CN209302221U - A kind of food and medicine analysis distilling apparatus - Google Patents

Abstract

A kind of food and medicine analysis distilling apparatus of the utility model, including jacketed flask and the curved ball of water conservancy diversion and condenser pipe, jacketed flask bottle body forms collet chamber, reaction chamber two chambers, the curved ball both ends have the interior outer grinding port for being mutually adapted sealing with jacketed flask and condenser pipe respectively, jacketed flask is that frosted is flat, admittance conduction oil oil bath in collet, the curved separating bulbs body portion of water conservancy diversion and upper and lower two horizontal conduits, apex is opened up lower horizontal conduit and is tilted down in terms of horizontal plane under the spherical part of the curved ball of water conservancy diversion, apex is opened up horizontal conduit and is tilted down in terms of horizontal plane on the spherical part of the curved ball of water conservancy diversion, in-line condenser pipe, distillate or reactant condensation to volatilization；Utility model device component Configuration is reasonable, and component organic unity is coordinated, overall coordination effect, the effective bumping for reducing food inspection environment cucurbit, vibration, prevent detection error, fraction water conservancy diversion is reasonable, device detection procedure safety, the data obtained are more reliable, are widely used.

Description

A kind of food and medicine analysis distilling apparatus

Technical field

The utility model belongs to food and medicine and examines detection and analysis instrument apparatus field, has related particularly to a kind of food Drug detects distilling apparatus.

Background technique

In the production in the fields such as food, drug, health care product and animal feed, the intermediate control of production and finished product Quality control or intermediate links are the key that one rings of relationship control of product quality, and testing and analyzing during control of product quality is Key means.In scientific research institutions, schoolman's experimental teaching or researcher's experimental study, coherent detection teaching, test Detection work is essential, and detection device reliability and data reliability are interrelated.The detection and analysis of any product quality, are removed It is also closely bound up with the rational structure of detection device or design outside the detection level for relying on testing staff.

Instantly most food drugs and health care products can add and declare to be rich in the being rich in nutrition medical efficacy of protein in the market.Albumen Matter is widely present in the food and medicine health care product or feed, additive after natural or processing.Protein content analysis is not It is only limitted to food service industry, a large amount of health care products or medicine field also there are many applications.Constant Kjeldahl method nitrogen (N) assay and In the distillation process of gross protein value measurement, kjeldahl determination distilling apparatus is commonly used.The measurement of sulphite in foods is each The required detection project of food light industry enterprise, the 2003 second method way of distillation of GB/T5009.34-are reacted using full glass distiller Distillation, is adapted to detect for sulfur dioxide residual quantity, is widely used by each factory and testing agency.The purposes of distilling apparatus includes egg For example zein detection, plumule or the detection of plumule cake protein, rich albumen drugs and health care products contain Protein Detection for white matter detection, also wrap Include volatilization distillation, the distillation of volatile solvent, the high-temperature chemical reaction of solution's solute and the distillation etc. of fermentation alcohol, it is seen that steam Distillation unit is the critical equipment of such detection or experimental provision.

But visible kjeldahl determination device, full glass distiller or other distilling apparatus are in application process currently on the market In, it is widely present before flask contents reaction ends that frequently acutely to seethe bumping because dispersing the factors such as irregular uneven heating existing As the flask of, bumping acutely beat or because acutely beat cause flask Fragmentation Phenomena, reaction content bumping to boil out caused by personnel The phenomenon that injury and corrosion surrounding expensive equipment, reaction volatile matter water conservancy diversion flow direction arrangement are unreasonable.

Existing equipment setting is unreasonable, boiling explosion phenomenon occurs and gently then causes measurement error extreme influence accuracy, heavy then make Distillation can not carry out and the failure measured or even vibration glass breaking initiation soda acid is caused to overflow to corrode to stab and personnel equipments is waited to pacify Full accident.Such situation, which such as eats user the various aspects related personnel such as medicine doctor detection, universities, middle and primary schools, biggish operation Security risk.In this case testing staff often can only remove earlier reaction flask before reaction thoroughly and terminate to distill, this Testing result deviation will be caused, the accuracy and credibility of detection is significantly impacted, also reduces detection efficiency, and then cause not The timely Instructing manufacture of energy, easily causes the reworked processing of many products；The flask heating equipment of another aspect kjeldahl determination device The high-temperature services such as electric furnace or alcolhol burner are mostly used, such equipment is in addition to laboratory peripheral facilities equipment cause of easily igniting is caught fire, also The shortcomings that temperature can not be adjusted accurately, the extensive control of temperature be also in flask reaction content bumping and bumping it is uncontrollable because One of element.Such heating equipment such as electric furnace, alcolhol burner etc. is instantaneous heating equipment simultaneously, is mentioned in the case where product is powered or lights state Apply heat for uninterrupted high temperature, and in unexpected power-off or sharp temperature drop when extinguishing, will lead in reaction flask temperature sharply The phenomenon that decline forms negative pressure and then the very fast suck-back of receiving liquid in receiving bottle is entered reaction flask before personnel make fast reaction, This is also detection failure and the uncontrollable factor for causing personal injury.

To sum up, bumping, flask bounce are acutely seethed in the unadjustable and flask contents of the heating temperature of existing apparatus Or Fragmentation Phenomena, device do not cooperate with unreliable then testing result to have deviation or detection failure and easily cause personal injury, are Such distilling apparatus urgent problem to be solved, and lack the effective solution of problems currently on the market.

Summary of the invention

The utility model provides a kind of food and medicine analysis distilling apparatus aiming at drawbacks described above.The utility model Rationally, component organic unity is coordinated for device assembly configuration, and overall coordination effect effectively reduces food inspection environment cucurbit Bumping, vibration prevent detection error, and fraction water conservancy diversion is reasonable, and device detection procedure safety, the data obtained are more reliable, using wide It is general, food Medicines and Health Product industry production circulation unit is greatly improved and school, scientific research institutions school index of correlation detects accurate water It is flat.

Technical solutions of the utility model are, including jacketed flask and the curved ball of water conservancy diversion and in-line condenser pipe, jacketed flask bottle body Collet chamber, reaction chamber two chambers are formed, the curved ball both ends, which have, is mutually adapted sealing with jacketed flask and condenser pipe respectively Interior outer grinding port, jacketed flask be frosted it is flat, admittance hot oil oil bath in collet, the curved separating bulbs body portion of water conservancy diversion with upper and lower two Horizontal conduit, apex is opened up lower horizontal conduit and is tilted down in terms of horizontal plane under the spherical part of the curved ball of water conservancy diversion, the ball of the curved ball of water conservancy diversion Apex is opened up horizontal conduit and is tilted down in terms of horizontal plane on body portion, distillate or reactant of the in-line condenser pipe to volatilization Condensation；Temperature controllable recycles oil-bath, and institute's admittance hot oil connection jacketed flask collet chamber is imported and exported to form closed cycle；Magnetic agitation Equipment, lower magnetic blender are stirred the magneton being placed in jacketed flask reaction chamber in the form of controllable magnetic and form agitation work With；And iron stand, connection hose, the fixation of receiving flask, connection, received combination.

Spatially there are bottleneck and bottle abdomen two parts down in the flat oil bath jacketed flask of frosted.Bottleneck port is interior frosted. The outer layer of bottle abdominal section is full clad type collet, and 200 ~ 1000ml of internal volume is to provide the inner cavity of thermal response in bottle abdomen, in bottle abdomen Bottom of chamber wall and collet bottom are flat circle, and bottle abdomen bottom wall of inner cavity is that 0.5cm ~ 1.5cm(forms collet away from collet distance from bottom For fluid thermal cycle), round collet bottom exterior layer makees frosted processing.

Opening is set on the downside of jackets outer wall as conduction oil oil inlet end, and it is fuel-displaced as conduction oil that opening is set on the upside of the jackets outer wall of opposite side End.Collet recycles oil bath pan, interior logical high temperature circulation conduction oil with the external temperature controllable of hose.Temperature controllable circulation oil bath pan of illustrating is optional With such as high-temperature circulator GX-2005.The heating range of temperature controllable circulation oil bath pan should be able to be controlled at 30 DEG C ~ 500 DEG C, and temperature controls Precision is ± 0.5 DEG C.

Connection hose materials are high temperature resistant silicon sebific duct.

Jacketed flask making material is conventional high temperature glass and/or high temperature resistant Pyrex.

Making material does not repel frivolous stainless steel etc. and is easy to cast material, is preferably advisable with pyroceram.

A magneton is placed in oil bath jacketed flask bottle abdomen, and the flat oil bath jacketed flask of frosted is placed on magnetic stirring apparatus On, place mat is less than or equal to 0.2mm bed course between magnetic stirring apparatus and the flat oil bath jacketed flask of frosted.The bed course is high temperature resistant material Material, is advisable with asbestos gauge.

Magneton internal layer is permanent magnet, straight or star, and outer layer coats heat resistant and wear resistant resistant material polytetrafluoroethylene (PTFE) entirely.

The range of speeds that magnetic stirring apparatus is adjustable is 0rpm/min ~ 800rpm/min, and it is ± 10rpm/ that revolving speed, which controls precision, min。

Apex conduit is tilted down 5 degree ~ 30 degree in terms of horizontal plane and opens downcomer under the spherical part of the curved ball of water conservancy diversion.

Apex conduit is tilted down 5 degree ~ 30 degree in terms of horizontal plane and opens downcomer on the spherical part of the curved ball of water conservancy diversion.

Upper conduit and the curved ball opposite side of downcomer point column water conservancy diversion.

Upper conduit and downcomer are calculated as 8cm ~ 15cm with chamfer length.

Upper conduit and downcomer are bent vertically sets up downwards bending longitudinal tubule (L tubule) separately, and the open end of two bending longitudinal tubule (L tubule)s is in the same water It is horizontal on planar end surface.Two bending the frosteds of longitudinal tubule (L tubule) port outer wall, and with the flat oil bath jacketed flask of frosted for being connected with interior ground or Condenser pipe forms size fit and seals piping connection.

In-line condenser pipe upper end tube nozzle is interior frosted, and lower port is that straight tube will submerge in receiving bottle in absorbing liquid.It is in-line cold Solidifying outer tube layer coats collet, connects coolant liquid with conventional hoses, selects using 1 DEG C ~ 15 DEG C tap water of temperature as coolant liquid.Array condensation Pipe is gripped with iron stand.Condenser pipe does not repel dish-type condenser pipe but recommends in-line condenser pipe.

All frosted interface sections specification of the present apparatus is strictly unified, interior outer grinding port rigid adaptation, and ground range 20 ~ 38mm。

Preferably, wherein the flat oil bath jacketed flask bottleneck port of frosted is interior ground 29/32(mm) [refer to lower edge/upper limb Diameter, other are same], in-line condenser pipe upper end tube nozzle is interior ground 29/32(mm), vertex bending longitudinal tubule (L tubule) and lower top on the curved ball of water conservancy diversion The port outer wall of point bending longitudinal tubule (L tubule) is ground 29/32(mm).Using when the present apparatus by each frosted mouth effectively connect sealing or it is auxiliary It is sealed with vaseline, vacuum silicon grease.

The invention has the benefit that the flat oil bath jacketed flask volume of frosted is big, bottle abdomen is coated entirely using collet, with can Temperature adjustment recycles the heating of oil bath pan accurate temperature controlling, with high precision magnetic stirring apparatus offer stirring, and installing is flexibly.

Without using open fire, it can be ensured that the abundant high efficiency dispersion of reaction content is mixed, is heated evenly, and detection process is not quick-fried Boiling, detect it is safer, greatly avoid flask contents acutely seethe bumping be forced too early reaction was completed, flask bounce Or Fragmentation Phenomena, favorable sealing property, then testing result is more acurrate reliable and stable, is more conducive to timely Instructing manufacture and stablizes production Quality.

And traditional zeolite or bead are replaced using magneton, eliminate the jump shake of traditional zeolite or bead in boiling The dynamic vibration limits to bottle body act on, but use the shockproof source disturbance of the Stirring mode of the concentric rotation of magnetic force magneton, bottle Body applied vibration source during the reaction potential leads to that flask is beated or broken factor is thoroughly eliminated or by magneton The agitation rotation of horizontal plane ensure that while content is fully dispersed to mix well and then such as distills, reacts more for device Add and reliable and stable provides guarantee.

And collet oil bath heating is used, since the heat storage capacity of conduction oil is especially strong, under the full cladding of collet, can keep away Exempt from the heating equipments such as electric furnace, alcolhol burner because of power-off suddenly or caused by extinguishing reaction flask because losing temperature form negative pressure for absorbing liquid suck-back Phenomenon has reserved more reaction time to testing staff, so that detection process is safely controllable reliably, avoids personal injury.

The spherical part of the curved ball of water conservancy diversion is conducive to buffering distillation impact air pressure.Spherical part is on upper vertex and lower vertex Diversion pipe and lower diversion pipe, two diversion pipe angled downward from horizontal certain angles are directly opened up, is more advantageous under the effect of gravity It is uninterrupted automatic clear to the positions such as the curved ball part of water conservancy diversion and diversion pipe, bending vertical tube with the spontaneous condensed water in distillation process Wash, analyte distillate sufficiently, tube wall residual also washed shunting recycling-reactant wall built-up stream and washed back reaction chamber by abundant stream automatically The reaction was continued, distillate wall built-up stream is washed till receiving bottle, so that reactant reaction is more abundant, distillate reception is more thorough, more favorably In the accuracy for improving testing result.

The frosted interface section specification of the present apparatus is strictly unified, assembly flexibly, sealing performance it is reliable, detection process is without letting out Dew is conducive to the accuracy for improving detection data, is suitable for the experiment links such as distillation, heating reaction, is particularly suited for albumen quality inspection It surveys.

Present apparatus making material in addition to iron stand, temperature controllable recirculated water bath, magnetic stirring apparatus is glass material, wherein Jacketed flask making material is conventional high temperature glass or high temperature resistant Pyrex, while can be made with frivolous stainless steel material. It is more advantageous to and improves equipment safety coefficient, be conducive to be recycled for a long time, be conducive to manufacture and popularize.

A kind of food and medicine analysis distilling apparatus of the utility model, adds that heating temperature is adjustable, flask contents are seethed Be uniformly dispersed mild, very big solution flask bounce and Fragmentation Phenomena, as a kind of anti-bumping distilling apparatus solution of food and medicine analysis Certainly existing practical problem is insufficient, and it is finer efficient to be suitable for detection.

Invention components configuration is more reasonable, and convenient for manufacture, each component organic unity is coordinated, and reactant volatile matter is flow conductivity Good, good airproof performance has overall coordination effect, and the effective bumping for reducing food inspection environment cucurbit, vibration prevent detection Error, device detection procedure safety, the data obtained are more reliable, can be widely applied to the industries albumen quality inspection such as food and medicine health care product All multioperation detection projects such as survey or distillation procedure are conducive to improve index of correlation detection precisely level.

Detailed description of the invention:

Fig. 1 show the basic structure schematic diagram of the utility model

Fig. 2, which is shown, existing determines nitrogen distilling apparatus structural schematic diagram

In figure, the flat oil bath jacketed flask of 1. frosteds；2. the curved ball of water conservancy diversion；3. temperature controllable recycles oil-bath；4. magnetic agitation Equipment；5. in-line condenser pipe；6. iron stand；7. connecting hose；8. receiving bottle.

Specific embodiment

Implementation example only to illustrate the invention below, including experiment scene or reagent sample and method choice etc., not Constitute the further limitation implemented to the present utility model.With the combination of the present apparatus and/or part combination for outside embodiment its His class chemical analysis detection scene is also the application to the present apparatus, but the production of the known present apparatus is answered to implement to fall into the utility model Protection scope.The utility model is illustrated with embodiment, but the utility model is not limited thereto.

Embodiment 1: device assembles seal tightness test

The related metering unified temperature condition of liquid is to place to measure at 20 DEG C of room temperature, between each component within unified ground standard Outer grinding port connection, the flat oil bath jacketed flask liquid storage of frosted, after being heated volatilization direction along the curved ball of water conservancy diversion and its two sides conduit, into Enter condenser pipe to receive into receiving flask.

A kind of food and medicine analysis distilling apparatus of the utility model, including jacketed flask (1) and the curved ball of water conservancy diversion (2) and straight Column condenser pipe (5), jacketed flask (1) bottle body form collet chamber, reaction chamber two chambers, and curved ball (2) both ends have difference The interior outer grinding port of sealing is mutually adapted with jacketed flask and condenser pipe, jacketed flask is that frosted is flat, admittance hot oil oil in collet It bathes, the curved ball of water conservancy diversion (2) bulb separation body portion and upper and lower two horizontal conduits, apex opens up down under the spherical part of the curved ball of water conservancy diversion (2) Horizontal conduit is tilted down in terms of horizontal plane, and it is downward in terms of horizontal plane to open up horizontal conduit for apex on the spherical part of the curved ball of water conservancy diversion Inclination, in-line condenser pipe (5) condense the distillate or reactant of volatilization；Temperature controllable recycles oil-bath (3), and institute's admittance hot oil connects Jacketed flask (1) collet chamber is connect to import and export to form closed cycle；Magnetic stirring equipment (4), lower magnetic blender is with controllable magnetic The magneton that the agitation of power form is placed in jacketed flask reaction chamber forms agitaion；And iron stand (6), connection hose (7), connect By the fixation of bottle (8), connection, received combination.

The jacketed flask is more specifically the flat oil bath jacketed flask (1) of frosted.

The device that is produced with pyroceram by Fig. 1 configuration is simultaneously linked in sequence according to figure, the specially flat oil bath of frosted Ground lower edge/upper limb diameter 29/32(mm in jacketed flask (1) bottle abdomen internal volume 500ml, bottleneck), it is built-in straightforward to cover polytetrafluoro Ethylene material rotor, bottle abdomen bottom wall of inner cavity are that 0.5cm ~ 1.5cm forms jacket space for admittance hot oil, folder away from collet distance from bottom Covering two hose of two-port (7) connection temperature controllable circulation oil-bath (3) is type selecting circulator GX-2005, the sphere of the curved ball of water conservancy diversion (2) Apex conduit is tilted down 7 degree in terms of horizontal plane and convinces pipe, water conservancy diversion curved ball longitudinal tubule (L tubule) part ground 29/32(mm by patient analysis above and below part) in Ground type, in-line condenser pipe (5) select adaptation 29/32(mm) it is interior ground type, fixed with iron stand (6), condenser pipe lower end is submerged Receiving bottle (8).Magnetic stirring equipment (4) revolving speed is set as 120rpm/min, and control precision is ± 2rpm/min.It is applied at all grounds Vaseline sealing.

200ml pure water is injected in the flat oil bath jacketed flask of frosted, adds bead 3, connection collet in-out end hose, Iron stand opens the peripheral devices such as high-temperature circulator, adjusts 130 DEG C of thermally conductive oil temperature, adjusts 6 DEG C of cooling water, receiving bottle prepares It receives.Pure water is heated in jacketed flask, by the diversion elbow of ground adaptation connection, on the liquid edge of bent tube section condensation 7 degree of oblique reflux fall into flask and continue by thermal response, and the volatile matter of steam state continues to push to condenser pipe and receiving flask direction, push The liquid further condensed in the process is eluted along 7 degree of oblique condenser pipe directions connected to adaptation ground.By the heating of 28min It volatilizees and receives, add up to receive condensate liquid 150ml, remaining non-volatile liquid meter volume 49.6ml in measuring flask, total to consume after cooling When the time it is short, device favorable sealing property is without friction or bumping, leakproofness and recyclability are good.

Embodiment 2: distillation apparatus nitrogen recovery checkout facility

Nitrogen recovery experiment is carried out according to by GB/T 5511-2008.Chemicals takes 0.05mol/L ammonium sulfate first Cucurbit is added in [(NH4) 2SO4] standard solution 10mL, adds 100mL distilled water, is cooled to room temperature.Measuring 50ml concentration is 10 drop bromocresol green-methyl red indicators are added into the receiving bottle of receiving end in the boric acid solution of 40g/L.By present apparatus array The end of condenser pipe is submerged completely in the boric acid absorbing liquid, and cooling water is opened.After present apparatus hose and each interface are connected in After slowly pouring into 40% analysis pure cerium hydroxide sodium water solution 50mL in the flat oil bath jacketed flask bottle abdomen of frosted, opens temperature controllable and follow Ring water-bath set temperature is 150 DEG C, is distilled.

Bumping and other phenomenons do not occur for observation distillation process whole process, and condensed water divides automatically in spherical elbow in distillation process Stream and tube wall cleaning are good.

Liquid product to be received is 100mL, and condensation pipe end lift-off liquid level is steamed 1 minute again, then stops distillation.It will be whole It distills receiving liquid and removes mixing progress titration operation.With sulfuric acid standard titration solution c(H2SO4)=0.05mol/L titrated, Observing color using visual colorimetry becomes pale red as terminal from blue-green, and measuring consumption sulfuric acid titrand is 20.00mL.It is 0.01mL that sample, which is similarly not added, and measures blank titration volume.Measuring sample nitrogen content according to calculating is 21.2015% (the 3rd, 4 decimal 15 is Infinite Cyclic decimal).It is that Infinite Cyclic is small according to ammonium sulfate theory nitrogen content 21.21%(decimal 21 Number) it calculates, the nitrogen recovery of this ammonium sulfate is 99.95%, higher than the requirement that the national standard rate of recovery need to be more than or equal to 99.80%.

Having done 10 groups of nitrogen recoveries simultaneously checks parallel test without boiling explosion phenomenon；Separately there are 10 groups of instruments to power off simultaneously It tests within 10 minutes, since distillate or absorbing liquid suck-back phenomenon does not occur by force in the heat storage capacity of conduction oil.

Embodiment 3: sulphur dioxide measuring is carried out using this device

Carrying out sulphur dioxide measuring concrete application using this device, steps are as follows:

1, it accurately weighs 0.2 ~ 0.3 gram of corn mixed feed (being accurate to 0.0001) to be placed in jacketed flask, 250mL is added Water, 3 ~ 5 drop defoaming agents.

2, distilling apparatus is connected, collet connects oil bath, and condenser pipe lower end is dipped in the 50mL lead acetate (20g/L) in iodine flask In, 10mL(1+1 is then added into jacketed flask) hydrochloric acid, it loses no time to cover tightly buffering ball, starts to distill.

3, distill: setting oil bath temperature is 105 DEG C, opens condensed water, when distillate about 200mL thing will condense in iodine flask Pipe lift-off liquid level, redistillation 1 minute, then distilled water flushing condenser pipe lower end, shifted sulfur dioxide completely.In detection sample While be not added sample blank experiment.

Bumping and other phenomenons do not occur for observation distillation process whole process, the sulfur dioxide smell evolution situation not being pungent, Favorable sealing property, in distillation process in spherical elbow condensed water automatic shunt cleaned automatically with tube wall it is all right.

4, titrate: sequentially adding 10mL concentrated hydrochloric acid into iodine flask, 1mL starch indicator solution (10g/L) shake up after with iodine mark It is blue that quasi- titration solution (0.010mol/L) is titrated to change, and it is non-discolouring in 30s until.

5, calculate: the content of sulfur dioxide is calculated by following formula in feed:

X=

In formula:

X --- the sulfur dioxide total content in feed, unit are grams per kilogram (g/kg)；

A --- the volume of iodine titrand (0.010mol/L) used in titration sample, unit are milliliter (mL)；

B --- the volume of iodine titrand (0.010mol/L) used in titer reagent blank, unit are milliliter (mL)；

M --- Feed Sample quality, unit are gram (g)；

0.032 --- the quality of 1mL iodine standard solution [c (1/2) I2=1.0mol/L] comparable sulfur dioxide, unit are Gram (g).

Through detecting, in 5 parallel Feed Samples content of sulfur dioxide detection be respectively 0.075%, 0.077%, 0.076%, 0.074&, 0.076%(w/w), it is good with present apparatus this method detection acquired results data reappearance.

Measurement with this device for content of sulfur dioxide in feed, the advantage is that flask has collet, can accurately control The temperature for making distillation, prevents distillate bumping, and sulfur dioxide is utmostly distilled out, the sulfur dioxide smell ease not being pungent Artificial situation, favorable sealing property solve the problems, such as that acetic acid lead solution absorbs not in time, so that measurement result is more accurate.

Reaction is mild in experimentation simultaneously, bumping does not occur and causes the problem of distilling bottle breakage, safety coefficient is effective It improves, reduces laboratory equipment loss, detection efficiency greatly promotes.

Embodiment 4: protein content detection is carried out using this device

The protein content detection that corn sample is done in distillation is carried out using the present apparatus, method uses GB5511-2008 cereal Kjeldahl method is calculated with beans nitrogen analysis and gross protein value, reagent and operating procedure press national regulations progress.

1.0529g grinding uniformly rear corn sample, 10g potassium sulfate, 0.3g cupric sulfate pentahydrate, 0.30g dioxy are weighed respectively Change titanium, 20ml sulfuric acid, is digested 2.5 hours for 420 DEG C in digesting.It is transferred in present apparatus jacketed flask bottle abdomen, 50ml is added Water, 50ml boric acid, 10 drop indicator, after this distilling apparatus is sealed in connection, are added 5ml excessive sodium hydrate.

Temperature controllable circulation oil bath pan is opened into collet for 120 DEG C of heat setting temperature, opens magnetic agitation.Absorption bottle absorbs After liquid fully absorbs, with the titration of 0.05mol/L sulfuric acid solution.

The protein content of the sample is calculated according to national standard formula, and does 5 Duplicate Samples.It is calculated through detection, 5 parallel samples Protein content result is 8.59%, 8.587%, 8.591%, 8.592%, 8.595%, and detection average value is 8.591%.

In distillation process, since collet is for conduction oil uniform temperature constant homogeneous, and opens magnetic agitation and mix well It ensure that the full and uniform reaction needs of reaction solution in jacketed flask bottle abdomen, diversion elbow have played the effect of washing of automatic stream respectively, Wall built-up substance sufficiently shunts, and reacts more thorough.

There is not boiling explosion phenomenon in reaction whole process, and reaction solution stirs evenly no bottle body vibration, slips out object and returns stream automatic automatically It cleans in receiving bottle, detection the data obtained is closer, and testing result is reliable.

Embodiment 5: protein powder detects example

Take commercially available mark that there is the protein powder 1000g(soybean protein isolate micro mist of alimentary health-care function) dress barrel sample 500g, making product nameplate declare every 100g containing protein not less than 80g.

Sampling 0.5000g is detected three times after mixing well with congenic method in example 4, and detection dry protein content is respectively 80.24%,80.26%,80.25%.Period equipment operation is flexible, and device accumulation of heat is good, no boiling explosion phenomenon, reaction distillation and collection Without loss.It is substantially accurate to identify, and equipment is accurate for detecting protein content, efficiently.

Claims (8)

1. a kind of food and medicine analysis distilling apparatus, which is characterized in that including jacketed flask and the curved ball of water conservancy diversion and in-line condenser pipe, Jacketed flask bottle body forms collet chamber, reaction chamber two chambers, and the curved ball both ends have respectively with jacketed flask and condenser pipe It is mutually adapted the interior outer grinding port of sealing, jacketed flask is that frosted is flat, admittance conduction oil oil bath in collet, the curved separating bulbs body of water conservancy diversion Part and upper and lower two horizontal conduits, apex is opened up lower horizontal conduit and is dipped down in terms of horizontal plane under the spherical part of the curved ball of water conservancy diversion Tiltedly, apex is opened up horizontal conduit and is tilted down in terms of horizontal plane on the spherical part of the curved ball of water conservancy diversion, and in-line condenser pipe is to volatilization Distillate or reactant condensation；Temperature controllable recycles oil-bath, and institute's admittance hot oil connection jacketed flask collet chamber is imported and exported to be formed Closed cycle；Magnetic stirring equipment, lower magnetic blender are stirred in the form of controllable magnetic and are placed in jacketed flask reaction chamber Magneton formed agitaion；And iron stand, connection hose, the fixation of receiving flask, connection, received combination.

2. a kind of food and medicine analysis distilling apparatus according to claim 1, which is characterized in that jacketed flask is flat for frosted Base oil bathes jacketed flask, 200 ~ 1000ml of internal volume in the bottle abdomen in the flat oil bath jacketed flask of frosted, bottle abdomen bottom wall of inner cavity away from Collet distance from bottom is 0.5cm ~ 1.5cm.

3. a kind of food and medicine analysis distilling apparatus according to claim 1, which is characterized in that jacketed flask making material For conventional high temperature glass and/or high temperature resistant Pyrex and/or frivolous stainless steel material.

4. a kind of food and medicine analysis distilling apparatus according to claim 1, which is characterized in that the spherical part of the curved ball of water conservancy diversion Apex conduit is tilted down 5 degree ~ 30 degree in terms of horizontal plane and opens downcomer under point.

5. a kind of food and medicine analysis distilling apparatus according to claim 1, which is characterized in that the spherical part of the curved ball of water conservancy diversion Divide upper apex conduit to tilt down 5 degree ~ 30 degree in terms of horizontal plane and opens downcomer.

6. a kind of food and medicine analysis distilling apparatus according to claim 1, which is characterized in that all frosteds of device connect Oral area divider lattice are strictly unified, interior outer grinding port rigid adaptation, 20 ~ 38mm of ground range.

7. a kind of food and medicine analysis distilling apparatus according to claim 1, which is characterized in that magnetic stirring apparatus can be turned Fast range is 0rpm/min ~ 800rpm/min, and it is ± 10rpm/min that revolving speed, which controls precision,.

8. a kind of food and medicine analysis distilling apparatus described according to claim 1 or 2 or 3 or 4 or 5, which is characterized in that frosted Internal volume 500ml in bottle abdomen in flat oil bath jacketed flask, bottle abdomen bottom wall of inner cavity are 1.0cm, collet away from collet distance from bottom Flask material high temperature resistant Pyrex, apex conduit is dipped down in terms of horizontal plane under the spherical part of the curved curved ball of ball water conservancy diversion of water conservancy diversion Oblique 7 degree are opened downcomer, and apex conduit is tilted down 7 degree in terms of horizontal plane and opens downcomer on the spherical part of the curved ball of water conservancy diversion.