The method of gas chromatography analysis
(57) Abstract:Usage: the invention relates to a gas mixture analysis, in particular gas chromatography, allowing complete separation of components of a gas mixture consisting of propane, air and carbon dioxide, in the presence of moisture at room temperature. The inventive method is based on the use of a chromatographic column filled with a sorbent-based media "Polisorb-1, which additionally contains "Selipar-600". The ratio of components, % 25 - 35 - "Polisorb-1", 75 - 65 - "Selipar-600". The column is filled approximately 1/3 of the length "Polisorb-1", else "Selipar-600, which is located along the gas for the "Polisorb-1". The analyzed mixture comes first "Polisorb-1", then "Selipar-600". 6 Il. The invention relates to chromatographic analysis of substances, in particular to a method of separating a mixture of gaseous substances by means of a chromatographic column filled with the adsorbent.Known methods of separating a mixture of gaseous substances in the presence of moisture by using a chromatographic column filled with the adsorbent, however, these methods require pre-heat carbendazime carrier  . However, such methods are complex, as they necessarily require back-flushing column to remove moisture after each unit of analysis.The closest technical solution of the invention is a method for the chromatographic separation of a mixture of air, propane, water and ethane on a column filled with adsorbent, based on the copolymer of styrene and divinylbenzene ("Polisorb-1"), optionally containing activated carbon  . This sorbent is subjected to conditioning in a stream of helium at a temperature of 180aboutC for 8 h, and the analysis is carried out by heating the column to the 90aboutC.However, the known method has the following disadvantages: first, you need to preliminary heat treatment of the sorbent (heating to 180aboutWith), and secondly, the separation of the mixture occurs at a temperature of 90aboutWith that requires the creation of special units ensure uniform heating of the column, tap-dispenser and detector. This leads to more complex devices capable of performing gas chromatographic analysis. In addition, the known method does not provide complete separation of the wet mixture of propane, air, carbon dioxide.CE is swetnam method of gas chromatographic analysis of a mixture of propane and air in the presence of moisture by separation on a chromatographic column, the last is filled with a sorbent-based media "Polisorb-1, which additionally contains, "Selipar-600 when the ratio of components, % : 25-35 - "Polisorb-1", 75-65 selipar-600, with "Selipar-600 is in the column in series along the gas flow after the "Polisorb-1".This gives you the opportunity to spend a complete separation of a mixture containing propane, air, carbon dioxide, in the presence of moisture, allows you to place a column at room temperature and to exclude pre-heat treated sorbents. Water exits in this case, very blurry peak. Ultimately, the presence in the analyzed mixture of moisture leads to a slight shift of the zero line of the chromatogram, which does not affect the conduct of the separation of other components of the analyzed mixture. In the column of water does not accumulate, therefore, does not require a back purge column after each unit of analysis. This method allows you to conduct several analyses and provides long-term repeated use of the column. This leads to simplification of the gas chromatographic analysis.In Fig. 1-6 presents the chromatogram obtained by separation of a gas mixture astasheerahum the gas chromatographic method of analysis is as follows. The analyzed mixture is prepared in the following ratio, wt. % : 20 air, propane 5; carbon dioxide 5; water 2; the rest is helium.As the analyzer uses a heat conductivity detector. The magnitude of the input dose of the analyzed mixture is chosen equal to 1 cm, as casinosites use helium. The speed of casinosites chosen equal to 20 cm/min. and the Column is carried out in a stainless steel tube with an inner diameter of 2 mm and set along the gas flow between the faucet spout and the detector without the intermediate connection elements. The analysis was performed at room temperature. The sorbents prepared fractions of 0.2-0,32.P R I m e R 1. The sorbent composition, % : "Polisorb-1" 25, "SIMOPOR-600" 75; column length 30 cm Analyzed the mixture comes first "Polisorb-1", then "Selipar-600". In Fig. 1 shows the chromatogram. which shows that the separation of the components of the analyzed mixture.P R I m m e R 2. The sorbent composition, % : "Polisorb-1" 30; "Selipar-600" 70; column length is 30 cm Analyzed the mixture comes first "Polisorb-1", then "Selipar-600". In Fig. 2 shows the chromatogram, which shows that the separation of the components of the analyzed mixture.P R I m e R 4. The composition of the sorbent similar to the previous one, the column length is 50 cm Analyzed the mixture comes first "Polisorb-1", then "Selipar-600". In Fig. 4 shows the chromatogram, which shows that the separation of the components of the analyzed mixture.Filling the column with a ratio of sorbents is outside the specified interval is not possible to obtain complete separation of the components of the analyzed mixture. This is confirmed by the following examples.P R I m e R 5. The sorbent composition, % : "Polisorb-1" 50; "Selipar-600" 50; column length is 30 cm Analyzed the mixture comes first "Polisorb-1", then "Selipar-600". In Fig. 5 shows the chromatogram. which shows that there is no complete separation of the components of the analyzed mixture (lack of separation between air and carbon dioxide).P R I m e R 6. The sorbent composition, % : "Polisorb-1" 10; "Selipar-600" 90; length of columns 30, see Fig. 6 shows the chromatogram, which shows that there is no complete separation between the components of the mixture.The separation between air and djok who did not provide complete separation of propane, air and carbon dioxide in the presence of moisture. The METHOD of gas CHROMATOGRAPHIC ANALYSIS by dividing the wet gas mixture containing propane and air, on a chromatographic column filled with a sorbent-based media Polisorb-1, characterized in that, to simplify the analysis, the sorbent further comprises SIMOPOR-600 when the ratio of the components Polisorb-1 - 25 - 35% , SIMOPOR-600 - 75 - 65% , and SIMOPOR-600 is in the column in series along the gas flow after Polisorb-1.
FIELD: chromatographic sorbents.
SUBSTANCE: invention relates to chromatographic sorbents, which can be used for analysis and preparative purification of optically active compounds. A novel sorbent for resolution of isomers of optically active compounds is developed containing, as chiral selector, macrocyclic glycopeptide antibiotic eremomycin, vancomycin, ristomycin A, teicoplanine, or their aglycons. Method of immobilization of macrocyclic glycopeptide antibiotics is also developed, which resides in that silica gel in aqueous buffer solution is first treated with 3-glycidoxypropyl(trialkoxy)silane and then, in alkaline aqueous or water-organic solution, above-indicated macrocyclic glycopeptide antibiotic is grafted to epoxy group-modified silica gel.
EFFECT: increased selectivity in enantiomer resolution and simplified preparation procedure.
9 cl, 12 dwg, 5 tbl, 9 ex
SUBSTANCE: specific area of silica surface reaches 300,2/g, porosity - up to 1,1 cm3/g, average pores diameter - 12,0-16,0 nm. For separating and property detection couples of substances and carrier gas are let through chromatography column, filled with silica powder, which is precipitated from hydrothermal solution, with receipt at output of column of sequence of special components, recorded in form of peaks. Absorbent, received on basis of silica, precipitated from hydro-thermal solution, in several cases has better separating ability then traditional absorbents.
EFFECT: higher efficiency.