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Coagulating point determinator and its determination method

A freezing point and measuring instrument technology, applied in the field of thermal analysis, can solve the problems of poor repeatability of the measurement method and large data error, and achieve the effects of accurate freezing point measurement, improving accuracy and expanding the scope of use.

Inactive Publication Date: 2010-11-17
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the repeatability of the measurement method using this instrument is poor, and the error of the tested data is relatively large.

Method used

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  • Coagulating point determinator and its determination method
  • Coagulating point determinator and its determination method
  • Coagulating point determinator and its determination method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] exist figure 1 Among them, the freezing point measuring instrument of this embodiment consists of a lower heating resistance wire 1, an upper heating resistance wire 2, a heating sleeve 3, an inner tube 4, an inner tube wall temperature sensor 5, a sample temperature sensor 6, an inner tube upper cover 7, an air Sleeve 8, cold trap upper cover 9, cold bath temperature sensor 10, semiconductor refrigerator 11, cold trap 12, magnetic stirrer 13, computer 14, electromagnetic switch 15 are connected to form.

[0034]The lower end of the cold trap 12 is fixedly installed with a magnetic stirrer 13 with a threaded fastening connector, and the magnetic stirrer 13 is connected with the electromagnetic switch 15 by a wire. The coolant in the cold trap 12 is stirred, and the outer wall of the cold trap 12 is bonded with a semiconductor refrigerator 11, and the semiconductor refrigerator 11 is connected with the electromagnetic switch 15 by a wire, and the semiconductor refrigerat...

Embodiment 2

[0051] The freezing point of the naphthalene solution was measured using the freezing point measuring instrument of Example 1, and the molecular weight of naphthalene was calculated.

[0052] In the measurement preparation process step 1 of embodiment 1, get solvent cyclohexane 24.0698g and join in the inner pipe 4, the cyclohexane liquid level is positioned at lower heating resistance wire 1 upper end ± 5mm, water is cooling liquid, and the consumption of water is 1.6L. In step 2 of the rough measurement of the freezing point of cyclohexane, the semiconductor refrigerator 11 controls the temperature of the cooling bath to be -3.5°C, which is 10°C lower than the theoretical freezing point of cyclohexane, and the lowest point of the temperature-time curve for the cooling of cyclohexane It is 6.42°C, and 6.46°C is determined to be the start-up temperature of heat dissipation compensation, which is 0.04°C higher than the temperature at the lowest point of the curve. The roughly ...

Embodiment 3

[0057] The freezing point of the naphthalene solution was measured using the freezing point measuring instrument of Example 1, and the molecular weight of naphthalene was calculated.

[0058] In the freezing point process step 4 of the mensuration naphthalene-cyclohexane solution of embodiment 2, naphthalene 0.7469g in the naphthalene-cyclohexane solution, the molar fraction of naphthalene in the naphthalene-cyclohexane solution is 0.02, other in this process step Step is identical with embodiment 2. Other steps are identical with embodiment 2. The freezing point of cyclohexane and the freezing point of naphthalene-cyclohexane solution are shown in Table 3.

[0059] Table 3 Example 3 cyclohexane freezing point and naphthalene-cyclohexane solution freezing point measured value

[0060]

[0061] In calculating the molecular weight process step 5 of naphthalene, the molecular weight calculated by formula (2) and formula (3) is 131.04, and the relative error with the theoreti...

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Abstract

The invention relates to a freezing point detector. A magnetic stirrer is arranged outside the lower end of a cold trap; the outer wall of the cold trap is provided with a semiconductor freezer; the magnetic stirrer and the semiconductor freezer are connected with an electromagnetic switch by wires; the upper end of the cold trap is provided with a cold trap cover; the cold trap cover is providedwith a cold bath temperature sensor; a heating tube with an inner tube is arranged in an air casing of the cold trap; the upper end of the inner tube is provided with an inner tube cover of a sample temperature sensor; the outside of the heating casing is connected with an upper heating resistance wire and a lower heating resistance wire by a wire and the electromagnetic switch; the electromagnetic switch is connected with a computer by a cable; the inner wall of the inner tube is provided with an inner tube wall temperature sensor; the inner tube wall temperature sensor, the sample temperature sensor and the cold bath temperature sensor are connected with the computer by cables. The method of determining the freezing point comprises preparing determination steps, roughly measuring the freezing point of a solvent, determining the freezing point of the solvent, measuring the freezing point of the tested sample solution, and other steps. The molecular weight of the tested item can be calculated according to the determined freezing point.

Description

technical field [0001] The invention belongs to the technical field of thermal analysis, and in particular relates to the determination of liquid freezing point and the determination of molecular weight of non-volatile solute by freezing point depression method. Background technique [0002] The freezing point is an important physical and chemical parameter of a substance, and it is of great significance to determine the freezing point of a substance. The molecular weight or molar mass of the solute can also be calculated by using the measured values ​​of the freezing point of the solvent and the solution. [0003] The freezing point depression method to determine the molecular weight of a substance is one of the classic methods for determining the molecular weight of a substance. It is based on the colligative property of dilute solutions, that is, for a solution formed by a solute that is non-volatile, non-dissociated, non-polymerizable, and does not form a solid solution...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N25/04
Inventor 白云山李世荣郭建中安洁
Owner SHAANXI NORMAL UNIV
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