JPS5864744A - Liquid chromatography mass spectrograph - Google Patents

Abstract

PURPOSE:To enable an eluent liquid and a sample, which constitute effluent solution, to be simultaneously vaporized continuously by providing a means of cooling an internal part of a conduit which is located inside an ion source, and a means of heating only the pointed end of the conduit from which the effluent solution is ejected. CONSTITUTION:An introduction cylinder 10, around which a heater 9 is wound, is connected to an introduction hole 4. A glass cylinder 11, whose end having a bottom is inserted into an ion source, is supported by a fast cylinder 13, which is fixed to the outer wall of the ion source through an insulating body 12, so that the cylinder 11 is movable in the direction indicated by the arrows. A conduit 14 which introduces liquid flowing out of a liquid chromatograph is installed and fixed in the center of the cylinder 11 in such a manner that the conduit 14 penetrates the bottom of the cylinder 11. The pointed end of the conduit 14 is inserted inside the cylinder 10. In addition, a cooling container 16 used for cooling the conduit 14 is installed at an internal part of the cylinder 11 which is inserted inside the ion source.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a device combining a liquid chromatograph and a quality analysis device.

A chromatograph is a useful device for separating and analyzing multi-component mixed samples, and in particular, when coupled with a quality analysis device as a detection means, information on molecular weight and molecular structure can be obtained. Devices that combine a gas chromatograph and a commercial analyzer have been put into practical use and are widely used, but devices that combine a liquid chromatograph and a quality 1 analyzer have not yet been put to practical use, although various methods have been attempted in recent years. The product is not yet complete〇By the way, the inside of the ion source of the purchase analyzer is kept in a high vacuum, and the effluent from the liquid chromatograph must be vaporized before being introduced.0 To vaporize this effluent, The essential conditions are (2) continuous vaporization of the eluent and sample constituting the +11 effluent at the same time. For example, if the eluent evaporates first, the chromatogram may become tailed, resulting in a tailing phenomenon, or in severe cases, the eluent may shrink.
C is deposited, and discontinuous vaporization causes fluctuations in the total ion concentration signal, both of which are undesirable.

The present invention involves inserting a conduit that guides the effluent from the liquid chromatograph into the ion source and ejecting it from the tip of the scissors conduit, which instantly vaporizes the effluent and introduces it into the ionizer to ionize it. In this case, a means for cooling the portion of the conduit inside the ion source and a means for heating only the tip portion from which the effluent is spouted should be provided.
The present invention will be explained in detail with reference to the following drawings. ◎ Figure #I1 is a sectional view showing the configuration of one embodiment of the present invention, and Figure 1 Here, 1 is an ion source whose interior is maintained at a high vacuum 6ζ Inside the ion source 1 is placed an ion source block 6 with an internal Cζ ionization chamber 2 ◎Cough block MK is a sample An introduction port 41 is provided with passage ports 5 and 6, and the sample introduced from the introduction port 4 into the ion exit chamber 2 is ionized by electrons generated from the filament 7 and directed toward the trap electrode 8. The opening 4 is connected to an introduction 1to around which an outer cap 1 and a heater 9 are wound. 011 is a glass tube whose bottom end is inserted into the ion source, and the glass gilt has an insulator 12. The glass 1liil is held slidably in the direction of the arrow by a mounting 111M fixed to the outer wall of the ion source through the
A conduit 14 is installed and fixed to guide the effluent from the liquid chromatograph (not shown) in a manner that penetrates through the bottom surface of the center 11i of the conduit 11, and the tip of the conduit 14 is inserted into the introduction [10]. 015 is a nut for adjusting the degree of insertion, and is screwed into a threaded portion provided at the atmospheric side end of the mounting tube and is rotatably held on the glass 1l1111. A portion Cζ inserted into the ion source inside the ion source 11 is a cooling tank 1 for cooling the primary conduit 14.
6 is provided. 17 and 18 are piping for flowing a cooling medium into the cooling tank 16.

In the configuration described above, the effluent from the liquid chromatograph has an allowable fI determined by the vacuum pumping capacity of the ion source.
L control, for example, several μl/min @ full, is adjusted, conduit 1
4 is spouted into the introduction tube 10 and vaporized. Generally, the inside of the ion source is kept at a high temperature of 11#c, but the effluent is cooled by the cooling tank 16 until just before ejection, so the temperature rise in the conduit 14 is small. Therefore, the eluent with a relatively low boiling point There is no chance that the sample will vaporize before the sample and bubbles will be generated in the conduit, causing the effluent to be sent intermittently.Therefore, it is called continuous vaporization! Condition 2) of Section II is satisfied.

The tip of the conduit 14 to the east is heated by the heater 9 and reaches a high temperature ε.
As a result, the ejected outflow is instantaneously vaporized, and the above-mentioned condition (1), which states that the eluent and sample are simultaneously vaporized, is also satisfied. Furthermore, if the tip of the conduit 14 is kept at a high temperature, the sample will not adhere to the tip, and the tip will always be kept clean, which is a great effect. In this embodiment, the degree of insertion of the tip of the conduit 14 into the introduction@10 can be varied by rotating the nut 15 and moving the glass sieve 11, so the temperature of the tip can be adjusted arbitrarily. O Figure 2 is a sectional view showing the configuration of another embodiment of the present invention.0 In the figure, the same components as in the embodiment of Figure 1 are given the same numbers. The glass tube 11 is slidably held in the mounting @15 like #1gl, but in this example, another glass tube 19 that houses the glass 11111 inside is fixed as the mounting tube IA#cII. There is. The tip of the glass 1119 has an inner diameter narrower than the portion housing the glass tube 11 so as to communicate with the sample introduction port 4, and an entrance nozzle is provided at the portion where the inner diameter changes to face the tip of the conduit 14. 20 are provided. A heating ring 22 around which a heater 21 is wound is fitted into the tip of the conduit 14, and a heater 26 is also wound around the tip of the glass sieve 19. 24 is a terminal for supplying power to the primary heater 21. Further, 25 is an exhaust pipe for evacuating the space between the glass 11111 and the glass sieve 19, and is connected to a rotary pump.

In this embodiment, a separator is formed by the ejection end of the conduit 14 and the inlet nozzle 20 disposed opposite thereto, so that it is possible to concentrate the sample components.

That is, the effluent (sample + eluent) is discharged from the tip of the conduit 14 in the form of an extremely fine mist. This fog is heated by heater 26
Although the eluent is heated and vaporized by the radiant heat from the lis kept at a high temperature, the eluent, which is a relatively light component, expands at a high speed and moves toward the exhaust pipe 25. On the other hand, since the sample component, which is a relatively heavy component, moves straight in the jetting direction, the gas entering the nozzle 20 contains a large amount of the sample component, and the sample component flows into the ionization chamber 2 in a concentrated state. However, it is ionized by electron impact I.

In this implementation f4jlc, the part of the conduit 14 that is inserted into the ion source is cooled, so no bubbles are generated in the conduit, and the tip of the conduit is heated, so the ejected liquid is instantly It is vaporized and there is no sample attached to the tip.In addition, with this real hook, turn the nut 15 once and attach the glass fI11.
Since the distance between the nozzle 20 and the conduit 14 can be changed by moving the separator 1, the state of the separator can be varied according to the required gI.

[Brief explanation of the drawing]

FIGS. 1 and 2 are #tJ diagrams each showing the configuration of an embodiment of the present invention. 1: Ion source, 2: Ion source, 6: Ion source pump, 9, 21.2M: Heater, 10: Introduction tube, It, 1
9 glass tube, 12: insulator, 16: mounting tube, 14: conduit, 15: nut, 16: cooling tank, 17° 18: piping,
20: Inlet nozzle, 22: Heating ring. Patent applicant JEOL Ltd. Representative Tadao Kase

Claims (1)

[Claims] A conduit that guides the effluent from the liquid radiator is inserted into the ion source, and the effluent is gasified by jetting it out from the tip of the ionizing tube, and the gas is introduced into the ionization chamber for ionization. A liquid chromatograph characterized in that a hot IIL body chromatograph mass spectrometer apparatus is provided with means for cooling a portion of the conduit located inside the ion source and means for heating a tip portion of the conduit. Mass spectrometer.