RU194141U1 - DEVICE FOR RESEARCH BY METHODS OF GAS ELECTRONOGRAPHY AND INFRARED FOURIER SPECTROSCOPY COMPONENTS OF SUBSTANCE, SEPARATED BY A GAS CHROMATOGRAPH - Google Patents

Abstract

The utility model relates to the field of research and analysis of materials. A device for electron diffraction studies of molecules in the gas phase includes series-connected units: a gas chromatograph; molecular separator; a gas electronograph, the results of which are recorded by a gas electronograph detector; and an infrared Fourier spectrometer (IRF spectrometer), the results of which are recorded by the detector of the IRF spectrometer, while all of these units are connected to a computer that controls the operation of each unit, stores and processes the results of their work using a common computer program that takes into account the results, obtained from a gas electron diffractometer and an IRF spectrometer. The technical result is to increase the accuracy and reliability of all parameters of the free molecules of the analyte. 1 ill.

Description

The technical field to which the utility model relates.

The proposed utility model relates to the field of research and analysis of materials, namely, to a device for determining the structure of a free molecule by gas electron diffraction (its spatial configuration, internuclear distances, valence angles, vibration amplitudes) and infrared Fourier spectroscopy (presence of isomers, presence and number of atoms carbon in the molecule, determination of individual groups of atoms, identification of substances) for pure substances obtained by separation of the analyzed material by gas chromatography.

State of the art

The prior art device is known combining gas chromatography (GC) and gas electron diffraction (GE) [Ewbank J.D. et al. Real-time data acquisition for gas electron diffraction / Review Scientific Instruments, 1984, V. 55, N. 10, pp. 1598-1603; Ewbank J.D. et. al. Improvements in real-time data acquisition for gas electron diffraction / Review Scientific Instruments, 1986, V. 57, N. 5, pp. 967-972].

The disadvantages of such a device are the impossibility of obtaining infrared Fourier spectra (IRF spectra) of the studied samples, which are especially important for studying the structures of polyatomic organic molecules, since the distance between the hydrogen nuclei in a molecule is practically impossible to determine by the GE method [L. Vilkov ., Mastryukov BC, Sadova N.I. Determination of the geometric structure of free molecules. - L .: Chemistry, 1978.- 224 p., P. 32], and infrared Fourier spectroscopy (IRFS) just gives the information associated with it (characteristic bands of hydrocarbon groups and molecules of organic substances).

On the other hand, the data obtained by the HE method in combination with the preliminary separation of the analyzed gas by the GC method provide important information for the IRFS method on the skeletal structure of a free molecule, the presence and number of certain groups of atoms in it. This helps the correct interpretation of the IRF spectrum. Taking into account the results of the GE method makes the results of the ICFS method more reliable and reasonable, that is, these methods are mutually complementary.

Utility Model Disclosure

The technical result of the proposed utility model is to increase the accuracy and reliability of all parameters of the free molecules of the analyte, determined by the GE method (that is, data on the spatial configuration of free molecules, internuclear distances in it, the value of valence angles and vibration amplitudes of atoms in this molecule).

The specified technical result is achieved by a device for electron diffraction analysis of molecules in the gas phase, which includes series-connected blocks: gas chromatograph; molecular separator; a gas electronograph, the results of which are recorded by a gas electronograph detector; and an infrared Fourier spectrometer (IRF spectrometer), the results of which are recorded by the detector of the IRF spectrometer. All of these blocks are connected to a computer that controls the operation of each block, remembers and processes the results of their work using a common computer program that takes into account the results obtained from a gas electron diffractometer and an IRF spectrometer.

Brief Description of the Drawing

A block diagram of the proposed device is shown in FIG. one.

Utility Model Implementation

The test sample 1, together with the carrier gas 2, enters the gas chromatograph (GC) 3, where the analyzed sample is separated into the components of which it can consist (impurities, isomers, conformers, rotamers, unstable molecules). As the carrier gas, helium should be used, which does not contribute to the electron diffraction pattern and does not react with the components of the sample (although other gases, for example, H ₂ , can also be used, which is solved taking into account the properties of these gases and the analyzed sample). From the gas chromatograph 3, the gas enters the molecular separator 4, which separates most of the carrier gas from the sample. The separated components of the sample gas enter the inlet system of the gas electron diffractor 5, and then into the chamber of the gas electron diffract 5 ₁ , where they interact with the electron beam, and the result is recorded by the gas electronograph detector 5 ₂ . The analyzed gas exits the nozzle of the gas electron diffraction system inlet 5 with a diameter of about 0.2 mm at a pressure of about 1 mm Hg, which is controlled by the valve of the gas electron diffraction inlet system 5. Next, the gas enters the measuring cell (“light tube”) of the IRF spectrometer 6, and its spectrum is recorded by the detector of an IRF spectrometer 6 ₁ . A source of infrared radiation, together with mirrors, a beam splitter and a parabolic mirror, directing light into the measuring cell of the IRF spectrometer 6, are mounted in block 6 ₂ . All blocks are connected to a computer 7, which controls the operation of each block, remembers the results of their work, and then processes the results according to a common computer program that takes into account the results of GE and IRFS. To ensure a working vacuum in all blocks, they are tightly interconnected (excluding a computer) through vacuum gaskets, have a common pumping system with forevacuum and high vacuum pumps, a piping system with valves, which allows to obtain the necessary pressure in each block and measure it with the required accuracy.

Claims (1)

A device for electron diffraction studies of molecules in the gas phase, including serially connected blocks: gas chromatograph; molecular separator; a gas electronograph, the results of which are recorded by a gas electronograph detector; and an infrared Fourier spectrometer (IRF spectrometer), the results of which are recorded by the detector of the IRF spectrometer, while all of these units are connected to a computer that controls the operation of each unit, stores and processes the results of their work using a common computer program that takes into account the results, obtained from a gas electron diffractometer and an IRF spectrometer.

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