CN202757899U - Molar mass measurement device utilizing freezing point depression method - Google Patents
Molar mass measurement device utilizing freezing point depression method Download PDFInfo
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- CN202757899U CN202757899U CN 201220172901 CN201220172901U CN202757899U CN 202757899 U CN202757899 U CN 202757899U CN 201220172901 CN201220172901 CN 201220172901 CN 201220172901 U CN201220172901 U CN 201220172901U CN 202757899 U CN202757899 U CN 202757899U
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- cryogenic liquid
- temperature
- freezing point
- interlayer
- measurement device
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Abstract
A molar mass measurement device utilizing a freezing point depression method comprises a stirring rod and a sample tube. The sample tube is a test tube with double layers of jackets, a cryogenic liquid inlet and a cryogenic liquid outlet are reserved on an interlayer, the cryogenic liquid inlet and the cryogenic liquid outlet are connected with an inlet and an outlet of a cryogenic liquid container, and the stirring rod is mechanically controlled to automatically vertically stir at a constant speed. The molar mass measurement device utilizing the freezing point depression method has the improvement that a circulating unit utilizing bath lotion in the cryogenic liquid container to refrigerate is additionally arranged, and an external refrigerating device with temperature controllable is utilized to feed circulating cryogenic liquid to the interlayer of the sample tube so as to realize temperature adjustment in an ice groove. Temperature of the circulating cryogenic liquid can be set according to needs, the limit that an original molar mass measurement device can only measure sample freezing point higher than zero DEG C is avoided, and temperature range of the sample freezing point is widened.
Description
Technical field
The utility model relates to a kind of kryoscopy instrument, especially cryoscopic method molal weight measurement mechanism.
Background technology
Why cryoscopic method can produce supercooling phenomenon if being measured molal weight, supercooling phenomenon is owing to being dissolved in solvent in the solution after temperature drops to solidifying point, do not have crystal to separate out and reach the phenomenon of hypersaturated state, reason generally is because cleaner in lower the temperature too fast or the solution, do not have the impurity nucleus, prevented from coldly at first will slowing down cooling rate, and then agitation as appropriate or add crystal seed, only needed slowly cooling just, had crystal and separate out; The solidifying point that is lower than in the cooling curve in the textbook partly represents to have occured supercooling phenomenon, be that solvent is chilled to below the solidifying point still without solid separation, this be since the saturated vapour pressure of the tiny crystal grains that goes out of beginning crystallization greater than the saturated vapour pressure of synthermal lower common crystal, so often produce supercooling phenomenon, be that the temperature of liquid will be reduced to below the solidifying point and just can separate out solid, temperature goes back up to solidifying point more subsequently.
Existing cryoscopic method molal weight measurement mechanism comprises digital Beckman thermometer (or temperature-difference instrument); Common thermometer; Stirring rod, ice groove (1000ml); Measure pipe, outer tube; Also comprise in addition transfer pipet (25cm
3); 1 of analytical balance; 1 in magnifier; 1 of sheeter.The reagent that adopts is analytically pure benzene and naphthalene (or pure water and sucrose or other sample that need study); Trash ice.Schematic diagram is Fig. 1.
Experimental procedure is: experimental provision is installed, and pack in the ice groove 1/3rd ice and 1/3rd water make ice groove (bath) temperature be lower than 2-3 ℃ at fluid to be measured solidifying point by salt adding.In mensuration, pack into benzene approximately 20g(be accurate to ± 0.02g).Or move into 25.00cm with transfer pipet
3Benzene is again according to its quality of density calculation of benzene under the temperature at that time.Notice that ice-water liquid level will be higher than the benzene liquid level of measuring in the pipe.Digital Beckman thermometer sensor dried insert to measure pipe, check little stirring rod, enable free movement and not with the temperature sensor friction.
Measure first the approximate solidifying point of neat solvent benzene.To measure pipe and directly immerse in the ice-water bath, manually rapid stirring.When fluid temperature decline almost pauses, take out and measure pipe, put into outer tube and continue stirring, write down finally stabilised temperature value, namely be approximate solidifying point.Measure once and can needn't repeat.
Take out and measure pipe, constantly stir, with its low-grade fever, crystallization is melted with hand fully.To measure and put into immediately outer tube after pipe soaks in frozen water, rapid stirring, the at this moment drop in temperature of liquid benzene.Stop 0.2 ℃ the time stirring more than temperature is down to solidifying point, the temperature of liquid benzene continues to descend.Cross when being as cold as following 0.05 ℃ of solidifying point and stir rapidly, temperature descends first and rises rapidly subsequently, when treating that temperature stabilization is constant, shows the numeral from digital Beckman thermometer and to read temperature value, is the solidifying point of benzene.Replication, until obtain three deviations and be no more than ± 0.005 ℃ test data.
With the about naphthalene sheet of 0.3g of analytical balance weighing, put into and measure pipe and stir, the naphthalene sheet is all dissolved.The same method is measured the approximate solidifying point of solution, again Accurate Determining solidifying point.Mistake is cold in the mensuration process must not be above 0.2 ℃.
After being finished, benzene liquid must pour returnable bottle into.
As measure the solidifying point of other sample, assay method is similar.
The main deficiency of existing apparatus is: one, the temperature in the ice bath otherwise the open close salt adding of crossing are regulated, and temperature is difficult to all even constant, and experimentation is pretty troublesome, thereby disperses basic experiment mechanism process.If the sample solidifying point of measuring is low many than 0 degree, then the method for this adjusting ice bath temperature is with infeasible.Two, the artificial speed that stirs is non-constant, and stirring rate is difficult to control.Three: for above-mentioned reasons, cause supercooling phenomenon and drop in temperature rate variation indefinite, make experimental data uncontrollable in crossing cold 0.2 ℃, cause not preparing of sample freezing point temperature measurement.
Summary of the invention
The utility model purpose is, a kind of cryoscopic method molal weight measurement mechanism is proposed, overcome that existing apparatus need to ice that body lotion in the groove carries out constantly artificial adjustment and the artificial deficiency such as unstable of bringing stir speed (S.S.) that stirs of the inhomogeneous and original device of the operation inconvenience that brings and temperature, more can concentrate on the analyzing and processing of experimentation and the accuracy of DATA REASONING.
The technical solution of the utility model is: a kind of cryoscopic method molal weight measurement mechanism comprises stirring rod, sample hose; It is characterized in that described sample hose is the test tube with double-jacket, interlayer is provided with the turnover port of cryogenic liquid; Interlayer is imported and exported output and the input port that connects a cooling liquid container; Stirring rod is by the automatic uniform speed vertical stirring mode of machinery control.Improvement of the present utility model is: other is provided with the Cycle Unit that the cooling liquid container body lotion freezes, and by the controlled external refrigerating plant of temperature, sends into the cold liquid of circulation to reach the adjustment in the ice groove to the sample hose interlayer.
The utility model industry, be provided with the stirring rod of vertical stirring in the sample hose, driven by mechanical hook-up, at the uniform velocity steady.
The beneficial effects of the utility model are: constant outer loop and at the uniform velocity stir the analyzing and processing equipment more can concentrate on experimentation, external low-temperature circulating liquid temp is adjustable, the circulation fluid temperature can be set as required, avoided original device can only measure the limitation that the sample solidifying point is higher than 0 degree, opened up and expand institute's test sample product freezing point temperature scope.
Description of drawings
Fig. 1 is structural representation of the present utility model.
Embodiment
Cryoscopic method molal weight measurement mechanism comprises that stirring rod 8(machinery control automatic vertical stirs), sample hose 2, air blanketing 5, interlayer import and export 1,4, liquid coolant 3, digital display Beckman thermometer sensor 6, gland bonnet 7.Wherein interlayer is imported and exported 1,4 connection (external) Cryo Equipments, and Cryo Equipment is supplied with liquid coolant, and interlayer is imported and exported output and the input port that connects a liquid coolant; The interior temperature that can keep sample hose 2.Stirring rod is by the automatic uniform speed vertical stirring mode of machinery control, and the automatic uniform speed vertical stirring of this machinery control can be adopted useful existing structure, by driven by motor.
Can be provided with in addition the Cycle Unit that the cooling liquid container body lotion freezes, by the controlled external refrigerating plant of temperature, send into the cold liquid of circulation to reach the adjustment in the ice groove to the sample hose interlayer.
Claims (1)
1. a cryoscopic method molal weight measurement mechanism comprises stirring rod, sample hose; It is characterized in that described sample hose is the test tube with double-jacket, interlayer is provided with the turnover port of cryogenic liquid; Interlayer is imported and exported output and the input port that connects a cooling liquid container; This measurement mechanism is provided with the Cycle Unit that the cooling liquid container body lotion freezes in addition, by the controlled external refrigerating plant of temperature, sends into the cold liquid of circulation to reach the adjustment in the ice groove to the sample hose interlayer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220172901 CN202757899U (en) | 2012-04-23 | 2012-04-23 | Molar mass measurement device utilizing freezing point depression method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220172901 CN202757899U (en) | 2012-04-23 | 2012-04-23 | Molar mass measurement device utilizing freezing point depression method |
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| Publication Number | Publication Date |
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| CN202757899U true CN202757899U (en) | 2013-02-27 |
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| CN 201220172901 Expired - Lifetime CN202757899U (en) | 2012-04-23 | 2012-04-23 | Molar mass measurement device utilizing freezing point depression method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2554621C2 (en) * | 2013-08-06 | 2015-06-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Кемеровский технологический институт пищевой промышленности" | Method of determination of freezing beginning temperature at freezing of water solutions and moisture containing products and materials and device for its implementation |
-
2012
- 2012-04-23 CN CN 201220172901 patent/CN202757899U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2554621C2 (en) * | 2013-08-06 | 2015-06-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Кемеровский технологический институт пищевой промышленности" | Method of determination of freezing beginning temperature at freezing of water solutions and moisture containing products and materials and device for its implementation |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130227 |
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| CX01 | Expiry of patent term |