Patent Publication Number: US-4059769-A

Title: Starting material radiation source for Mossbauer investigations of tellurium compounds

Description:
This is a divisional of application Ser. No. 554,705, filed Mar. 3, 1975, now U.S. Pat. No. 4,004,970. 
    
    
     BACKGROUND OF THE INVENTION 
     The present invention relates to radiation sources adapted for Mossbauer investigations of chemical compounds employed for investigating structures of chemical compounds, studying chemical transformations of organic and inorganic chemical compounds as well as for analytical applications and in industry. 
     More specifically, the present invention relates to a radiation source for Mossbauer investigations of tellurium compounds. 
     Known in the art are radiation sources for Mossbauer investigations of tellurium compounds such as the binary tellurium compounds Zn 67  Te 125m  and PbTe 125m  and such sources as Sb 125  in Cu, l 125  and β --Te 125m  O 3 . 
     There are various methods of preparing such radiation sources. In the preparation of sources such as ZnTe and PbTe after the production of a chemical matrix from inactive compounds such as Zn 67  Te 124  and PbTe 124 , the matrix is exposed to irradiation in a reactor by means of thermal neutrons, whereafter, to eliminate radiation defects, the matrix is annealed at a temperature within the range of from 400° to 500° C for a period of from 1 to 3 hours. 
     Sources made of Sb 125 , l 125  and β--Te 125m  O 3  require pre-irradiation of an isotopic raw material in a reactor, followed by special radio-chemical synthesis to obtain a required chemical form of the source. 
     The prior art sources and the methods of preparing the sources feature some disadvantages, among which the most essential are the following: 
     1. Sources such as ZnTe and PbTe, Sb 125  in Cu have but a small probability of Mossbauer effect which, even at the temperature of liquid nitrogen, does not exceed 0.2 and at room temperature is at most 0.05. Furthermore, these sources have, as a rule a widened emission line as compared to the natural one (2Γ n  = 5.3 mm/sec) which is due to difficulties of obtaining a strict stoichiometric composition of these compounds used as a chemical form of the sources. 
     Sources using l 125  also have a small probability of Mossbauer effect and may be used only in emission spectroscopy. 
     2. The source β--TeO.sub. 3, though having good Mossbauer parameters, is difficult to prepare. To produce it, one should perform a complex radio-chemical synthesis of an unstable compound, viz. β--TeO.sub. 3 which already at a temperature of about 100° C is transformed into other modifications, whereby the effect becomes less pronounced and the emission line is widened. Moreover, to prepare this compound, conditions of a specialized radio-chemical laboratory are necessary. 
     SUMMARY OF THE INVENTION 
     It is an object of the present invention to provide a radiation source for Mossbauer investigations of tellurium compounds with a high probability of Mossbauer effect and a natural width of the emission line. 
     This object is accomplished in that the radiation source for Mossbauer investigations of tellurium compounds is prepared, in accordance with the present invention, on the basis of a chemical compound of tellurium, viz. 5MgO.Te 124  O.sub. 3. 
     The process of preparing the radiation source is by way of irradiating a chemical compound of tellurium in a reactor by means of thermal neutrons, followed by annealing this compound, which according to the present invention is 5MgO.Te 124  O.sub. 3, and annealing is performed at a temperature within the range of from 600° to 1,100° C for a period of from 5 to 10 hours. 
     It is preferred, however, to perform the annealing at a temperature within the range of from 900 to 1,000° C for 6 hours. 
     The radiation source for Mossbauer investigations of tellurium compounds prepared in accordance with the present invention on the basis of 5MgO.Te 124  O.sub. 3 has a high probability of Mossbauer effect equal to 0.20 at room temperature and therewith 0.51 at the temperature of liquid nitrogen; therewith, it has a natural width of the emission line. The method of preparing this radiation source is readily accessible for practically any laboratory and, which is most important, does not require a radiochemical synthesis under specialized conditions. For this purpose, it is necessary to prepare, once, a stable nonradioactive compound 5MgO.Te 124  O.sub. 3 in the required amount and to irradiate the compound in the reactor as necessary. 
     DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT 
     Given hereinafter is a description of the preferred embodiment of the method of preparing a radiation source for Mossbauer investigations of tellurium compounds based on 5MgO.Te 124  O.sub. 3. The latter compound in a powder-like form is placed into a quartz ampule to be irradiated in a reactor. The flux of thermal neutrons and the irradiation time depend on a desirable source activity. It is advisable that the source activity be within the range of from 10 mC to 10 C at a flux of thermal neutrons of from 10 13  to 10 15  thermal neutrons/cm 2 .sec, while the irradiation time per se is varied from 10 hours to 1,000 hours. In doing so, a radioactive compound of 5MgO.Te 125m  O.sub. 3 is produced. After irradiation, the radioactive compound 5MgO.Te 125m  O.sub. 3 is annealed at a temperature within the range of from 600° to 1,100° C for a period of from 5 to 10 hours and then gradually cooled to room temperature. The annealed finely-divided powder of 5MgO.Te 125m  O.sub. 3 is uniformly distributed over the surface of a substrate using an adhesive such as BF-2 as a binder and coated with an aluminium foil on a cement. At this stage the procedure of making a radiation source is finished. 
     A method of preparing the above-mentioned compound 5MgO.Te 124  O.sub. 3, if it is not available, contemplates a simple chemical synthesis. As the starting material therefore use is made of a stable isotope Te 124  (with a high enrichment of Te 124 , i.e. about 90% and above). The synthesis is effected in the following manner: 
     
         Te.sup.124 + 3H.sub.2 O.sub.2 + 5MgSO.sub.4 + 10 KOH → 5 MgO.Te.sup. 124 O.sub.3 + 5K.sub.2 SO.sub.4 + 8H.sub. O 
    
     5mgO.Te 124  O 3  in the form of a residue resulting from the reaction is dried at a temperature of from 120° to 140° C for 1 hour and then calcined for 2 hours at 1000° C. Thereafter the compound is ready to be irradiated in the reactor. 
    
    
     For a better understanding of the present invention, the following are specific Examples illustrating the method of preparing the radiation source according to the invention. 
     EXAMPLE 1 
     A weighed portion of 165 mg of ground Te 124  was placed into a 100 ml beaker and mixed with 3 ml of a 5N solution of KOH. The mixture was heated to a temperature of 60 to 70° C and a 30% solution of H 2  O 2  was added thereto under stirring. Therewith, an intensive oxidation of the tellurium occurred with the formation of K 2  H 4  TeO 6  which is completed after 10-15 minutes; the excess of hydrogen peroxide is then decomposed by heating at reflux. The potassium tellurate solution was diluted with distilled water to 50 ml and gradually mixed with a solution of 1.63 g of magnesium sulphate (MgSO 4 .7 H 2  O) in 30 ml of water. In doing so, a mixture of magnesium tellurate with magnesium hydroxide precipitated. To minimize the adsorption of impurities and enlargening of the precipitate particles, the mixture was boiled, right after precipitation, for 10-15 minutes and the residue, without allowing the mixture to be cooled, was separated on a dense paper filter under suction. The residue was washed with several portions of hot water till no SO 4   =   ions were detected. Then, the residue was washed with 10 ml of absolute ethanol and 40-50 ml of diethyl ether, whereafter air was purged therethrough for 5-10 minutes. The residue was dried at a temperature of from 120° to 140° C, placed into a corundum crucible and calcined for 2 hours at a temperature within the range of from 900° to 1,000° C. The calcined residue of 5MgO.Te 124  O 3  was ground, sealed into a quartz ampule and irradiated for 360 hours in a reactor with a flux of 3 to 10 13  thermal neutrons/cm.sup. 2 sec. The resulting 5MgO.Te 125m  O 3  was annealed at a temperature within the range of from 900 to 1,000° C for 6 hours, whereafter it was gradually cooled to room temperature. 
     As a result, a radiation source was obtained with an activity of 100 mC and with a natural width of the emission line. 
     EXAMPLE 2 
     A weighed portion of 500 mg of ground Te 124  was taken for the experiment. Further operations were performed in accordance with the procedure of Example 1, excluding the manufacture of the source 5MgO.Te 125m  O 3  per se. To this end, a weighed portion of 100 mg of 5MgO.Te 124  O 3  was placed into a quartz ampule. Irradiation was effected in the reactor with a flux of thermal neutrons of 8·10 4  thermal neutrons/cm.sup. 2 sec for 500 hours. Annealing of the resulting 5MgO.Te 125m  O 3  was conducted at a temperature of 800° C for 7 hours. Further operations were similar to those of Example 1. 
     Two sources were prepared from the thus-prepared active compound: the former with an activity of 1C for experiments of nuclear coherent dissipation on tellurium single cyrstals and the latter with an activity of 200 mC for experiments on resonance absorption. 
     EXAMPLE 3 
     The experiments in this Example performed in accordance with the procedure of Example 1, with the only difference that annealing of 5MgO.Te 125m  O 3  was conducted at a temperature of 600° C for 10 hours. 
     As a result, a radiation source was obtained with activity of 100 mC and with a width of the emission line slightly more than the natural one: 2 Γ =  6 mm/sec.