Manufacture of high purity alpha mercuric iodide

[Detailed Description of the Invention]

Field of the Invention the X-rays to which the present invention operates with ambient air temperature, and gamma ray radiation -- a spectrum -- it is related with the manufacturing method of the 2nd mercury of high purity alpha iodination used as a starting material for growth of the 2nd mercury single crystal of alpha iodination which can be used for manufacture of the total and a detector. Conventional technology □ In order to manufacture X-rays, a gamma ray radiation spectrum photometer, and a detector, the 2nd mercury of high purity alpha iodination for attaining growth of an alpha-HgL single crystal without the defect which has the ingredient ratio completely controlled by high purity is required. In order to obtain a satisfying result, it is important that a single crystal does not have a trapping center of a low level in a prohibition belt. It is because a Charge career will be captured at the center of a low level. Trapping center - of a low level generally produces by content of the impurities which arise during the error about the ingredient ratio of a single crystal, and plastic deformation (transposition) or growth of a single crystal. The manufacturing method of alpha-Hg I 2 single crystal which makes it possible to control the ingredient ratio of a single crystal and to make plastic deformation into the minimum is publicly known. Although the method is indicated in the France patent application box No. 7916418 dated June 26, 1979, the solution which dissolved t1gI2 in 2nd mercury [ of alpha iodination ] many crystals, organic Sulfoxide currently beforehand refined by electrolysis, and methanol is used as a starting material. According to the method, the crystal of satisfying character can be obtained, but it is desirable to use the many crystals of high purity for crystal growth, and to improve the character of a single crystal further further. It is because there are still too many impurities contents of metallic, the quality of nonmetallic, and the quality of organicity during the many crystals obtained from the element of high purity by the conventional synthesizing method. alpha Boss which can be used for quality crystal growth (the refining method of gI2 is also known.) Although the method is indicated to the France patent application No. 2316192, The 1st process of compounding the 2nd mercury of iodination from mercury and iodine, the 2nd purification process including repeating and sublimating the 2nd mercury of iodination obtained by composition, and the 3rd purification process including Zone Melchi, Inc. of the 2nd mercury refined by sublimation of iodination are included. However, the method has many faults which are described below. a) In dry type composition, since there is danger of explosion, the quantity of alpha-11g12 which cannot obtain a lot of alpha-HgL, therefore are obtained by the method is restricted to 100 g by one charge. b) Since there is much number of times of sublimation and a zone Melchi ink process, execution is difficult, and efficiency and yield are bad. In order to obtain the thing of high purity, 6~30 continuous sublimation and 30~100 zone-melting operations are required. C) The efficiency of the impurities separation in a sublimation process is low. It is because, as for almost all organic impurities, 1g of alpha Boss form 12 and a stable complex and their steam pressure of the complex corresponds with the steam pressure of alpha-11gI2 mostly at the sublimation temperature of 100~140 degreeC. Therefore, these complexes are sublimated and condensed with alpha-Hg I 2. Similarly, organic impurities are not partially disassembled at the temperature used for sublimation. In the 2nd mercury single crystal of alpha iodination which is refined by analysis of a mass spectrum by repetition of sublimation, and is obtained with vapor phase epitaxy in this way, they are at least 10 elements (C, N, 0.AA, Ca.). Mn, Na, K, Cr, and Fe are contained, and organic impurities are seven sorts of hydrocarbon groups (C11, C2H). Having decomposed at high concentration comparatively became clear to C3H5, C3H, C, H4, C, H7, C, and H8. It is because the analytical value was averaged and is over the 50~1100pp atom per each element and hydrocarbon group. d) Since the steam pressure of a zone melting of fusion HgI2 is high, it is difficult to carry out. Especially Hg12 [ refined by sublimation ] contains a lot of organic impurities, and it disassembles the impurities, It is because gas-like output with a possibility of breaking the A seal pipe containing lIgL which produces carbon and a tar suspension thing inseparable depending on a zone melting, and should be refined by overpressure is produced. The 1st process that other refining methods are known, re-crystallizes the method by about 100 degreeC from alpha-Hg 12 saturated chloride solution (1:1), and it refines, The thermochemical '" -- distillation (vacuum evaporation is carried out by about 200 degreeC, and the 2nd process of 400~5 (l1gI2 steam is overheated by 10 degreeC, and, subsequently alpha-HgI 2 is condensed by 40~50 degreeC) and the 3rd purification process repeatedly sublimated by 120~130 degreeC are comprised.) However, there are many faults which are stated also to this method below. a) Chlorine is mixed in output. b) Output is nonstoichiometric (it is rich in Hg). C) It is necessary to sublimate the last 6~8 times at a sublimation speed very low [ o'clock ] 2g /, and the whole yield is also only 10~12%. The object of an invention The object of the present invention is to provide the manufacturing method of the 2nd mercury suitable for making it possible to conquer the fault of the conventional method mentioned above, and to remove all impurities (metallic, quality of nonmetallic, and quality of organicity) by good efficiency or yield, and carrying out on an industrial scale of high purity alpha iodination. Constitution of an invention That is, if it says in more detail, the present invention will compound the 2nd mercury of a alpha iodination, h) Give the 2nd obtained mercury of alpha iodination to the refining processing which comprises at least 1 time of the vacuum distillation process performed by at least 255 degreeC, and it is the distillation process, It is carried out in the reaction machine which has three continuous fields maintained at a different temperature, and is maintained by the vacuum with a vacuum pump, The 1st field is maintained at the triple point temperature of alpha-f 1gI2, i.e., 255 degreeC, and the 2nd mercury of alpha iodination that should be refined in it is put in, The 2nd field is maintained at 255~300 degreeC, the 3rd field is maintained at a temperature lower than other two fields in order to condense the 2nd mercury of alpha iodination that evaporated, namely, the 3rd field provides the manufacturing method of the 2nd mercury of high purity alpha iodination that comprises carrying out air cooling. After distillation is completed, alpha-1gI2 crystallized into the wall of the 3rd field of a reaction machine are collected. Generally, several distillation is performed and the crystal of the 2nd mercury of alpha iodination obtained by the last condensation is used in each distillation cycle, respectively. The number of times of distillation is usually 6~12 times. By performing this vacuum distillation process, the impurities of Okay. are removed and it becomes possible to control the stoichiometric composition of the 2nd mercury of iodination simultaneously. In this way, it exists in the form of the complex of HgI2, most inorganic impurities which have the steam pressure which is equal to the steam pressure of 11gI2 decompose by 255~300 degreeC, and the steam pressure of the decomposition output becomes lower enough than the steam pressure of HgL. As a result, these impurities remain in the bottom and side wall of a reaction machine as a residual substance. Similarly, organic impurities are also disassembled at this temperature and it is N2.+ (the gas of 20, N2.NH3, CH, Co, and Co2 grade is eliminated with a vacuum pump, and carbon or tar of a certain kind remains into a residual substance.). The distillation based on the difference of impurities and the partial pressure of Hg12 is more effective than the sublimation only based on the difference of impurities and the steam pressure of Hg12. In this way, it Existence 1 as an iodide in a residual substance, and distillation is i. Na K, Mg Ca Cr (U) Mn nickel. P which exists as Co, Ag, Ba, Ph, A1 and SI that exist as silicate, and a B1 phosphate which exists as borate salt -- it is very effective in As which exist as salt, Ti which exists as an oxide, and Zr# calling and removing ■. Re to which similarly distillation exists as an iodide in a residual substance (In), Cu (1), Zn, Cd, and 5n(II). It is effective also in order to separate S and Se which exist as HgS and HgSe, respectively. Since Lynn, boron, and iodine are volatility very much, these are condensed as PI3, BI3, and I2 by the trap cooled by the liquid nitrogen between a pump and a reaction machine, respectively. The fluoride, chlorine, and bromine which exist rather than HgI2 in the form of halogenation mercury which is volatility are partially condensed in a trap. The same may be said of titanium and tin (IV) and mercury (1) which exist as an iodide. A.I. Artificial Intelligence and Si in which distillation exists as an iodide, Cr (III), and 2As -- it V# calls and is not so effective in separation of 2r. It is because these iodides have the steam pressure which is equal to t1gI2. In this way, the method of the present invention is very effective. According to one advantageous feature of the method of the present invention, composition of the 2nd mercury of alpha iodination is performed by making mercury and iodine react in the organic Sulfoxide solution containing methanol. The reaction is performed in the quartz reaction machine for semiconductors with the ambient air temperature of about 20 degreeC. The iodine which has the high purity, i.e., the purity of m5N5, dissolved in the organic Sulfoxide solution of the spectrophotometrical purity containing mercury of high purity, i.e.,n [ m7 ] purity, and methanol of electronic purity was used. In order to avoid the rise in heat of solution, mercury is gradually added until it cools with water and all iodine is consumed, agitating. As for the solution, it is preferred that iodine is superfluously included as compared with a quantity required in order to obtain HgI2 of stoichiometric composition. As for molar ratio [organicity Sulfoxide]/([Sulfoxide]10 [methanol]) in the solution used for the composition, it is advantageous that it is within the limits of 0.6~0 and 8. In this way, 11g of saturated solutions of 12 are obtained, and in order to enable refining by next distillation, 11gI2 is recoverable from the saturated solution at the time of the end of the operation, by making it precipitate by a usual state method, for example, underwater. Although the composition mentioned above is desirable for obtaining the thing of high purity, it is possible to follow the present invention and to compound the 2nd mercury of alpha iodination also by other methods, for example, the composition in solution, a double exchange reaction, or dry type composition. According to the present invention, the obtained output passes through the refining processing which comprises at least 1 time of a vacuum distillation process next. As for the 2nd mercury of alpha iodination, if the present invention is followed, before performing the distillation process, it is preferred to pass through the interim electrolytic refining processes in the state where it dissolved in organic Sulfoxide, and/or the interim re-crystal process of the 2nd mercury of alpha iodination from the organic Sulfoxide solution of the 2nd mercury of iodination. The solution used for electrolytic refining and a re-crystal contains methanol like the solution used for composition. It is made for Mol Specification [Sulfoxide] ([Sulfoxide]10 [methanol]) /to serve as the range of 0.6~0.9 for electrolytic refining in addition of methanol. Electrolytic refining processes can also be directly performed using t1gI2 saturated solution obtained when compounding from mercury and iodine in solution. If the present invention is followed, electrolytic refining processes will be performed so that less than 100microScm-' may become with the minimum degree of conduction of solution, i.e., 20 degreeC. The refining is C, E, and A on June 26, 1979. It is advantageous to carry out under the conditions indicated in the France patent application box No. 7916418 for which it applied "Be alike." If modification of the present invention is followed, it is possible to use for electrolytic refining the 2nd mercury solution of alpha iodination prepared by dissolving the 2nd mercury single crystal of alpha iodination collected from l1gI2 saturated solution obtained by composition by precipitation in organic Sulfoxide and methanol. In this case, in order to settle l1gI2, conductivity water is added to the saturated solution. Precipitation is filtered, and it dissociates and carries out true 5 sky dryness by 80 degreeC, using the quartz container for semiconductors. Electrolysis is a method effective in refining HgI2 by removing all the impurities that have dissociated in electrolysis in solution. Since the organic impurities originating in iodine composition do not dissociate in electrolysis, they are inseparable by electrolysis. In order to attain purity satisfying at the time of the end of electrolytic refining processes, it is desirable to perform several cation separation operations, several anion separation operations, i.e., 8~24 cation separation operations, and 2~6 anion separation operations. Alpha-Hglz is collected by making it precipitate using water, as mentioned above after the electrolytic refining processes. As for this process, although the alpha-HgI 2 ranks next and it passes through a vacuum distillation process, it is desirable to carry out after the interim refining processing which consists of re-crystallizing from the organic Sulfoxide solution containing methanol. As for molar ratio [Sulfoxide]/([Sulfoxide]10 [methanol]), it is desirable that it is the range of 0.1~0.2. A re-crystal is usually performed within the limits of 65 degrees C~15 degreeC. From the fact to say that the increase in the solubility of l1gI2 in the solution as six functions of temperature is restricted, A container with two fields maintained at the temperature from which this re-crystal differs, i.e., the 1st dissolution field, is heated by 60~65 degreeC, and the 2nd re-crystalline region is performed in the reaction machine maintained below at about 15~20 degreeC. The reaction machine used may have a double wall with the quartz reaction machine for semiconductors. The 2nd mercury of re-crystal To be alpha iodination is put into the bottom of the reaction machine, this is heated with water, and, on the other hand, the side wall upper portion of the reaction machine is cooled with cold water. Then, the crystal of alpha-Hg I 2 is dissolving at the bottom, and it becomes a dense lump of many crystals with a size of an average of 2~3 mm, and crystallizes in a side wall part. Movement of a substance takes place automatically by a heat convection. In order to prevent returning 1g of HgL(s) to 2I2, it is preferred to add iodine to re-crystal solution superfluously. In this way, the soluble impurities condensed in solution are removed. However, it is more difficult to remove Cu, Ag, Br, and Cd. It can say that the same may be said of the heavy organicity iodide originating in iodine composition (or HgL used as a starting material). Usually performing several re-crystals, in order to raise purity, generally the number of times is 3~6 times. Organic Sulfoxide which can be used with the solution for composition, the solution for electrolytic refining, and the solution for re-crystal refining if the present invention is followed, They are Dialkyl sulfoxide, such as Dimethyl sulfoxide (DMSO), methylethyl Sulfoxide, Diethyl sulfoxide, and tetramethylen Sulfoxide. Usually, Dimethyl sulfoxide is used. EXAMPLE The example indicated referring to an accompanying drawing below explains the present invention still more concretely. However, how many present invention is not restricted by these examples. Electrolytic refining of the 2nd mercury of being [ this example performs the first synthetic process in the 2nd mercury solution of iodination and / alpha ] the iodination in Sulfoxide, It is related with obtaining the 2nd mercury of alpha iodination of high purity by performing three purification processes which comprise the re-crystal and vacuum distillation of alpha-HgI 2 from the organic Sulfoxide solution of l1g I 2. a) Composition of alpha-11gI2 Composition of alpha-HgL is performed in the 3-liter quartz reaction machine provided with the dropping funnel which penetrates the lid of the stirrer of the direction of an axis, and a reaction machine, or a cap. 26.5 mol of DMSO(s) for spectra (product made from AIdrich) diluted with methanol (MeOII) with an electronic purity of 6.5 mol are put in a reaction machine. At this time, molar ratio CDMSO1/(CDMSO)+ [:Meol-1] is equivalent to 0.8. The iodine 8g atom which has the purity of m5N5 is dissolved in the solution. Subsequently, it adds gradually, agitating the mercury 4g atom which has the purity of m7N. Mercury reacts to iodine at the bottom of a reaction machine, 8gI2 is produced, and this dissolves into solution. A reaction will be ended if all either of the two elements is consumed. Mercury of a little additions is added after an appropriate time, and the terminal point of a reaction is shown by when the color of solution changes from brown to the yellow of straw. then, iodine of an 8g atom and mercury of a 4g atom -- 9 -- it adds again and adds iodine of an 8 moreg atom, and mercury of a 4g atom at the time of the end of the reaction. The solution containing HgI2 [ 12-mol ] is obtained in 24 hours. In order to control or check the chemicals stoichiometry of Hg12 obtained in this way, iodine (0, 5~Ig) of a little additions is added at the end of the operation. In order to remove the white impurities (organic output) of a trace which had appearance like grease and have floated in the surface, it has a filter of quartz and filters the solution on the filter of the degree 4 of porous. By adding and settling 250-mol conductivity water, it is possible to collect solid alpha-f 1gIz from the solution. The sediment which sediments easily is washed while being dropped 6 times with 250-mol conductivity water on the filter which has a filter of quartz, and it is dried within the oven of 80 degreeC under a 1350-Pa vacuum for 48 hours. The 1st column of the attached table expresses the impurities content of the 2nd mercury of alpha iodination obtained in this way. 0 b) Refining by electrolysis Alpha-HgI 2 crystal is again dissolved in DMSO and MeOH solution for the process made from wood alcohol. It is also possible to use directly the saturated solution of the 2nd mercury of iodination obtained at the time of the end of the above-mentioned synthetic process. Refining is performed in the instrument shown in Drawing 1. The instrument comprises 10-liter silica tube 2 of capacity 100 rr+j! which calls globular form flask 1'J3 and constitutes the negative pole space of an electrolysis slot which constitutes the anode space of an electrolysis slot. Stirrer 3 of quartz is formed in an anode room, and negative pole 4 of graphite is provided in a negative pole room. The anode of an anode room comprises superfluous mercury 5 set at the bottom of flask 1, and is connected with the direct current generator with the tungsten wire. Negative pole space is connected with anode space with fritting quartz board 7 which forms a partition. The 2nd mercury solution of iodination that should be refined is introduced into anode space, the voltage of 200■ is applied between two electrodes, on the other hand, in order to restrict temperature to 20 degreeC, quartz coil 8 which crosses a globular form flask is made to circulate through cold water, and the solution is cooled. The above-mentioned current changes between 20~loomA(s). Under such conditions, current is 2nd mercury anion [ of iodination ] [Hgl. As for the cation and a certain grade of]-1 impurities, it is carried by cation l:l1gI]+. All these ion is reactions in a general reaction following type, for example, the case of sodium iodide,: Nal+ 11g12- Na"+[:lIgL : Or [ according to l -, the iodide of impurities forms the 2nd mercury of iodination, and a complex ], Or it is I]"+[l (it produces, when the 2nd mercury of iodination performs Self-complex-ization of a certain kind according to glJ-.) to reaction;28g12-CI-1. In the anode, the 2nd mercury anion of iodination discharges and it supplies iodine. In order to prevent accumulation of iodine, 7N mercury of high purity of raw horse meat is placed on the bottom of a globular form flask, and this reacts to iodine and forms the 2nd mercury of iodination again. Solution is often diluted, in order to avoid super saturation in this case. In the negative pole, the cation of impurities, i.e., Na", K", Re", N12+, Cu", Cu", Cr3+, Ca 2+, Ag", etc. pile up negative pole space 2. A CflgD" cation is discharged, serves as insoluble mercurous iodide mud 9, and precipitates. A certain kind of impurities cation precipitates simultaneously with mercurous iodide mud, or is absorbed into a mercurous iodide. accumulation of the impurities which ionized the electric conduction rate of negative pole space -- 1 -- or it increases double figures. Subsequently, space 2 is used under pressurization and electrolysis is continued. This value is approximate, although the electric conduction rate of anode space decreases gradually as a result of refining and it becomes fixed in 20degreeC at 110microScm-'. 1 (if it is To, it is because an electric conduction rate is affected not only with self-dissociation of the 2nd mercury of active iodination but with the quantity of the ionized mercury salt of the others which accompany the 2nd mercury of iodination, for example as impurities, such as other halogenation things, a nitrate, sulfate, and cyanide.) Refining is continued until the electric conduction rate of negative pole space does not increase any longer or it comes to increase very slowly. Then, if an impurities cation is removed from solution, purity will amount to m6-7N. Impurities 3 In order to also remove an anion, additional refining is performed and the same technique as the above can be performed. However, polarity is made reverse. Thus, in order to attain the good degree of refining, in order to remove a cation, 24 refining operations are performed, and in order to remove an anion, six refining operations are performed. In other examples, eight refining operations are performed to remove a cation and two refining operations are performed to remove an anion. It points out meaning the operation corresponding to a term called refining operation performing electrolysis once in both a cation and anion removal, and subsequently to Partition room 2 carrying out it here. In these examples, each operation is continued for about seven days, and the impurities solution of 1 is obtained 65 m by using Partition room 2 at the time of the end of each operation. It is made to precipitate with conductivity water, as the 2nd mercury of iodination after electrolytic refining operation of these versatility and in solution was mentioned above. The impurities content of alpha-Hgla obtained in this way is an example in the attached table (the 2nd column and the 34th column). c) The re-crystal process of Hg12 This process is performed using the reaction vessel shown in Drawing 2. The reaction vessel is provided with the double wall designed to raise the field of 10a and 10b in a reaction machine to the temperature which changes with circulation of water including quartz container 10. Reflux condenser 11 is formed in the upper part of the reaction machine. alpha-11g 1210 mol obtained in process a, and A JL / upper To [DMSO:] / ([DMSO] + [MeOH]) puts DMSO and 40 mol (1740m Il) of MeOH solution of 0.1 in a reaction machine. If a heat water cycle maintains lower part 10a of a reaction machine at 65 degreeC, the crystal of HgI2 will dissolve in field 10a. Cold-water circulation maintains upper part 10b of a reaction machine at 15 degreeC. In this way, alpha-11gL re-crystallizes as a dense lump on the wall of field 10b of a reaction machine in five days. The efficiency of re-crystal operation is about 95%. If this re-crystal is completed, the solution which remains in field 10a will be removed, and the 2nd mercury of iodination re-crystallized on the side wall of field 10b will be collected. These crystals are again put into the lower part of a reaction machine. New DMSO/ MeOH solution is added and a re-crystal is performed further. Four re-crystal operations were performed in this example. alpha-11g is shown in the 4th column of the table which was refined in this way and which the impurities content of 12 attached. After the last re-crystal operation, before the crystal of alpha-Hg 12 collected by the side wall of field 10b of a reaction machine performs the last purification process by vacuum distillation, it is dried under a 1350-Pa vacuum in the oven of 80 degreeC. d) Vacuum distillation process This process is performed using the device illustrated to three continuous fields 12a and 12b and Drawing 3 containing 3-liter quartz reaction machine 12 which wears and has 12c. Field 12a located in the lower part of a reaction machine can be raised to the temperature of 255 degreeC by electric heating. Field 12b is maintained at 300 degreeC by electric heating, and air cooling of the 3rd field 12c is carried out by the natural convection. The inside of a reaction machine is made into a vacuum with the vacuum pump connected with upper part 13. 125 kg of alpha-Hg is put into field 12a of the bottom of a reaction machine, and it changes into the vacuum state of 10-'Pa by continuation exhaust air. A crystal melts and distillation takes place by 255 degreeC. Steam of HgI2 is condensed on the wall of top field 12c, and the crystal of alpha-11gI2 is formed there. Distillation is continued for about 4 hours. Shortly after the distillation finishes, after [ which removed the residual substance of the 1st distillation ] removing the crystal layer re-crystallized on the wall of field 12c and remaining in the container wall of the bottom of a reaction machine, and middle field 12b, in order to perform 2nd distillation operation, the above-mentioned crystal layer is put into the bottom of a reaction machine. The efficiency of each distillation operation is about 99%, and performs about 12 distillation refining operations. The impurities content of alpha-HgL obtained by 12 distillation refining operations in the attached table is an example. 7 9 8 1: The list of elements under 24 cation refining operations [ eight cation refining operation and two anion refining operations two : ] and first half [ of 6th inning ] anion refining operation expresses all the impurities contained in alpha11gL with the used analysis except for C10, N, and H which cannot be quantified (refer to table). Considering the result given to the table, it can be said that each process of the present invention method is very effective in decreasing the impurities content in the 2nd mercury of alpha iodination. Although all the impurities contents of the 2nd mercury of alpha iodination obtained by the composition in solution were 376 ppm in this way, This impurities content decreases to 19 ppm after the according to 83 ppm and 30 electrolysis in after ten refining operations refining operation by a electrolysis, decreases to 53 ppm after four refining operations by b re-crystal, and decreases into 9 ppm after distillation operation of C12 time. Among the impurities which were not made in fixed quantity with a mass spectrum, there is much C overwhelmingly. C content under compound alpha-Hg I 2 crystal is about 500 ppm. It decreases to about 200 ppm after four re-crystal operations, and is set to only several ppm after 12 distillation operations. When the process from which the method of the present invention differs is performed continuously, it is possible to make alpha-11g of impurities contents of 12 below into 1 ppm after ten electrolysis, four re-crystals, and 12 vacuum distillation. The refining method by the present invention can remove alpha-11g of all the impurities of 12 by combining the three above-mentioned purification processes. In this way, although organic impurities are unremovable in electrolysis, they are removable by a re-crystal and distillation. Cu, Ag. Although 8r and Cd are effectively unremovable depending on a re-crystal, it is removable by electrolysis and distillation. A1, Si, Cr (II[), As. ■ And although Zr is effectively unremovable depending on distillation, it is removable by electrolysis and a re-crystal. Refining alpha-Hg I 2 crystal obtained by the method according to the present invention is put in and saved into quartz, polyethylene, or the bottle of Teflon in inactive gas atmosphere. the crystal can be used as a starting material provided with sufficient pure 1 degree and ingredient ratio for obtaining by growing up the single crystal of the 2nd mercury of alpha iodination that sees in the quality required of nuclear detection, and suits it in the liquid phase or the gaseous phase.

[Brief Description of the Drawings]

Drawing 1 is a figure for explaining the instrument used for electrolytic refining, Drawing 2 is a figure for explaining the instrument used for refining by a re-crystal, and Drawing 3 is a figure for explaining the reaction machine used for refining by vacuum distillation of 11g1. (The main reference numbers) 1: Globular Form Flask 2: Silica Tube 3: Stirrer 4: Graphite Negative Pole 5: Mercury 6: Tungsten Wire 7 : Fritting Quartz Board 8: Quartz Coil 9: Mercurous Iodide Mud 2 IO110a110b= quartz container 11: Reflux Condenser 12.12a, 12b, 12c : Quartz reaction machine 13: Exhaust port applicant for a patent for vacuum pump connection Commissa reata Renel G atomic representative Patent attorney Masahiko Arai