COMPACT SEPARATION SYSTEM WITH SNAP-IN COLUMNS

Abstract: The present invention is projected for use in chemical analyses based on separation techniques such as used in gas chromatography. The invention has a separating column encapsulated in a closed container of small volume, through which a temperature control fluid is circulated by means of a small pump, when the capsule is coupled to the instrument. This fluid is heated with temperature control and monitoring carried out electronically. The instrument also has a sample injector, a detector to indicate the separated components of the sample after their passage through the column and an electronic system to amplify and store the signal originated in the detector. An external control panel permits command of all its functions by an operator.

Description: "COMPACT SEPARATION SYSTEM WITH SNAP-IN COLUMNS" DESCRIPTION OF PROJECT r ieid ~ ~ pooli c. tion Tne i n 2 - rumen t neraiπ αescriPed is proposed for D 5- aculicaticn in cremicai analysis involving separation tecnπiquss such as in Gas Chromatαr.raohy. Prior knowledge Systems presently in use for cnrcmatp graphic analysis, using g-2ses or supercritical fluids -as the mooile phase, 10- utilize large ovens, with vplumes on the order of various cubic decimeters, sufficient to acco odate one or more columns end to adequately control the temoerature, or the -rogramiπα of tne temperature, using confined hot air. The columns are installed using different ty-es of threaded 5- connectors normally containing aoprppriate ferrules to avoid fluid loss. A complete description of such equipment can be found in the literature on Chromatography. We suggest the book "Modern Practice of Gas Chro tojraphy" , R. t. Grob, ed. , 0- 2 edition, John Wiley and Sons, New York, 1985. General description of the invention The present invention has two parts. The analytical column is contained in a replaceable capsule through which circulates a temperature-controlling fluid. Whether connected 5- to the system or simply being stpred, the analytical cplumn is prptεcted against mechanical damage by the capsule container. The small volume of the capsule container permits better temoerature control and more raoid and reliable temperature orogra ing when in use. The attachment, and 0- removal, of the column capsule from the instrument is carried out manually, withcut the need of tools, using planar or spherical connectors without tnreads. Two connections are for the entrance and exit of tne analytical fluid. Two other connections permit tne circulation of tne temoerature control 5- fluid. The instrument has a unit which activates the circulation of this fluid, which may ce neateα cr cooled, and for control and monitoring of the temperature, controlled through appropriate electronic cir.cuitry. The instrument also has systems to permit the entrance of the analytical fluid, sample injection into this analytical fluid, and a G5- detector for the partially or completely separated original components, whose signal is transferred, by appropriate electrical connections, to an electronic amplifier, for simultaneous or posterior display. Description of the diagrams 10- Figure 1 shows de proposed instrument coupled to the cclumn capsule (1) which contains the analytical column (2). The analytical fluid, such as a gas, enters the instrument through opening (3). The sample is introduced into the fluid stream through the injector (4) which has its own independent 15- temperature control system. The sample is completely or partially separated during its passage through the column and exits from the column into a detector (5), which indicates the presence of the separated comooπents by means of an electronic signal that is received, 20- processed and then registered and stored (6). After passing through the detector the analytical fluid and sample exit through opening (7). The temoerature control fluid circulates through ducts (B), propelled by a pump (9) activated by a motor (10). The 25- he≤ting or cooling of this fluid is carried out in a small chamber (11) equipped with a heating element, such as a resistor, and with a system to exchange heat with external atmosphere, by convection or forced air circulation. Control of temperature is done by means of appropriate electronic 30- circuitry and monitored by a thermometric system, such as a thermccouple (12). The operation -arameters are controlled and monitored by use of a small αanel (13) and appropriate electronics and the resulting information is displayed and/or stored. The 35- equipment operates in alternating current (110/220 volts and 50/βθ hertz) with an internal transformer. (14) . figure ϊ snows oet^ils of the connections oetwesn the column capsule and tne instrument with the column ends (15), and the tsm- er jture control fluid fittings (15). Construction cf the instrument C 5- The column, usually in the form of a capillary tube, is made of glass, fused silica, or metal, with lenghts from few centimeters to many meters, and has usually received special treatment on the inner surfsce to permit sample- separation to occur. The column is supported within the caosule in such 10- ~ v.aππer ≡s to permit easy circulation of the temperature controlling fluid. The cacsuia is made of metal or other material that .has a good resistance against the working limit of temperature, which is aoout 5C0 C for some columns and is expected to be 5- higher as column technology improves. The capsule inner wall is made reflective and the external one is coated with a thermal insulating cover. The instrument container itself is made of metal or a mechanically resistant p lastic. The temperature controlling 0- fluid is contained in a thermally insulated metal tubing loop and the connections between the caosule and the instrument itself are made of tantallum, glass or quartz, with highly polished, smooth surfaces. The injector and detector may be anyone of many already 5- available commercially and will be incorporated into the instrument as required. The electronic control of the whole system is carried out using an already available board from a microcomputer. The results are displayed in an external device, not shown on the drawing, that can be a screen or a D- printer/plotter recorder. Applications The instrument may- be used in any determination which involves separation and qualitative/quantitative analysis of gases or volatile species in a fluid stream, either in a 5- laαorstory environment or directly coupled to a orαcess line.

Claims: AMENDED CLAIMS [received by the International Bureau on 21 May 1990 (21.05.90); original claim 3 amended; other claims unchanged (1 page)] 1- The invention herein described is characterized. by the presence of an encapsulated column, to be attached to the instrument itself by smooth fittings, containing a freely - circulating temperature control fluid. 2- The invention herein describe is characterized by the presence of a circulating temperature control fluid, with devices for pumping, heating/cooling and monitoring its temperature along the flowing tubing. - 3- The invention herein described is characterized by the mounting of the column capsule directly onto a compact system containing a injector, a detector, and a tubing for the temperature control fluid circulation. - 4- The invention herein described is characterized by the presence of the heating element inside a closed system, with no direct contact with external atmosphere.

Inventors: MANFREDI JOSE FELIX, MENDONCA JOSE EDUARDO DE, MANFREDI, JOSE, FELIX, MENDONCA, JOSE, EDUARDO DE
Applicants: MANFREDI JOSE FELIX, MENDONCA JOSE EDUARDO DE, MANFREDI, JOSE, FELIX, MENDONCA, JOSE, EDUARDO DE
Application year: 1989
Main classification: G01N30
IPC codes: G01N30