CN110132793A - A kind of polymer molecular weight test device and test method - Google Patents
A kind of polymer molecular weight test device and test method Download PDFInfo
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- CN110132793A CN110132793A CN201910315499.8A CN201910315499A CN110132793A CN 110132793 A CN110132793 A CN 110132793A CN 201910315499 A CN201910315499 A CN 201910315499A CN 110132793 A CN110132793 A CN 110132793A
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- necked flask
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- ubbelohde viscometer
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
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Abstract
The present invention discloses a kind of polymer molecular weight test device and test method, it is made of dissolution mechanism and mechanism for testing two parts.Dissolving mechanism includes heat collecting type constant-temperature heating magnetic stirring apparatus, iron stand, test tube clamp, three-necked flask, air inlet pipe, escape pipe, rubber tube, nitrogen cylinder, thermometer, and three mouths of three-necked flask tap into tracheae, escape pipe and thermometer respectively.Testing structure includes intelligent constant-temperature slot, iron stand, test tube clamp, Ubbelohde viscometer, air-bubble level, rubber tube, Ubbelohde viscometer is vertically fixed in intelligent constant-temperature slot by test tube clamp, and more Ubbelohde viscometer height are consistent, the accurate time for measuring solution and flowing through Ubbelohde viscometer measurement ball or more graduation mark, the intrinsic viscosity for acquiring solute goes out the viscosity-average molecular weight of solute according to mark's-Huo Wenke equation calculation.
Description
Technical field
The present invention relates to measuring instrument technical field more particularly to a kind of polymer molecular weight test device and test sides
Method.
Background technique
High molecular polymer refers to relative molecular mass in 10-106Above macromolecular substances, high molecular weight assign poly-
The many excellent performances of object are closed, therefore the test of polymer molecular weight is just particularly important.
There are many kinds for the method for molecular weight test, such as terminal group titration, membrane osmotic pressure method, light scattering method, supercentrifugal process,
Exclusion chromatography etc., these methods or cumbersome or surveying range is limited or measuring device is expensive, it is many-sided because
Element makes these methods not to be used widely in the detection of industrial products again.And viscosimetry is because its is easy to operate, test week
Phase is short, accuracy feature with higher and by favor, but the device price of accurate viscosimetry test molecule amount is same
Sample is sufficiently expensive, and testing cost is high, it is desirable to be widely applied in the detection of industrial products still relatively difficult.
Summary of the invention
The object of the present invention is to provide a kind of polymer molecular weight for the particular/special requirement of industrial products measurement molecular weight
Test device and test method realize the quick, accurate, inexpensive of industrial products molecular weight test process.
The object of the present invention is achieved like this, a kind of polymer molecular weight test device, including heat collecting type heated at constant temperature
Magnetic stirring apparatus, iron stand, test tube clamp, three-necked flask, air inlet pipe, escape pipe, rubber tube, nitrogen cylinder, thermometer, intelligent constant-temperature
Slot, Ubbelohde viscometer, air-bubble level；It is characterized in that heat collecting type constant-temperature heating magnetic stirring apparatus, iron stand, test tube clamp, three
Mouth flask, air inlet pipe, escape pipe, rubber tube, nitrogen cylinder, thermometer have collectively constituted dissolution mechanism, in heat collecting type heated at constant temperature
It is put into three-necked flask in magnetic stirring apparatus, is equipped with iron stand in heat collecting type constant-temperature heating magnetic stirring apparatus side, three-necked flask
Neck is clamped by test tube clamp and is fixed on iron stand, and air inlet pipe one end is connected by rubber tube with nitrogen cylinder, and the other end is stretched
Enter the liquid level of solution in three-necked flask hereinafter, escape pipe one end is connected with air, the other end is placed in the solution liquid in three-necked flask
More than face, thermometer is inserted into three-necked flask in solution, can accurately measure the real time temperature of solution in three-necked flask, nitrogen pass through into
Tracheae is passed into three-necked flask bottom, and the air being discharged in three-necked flask simultaneously promotes solute to dissolve and disperse；Intelligent constant-temperature slot, iron
Pallet, test tube clamp, Ubbelohde viscometer, air-bubble level, rubber tube have collectively constituted mechanism for testing, and Ubbelohde viscometer is placed in intelligence
It is clamped and is fixed on iron stand with test tube clamp in thermostat, the c ball of Ubbelohde viscometer will be placed in oil bath liquid in intelligent constant-temperature slot
Face is hereinafter, air-bubble level covers on the B pipe of Ubbelohde viscometer, for determining whether B pipe is disposed vertically.
The above-mentioned ubbelohde viscosity count number being placed in intelligent constant-temperature slot is 2-4, and placing height should be consistent, for sentencing
Whether disconnected solute is completely dissolved and evenly dispersed.
The Ubbelohde viscometer can be collocated with sand core funnel filter device, for joined the insoluble solute of inorganic filler
The measurement of composite material.
The capillary caliber of provisioned Ubbelohde viscometer be it is variable, adapt to the test request of different polymer.
The air-bubble level is bushing type, can dismantle and replace, and facilitates the cleaning of Ubbelohde viscometer.
It is passed through nitrogen inert gas in above-mentioned course of dissolution, for excluding air, prevents sample from aoxidizing, while rising and dividing
Dissipate effect.
The test method of a kind of polymer molecular weight test device of the present invention, which is characterized in that steps are as follows:
1) pure solvent is transferred in Ubbelohde viscometer with pipette, is measured under test temperature the same terms with solute to be measured
Delivery time of the pure solvent in Ubbelohde viscometer；
2) solvent of the solute and corresponding volume of the appropriate quality of precise, the antioxidant for being equipped with corrresponding quality are added three mouthfuls together
In flask；
3) three-necked flask is placed on constant temperature in water-bath or oil bath pan to dissolve, by air inlet pipe one end insertion liquid level of solution hereinafter, another
End is connected by rubber tube with nitrogen cylinder, and nitrogen valve is rotated, and the one end for being inserted into air inlet pipe under liquid level of solution has bubble uniform
It emerges；
4) it after solute is completely dissolved, is transferred the solution into the pipette of heat preservation glutinous with the Ubbelohde of pure solvent rinse and drying
In degree meter, constant temperature appropriate time is stabilized to test temperature to solution temperature, with the delivery time of stopwatch test solution, repeatedly surveys
Measuring time error should be within 0.02.s；
5) intrinsic viscosity is gone out according to one point method empirical equation or calculation by extrapolation, further according to mark's-Huo Wenke equation calculation solute
Viscosity-average molecular weight.
The beneficial effects of the present invention are: polymer to be measured can be effectively prevent to degrade in atmosphere of inert gases, held
Continuous bubble facilitates the dispersion of solute, and more viscosmeters measure the accuracy that can verify that result, the air-bubble of bushing type simultaneously
Level is detachable and replaces, also convenient to clean to viscosmeter.Package unit structure is simple, easy to operate, and measurement result is quasi-
Really stablize, the test of different molecular weight polymers may be implemented.
Detailed description of the invention
Fig. 1 is the schematic diagram of this polymer molecular weight test device dissolution mechanism；
Fig. 2 is the schematic diagram of this polymer molecular weight test device test structure；
Fig. 3 is the schematic diagram of Ubbelohde viscometer in this polymer molecular weight test device test structure.
Specific embodiment
With reference to the accompanying drawing and pass through specific embodiment to further illustrate the technical scheme of the present invention:
As shown in the picture, the present invention is a kind of polymer molecular weight test device, including heat collecting type constant-temperature heating magnetic stirring apparatus
1, iron stand 2, test tube clamp 3, three-necked flask 4, air inlet pipe 5, escape pipe 6, rubber tube 7, nitrogen cylinder 8, thermometer 9, intelligent constant-temperature
Slot 10, Ubbelohde viscometer 11, air-bubble level 12.The heat collecting type constant-temperature heating magnetic stirring apparatus 1, iron stand 2, test tube clamp
3, three-necked flask 4, air inlet pipe 5, escape pipe 6, rubber tube 7, nitrogen cylinder 8, thermometer 9 have collectively constituted dissolution mechanism, in thermal-arrest
It is put into three-necked flask 4 in formula constant-temperature heating magnetic stirring apparatus 1, is equipped with brandreth in 1 side of heat collecting type constant-temperature heating magnetic stirring apparatus
Platform 2, the neck of three-necked flask 4 are clamped and are fixed on iron stand 2 by test tube clamp 3,5 one end of air inlet pipe by rubber tube 7 with
Nitrogen cylinder 8 is connected, and liquid level of solution that the other end protrudes into three-necked flask 4 is hereinafter, 6 one end of escape pipe is connected with air, the other end
It is placed in the liquid level of solution in three-necked flask 4 or more, thermometer 9 is inserted into three-necked flask in solution, can accurately measure three mouthfuls of burnings
The real time temperature of solution in bottle.Nitrogen is passed into 4 bottom of three-necked flask through air inlet pipe 5, and the air in three-necked flask 4 and rush is discharged
It dissolves and disperses into solute.To solution in three-necked flask without precipitating or gel, with the pipette of heat preservation by solution fast transfer extremely
In the A ball of the A pipe of Ubbelohde viscometer 11, constant temperature to test temperature.Intelligent constant-temperature slot 10, iron stand 2, test tube clamp 3, ubbelohde viscosity
Meter 11, air-bubble level 12, rubber tube 7 have collectively constituted mechanism for testing, and Ubbelohde viscometer 11 is placed in intelligent constant-temperature slot 10 simultaneously
It is clamped and is fixed on iron stand 2 with test tube clamp 3, the C ball of Ubbelohde viscometer 11 will be placed in oil bath liquid level in intelligent constant-temperature slot 10
Hereinafter, air-bubble level covers on the B pipe of Ubbelohde viscometer 11, it is ensured that B pipe is disposed vertically, by the C seal of tube, with ear washing bulb by C
Solution is drawn to C ball in ball, then C pipe is connected to air, so that solution is slowly flowed to D ball once, rinse starts timing afterwards three times.
Test method using a kind of polymer molecular weight test device of the invention, which is characterized in that steps are as follows:
1) pure solvent is transferred in Ubbelohde viscometer with pipette, is measured under test temperature identical with solute to be measured pure molten
Delivery time of the agent in Ubbelohde viscometer；
2) solvent of the solute and corresponding volume of the appropriate quality of precise, the antioxidant for being equipped with corrresponding quality are added three mouthfuls together
In flask；
3) three-necked flask is placed on constant temperature in water-bath or oil bath pan to dissolve, by air inlet pipe one end insertion liquid level of solution hereinafter, another
End is connected by rubber tube with nitrogen cylinder, and nitrogen valve is rotated, and the one end for being inserted into air inlet pipe under liquid level of solution has bubble uniform
It emerges；
4) after solute is completely dissolved, this solution is transferred to the Ubbelohde with pure solvent rinse and drying with the pipette of heat preservation
In viscosmeter, constant temperature appropriate time is stabilized to test temperature to solution temperature, the delivery time of solution is tested with stopwatch, repeatedly
Time of measuring error should be within 0.02.s；
5) intrinsic viscosity is gone out according to one point method empirical equation or calculation by extrapolation, further according to mark's-Huo Wenke equation calculation solute
Viscosity-average molecular weight.
Claims (7)
1. a kind of polymer molecular weight test device, including heat collecting type constant-temperature heating magnetic stirring apparatus, iron stand, test tube clamp, three
Mouth flask, air inlet pipe, escape pipe, rubber tube, nitrogen cylinder, thermometer, intelligent constant-temperature slot, Ubbelohde viscometer, air-bubble level；Its
Be characterized in that heat collecting type constant-temperature heating magnetic stirring apparatus, iron stand, test tube clamp, three-necked flask, air inlet pipe, escape pipe, rubber tube,
Nitrogen cylinder, thermometer have collectively constituted dissolution mechanism, are put into three-necked flask in heat collecting type constant-temperature heating magnetic stirring apparatus, are collecting
Hot type constant-temperature heating magnetic stirring apparatus side is equipped with iron stand, and the neck of three-necked flask is clamped by test tube clamp and is fixed on brandreth
On platform, air inlet pipe one end is connected by rubber tube with nitrogen cylinder, and the other end protrudes into the liquid level of solution in three-necked flask hereinafter, outlet
Pipe one end is connected with air, and the other end is placed in the liquid level of solution in three-necked flask or more, and thermometer is inserted into solution in three-necked flask
In, the real time temperature of solution in three-necked flask can be accurately measured, nitrogen is passed into three-necked flask bottom through air inlet pipe, is discharged three mouthfuls
Air in flask simultaneously promotes solute to dissolve and dispersion；Intelligent constant-temperature slot, iron stand, test tube clamp, Ubbelohde viscometer, bubble level
Instrument, rubber tube have collectively constituted mechanism for testing, and Ubbelohde viscometer, which is placed in, to be clamped with test tube clamp in intelligent constant-temperature slot and be fixed on iron
On pallet, the c ball of Ubbelohde viscometer will be placed in intelligent constant-temperature slot oil bath liquid level hereinafter, air-bubble level is covered in Ubbelohde viscometer
B pipe on, for determine B pipe whether be disposed vertically.
2. a kind of polymer molecular weight test device according to claim 1, it is characterised in that be placed in intelligent constant-temperature slot
Ubbelohde viscosity count number be 2-4, placing height should be consistent, for judging whether solute is completely dissolved and uniformly divides
It dissipates.
3. a kind of polymer molecular weight test device according to claim 1 or 2, it is characterised in that the ubbelohde viscosity
Meter can be collocated with sand core funnel filter device, the measurement of the composite material for joined the insoluble solute of inorganic filler.
4. a kind of polymer molecular weight test device according to claim 1 to 3, it is characterised in that provisioned crow
The capillary caliber of family name's viscosmeter be it is variable, adapt to the test request of different polymer.
5. a kind of polymer molecular weight test device according to claim 1 to 4, it is characterised in that the bubble
Level meter is bushing type, can dismantle and replace, and facilitates the cleaning of Ubbelohde viscometer.
6. -5 any a kind of polymer molecular weight test device according to claim 1, it is characterised in that in course of dissolution
It is passed through nitrogen inert gas, for excluding air, prevents sample from aoxidizing, while playing peptizaiton.
7. a kind of test method using a kind of any polymer molecular weight test device of claim 1-6, feature
It is, steps are as follows:
1) pure solvent is transferred in Ubbelohde viscometer with pipette, is measured under test temperature the same terms with solute to be measured
Delivery time of the pure solvent in Ubbelohde viscometer；
2) solvent of the solute and corresponding volume of the appropriate quality of precise, the antioxidant for being equipped with corrresponding quality are added three mouthfuls together
In flask；
3) three-necked flask is placed on constant temperature in water-bath or oil bath pan to dissolve, by air inlet pipe one end insertion liquid level of solution hereinafter, another
End is connected by rubber tube with nitrogen cylinder, and nitrogen valve is rotated, and the one end for being inserted into air inlet pipe under liquid level of solution has bubble uniform
It emerges；
4) it after solute is completely dissolved, is transferred the solution into the pipette of heat preservation glutinous with the Ubbelohde of pure solvent rinse and drying
In degree meter, constant temperature appropriate time is stabilized to test temperature to solution temperature, with the delivery time of stopwatch test solution, repeatedly surveys
Measuring time error should be within 0.02.s；
5) intrinsic viscosity is gone out according to one point method empirical equation or calculation by extrapolation, further according to mark's-Huo Wenke equation calculation solute
Viscosity-average molecular weight.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910315499.8A CN110132793A (en) | 2019-04-19 | 2019-04-19 | A kind of polymer molecular weight test device and test method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910315499.8A CN110132793A (en) | 2019-04-19 | 2019-04-19 | A kind of polymer molecular weight test device and test method |
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| CN110132793A true CN110132793A (en) | 2019-08-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910315499.8A Pending CN110132793A (en) | 2019-04-19 | 2019-04-19 | A kind of polymer molecular weight test device and test method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413254A (en) * | 2020-04-21 | 2020-07-14 | 回音必集团安徽制药有限公司 | Method for testing thick paste viscosity |
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|---|---|---|---|---|
| US3837217A (en) * | 1972-10-19 | 1974-09-24 | Exxon Research Engineering Co | Measurement of polymer molecular weight distribution |
| US4258564A (en) * | 1979-03-28 | 1981-03-31 | Polysar Limited | Polymer characterization apparatus |
| CN102353618A (en) * | 2011-06-22 | 2012-02-15 | 上海化工研究院 | Method for qualitatively testing molecular weight distribution of ultrahigh molecular weight polyethylene (UHMWPE) |
| CN102455274A (en) * | 2010-10-18 | 2012-05-16 | 袁俊海 | Method for measuring intrinsic viscosity of polymer |
| CN204735217U (en) * | 2015-05-29 | 2015-11-04 | 南京科技职业学院 | Preparation cyclodextrin polymer experimental apparatus |
-
2019
- 2019-04-19 CN CN201910315499.8A patent/CN110132793A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3837217A (en) * | 1972-10-19 | 1974-09-24 | Exxon Research Engineering Co | Measurement of polymer molecular weight distribution |
| US4258564A (en) * | 1979-03-28 | 1981-03-31 | Polysar Limited | Polymer characterization apparatus |
| CN102455274A (en) * | 2010-10-18 | 2012-05-16 | 袁俊海 | Method for measuring intrinsic viscosity of polymer |
| CN102353618A (en) * | 2011-06-22 | 2012-02-15 | 上海化工研究院 | Method for qualitatively testing molecular weight distribution of ultrahigh molecular weight polyethylene (UHMWPE) |
| CN204735217U (en) * | 2015-05-29 | 2015-11-04 | 南京科技职业学院 | Preparation cyclodextrin polymer experimental apparatus |
Non-Patent Citations (1)
| Title |
|---|
| 周天楠 等: "《聚合物材料结构表征与分析实验教程》", 31 May 2016, 四川大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413254A (en) * | 2020-04-21 | 2020-07-14 | 回音必集团安徽制药有限公司 | Method for testing thick paste viscosity |
| CN111413254B (en) * | 2020-04-21 | 2023-03-21 | 回音必集团安徽制药有限公司 | Method for testing thick paste viscosity |
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Application publication date: 20190816 |