CN1425129A

CN1425129A - Sample testing

Info

Publication number: CN1425129A
Application number: CN00818569A
Authority: CN
Inventors: 尼古拉斯·布拉德肖
Original assignee: Individual
Current assignee: Individual
Priority date: 1999-11-25
Filing date: 2000-11-24
Publication date: 2003-06-18
Anticipated expiration: 2020-11-24
Also published as: CN1219200C; WO2001038847A1; ZA200204137B; AUPQ422299A0

Abstract

Method and apparatus for producing a specimen bead in a mouldible (9) for future analysis wherein a halogen gas is passed over the surface of the specimen whilst molten to increase surface tension thereof thus enabling the bead to be released from the mouldible. A furnace (1) has a cradle (8) to support the mouldibles (9) and an injector (12) delivers halogen gas through nozzle 17. Alternatively, a halogen source may be located in the cap or lid of the mouldible.

Description

Sample testing

The present invention relates to sample testing, more particularly, relate to the preparation of the sample that is used for analytical test.

The mineral sample that is used to test in preparation or when having processed the mineral sample, the mineral sample is preparation like this, promptly, the need of specified quantity are handled sample (by volume or weight) to be mixed mutually with the flux (flux) of for example lithium tetraborate or lithium metaborate and so on, and in a heating furnace, potpourri is heated, use the sample that generation will be analyzed subsequently.Then, will be placed in sample in carbon, gold or platinum mould or the mould (mouldible) is put in the heating furnace and heats.Yet so serious problem is arranged: the potpourri of fusion can adhere to the inside surface of mould or mould, can not be shaped and discharge a bead-like body that is used for next analyzing (bead) or specimen sample.For overcoming this problem, can in sample, introduce the capillary reagent that release agent maybe can increase melted material.Yet these materials can pollute sample, and then have a strong impact on the accuracy of sample analysis.

Also have, often need in heating, stir sample lentamente, to guarantee that material and flux mix fully, if the sample of fusion adheres to or tends to adhere to the inwall of mould or mould, then bubble be may in sample, produce, sample microscope, X ray and other inspection carried out thereby seriously influence.

As mentioned above, well-known is can adopt release agent when preparation bead shape X.R.F. sample.Used reagent is the compound of halogens group normally, and halogenide (being fluorine, chlorine, bromine, iodine) is active component.These reagent add in the fused mass with the form (for example sodium bromide, ammonium iodide, potassium iodide and hydrobromic acid) of compound.

Yet release agent can become the part of sample subsequently, often is to react with out of contior mode and sample in some cases, thereby causes sample that undesirable variation takes place, and then causes analyzing inaccurate.

Therefore, the objective of the invention is to, a kind of method and apparatus that is used to overcome one or more problems of above-mentioned prior art is provided.

Test is performed such, and, in heating and/or fusion process, and/or in the cooling procedure of mixing and/or fusion bead-like body, specimen surface is added pure halogen gas that is.Found that under this mode, halogen can not become the part of sample or reaction with it.

Test is carried out with iodine, can provide the system of iodine to test to two.One of them system generates iodine gas from solid-state iodine, and in heating and mixed process, this gas is transferred into specimen surface.

Second kind of system transmits iodine gas to its surface when the fusion bead-like body cools off.

These two systems all are satisfactory, depend on the sample of being tested, and can test with one of them or two systems a sample.

Therefore, the invention provides a kind of method that needing to be used for the sample of test material and flux mould manufacturing, described method comprises the steps: the surface of the sample that is in molten condition in the described mould is applied a halogen, to reduce the surface tension of fusion sample, this can carry out in the fusion process in heating furnace, and/or carries out after taking out from heating furnace.

According to the present invention, a kind of heating furnace that is used for manufacturing test with sample also is provided, described heating furnace has: one is used to admit the device of a mould, contains the material and the flux that need test in the described mould, uses the generation sample; Heating arrangement in the heating furnace; And be used to that halogen gas was sprayed or the device on the surface by fusion or partial melting sample, use the surface tension that improves melted material, thereby produce a sample bead-like body that can not adhere to the mould inwall.

Preferably, described halogen is a gaseous iodine.

Preferably, described mould is stirred lentamente, and iodine gas periodically flows through the surface of melted material.

In another kind of form of the present invention, comprise the steps: after mould is taken out from described heating furnace, the surface of melted material is applied halogen gas.

Preferably, the present invention also comprises the steps: mould is taken out from heating furnace, part to end cap applies the iodine that is solution or solid form, this end cap is put on the mould, heat in mould and the sample makes the surface evaporation of halogen species at sample, vaporized gas contacts with the specimen surface of fusion, uses and improves its surface tension.

Below in conjunction with accompanying drawing the present invention is described better, in the accompanying drawing:

Fig. 1 is the stereographic map that can be used for a heating furnace of the present invention;

Fig. 2 is the view of the part after the lid of heating furnace is raised;

Fig. 3 is a kind of cut-open view of iodine thrower of form;

Fig. 4 (a), 4 (b) and 4 (c) are the cut-open views of another kind of form iodine thrower;

Fig. 5 is the view of mould and end cap;

Fig. 6 is the view that is placed in the end cap of the another kind of form on the mould;

Fig. 7 is the cut-open view of the end cap on the mould;

Fig. 8 is the view of the thrower of another kind of form; And

Fig. 9 is the cut-open view of thrower shown in Figure 8;

At first see also Fig. 1 and 2, wherein show a heating furnace 1, this heating furnace has a lid 2 that is used to seal its inner chamber 3, and in the case, inner chamber 3 is heated by electrical equipment (not shown).Lid is supported by the parallel rod 4 around pivoting point 5, uses that lid is flushed with heating furnace upper surface 7.Be provided with handle 6, use making the lid lifting.The inner chamber of heating furnace comprises that one can hold the carriage 8 of a plurality of moulds 9, this bearing bracket is on pivot 10, one of pivot can be by motor and crank-driven, thereby carriage can be vibrated or swing lentamente, uses sample can be mixed fully in its heating and melting stage.Heating furnace comprises several pallets 11, at the cooling stage of sample, mould can be placed on these pallets.

Heating furnace comprises a thrower 12, uses the halogen that is the iodine gas form to the sample transmission.Fig. 3 shows a kind of form of thrower.Solid-state iodine can be put into a groove 13, these iodine are by the heating of an electrical equipment 14, and described electrical equipment is by lead 15 power supplies.Can pass through air pipe line 16 air supplies, these air can be blown into the iodine of gaseous state the top of mould 9 by nozzle 17.This thrower 12 comprises that also one is positioned at the reverberator 18 of electrical equipment 14 tops.

As mentioned above, carriage can be vibrated or be swung, when the top of opening wide of mould faces toward nozzle, one control module (not shown) starts electrical equipment so that the evaporation of a part of iodine, and cause one air to flow through the surface of iodine, collect iodine gas, and make iodine gas enter the top of opening wide of mould, and then arrive the surface of sample.

Fig. 4 (a) and 4 (b) show the thrower 26 of another kind of form, and its structure is comparatively simple, is easy to iodine is added in the thrower.Thrower 26 has a body 27, and this body has a bottom of opening wide, and this bottom is by a ship shape part or a channel 28 sealings, and body 27 also has an inlet attack 29 that is used for supplying with injection air.Body is supporting electrical equipment 30 and electric connection terminal 31,32.One reverberator 33 is positioned at the top of element 30, so that will guide to iodine downwards from the heat of this element.Iodine is placed in ship shape part or the channel 28, and this ship shape part can put in place by the securing member that passes hole 34 is fastening, and a sealing ring 35 is sealed in body 27 with ship shape part or channel 28.

Fig. 5 (a) and 5 (b) have shown the second embodiment of the present invention, show mould 9 and the end cap or the lid 19 that are placed on the mould 9.The lower surface of lid has a liquid keeper cavernous body or a gauze 20 in order to keep a small amount of iodine.Lid has one and is positioned at the flange 22 that edge 21 and on the mould 9 is resisted against the mould upper flange.This lid or end cap have one handle 2, and this handle is made of disk 24 that be used to cool off, the space, and these disks are isolated by heat-barrier material 25 and flange 22.

When mould was taken out from heating furnace, lid or end cap tegmentum were on mould, and the iodine in the metal sponge is by heat of vaporization remaining in mould and the sample, and when sample cooled off, iodine gas was stopped in the mould, up to lid is opened.

Fig. 6 shows the end cap 36 of the another kind of form that is used for mould 9.End cap 36 has two parts, i.e. inner cap 37 and enclosing cover 38.These two parts are separated by a clearance 39, mutually combine by a latching 40 that is positioned on the metal sponge 41 in their upper end simultaneously.Metal sponge 41 is resisted against the upper end of inner cap, and enclosing cover is also passed in a hole that covers in latching passes, and a nut 42 keeps together inner cap and enclosing cover.

Inner cap has an edge part 43 that can enter mould, and a upright flange 44.The end 45 of enclosing cover terminates in the top of flange 37, so that a gap 46 to be provided.Enclosing cover has an air intake 47 that leads to air nozzle 48.In use, end cap is put on the mould, and air supply pipe is connected in air intake.Airflow is gone into around the space between inner cap and the enclosing cover, thereby makes enclosing cover and inner cap isolated effectively, therefore, in the time end cap must being taken off, can catch enclosing cover that end cap is removed.

Fig. 8 and 9 shows the thrower 50 of another kind of form.This thrower 50 comprises that a body part 51, one evaporation cavities 52 and a nozzle 17 are connected in this body part.Evaporation cavity 52 comprises an air jet hole 53 and air supply flexible pipe 54.One electrical equipment 55 is connected in supply lines 56.Thrower 50 has the locking collar 57 and a latching 58, so that this thrower is installed in the heating furnace.The end of evaporation cavity 52 is installed with electrical equipment 55 by a chock plug 59 sealing on this chock plug, and have an attached air hose 54 connect mouth 60.Chock plug 59 is detachable, and it is held in place by a locking latching 6.During use, chock plug is removed, a certain amount of iodine crystal is put into the bottom of evaporation cavity, then chock plug is put back to.Preferably, heating element is a lampet, and enough heats can be provided this lamp so that the iodine crystal evaporation.By lamp, can protect heating element to avoid the corrosive attack of iodine gas.

This shows that the invention provides a kind of system, wherein the analysis that is generated does not have bubble with bead-like body, and can not stained by release agent material.In the melting stage, (demoulding) releasing agent of for example halogen gas and so on is supplied to the surface of fusion sample, this can carry out in the heating of sample and mixed process, perhaps can carry out the process of the cooling in that sample is taken out from heating furnace.

Though describe various forms of the present invention above in detail, be appreciated that the present invention is not limited to these details, but can comprise variation and the remodeling that falls in the present invention's spirit and the essential scope.

Claims

1. method that make needing to be used for the sample of test material and flux at mould, described method comprises the steps: the surface of the sample that is in molten condition in the described mould is applied a halogen, to reduce the surface tension of fusion sample, this can carry out in the fusion process in heating furnace, and/or carries out after taking out from heating furnace.

2. the method for claim 1 is characterized in that, described halogen is a gaseous iodine.

3. one kind is used for the heating furnace that sample is used in manufacturing test, and described heating furnace has: one is used to admit the device of a mould, contains the material and the flux that need test in the described mould, uses the generation sample; Heating arrangement in the heating furnace; And be used to that halogen gas was sprayed or the device on the surface by fusion or partial melting sample, use the surface tension that improves melted material, thereby produce a sample bead-like body that can not adhere to the mould inwall.

4. heating furnace as claimed in claim 3 is characterized in that, described halogen is the iodine of gaseous state.

5. as claim 3 or 4 described heating furnaces, it is characterized in that, also comprise being used for the device that sample slowly stirred at mould.

6. as each described heating furnace in the claim 3 to 5, it is characterized in that, also comprise being used to make halogen gas periodically to flow through the device of sample.

7. heating furnace as claimed in claim 6 is characterized in that, the device that is used to make halogen gas periodically flow through sample comprises a thrower.

8. heating furnace as claimed in claim 7 is characterized in that, described thrower comprises the heating arrangement that is used to make the iodine evaporation, and the device that is used to provide the air that periodically flows through thrower.

9. the method for claim 1 is characterized in that, also comprises the steps: mould is taken out from described heating furnace, and the surface of the sample of molten condition is applied halogen gas.

10. method as claimed in claim 9 is characterized in that, also comprises the steps: the inner chamber of an end cap is applied solid-state or liquid halogen species, and this end cap is put on the mould, and the heat in mould and the sample makes the surface evaporation of halogen species at sample.

11., it is characterized in that described halogen gas is selected from iodine, fluorine, chlorine and bromine as claim 1,2,9 and 10 described methods.