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Do you really understand "microwave digestion"?
Microwave digestion generally refers to the use of microwave heating to close the digestive solution (various acids, partial lye and salts) and samples in the container to rapidly dissolve various samples under high temperature pressurization conditions (also open containers) Microwave digestion, will not be discussed). The two characteristics of closed container reaction and microwave heating determine the advantages of complete, fast and low blank, but inevitably bring about high pressure (his potential hazard of overpressure) and insufficient sample size. High pressure (up to 100-150 bar), high temperature (usually 180-240 ° C), and strong acid vapor bring safety stress to the experimenter. Today's commercial microwave digestion systems generally have temperature measurement/pressure measurement and even temperature control/pressure control technology, so there is a greater guarantee in safety. But as a potential user (or user), you should still understand some of its characteristics, not only for the choice of microwave digestion system, but also for safer use, the following points are listed:
1, the principle
Multiwave PRO, the first two-dimensional dual magnetron technology, has become the only microwave device in the world to receive ETL and GS dual safety certification.
2, intelligent integration
One-button intelligent integration: Automatic identification of the type, number and location of reactors in the reaction chamber, and automatic detection of the installation of the temperature control system. Then, according to the characteristics and equivalent of the sample, the application method database is automatically retrieved, and the automatic energy optimization data matching calculation is performed. The whole process intelligent control does not need to be set, but at the same time, the whole process of temperature, pressure and power adjustment curves is displayed, 0-40 cans. The target tracks the real-time temperature status display.
3, safety pressure relief
Whether it is timely and safe to release pressure related to safety is the most important. Generally, the microwave digestion system controls the microwave heating when the temperature/pressure reaches the target temperature/pressure. However, the chemical reaction in the actual digestion tank does not necessarily stop immediately, so it may cause overpressure and must be safe in time. Relieve pressure. If there is no pressure relief method, the pressure resistance of the digestion tank must be much greater than the maximum working pressure to ensure a sufficient safety factor. At present, the microwave digestion tanks produced by several major imported microwave digestion manufacturers have adopted corresponding measures for passive pressure relief. Anton Parr (Austria) and Berghof (Germany) use metal explosion-proof membranes, and PreeKem (屹尧) adopts The plastic explosion-proof membrane, Milestone (Italy) reaction tank is a single spring piece automatic pressure relief type, CEM (United States) uses the explosion-proof membrane and shrapnel pressure relief, Sineo (China) uses explosion-proof membrane and burst rupture.
4, temperature measurement method
The temperature measurement method can be divided into contact type (fiber temperature measurement), non-contact type (infrared temperature measurement) and platinum resistance temperature measurement according to whether it is in contact with the inside of the digester. Each of the three methods has its own advantages and disadvantages. The user can examine the accuracy of the test, the uniformity of the sample test, and the speed of the test. In the pressure measurement method, it is divided into contact pressure measurement and non-contact pressure measurement.
5, container material
There are generally fluoroplastics such as TFM, PTFE, PFA and quartz. TFM is a modified PTFE. Melting point 320-340 ° C. In addition to all the advantages of PTFE, there are some notable improvements in properties: smaller deformation at higher temperatures and pressures, less permeability, better recovery from heavy pressure at high temperatures, and high surface finish. PFA, although translucent, has a lower maximum temperature than PTFE. Therefore, TFM is the preferred material for digesting containers. The PTFE digestion tank can only be used for medium and high pressure, while the TFM digestion tank can be used for ultra high pressure microwave digestion.
6, container selection
The outer casing (sheath) of the combined can and the insert dig can be separated. The one-piece can may be made of a single material, but it may be composed of one, two or three materials, but it has been combined and cannot be disassembled. The combination tank generally has a casing, a frame (intermediate layer), an interpolating digester, and some combination tanks do not use an intermediate layer. The outer casing is made of composite fiber (CEM patent), PEEK, high temperature ceramic, Ultem-100 (Ultem material has been basically eliminated). The frame is mainly made of PFA and high strength engineering plastics. The interpolated digestion tank is in direct contact with the sample and acid, and acid resistance, temperature resistance and high pressure performance are the primary considerations.
Comparison of the advantages and disadvantages of the two: the integrated tank is more resistant to pressure than the single material, and the interpolation digester can be taken out and replaced (at a small cost). However, the combination tank needs to be disassembled, the acid resistance of the outer casing is always inferior to that of fluoroplastic, and some shells are brittle at high temperatures. One-piece cans do not need to be disassembled, but they are costly, heavy, and slow to cool down. The single material integrated tank can only be made of TFM or PTFE, which is acid resistant and has a long service life. Fluoroplastics are tough materials that are not susceptible to bursting.
Interpolated digester material, used as an interpolation digester (or integrated digestion tank), there are generally four kinds of materials, PTFE, TFMTM PTFE, PFA, quartz, the first three are fluoroplastic type. PTFE: polytetrafluoroethylene, melting point 320-340 ° C; TFMTM PTFE (referred to as TFM): made of PTFE added less than 1% of additives, is a modified PTFE. Melting point 320-340 ° C. In addition to all the advantages of PTFE, there are some notable improvements in properties: smaller deformation at higher temperatures and pressures, less permeability, better recovery from heavy pressure at high temperatures, and high surface finish; PFA: perfluorinated Alkoxyethylene, translucent, melting point about 308 ° C, high surface finish; quartz: very good thermal stability, high melting point, but brittle under high pressure, can not be used in the case of HF sample. Quartz digestion tanks cannot be used alone and should be sheathed.
For the highest practical use temperature, TFM is the same as PTFE at 260 °C. PFA is 10-20 ° C lower than the first two. Although the use temperature of quartz can be very high, it is limited by materials such as seals and brackets. Generally, the maximum temperature of the quartz digestion vessel is 300 °C. The maximum use temperature is generally achieved when sulfuric acid is used, and the usual digestion temperature is 170-220 °C.
Compared with the three kinds of fluoroplastics, TFM is undoubtedly the best digesting material. Therefore, the interpolation digester of the high-pressure digestion tank that is generally imported into the microwave digestion system is TFM material. PFA and PTFE can generally only be used as medium and low pressure digestion vessels. Of course, if you have to ask for transparency, you can only use PFA.
7, sheath material
Generally, there are composite fiber materials, PEEK, ceramics, and Ultem-100, and their strengths are much larger than TFM, but any material that is resistant to acid corrosion cannot be compared with fluoroplastics such as TFM, PTFE, and PFA.
8, digestion tank
Maximum temperature The maximum operating temperature cannot exceed the maximum operating temperature of the digested container material. Therefore 260 ° C is generally the highest temperature of use of all fluoroplastic digestion tanks. Although some companies' products can reach 300 ° C, but can not reach the highest pressure at the same time, 300 ° C will definitely affect the service life of fluoroplastic digestion vessels. The maximum operating temperature of the quartz digestion vessel can be very high, but it is generally limited to 300 ° C due to its sheath or bracket. Usually, most of the microwave digestion can be completed at 160-220 °C.
Maximum pressure The pressure in the digester is mainly determined by the organic matter content of the sample, the vapor pressure of the acid, and the temperature. The higher the organic matter content of the sample, the greater the pressure in the digester.
Digestion with acid or alkali solution microwave digestion usually uses nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid and hydrogen peroxide. Sulfuric acid has the lowest volatility, and the highest temperature is generally achieved when sulfuric acid is used, but it is extremely easy to damage the digesting tank after 210 °C. Sometimes, some samples (silicon aluminum alloy) are often digested with potassium hydroxide or sodium hydroxide solution.
Digestion Amounts Different types of digesters can differ in the maximum amount of sample that can be digested. The maximum amount of sample that can be digested depends on the organic matter content of the sample, the type of acid field, the set temperature, the volume of the digestion tank, and the maximum working pressure of the digestion tank. For microwave closed digestion, the maximum amount of sample that can be digested is always the relative weakness of all microwave digestion systems.
9, consumables savings
After using the microwave of CEM MARS5, I found that by putting a translucent cover on the upper and lower ends of the jacket, it can reduce the wear of acid and pressure, and can reduce the loss by 3/4 in the case of heavy use. CEM is more than 1,000 in South China. If it is used frequently, the average loss per 5,000 yuan per coat can be saved by 500W. These jackets are all imported from the United States and can save a lot of foreign exchange.
10. Industry application
The cost of conversion of elemental analysis methods in the pharmaceutical industry is enormous, including instrument procurement, microwave digestion methods and ICP method development, test project determination, training and documentation. Some samples are easy to digest, but some raw material samples containing biomolecules are not so easy. CEM's goal is to allow technicians to go to the microwave digestion device, safely and quickly assemble the digestion tank, add appropriate amounts of sample and acid reagents, and place them in the microwave digestion chamber to complete the digestion process. Jason Keith, CEM's Analytical Chemistry Product Line Product Manager, said: "CEM's extensive range of built-in training tutorials and pre-programmed methods can help achieve this goal."
It can be used for digestion of various samples in industrial, agricultural, environmental protection, sanitary inspection, metallurgy, geology, medicine, chemical and other sectors; especially suitable for atomic spectroscopy such as atomic absorption spectrometer, ICP-emission spectrometer, atomic fluorescence spectrometer, ICP-mass spectrometry Accurate determination of trace, trace and ultra-trace elements in various samples, such as instruments and anode dissolution apparatus. APL's microwave digestion instruments are widely used in these fields!