MXPA97004434A - Device for conducting electrochemical measurements in glass or fundi sales - Google Patents
Device for conducting electrochemical measurements in glass or fundi salesInfo
- Publication number
- MXPA97004434A MXPA97004434A MXPA/A/1997/004434A MX9704434A MXPA97004434A MX PA97004434 A MXPA97004434 A MX PA97004434A MX 9704434 A MX9704434 A MX 9704434A MX PA97004434 A MXPA97004434 A MX PA97004434A
- Authority
- MX
- Mexico
- Prior art keywords
- tube
- further characterized
- noble metal
- heat
- reference electrode
- Prior art date
Links
- 239000011521 glass Substances 0.000 title claims abstract description 9
- 238000002848 electrochemical method Methods 0.000 title claims description 4
- 235000005459 Digitaria exilis Nutrition 0.000 title 1
- 240000008570 Digitaria exilis Species 0.000 title 1
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 32
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 14
- 239000000956 alloy Substances 0.000 claims abstract description 14
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 14
- 239000000155 melt Substances 0.000 claims abstract description 14
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000575 Ir alloy Inorganic materials 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 239000011780 sodium chloride Substances 0.000 claims abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N al2o3 Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- 238000007654 immersion Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 210000001736 Capillaries Anatomy 0.000 claims description 7
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910000599 Cr alloy Inorganic materials 0.000 claims description 5
- 239000007784 solid electrolyte Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000001808 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 14
- 235000008733 Citrus aurantifolia Nutrition 0.000 abstract 1
- 235000015450 Tilia cordata Nutrition 0.000 abstract 1
- 235000011941 Tilia x europaea Nutrition 0.000 abstract 1
- 239000004571 lime Substances 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 241001392754 Calliostoma iridium Species 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- XIKYYQJBTPYKSG-UHFFFAOYSA-N [Ni].[Ni] Chemical compound [Ni].[Ni] XIKYYQJBTPYKSG-UHFFFAOYSA-N 0.000 description 1
- WZOZCAZYAWIWQO-UHFFFAOYSA-N [Ni].[Ni]=O Chemical compound [Ni].[Ni]=O WZOZCAZYAWIWQO-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- -1 chromium-nickel Chemical compound 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Abstract
The present invention relates to a device for conducting electromechanical measurements in glass or molten salts having at least one indicating electrode and a reference electrode arrangement. To be able to conduct very accurate measurements, the tip of the indicator electrode made to immerse in the melt is made of a noble metal or a noble metal alloy with at least one of the other noble metals, preferably iridium or an iridium alloy with another noble metal, and it is sealed gas tight in a heat resistant tube. The indicator electrode is passed through the lime-resistant tube
Description
DEVICE PRRfl CONDUCT ELECTROCHEMICAL MEASUREMENTS IN GLASS OR FUNDIDRS SRLES.
BACKGROUND OF THE INVENTION
The invention relates to a device for conducting electrochemical measurements in glass or molten salts with at least one indicator electrode and a reference electrode arrangement. Such devices are widely known, especially from GB 2 057 695. Plquí, a measurement of the partial pressure of oxygen takes place by means of an electrochemical measuring cell, also called the reference electrode arrangement, which is connected to ? n counter electrode (indicator electrode) through? n typical indicator and / or evaluation means (measurement system). A platinum wire is used as an indicator electrode, which passes through a body of aluminum oxide. The platinum wire is freely exposed at the tips of the aluminum oxide body, so that it can come into contact with the melt as soon as the counter electrode is immersed in it. The aluminum oxide body is mounted on a + aluminum oxide bulb. In practice, it has become apparent that it is not possible to create a gas-tight seal by means of lead between the platinum electrode and the aluminum oxide body. In this way, the oxygen in the atmosphere above the melt penetrates the part of the indicator electrode which remains in contact with the melt, so that the values measured there do not correspond to the actual conditions within the melt, and the measurements by so + o are wrong. Similar measurement arrangements are known, for example, to par + from DE 38 11 915 01. Thus far, the indicator electrode is made of platinum. The determination of iron, sulfur or chromium melts by means of vol + arnetp co analysis with three electrodes is known, for example, from Glastech, Ber. Glass Sci. Technol.
68 (9), pages 273-277 (1995). Even here, the mentioned problems occur. For example, in this way the size of the electrode surface in the glass must be known exactly.
BRIEF DESCRIPTION OF THE INVENTION
Starting from the devices known from the prior art, an object of the present invention is to improve the accuracy of the measurement of, for example, measurement of partial pressure of oxygen in glass or molten salts. According to the invention, the object is achieved with the tip of the indicator electrode made of a noble metal or an alloy having two or more noble metals and mounted gas-tight in a heat-resistant tube designed to be submerged in melts, of this mode the indicator electrode is passed through the heat-resistant tube (out of the melt and into the evaluation medium) A gas-tight rnon-i means that oxygen does not penetrate through the tube from the outside to the melt q? e is to be measured (especially a glass melt) in an amount such as to influence the measurement. The noble metal or noble metal alloy may be selected from metals of the iridium, platinum, palladium, rhodium or alloy group of at least one of these metals with at least one other noble metal (possibly also from this group). Preferably, the noble metal or the alloy thereof is iridium or an iridium alloy with at least one other noble metal. Iridium and iridium alloys have a high melting point and for this reason they can be connected in a gas-tight manner to the heat-resistant tube by means of heat-based treatment. Advantageously, the heat-resistant tube can be a quartz glass tube. In the case of iridium and iridium alloys, ceramic tubes, for example aluminum oxide, are also possible. When using a ceramic tube, of course it is necessary that the material is not an ion or electron conductor at temperatures of approximately 1000 to 1500 ° C. Iridium or iridium alloys can be sintered or fused properly into the heat resistant tube. Iridium has a melting point of 2447 ° C. This maintains the heating that is necessary for the dense casting or sintering of aluminum oxide or for softening the quartz glass. For other noble metals or alloys of noble metals with lower melting points, the fusion of the metal tip in a quartz glass tube is appropriate. It is reasonable to use indicator electrodes especially for short-term measurements in the case of a fusion in a quartz glass tube, while the indicator electrodes that are melted or if they are not placed inside aluminum oxide tubes can also be used for measurements at a long term (with the so-called continuous exams). It is convenient that it be gas-tight for the connection between the indicator electrode and the heat-resistant tube at the tip of the tube intended for immersion. The tube can be opened backwards, away from the melt. It is also convenient that the tip of the indicator electrode, which is made of noble metal or noble metal alloy, be made inside the tube with a measuring wire, preferably made of molybdenum, tungsten or a nickel and chromium alloy (e.g. , cronix). In this way, the length of the metal wire used as an electrode can be kept short to save noble metal. In the case where the measuring wire is made of molybdenum or tungsten, it is possible to install a strip of molybdenum metal on the tip of the indicator electrode which is made of noble metal or noble metal alloy and the measuring wire. The connection between the noble metal and the measuring wire can be melted in a heat-resistant tube. In particular, a molten strip of rnolybdenum metal ensures that it is almost perfectly airtight to the gas. A chrome-nickel wire can not be melted in the heat-resistant tube without much difficulty, since there is a danger that the tube will melt at the required temperature. Therefore, the connection should preferably be arranged before the melting point in the tube. It is advantageous for a high precision measurement that a reference electrode can be arranged in a solid capillary tube, closed at one end, which is mounted on a ceramic tube with its end moving away from the closed end through the which is passed the reference electrode. It is also advantageous that the end of the reference electrode in the solid electrolyte capillary tube is surrounded by a reference material which is made of a metal-metal oxide, preferably a mixture of nickel-nickel powder oxide. The reference electrode itself is suitably made of an alloy of chromium and nickel. It is still more convenient that the heat-resistant tube and the ceramic tube are filled with corundum. In addition, it is advantageous that the heat-resistant tube and the ceramic tube are mounted on a common conveyor tube, which is preferably made of ceramic and has a connection piece of the usual type at the end moving away from the immersion end. for mechanical coupling and for connection of the indicator electrode and the reference electrode with a measuring system. The transporter tube can be made of aluminum oxide and can be filled with corundum spheres.
BRIEF DESCRIPTION OF THE DRAWINGS
The above summary, like the following detailed description of the preferred embodiments of the invention, will be better understood when read in conjunction with the accompanying drawings. For the purpose of illustrating the invention, they are shown in two embodiments of the drawings, which are currently preferred. However, it should be understood that the invention is not limited to the precise arrangements and the means shown. In the drawings: Figure 1 shows a representation of the device of the invention; Figure 2 is a longitudinal section through the device of the invention; Figure 3 is a longitudinal section through the indicator electrode fused in the heat resistant tube; and Figure 4 is a section through a device with three electrodes.
DETAILED DESCRIPTION OF LR INVENTION
The device for measuring the partial pressure of oxygen, shown in Figure 1, has a conveyor tube 1, which is made of aluminum oxide. A connecting piece 2 is arranged in the conveyor tube 1 at the end moving away from the immersion end, which is inserted in a support (not shown in the figure), for example a metal rod. The wires that pass through the conveyor tube 1, the measuring wire 3 and the reference electrode 4 are connected through the connecting piece 2 with a measuring system, this means with a common indicator and / or an evaluation unit . Inside the conveyor tube 1, the measuring wire 3 and the reference electrode 4 is passed through the quartz glass capillary tubes 5 and inserted into spherical or ball-shaped corundum 6. At the end of the device facing the immersion end of the conveyor tube 1 are the disposition of the reference electrode 7 and the quartz glass tube 8 as a heat-resistant tube. The arrangement of the reference tube 7 has a ceramic tube 9 of aluminum oxide, through which the reference electrode 4 is passed to the capillary tube of solid electrolyte 10. The solid electrolyte capillary tube 10 of zirconium oxide which it has inside it, as a reference material, a mixture of nickel nickel-oxide powder, in which the electrode 4 is mounted, which is made of a chromium-nickel alloy (cronix). The indicator electrode with the Meter wire 3 is passed through the quartz glass tube 8. Tip 11 of the indicator electrode is made of iridium wire. However, it can be made of another noble metal or a noble metal alloy, preferably an alloy containing predominantly iridium and other noble metals. The iridium tip 11 projects into the quartz glass tube 8. The tip 11 melts gas-tight at the end 12 of the quartz glass tube 8 over a length of about 2 cm. After this, the indicator electrode material changes. To save on the relatively high cost of the iridium wire, the remainder of the indicator electrode is a measuring wire 3 made of cronix (chromium and nickel alloy). For example, measuring wire 3 can be used instead of cronix molybdenum or tungsten. Another possibility of construction of the indicator electrode is shown in figure 3. Here, the iridium tip 11 inside the quartz glass tube 8 is connected to a strip of molybdenum 13, which is connected at its other end to the measuring wire 3. In this case the measuring wire 3 can, for example, be made of molybdenum or tungsten. In the example shown, the strip of molybdenum 13 is completely melted at the end 12 of the quartz glass tube 8. In this way, it can be achieved that it is perfectly hermetic to the gas. The possibility of driving the molybdenum strip 13 out of the molten-closed end 12 of the quartz glass tube 8 and first connecting it with the measuring wire 3 in the open tube is not represented in the figures. In that caseIt would also be possible to use cronix as the measuring wire 3. The quartz glass tube 8 and the ceramic tube 9 are provided with corundum packing which stabilizes the position of the wires inside the tubes. The device shown in FIG. 4 is suitable for voltammetric measurement, for example, of the content of iron, sulfur or chromium in a molten glass. The procedure for this is described, for example, in Glastech. Ber. Glass Sci. Technol. 68 (9), p. 273-277 (1995). An indicator electrode and a reference electrode 4 are disposed on the aluminum oxide transport tube 1. The tip 11 of the indicator electrode is made of iridium and melts in a quartz glass tube 8. The reference electrode 4 of platinum is arranged in a ceramic tube 9, and a platinum counter electrode 14 is disposed at the immersion end of the conveyor tube 1. Measurement with the described device makes it possible to have very reliable results, first and foremost in operations to short term. Because the device can be manufactured very economically, it is possible to make a disposable examination (? N use). When an aluminum or aluminum heat resistant tube 8 is used, long-term use is also conceivable. Those who are experts in the art will realize that changes can be made to the modalities described above without departing from the broad concept of invention thereof. Therefore, it is understood that this invention is not limited to the particular embodiments described, but is intended to encompass modifications within the spirit and scope of the present invention as defined by the appended claims.
Claims (3)
- NOVELTY OF THE INVENTION CLAIMS 1. - A device for conducting electrochemical measurement in glass or molten salts, comprising at least one indicator electrode and a reference electrode arrangement, further characterized in that a tip (11) of the. Proposed indicator electrode for the immersion in the melt is made of a noble metal or a noble metal alloy with at least one other noble metal, where the tip (11) is gas-tight mounted in a heat-resistant tube (8) , and where the indicator electrode is passed through the heat resistant tube (8).
- 2. The device according to claim 1, further characterized in that the heat-resistant tube (8) is a quartz glass tube.
- 3. The device according to claim 1, further characterized in that the noble metal or noble metal alloy is melted in the heat-resistant tube (8). * • "The device according to claim 1, further characterized in that the connection between the indicator electrode and the heat-resistant tube (8) at one end (12) of the tube (8) intended for immersion in the melt It is gas tight. 5. - The device according to claim 1, further characterized in that the tip (11) is connected with a measuring wire (3) inside the heat resistant tube (8). 6. The device according to claim 5, further characterized in that a metal band (13) of molybdenum is arranged between the tip (11) and the measuring wire (3). 7. The device according to claim 6, further characterized in that the measuring wire (3) is made of molybdenum or tungsten. 8. The device according to claim 5, further characterized in that the connection between the tip (11) and the measuring wire (3) is melted in the heat resistant tube (8). 9. The device according to claim 5, further characterized in that the measuring wire (3) is made of an alloy of chromium and nickel. 10. The device according to claim 1, further characterized in that the arrangement of the reference electrode comprises a reference electrode (4) arranged in a capillary tube of solid electrolyte closed at one end, the capillary tube at the opposite end to the The closed end is mounted on a ceramic tube (9) through which the reference electrode (4) is passed, and wherein one end of the reference electrode (4) in the solid electrolyte capillary tube (10) is surrounded by a reference material which comprises a mixture of nickel and nickel oxide powder. 11. The device according to claim 10, further characterized in that the reference electrode (4) is made of an alloy of chromium and nickel. 12. The device according to claim 10, further characterized in that the heat-resistant tube (8) and the ceramic tube (9) are filled with spherical corundum. 13. The device according to one of claim 10, further characterized in that the heat-resistant tube (8) and the ceramic tube (9) are mounted on a common conveyor tube (1) having a connecting piece (2) at the end moving away from the immersion tip for the mechanical coupling and for connecting the indicator electrode and the reference electrode and the reference electrode (4) with a measuring system. 14. The device according to claim 13, further characterized in that the conveyor tube (1) is made of aluminum oxide and filled with spherical corundum (6). 15. The device according to claim 13, further characterized in that the conveyor tube (1) is made of ceramic. 16. The device according to claim 1, further characterized in that the noble metal or noble metal alloy is selected from the group consisting of iridium, platinum, palladium, rhodium and alloys thereof. 17. The device according to claim 1, further characterized in that the noble metal or the noble metal alloy is iridium or an iridium alloy with at least one of the other noble metals. 18. The device according to claim 17, further characterized in that the heat-resistant tube (8) comprises ceramic. 19. The device according to claim 18, further characterized in that the ceramic comprises aluminum oxide. 20. The device according to claim 18, further characterized in that the iridium or the iridium alloy is sintered or melted in the heat resistant tube (8).
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19623683A DE19623683C1 (en) | 1996-06-14 | 1996-06-14 | Device for carrying out electrochemical measurements in glass or salt melts |
| DE19623687.8 | 1996-06-14 | ||
| DE19623683.5 | 1996-06-14 | ||
| DE19623687A DE19623687C1 (en) | 1996-06-14 | 1996-06-14 | Inexpensive precision electrochemical measuring probe |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| MX9704434A MX9704434A (en) | 1998-07-31 |
| MXPA97004434A true MXPA97004434A (en) | 1998-11-09 |
Family
ID=
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