JPS5845552A - Novel detector used for chromatographic method - Google Patents

Abstract

PURPOSE:To eliminate the variance in a circumferential direction and to detect developed materials quantitatively with high reproducibility by rotating a bar- like developing element around its axial center, and moving a detector in the axial center direction of the element. CONSTITUTION:A motor 6 of a driving part 3 for a developing element and a motor 11 of a driving part 4 for a detector are run under control of an op amplifier 15 of differential input type to move a detector 10 in the axial direction of an element according to the revolutions of the element 7, gripped by chuck 5. In the case of using a spiral element B as the element 7, the detecting position of the detector 10 consisting of a hydrogen flame burner 13 and an ion collector 14 moves along the developing line of a thin spiral layer 2. The detected output of the detector 10 is supplied through an op amplifier 16 of single input type to a pen recorder 17, by which said output is recorded on a chart.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a detection device used in chromatography, and more particularly to a detection device for a substance developed with a rod-like development element. The purpose is to propose a device that is capable of quantitative detection with high reproducibility and without variation in the circumferential direction even in the case of a rod-shaped deployable element or a deployable element provided with a spirally detoured deployment path.

Conventionally, there have been rod-shaped deployment elements in which a thin layer of an adsorbent or a distributing agent is provided on the surface of a long support such as a rod or a tube.

A conventional method for detecting a substance developed by a rod-shaped deployment element involves moving the deployment element or a detection device in the axial direction of the element to sweep and detect one side of the deployment path of the element. For this reason, it is not possible to detect variations in the development along the circumferential direction of the development path.
It was not possible to perform highly accurate detection.

Furthermore, the present inventors have proposed a deployment element having a spirally detoured deployment path on the surface of a long support (Japanese Patent Application No. 56-121-520). This deployment element has a long deployment path compared to the element dimensions, and it is possible to achieve efficiency in the deployment operation, such as miniaturization of the deployment tank and easier control of the vapor pressure of the developing solvent. However.

There is no suitable method for detecting the developed substance, and highly accurate quantitative detection cannot be performed without relying on visual detection.

This invention was made by paying attention to the above-mentioned problems. The gist of this is that in a device for detecting a developing substance using a chromatography method, a rod-shaped developing element is used, the developing element is rotatable around its axis, and the rotation is performed in order to sweep and detect the deployment phase of the developing element. This is a detection device characterized in that the detector or the unfolding element can be moved in the element axis direction following the detection device.

The deploying element used in this detection device is a uniformly deployable amateur device which is made by uniformly deploying a thin layer 1 of adsorbent or distributing agent on the surface of a long support such as a rod or tube as shown in FIG. , a spirally developed element B in which a spiral thin layer 2 is provided on the surface of an elongated support with curves surrounding it in a spiral, as shown in FIG. 2, or a spiral thin layer with two or three or more strips as shown in FIG. The detection device of the present invention usually uses a flame ionization detector, but other than this, a detector that transmits visible light, ultraviolet light, reflects light, or uses fluorescence can also be used. It can be used.

A description will be given below based on an example of the embodiment of this detection device shown in the drawings.

In FIG. 4, this detection device consists of a deployment element drive section 3 and a detector drive section 4. The unfolding element drive unit 3 has a chuck 5 and a motor 6, and the element 7 gripped by the chuck 5 is driven by the motor 6 via a gear 8° 81 and is rotatable about the element axis. The detector drive unit 4 includes a support base 9 and a flame ionization detector 10 fixed thereon.
The support stand 9 is provided with a linear gear on its lower surface (
(not shown), the element 7.0 can be moved in the axial direction by means of the motor 11 via the gear 12.12'. The flame ionization detector 10 consists of a lower hydrogen flame burner 15 and an upper ion collector 14 that form a pair, and a burner 13.
The element 7 is arranged between the collector 14 and the collector 14.

The motor 6 of the deployment element drive section 5 and the motor 11 of the detector drive section 4 are controlled by a differential input type operational amplifier 15 to rotate, and the detector 10 is moved in the element axis direction in accordance with the rotation of the element 7. .

For example, when spiral element B is used as element 7, detector 1
The detection position of 0 moves along the development path of the spiral thin layer 2,
The entire unfolding path can be swept and detected. Also, for example, if a uniformly developed amateur is used as element 7, element 7
The entire circumferential surface of the element 7 is swept by controlling the running speed of the detector 10 with respect to 0 rotation speed so that the detection position forms a spiral with a pitch equal to the detector detection width (in the element axis direction). Can be detected. The results detected by the detector 10 in this way are passed through a single human-powered operational amplifier 16 to a Ben recorder 1.
7 is recorded in the chart.

The apparatus shown in FIG. 5 is also an embodiment of the present invention.

In this case, the deployment element drive unit 3 is placed and fixed on the support stand 18, and the foot support stand 1B is driven by the motor 19 to drive the gear 20.
, 20', it is possible to run in the axial direction of the element 7 attached to the chuck 5.

Further, the element 7 attached to the chuck 5 can be rotated by the motor 6 about the υ axis. In this device,
Fluorescence detector 2 consisting of an ultraviolet light emitting section 21 and a light receiving section 22
3 is fixed above the element, and the element 7 rotates around its axis and moves in the axial direction in accordance with this rotation to cover the entire development path of the uniform thin layer 1 of the element or the spiral thin layer 2 of the element B. The peripheral surface can be scanned and detected by the fluorescence detector 23.

The apparatus shown in FIG. 6 is also an embodiment of the invention.

This device consists of multiple chucks 5+, '5*...
..., and is driven by one motor 24 via the υ belt 25 and attached to the chuck 5.
'! ... can be rotated around its axis. The detector 10 fixed to the upper surface of the support stand 9 is movable in the element axis direction as in the case of the fourth @, and the support stand holder 26 that supports the support stand 9 from below is perpendicular to the axis of the element 7. It can be moved by riding on the rails 27.27. Therefore, after sweeping and detecting the deployed peripheral surface of one element 71 from the distal end to the proximal end, the position of the detector 10 is
1, and the detector 10 is positioned beyond the tip of element 7.
The element 7.2 is moved to the distal end position of element 7.2, and moves from the distal end of element 7□ toward the proximal end to perform sweep detection of element 7.2. This can be repeated to continuously sweep and detect multiple elements. Also, instead of moving the detector in the direction perpendicular to the element axis, multiple chucks are arranged in parallel! 5. ,5. ... Even if the group is moved in a direction perpendicular to the element axis, similar effects can be obtained.

In the detection device according to the present invention, it is preferable to use pulse motors for the motors that drive rotation or travel because the movement can be accurately and easily controlled. Furthermore, when the proximal end of the deploying element is gripped by a chuck and rotated, the distal end may be supported by a removable spring type bearing or the like to prevent the distal end from curling.

(Example) Developing element: diameter 10 mm, length 6 (] m+, silica gel powder was sintered on the surface of a glass rod support made by Ilex
A helical expansion element B was used, in which a thin film with a thickness of 0.11111% and a width of 2 m was spirally provided.

Developed sample: phenyltrimethylamine, triyneoctylamine, laurylamine mixture Development: After loading 1μ of the sample onto a thin film located 10m from the end of the developing element, place it in a test tube with an inner diameter of 15111II+ and a height of 80cm,
Add 1 ml of developing solvent to the bottom, and after developing for about 30 minutes,
The developing element was dried in a conventional manner and transferred to detection.

Detection: The detection device shown in FIG. 4 was used. The expansion element is 1
The flame ionization detector was rotated for 5 seconds, and the flame ionization detector was run from the tip to the base at a speed of 15 seconds to create a spiral development phase of 22.5 seconds.
Sweep detection was performed in seconds and the results were recorded on a chart, allowing for highly accurate and efficient detection.

The present invention has the above-mentioned features and is capable of detecting a substance spread using a rod-shaped spreading element with high accuracy and efficiency.

[Brief explanation of drawings]

Figures 1, 2, and 3 are side views of a uniform deployable element, a spiral deployable element, and a double helix deployable element that can be used in this device, and Figures 4 and 5 are side views of a detector traveling type and an element, respectively. FIG. 6 is a schematic perspective view of the entire traveling type device, and FIG. 6 is a schematic plan view of an embodiment of the detection device capable of continuously detecting a plurality of parallel deployed elements. A.. Uniform development element, B. Town spiral development element, C.. Compound spiral development element, 1.. Uniform thin layer, 2.. Spiral thin layer, 3..
Deployment element drive unit, 4...detector drive unit, 5...chuck, 6...motor, 7.7. ．． 7.・Development element,
8, 81...Gear, 9...Support, 10...Flame ionization detector, 11...Motor, 12.12'...Gear, 13...Hydrogen flame burner, 14...Ion collector, 1511・OP Amplifier, 16a 60p amplifier, 1
7. Pen recorder, 18. φ support stand, 19. Fist motor, 20, 20'... Gear, 21. Light emitting part, 2
2...Light receiving section, 23...Fluorescence detector, 24...Motor, 25...Belt, 26...Support pedestal, 27...Rail. Patent applicant: Asahi Kasei Industries, Ltd. Figure 1 Figure 5 Figure 6

Claims (1)

[Claims] (11) A detecting device for a developing substance using a chromatography method, in which a rod-shaped developing element is used, the developing element is rotatable around its axis, and the developing phase of the developing element is swept. A detection device used in a new chromatography method characterized in that a detector or a developing element can be moved in the element axis direction to follow the rotation for detection. (2) A plurality of developing elements are arranged in parallel. Claim 1, characterized in that the parallel deployment element group or the detector is movable in a direction perpendicular to the deployment element axis so as to be able to detect a plurality of deployment elements in succession. Detection device used in the new chromatography method described in Section 1.