SU1497535A1 - Apparatus for making specimen holder for x-ray fluorescence analysis of solutions - Google Patents

Abstract

The invention relates to the analysis of materials by sodic-physical methods, in particular, to the preparation of samples for X-ray fluorescence analysis. The goal is to improve the quality of the holder. The device is made in the form of an overturning table, on the working plane of which there is an annular slot for the flow of hydrophobic material from the tank, which is in contact with the heater. A wedge-shaped ledge with a chamfer is made around the gap. On the working plane of the table there are centering and clamping means. 1 il.

Description

The invention relates to the analysis of materials by nuclear-physical methods, in particular, to the field of sample preparation for X-ray fluorescence analysis.

The purpose of the invention is to increase the quality of the holder.

The drawing schematically shows the device, the cross section.

The tilting table 1 has an annular slit 2 on the working surface with a wedge-shaped annular protrusion 3 formed by protruding edges of the annular slit 2 and directed perpendicular to the working surface of the table 1. The wedge-shaped annular protrusion 3 is provided with a bevel at the top that eliminates its cutting properties. From below, removable tank 4 is hermetically attached to table 1, for example, by means of a threaded joint. To the bottom of the tank 4 attached removable heater 5 in the form of low-power stove. The cavity of tank A communicates with the annular gap 2 through channels 6. Coaxially with the annular gap 2 on table 1, the centering ring 7 and clamp 8 are mounted on top. Ring gap 2 is made in the form of a gap between the walls of the axial hole in table 1 and the COE installed in this hole, for example , with

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by means of a threaded joint, an inverted cup 9. The channels 6 are made; in the form of several through holes evenly spaced in the walls of the cup 9 in the gap between the connecting thread and the bottom of the cup 9. The tightness of the connection of the tank 4 with the table 1 is provided with a sealing gasket 10. The centering ring 7 is installed by putting the centering ring on the bottom of the working surface table 1, located outside the annular gap 2, with a small effort, ensuring the centering ring 7 maintains its position when tilting 1. The centering ring 7 is provided with an upper-sided outboard 11, the dimensions of which ensure the edge of the paper disk 12 located inside the centering ring 7 with a pair of tweezers. The clamp 8 is made in the form of a spring-loaded piston 13 in the glass 14. The glass 14 with its open side is fixed on the second (peripheral) cylindrical ledge of the working surface of the table 1, equipped with a tag insulating gasket 15, made in the form of a flange attached to the ledge by means of, for example, countersunk screws or heat-resistant glue, and having the thread for attaching the cup 14. The piston 13 for pressing against the wedge-shaped annular protrusion 3 is provided with a flat elastic gasket 16 made, for example, of Teflon. The outer dimensions of the pressing (lower) part of the piston 13 ensure its free passage through the centering ring 7. C. the opposite side of the piston 3 has a rod. 17 with the compression spring 18 attached to it, the end of the stem 17 goes out through the axial hole in the bottom of the cup 14 and is connected to the lever 19 by means of an axis 20 and a notch 21 at the end of the lever 19, providing the lever 19 with a given free stroke. The support for the lever 19 is the bracket 225 located on the edge of the bottom of the glass 14 from the outside. The lever 19 and the bracket 22 are connected by a supporting axis 23. The outer end of the lever 19 is equipped with a heat insulating handle 24. On the side opposite to the lever 19, a side cutout 25 is made in the wall of the glass 4;

the passage through it of the centering ring 7 and the paper disk 12. The Upper Leg edge 11 of the centering ring 7 mounted on table 1 is directed toward the side cutout 25, Table 1 is equipped with two side symmetrical semi-axes 26, located 1zimi- on one line intersecting the longitudinal the axis of the table 1 at a right angle ,, and located in the same plane with the lever 19 and the bracket 22. With the help of semi-axes 26, the table 1 is attached to two support posts 27 mounted on the base 28. The rack 27 located under the lever 19 is made extended to e on the longitudinal axis in the upper free position of the lever 9. The height of the position of the table 1 above the base 28 ensures unimpeded tilting of the table 1 relative to the axes 26 together with the tank 4 attached to it, the heater 5, the clamp 8 at an angle of about 180 ° until the lever 19 stops against the base an extended stand 27. The upper part of the extended stand 27 is provided with a longitudinal notch 29 for positioning and moving the lever 19 therein from the free upper to the lowermost positions corresponding to the range of movement of the pores n 13 in the glass 14. The elongated rack 27 is provided with a hook 30, whose size and location provide putting the hook 30 on the lever 19 finds schiys at the lowermost position in the recess 29.

The device works as follows.

The tank 4 (together with the heater 5 attached to it) is removed, filled with low-melting hydrophobic material and again attached to the table 1 using a gasket 10 to seal the joint. A heater 5 is turned on, which creates in the tank 4 a temperature sufficient to melt the low-melting hydrophobic material and keep it in a liquid state during operation of the device.

The device is reset to its original position (with the annular gap 2 upwards) by moving the lever 19 to the longitudinal section 29 of the elongated support 27, using a free stroke at the junction of the lever 19 with the rod 17, providing the required additional

raising the lever 19 (not less than half the height of its cross section) above the elongated strut 27 as it is transferred to or from the longitudinal notch 29. In this position of the device, the rotation (swinging) of the table 1 relative to its semi-axes 26 5 interfering when working with clamp 8 is excluded. Press down the heat-insulated handle 24 of the lever 19, which, lowering in the longitudinal notch 29, raises the piston 13 in the glass 14, thereby opening access to the annular gap 2 and the centering ring 7 through the side cutout 25. A paper disk 12 is placed in the centering ring 7 and the heat insulating handle 24 of the lever 19 is released. Under the action of the compression spring 18, the lever 19 moves to its upper free position, and s 13 is lowered in the glass 14 and tightly presses a paper disk 12 to wedge the annular flange 3 of the annular gap 2 of its resilient gasket 16. Thus the force provided constancy and uniformity of paper disk 12 to compress the wedging annular flange 3

The lagging (in Crown from the annular slit 2) is limited, which ensures the constant dose of the low-melting hydrophobic material and the same size of the restrictive ring for each paper disk. The heat insulating handle 24 of the lever 1 located in the longitudinal notch 29 is again pressed to allow access to the paper disk 12 through the side cut 25. Grip the edge of the paper disk 12 accessible through the upper side of the centering ring 7 and remove the paper disk 12 s with tweezers a restrictive ring deposited on it from the centrifugal ring 7 and clamp 8. The resulting paper disk (sample) is ready for

analytical application. If necessary, the open position of the col-, virgin slit 2 (for example, for cleaning it from contamination) can be fixed by hooking the hook

30 to the lever 19, which is in the longitudinal notch 29 in the lowest position.

The use of the proposed device provides stada, rt {-s

and their alignment. At the same time, the work does not take place, namely, the coaxiality wakes up the paper with a wedge-shaped annular protrusion 3, since it is provided with a bevel. Holding the heat-insulating handle 24, remove the lever 19 using a free move in place: its connection with the rod 17, from the longitudinal notch 29 and the rotational movement relative to the semi-axes 26 overturn the table 1 together with the elements attached to it up to the stop of the lever 19 into the base of the extended stand 27 and immediately return table 1 to its original position. In the upturned position of table 1, molten low-melting hydrophobic material due to its own weight flows out of reservoir 4 through channels 6 and annular slit 2 into a section of paper disk 12, adjacent to wedge-shaped annular protrusion 3, on this section of paper disk 12 along both sides of the annular gap 2, the paper is sealed with a wedge-shaped annular protrusion 3 (with its symmetrical halves) concentrating on the paper the force of the spring -18 grip. Therefore, the penetration of low-melting hydrophobic material into the pores of the paper in this area in the radial direction of the disk and the ring neck, the constancy and uniform distribution of the force of pressing the paper disk to the wedge-shaped ring protrusion, the dose of the low-melting g and the fiber-repellent material to obtain the restrictive ring.

In addition, the device has become convenient and productive because manual operations are excluded — applying a low-melting hydrophobic material to the end of the tube, centering the paper disk and pressing it to the end of the tube by using a reservoir with a reserve of fusible hydrophobic material and an annular gap on the tilting the time for resuming a dose of low-melting hydrophobic material in the zone of formation of a restrictive ring after each working cycle was significantly reduced; nna device is ready to work for a long time and economical consumption fusible hydrophobic material.

The proposed device can be used in conjunction with X-ray fluorescence spectrometers

quality (type SPARK, CPM) or foreign (firms ARL, PHILIPS, etc.) mass production.

Claims (1)

Invention Formula A device for the manufacture of a sample holder for X-ray fluorescence analysis of solutions, including an annular cliche and a heater, in which, in order to improve the quality of the holder, the annular cliche is made in the form of A table with an annular slit, the working surface of which is provided with a wedge-shaped protrusion around the slit, equipped with a chamfer, centering ring and clamp, an additional reservoir is inserted, hermetically connected to the table from the side opposite to the working surface, provided with channels, connecting it with the annular gap, while the table is made with the possibility of tilting.