 immersion Methods 0.000 claims description 56
- 238000010276 construction Methods 0.000 claims description 27
- 238000000926 separation method Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 99
- 238000007789 sealing Methods 0.000 description 48
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 36
- 235000019784 crude fat Nutrition 0.000 description 26
- 229910001220 stainless steel Inorganic materials 0.000 description 21
- 239000010935 stainless steel Substances 0.000 description 20
- 230000000007 visual effect Effects 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 235000019197 fats Nutrition 0.000 description 8
- 239000000284 extract Substances 0.000 description 6
- 238000002386 leaching Methods 0.000 description 6
- 238000009423 ventilation Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 210000000969 egg white Anatomy 0.000 description 4
- 210000002969 egg yolk Anatomy 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 3
- 102000002322 Egg Proteins Human genes 0.000 description 3
- 108010000912 Egg Proteins Proteins 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 235000014103 egg white Nutrition 0.000 description 3
- 235000013861 fat-free Nutrition 0.000 description 3
- 238000000855 fermentation Methods 0.000 description 3
- 230000004151 fermentation Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000013013 elastic material Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229930182558 Sterol Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 210000000991 chicken egg Anatomy 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; 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)
- Immunology (AREA)
- Pathology (AREA)
- Centrifugal Separators (AREA)
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
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.
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Citations (4)
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 |
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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2016
- 2016-06-23 CN CN201610492877.6A patent/CN106198153B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Non-Patent Citations (2)
Title |
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