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Apparatus for monitoring fluid sample produced under low temperature and method thereof

A monitoring device and fluid preparation technology, applied in the preparation of test samples, measuring devices, and material analysis through optical means, to achieve safe and reliable adjustment of the cooling rate

Inactive Publication Date: 2009-10-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The device solves the problem of the preparation of liquid and liquid-liquid mixture high-purity samples of transparent small molecule materials, the state of liquid phase samples, the full filling volume and the phase change process in a multi-working layer low-temperature sealed vacuum environment under the action of liquid nitrogen and other refrigerants. It has the characteristics of simple structure, convenient operation, safety and reliability, and low cost; the method of preparing fluid samples at low temperature using this device is easy to operate, ensuring the preparation of single-component transparent small molecule materials below 273K and above 77K. Pure fluid samples, for those two-component samples with close physical properties, can also reliably achieve uniform mixing and preparation

Method used

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  • Apparatus for monitoring fluid sample produced under low temperature and method thereof
  • Apparatus for monitoring fluid sample produced under low temperature and method thereof
  • Apparatus for monitoring fluid sample produced under low temperature and method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] The CO high-purity liquid sample is prepared by using the monitoring device of the present invention. according to figure 1 Connect the components in the middle structure, check the conduction status of the entire device, and detect the leakage of the low-temperature pipeline. Avoid leakage and operate in a well-ventilated environment. Fill 20 liters of liquid nitrogen in the liquid nitrogen container 8, the light source 14 used is an incandescent lamp, and the first temperature sensor 21 uses a copper-constantan thermocouple. The specific operation steps are:

[0045] 1. Open flushing valve 24, use 2kg / cm 2 The sample chamber 5 is purged with CO sample gas to ensure that the residual gas sample does not affect the purity of the sample preparation;

[0046] 2. Utilize the first temperature sensor 21 to control the heater 11 to heat the liquid nitrogen in the liquid nitrogen container 8, so that the liquid nitrogen in the liquid nitrogen container is not greater than ...

Embodiment 2

[0051] Use the monitoring device of the present invention to prepare CO+N 2 High-purity mixed liquid samples. The experimental equipment and experimental environment used are the same as those in the first embodiment, but the process is slightly different. The second temperature sensor 26 also uses a copper-constantan thermocouple.

[0052] Wherein step 1-3 is identical with embodiment one, guarantees to mix sample CO+N in liquefaction 2 In order to ensure the safe operation of the system and the accuracy of cooling control during the process, perform the following operations:

[0053] a. First use 1.4×10 5 N of Pa 2 Fill the cryogenic sample chamber 5, when the liquefied N 2 When the indication value of the second temperature sensor 26 placed on the radius height of the front panel of the optical fiber sensor changes suddenly, it indicates that the sample liquid nitrogen has filled 1 / 2 of the sample chamber volume, and at this time, the CO gas sample tank 12 is replaced w...

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Abstract

The invention relates to a monitoring device and a method for preparing fluid samples at low temperature. The device mainly includes a low-temperature refrigeration unit composed of a low-temperature sample preparation target, a liquid nitrogen container, a bellows and a rubber tube; a low-temperature control unit composed of a flushing valve, a safety valve, a controller, a heater and a computer monitoring system; a fiber optic sensor , a temperature sensor, a photomultiplier tube and a computer monitoring system constitute a non-contact phase monitoring device for a low temperature monitoring unit. The device is used to solve the method of preparing high-purity samples of transparent small molecule materials above 77K in a low-temperature sealed vacuum environment. The invention not only can directly operate and monitor the state and phase change process of the fluid sample to be prepared, but also has the characteristics of simple structure, convenient operation, safety and reliability, low cost, uniform and reliable effect of repeated sample copying, etc.; it is used in aerospace, petrochemical and light industries Daily chemical and other fields have a wide range of practical value.

Description

1. Technical field [0001] The invention relates to a monitoring device and method for preparing fluid samples at a low temperature, in particular to a method for performing liquid and liquid-liquid mixture transparent small molecule materials with high purity under the action of liquid nitrogen and other refrigerants in a multi-layer low-temperature sealed vacuum environment. A non-contact monitoring device and method for phase of sample preparation. 2. Background technology [0002] As we all know, when the temperature and pressure of the environment are changed appropriately, the basic particles—molecules, atoms, and electrons—that make up the substance will not only become inert, but also undergo overall or partial reorganization of their structure, that is, phase transition. Using this phenomenon, the research scope of materials can be extended to extreme conditions such as high temperature and high pressure, low temperature and low pressure, and low temperature and high...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/42G01N21/84
Inventor 孙悦陈先猛刘福生
Owner SICHUAN UNIV
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