Patent
Method of analysis of organic compounds in chromatography and apparatus for performing this method
| العنوان: | Method of analysis of organic compounds in chromatography and apparatus for performing this method |
|---|---|
| Patent Number: | 5,028,544 |
| تاريخ النشر: | July 02, 1991 |
| Appl. No: | 07/257,440 |
| Application Filed: | October 14, 1988 |
| مستخلص: | The objects of the invention are attained in an apparatus for performing a method of analysis of organic compounds in chromatography, comprising a chromatographic column sealingly connected with the housing of a surface ionization detector having coaxially arranged inside, a collector and a thermoemitter with current leads, the housing of the surface ionization detector being provided with an opening for an auxiliary gas feed line and an opening for delivering the spent gases. The thermoemitter includes a closed-end sleeve with a heating element in contact with the external non-working surface of the thermoemitter. The collector includes a hollow cylinder spaced from the inner ionizing surface of the thermoemitter, and the outlet portion of the chromatographic column being received inside and throughout the length of the collector. The end of the outlet portion of the chromatographic column and the auxiliary gas feed line are positioned and arranged such that the mixing of the components of the sample gas and the feed gas occurs immediately adjacent the ionizing surface of the emitter, with the auxiliary feed gas being thermolyzed by the collector prior to contacting the emitter. Another preferred arrangement of the apparatus includes a thermoemitter which consists of a refractory metal and an ionizing surface coated with oxidized tungsten. |
| Inventors: | Rasulev, Utkur K. (Tashkent, SUX); Nazarov, Erkinzhan G. (Tashkent, SUX); Sidelnikov, Valery O. (Tashkent, SUX); Evtukhov, Rustam N. (Tashkent, SUX); Alimkhodzhaev, Shavkat S. (Tashkent, SUX); Tashpulatov, Bakhtiyar M. (Tashkent, SUX); Khudaeva, Gulsara B. (Tashkent, SUX) |
| Claim: | What is claimed is |
| Claim: | 1. A method of analysis of organic compounds in chromatograhy, including |
| Claim: | separating chromatographically a gas mixture to be analyzed in a chromatographic column sealingly connected with a surface-ionization detector; |
| Claim: | passing components of said separated mixture through said surface-ionization detector having a thermoemitter and a collector; |
| Claim: | passing concurrently an auxiliary gas through said surface-ionization detector, said auxiliary gas flowing past the length of the collector prior to contacting the thermoemitter |
| Claim: | said components of said mixture under analysis and said auxiliary gas being passed into said surface ionization detector independently of one another and in one and the same direction; |
| Claim: | mixing said components of said mixture under analysis and said auxiliary gas in direct vicinity of the ionizing surface of the thermoemitter of said surface-ionization detector, the mixing of said components of said separated mixture under analysis and said auxiliary gas being conducted in quantities supporting substantial permanence of the surface ionization factor of said theroemitter of said surface-ionization detector within the predetermined range of working temperature thereof; |
| Claim: | measuring the ion current at the collector of said surface-ionization detector, and using the results of the measurements for assessing the presence and quantities of the individual ones of said components of said mixture under analysis. |
| Claim: | 2. An apparatus for performing a method of analysis of organic compounds, comprising |
| Claim: | a surface-ionization detector including a housing, a thermoemitter with current leads positioned in said housing and being in the form of a closed-end sleeve accommodating a heating element about the lateral non-working surface thereof, a collector positioned in said housing coaxially with said thermoemitter, in the form of a hollow cylinder arranged with a gap defined therebetween and the inner ionizing surface of said thermoemitter, and means for delivery of spent gases, mounted in said housing; |
| Claim: | a chromatographic column sealingly connected with said surface-ionization detector, the outlet portion of said chromatographic column extending within said collector throughout the length thereof, the outlet end of said outlet portion of said chromatographic column directly adjoining said ionizing surface of said thermoemitter; |
| Claim: | means for feeding in an auxiliary gas, mounted in said housing of said surface-ionization detector below the port of entry of said outlet portion of said chromatographic column into said housing of said surface-ionization detector, and being positioned and arranged so that the auxiliary gas is thermolyzed while passing along the collector prior to contacting the thermoemitter. |
| Claim: | 3. An apparatus for performing a method of analysis of organic compounds , comprising |
| Claim: | a surface-ionization detector including a housing, a thermoemitter made of a refractory material and having current leads, positioned in said housing and being in the form of a hollow cylinder accommodating a heating element about the lateral external surface thereof, a collector positioned in said housing by an insulator, extending coaxially with said thermoemitter and being in the form of a rod spaced from an inner ionizing surface of said thermoemitter throughout the length thereof, said ionizing surface being additionally coated with a layer of oxidized tungsten, and means for delivery of spent gases, mounted in said housing; |
| Claim: | a chromatographic column sealingly connected with said surface-ionization detector, the outlet end of the outlet portion of said chromatographic column being accommodated in said housing at the side thereof opposite to a securing of said collector in said housing of said surface-ionization detector, coaxially with said collector and adjacent to an end face of said collector and to said ionizing surface of said thermoemitter; |
| Claim: | means for feeding an auxiliary gas accommodated in the wall of said housing of said surface-ionization detector at the side of the accommodation therein of said end portion of said chromatographic column, for feeding the auxiliary gas adjacent to said ionizing surface of said thermoemitter. |
| Claim: | 4. An apparatus as claimed in claim 2, wherein said thermoemitter is made of a refractory metal, said ionizing surface thereof being additionally coated with a layer of oxidized tungsten. |
| Claim: | 5. A method of analysis of organic compounds in chromatography, including the steps of |
| Claim: | separating chromatographically a gas mixture to be analyzed in the chromatographic column sealingly connected with a surface ionization detector; |
| Claim: | passing components of said separated mixture through said surface-ionization detector having a thermoemitter and a collector, said thermo-emitter being made of a refractory metal and having an ionizing surface coated with a layer of oxidized tungsten; |
| Claim: | passing concurrently an auxiliary gas through said surface-ionization detector; |
| Claim: | passing said components of said mixture under analysis and said auxiliary gas into said surface-ionization detector independently of one another and in one and the same direction; |
| Claim: | mixing each of said components with said mixture under analysis and said auxiliary gas in direct vicinity of the ionizing surface of the thermoemitter of said surface-ionization detector, the mixing of said components of said separated mixture under analysis and said auxiliary gas being conducted in quantity supporting substantial permanence of this surface-ionization factor of said thermoemitter of said surface-ionization detector within a predetermined range of working temperature thereof; and |
| Claim: | measuring ion current at the collector of said surface-ionization detector, and using the results of the measurements for assessing the presence and quantities of each of said components of said mixture under analysis. |
| Current U.S. Class: | 436/161; 436/153; 422/89; 422/90; 422/98; 324/467; 324/468; 324/470; 73/234; 250/281; 250/379; 250/389 |
| Current International Class: | G01N 3300 |
| Patent References Cited: | 4651008 March 1989 Wells 4839143 June 1989 Vora et al. |
| Other References: | Zandberg, E. et al., "Emitters for Surface-Ionization Detection of Organic Compounds", Zh. Tekh. Fiz., 46(4), pp. 832-838, 1976. |
| Primary Examiner: | Lacey, David L. |
| Assistant Examiner: | Redding, David |
| Attorney, Agent or Firm: | Lilling and Lilling |
| رقم الانضمام: | edspgr.05028544 |
| قاعدة البيانات: | USPTO Patent Grants |
| الوصف غير متاح. |