Application of analytical instrument quartz spring thermobalance in thermal analysis Dong Zhongbing, Hu Zhen. Cao Yu. Deng Huiping. Wang Yang State Key Laboratory of Coal Conversion, Shanxi Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan, Shanxi, 31 Ming, in addition to the performance of the current commercial thermal balance, the device also has a unique reaction atmosphere, wide operation, simple working temperature, high corrosion resistance. Excellent performance such as strong sex, 1刖S thermogravimetry is a technique for measuring the relationship between mass and temperature under program-controlled temperature changes. The main feature of the thermogravimetric method is the quantitative and accurate measurement of the mass change of the substance and the rate of change. It is a routine analysis method necessary for the research, metallurgy paint, ink science, ceramics, food technology, inorganic chemistry, organic chemistry, biochemistry and geochemistry. It can be said that as long as the weight changes when the substance is heated, the change process can be studied by the thermogravimetric method. At present, the thermogravimetric method has been applied to the thermal analysis of inorganic organic substances and polymers; the metal is subjected to various bodies at high temperatures. Corrosion process; calcination and smelting of minerals; pyrolysis gasification process of coal; determination of volatile matter content of moisture content; research on reaction kinetics; research on reaction mechanism and many other physical and chemical processes.
The thermogravimetric method is a device that continuously weighs the sample while heating or cooling the sample on a thermobalance device, and its development process is only a few decades. China's existing thermal balance is mainly composed of temperature-controlled weighing records and atmosphere. It is said that the balance of the balance, the rule, the crucible, and the support of the sky sling supported by the sky sling, the balance of the balance of the spiral spring balance. The lever balance is a balance that uses the principle of equal arm balance. Due to its strict material requirements, it is expensive and difficult to process, limiting its application. The balance supported by the wire is a lever balance that uses a wire-supporting beam and is combined with an electromagnetic reset device. The disadvantage is that the wire is fragile, easy to break, and the weighing range is small. The balance supported by the sling is a lever balance supported by a sling as a middle knives. The disadvantage is that the width of the sling and the installation height of the sling seriously affect the sensitivity of the day. Spiral bombs operate under the atmosphere of yellow-etched species.
The quartz spring type thermal balance inherits all the characteristics of the existing hot flat, and can be used in all atmospheres except for the hydrogen fluoride gas, so it can work at higher temperatures, corrosion resistance and precision can be improved, 2 quartz Spring thermal balance structure and operating procedures 2.1 Structural features Quartz spring type thermobalance is mainly composed of quartz spring quartz reaction tube weighing system. The temperature control system gas is machined from the system, and the spring is accurately corrected by the broken code before use. The working principle is that the spring hangs the iron core of the differential transformer and the sample disk, and the heating furnace is linearly stretched when the sample is re-visited and the sample is changed. The differential transformer is caused to generate an electrical displacement signal proportional to the displacement, and the output signal is then subjected to transformation acquisition 5 to display the weight change relationship with time on the computer. The temperature was detected with a thermocouple close to the sample and recorded on a computer at the same time. The reaction process can achieve program temperature rise or rapid temperature rise, and the working temperature can reach about 1300. Since the device is made of quartz, it can be applied to low vacuum and various reaction atmospheres, except for gases. With a structure such as a cabinet 2.
The device can be adjusted according to different general rules; and the telescopic expansion of the 4-inch spring is adjusted to prevent the reaction gas from the top of the gas and the core of the corrosion displacement sensor. The top of the balance is protected by helium, and the outside of the core is closed by a quartz sleeve. In order to prevent the heat radiation of the heating sensor to the displacement sensor, in addition to keeping it away from the heating furnace as much as possible, the balance of the balance arm is also used to use the gold storm silk spring as the weighing method.
After being stabilized, the computer acquisition system and the heating furnace are started, the reaction starts, the reaction temperature of the sample is reacted and the reaction temperature is simultaneously collected by the computer, and the product gas can be taken online and sampled with the gas analyzer. Until the weight change amount is small enough to be considered as the end of the reaction, the reverse procedure is carried out as described above, and finally, the 1 after the reaction is taken out. Into the weighing and 1 liter of chemical points 1 则 1 1 3 quartz thermal balance measured the oxidation process in the atmosphere, the reaction gas mountain trial sulfur; implementation of the online weight change 妃 by the material heavy initial material 1 said More than that. It can be seen that at the beginning of the reaction process, the process of rapid weight reduction before 20 s. The weight then gradually increases until there is no weight change. Through material balance and reaction gas analysis, to record the conversion and reaction mechanism of calcium sulfide in the reaction process, the device can not only test the weight change of single reaction condition 1 . It is also possible to carry out a continuous reaction under different conditions. The 祀 祀 4 is a continuous oxidation reaction process of calcium sulphate under the atmosphere of 90,0 vulcanization. 4 Clear the results of material weight changes during the continuous vulcanization and oxidation process.
2 Operation procedure First, the quartz reaction tube is opened by the interface, and the quartz basket reactor is reset to the protective gas slave reaction gas, 1+3 å¡ æŸ¬ system source, the fan of the balance system keeps the sensor temperature as the chamber quartz reaction The lower part of the device is a two-layer casing structure inside and outside. The reaction gas is intermittently introduced by two casings, and enters the inner casing from the bottom of the reactor. The product gas and protection 41 are exported from the central outlet. 2. The quartz basket is also tested with other hot weather. Different materials, the same part or the xin part is wrapped by quartz wire milk. The reaction gas enters from the side blood and the bottom. 5 The chemical reaction occurs in the sample, which overcomes the shortcomings of the existing thermal balance reaction gas and the sample, which is very important for the reaction kinetics study. 2. For the fine particle sample, the quartz wire mesh can be used. Thin layer of quartz wool is laid on the top to prevent leakage of the sample.
The device can be used to meet the requirements of the sequence lift and rapid sweat conditions on the furnace. The acquisition system starts at the same time. The reaction is started from room temperature at a set heating rate, the constant temperature process, and when the temperature needs to be rapidly increased, the furnace is first raised to a set temperature, and then the furnace is rapidly raised to the reaction zone by the lifter, and Acquisition system, acquisition, 1 can be set according to the 12, the stored data is stored and suspended. Ying Yanshi basket stone basket analysis instrument vortex refrigeration application in styrene analysis system Li Bu Liu Yong 21. Luoyang Petrochemical Plant, Henan Luoyang 471012; 2. Tianhua Chemical Machinery and Automation Research and Design Institute, Lanzhou 730060, Gansu, China. After using the vortex cooling method. Solved this.
1Overview of our factory in the expansion of the 6 parent 5 styrene project, the application of a oxygen analyzer to analyze the oxygen content of the compressor outlet gas outlet as a compressor outlet leak detection measure, and participate in the interlocking alarm inch production device Crucial role.
In the application process, due to the high water content of the sample gas, the oxygen analyzer can not only be shipped to the factory and, accurate analysis, to solve this difficulty. We entrusted the ruler Huahua 1 Machinery and Automation Research Institute to use the lane sampling processing system. After years of operation, the effect is good, the development of lubrication and refrigeration, currently mainly for the development and application of ethylene plant cracking furnace outlet gas, in recent years, has been extended to the ammonia synthesis gas furnace catalytic cracking regeneration flue gas sampling and processing system in. The application object is mainly in the process of high temperature, low pressure, high water saturated steam or heavy carbon component containing solid impurities. Its biggest feature is 1 self-cleaning function 2 has no moving parts; 3 maintenance quantity is less than 4, hitting and reaching The sample is purified, the temperature is lowered, and the analyzer is provided with a continuous and reliable qualified sample gas, which ensures the normal operation of the process analyzer and guides the normal production process.
2 Process conditions and overview The process conditions of the benzene ethylene exhaust gas outlet are as follows 1.
It can be known from the process conditions that the normal operation and timely and accurate analysis of the online analyzer should be ensured. The sample gas must be paid into the chamber to cool the heart, remove water; in addition to the harmful components benzene toluene ethylbenzene styrene and water.
The styrene-mounted compressor exhaust gas outlet has a low card force of 0.059 and a high temperature of 87, so the cooling method can not be used. We use the boiling point of the physical properties of each component of the sample. Guang, Xuanling technology, sample; pieces of refrigeration to 5100 right summer is 5; winter is 10, 4 conclusions The above balance not only has the performance of the current commercial thermal balance, but also has some unique excellent performance heat resistance and The corrosion resistance is good; the structure of the device is simple and can be continuously weighed; the reaction gas is easy to sample; it can be operated except in any atmosphere; the reaction process and the change of the sample can be observed externally.
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