Tritium-marked nanodiamonds and method of obtaining thereof

FIELD: chemistry.

SUBSTANCE: method of obtaining tritium-marked nanodiamonds by method of thermal activation of tritium includes preparation of water suspension of nanodiamonds with average size of particles not more than 125 nm and content of dispersive phase from 0.15 to 0.6 mg, uniform application of obtained suspension on walls of vessel, which contains placed with possibility of electric current connection tungsten filament for tritium activation, with the following lyophilisation and air removal. In the process of carrying out reaction with atomic tritium temperature of walls of reaction vessel is supported in the range 291- 298 K, with its bottom being cooled to 77 K. Introduction of gaseous tritium and its activation on tungsten filament is carried out for 5-15 sec, after which remaining tritium is removed. Stage of introduction of gaseous tritium and its activation is repeated from one to eight times. Obtained are tritium-marked nanodiamonds, in which tritium is bound with nanodiamond by C-H bond, characterised by specific radioactivity not less than 1 TBq/g.

EFFECT: improvement of characteristics.

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The technical field

The invention relates to isotope-labeled substances and can be used for injection of radioactive label in nanodiamonds of detonation synthesis to study their behavior in various systems, including biological.

The level of technology

In the biochemical and physico-chemical studies are widely applied tritium-labeled substances as an indicator of their number. Method of introduction of tritium label in physiologically active compounds using the method of thermal activation of tritium was first used in [Shishkov A. C., Filatov, E. S. Simonov, E. F. and others, " Dokl. THE USSR ACADEMY OF SCIENCES. 1976. So 228. S. 1237-1241]. Currently this method is used for the introduction of tritium label in various organic substances. The method was used for injection of radioactive label in humic substances with uniform distribution of tritium components of a complex mixture of molecules comprising the composition of these substances [Badan, A., Pozdnyakov C. Yu, M. Chernyshova,, Kulikova N. A., Perminova, I. C., Schmitt-Kopplin F. a Method of obtaining tritium-labeled humic and humanophobia substances. Patent for invention No. 2295510. Application No. 2005139586. Priority of invention 19.12.2005]. Typical conditions for the introduction of tritium into the molecules of substances of different classes using the method of thermal activation of tritium: the temperature of the walls of the reaction with the UDA 77 K (liquid nitrogen cooling), the gas pressure in the system is 0.5 to 2 PA, the temperature of the atomizer (tungsten wire) 1500-2000 K, the exposure time from 10 seconds to several minutes.

In the works [Alcobev C. N., Eremenko, L. A., Mazanova A. A. Pronin, A. S., Beketova D. H., Dyadischev N. R., Borovik R. C., Kuchava L. D., Chervonohrad S. P., Burchak, F., Baden, A., Tasto H. A., M. Chernyshova, / / Sat. abstracts of scientific-technical sections of the international forum on nanotechnology. 2008. S. 314-315] and [A. G. C. // Int. the scientific. proc. "Nanostructured materials-2010: Belarus-Russia-Ukraine". Mat.-Kyiv. 2010. S. 538] shows the principal possibility of introducing a radioactive label in carbon nanomaterials using the method of thermal activation of tritium examples of carbon nanotubes and nanodiamonds. Also was shown the possibility of using such substances in physico-chemical [butchers I. Y. // International. the scientific. proc. students, postgraduates and young scientists "Lomonosov". 18-I. - M. 2010; Yakovlev RJu., Badun G. A, Chernysheva M. G., Selezenev N. G., Leonidov N. B. // Int. Symp."Modern problems of surface chemistry and physics". Kyiv. Ukraine. 2010. P. 439-440; M. G. Chernysheva, I. Yu. Myasnikov, G. A. Badun // Mend. Comm. 2012. V. 22. P. 290-291] and biochemical [Alcobev B. H., Eremenko, L. A., Mazanova A. A., Beketova D. H., dyadischev N. R., Rybalkin S. P., Kuchava L. D., Baden, A., Chervonohrad S. P., Muradyan C. E., Maslikov A. A. // Nanotechnology and health. 2011. So 3, No. 2. C. 16-23] study is the be.

Described in the prototype [Yakovlev R. Ju., Badun G. A, Chernysheva M. G., Selezenev N. G., Leonidov N. B. // Int. Symp. "Modern problems of surface chemistry and physics". Kyiv. Ukraine. 2010. P. 439-440; M. G. Chernysheva, I. Yu.Myasnikov, G. A. Badun // Mend. Comm. 2012. V. 22. P. 290-291] tritium-labeled nanodiamonds were obtained in the processing of tritium atoms of the diamond powder. The radioactive label was introduced in the SN-due on the surface of nanodiamond using the method of thermal activation of tritium. The specific radioactivity of the product was 34 GBq/year

The present invention provides a method of obtaining tritium-labeled nanodiamonds with a specific radioactivity of the product was not less than 1 TBq/g for their visualization in different systems.

Disclosure of inventions

The problem to be solved by the authors of the present invention is to develop a method of producing tritium-labeled nanodiamonds with high specific radioactivity.

The technical result of the present invention is to increase the specific radioactivity of tritium-labeled nanodiamond 34 GBq/g to at least 1 TBq/g, in particular to 2.6 TBq/year the Proposed method allows to obtain tritium-labeled nanodiamond tightly bound with the label due to the fact that binding of tritium occurs on connection C-H.

This technical result is achieved due to the fact that the introduction of tritium do not use powder of nd, and the aqueous suspension of nanodiamond with concentration the Oia from 0.15 to 0.61 mg/ml and an average particle size of not more than 125 nm according to dynamic light scattering. In addition, if the reaction tagging part of the vessel not containing nanodiamonds, cooled to a temperature of 77 K, while the walls of the vessel caused by nanodiamonds support at a temperature 290-298, and the atomization of tritium perform a short (5-15 seconds) pulses, which ensures an increase in the specific radioactivity of the labeled product in 30-76 time.

The problem is solved in that a method of obtaining tritium-labeled nanodiamonds by the method of thermal activation of tritium includes: preparation of an aqueous suspension of nanodiamonds with an average particle size of not more than 125 nm and the content of the dispersed phase from 0.15 to 0.6 mg, uniform application of the obtained suspension of the vessel wall with subsequent lyophilization and removal of air, and the said vessel contains installed with the possibility of connecting an electric current tungsten filament to activate tritium, the cooling of the bottom of the vessel, not containing nanodiamonds, to a temperature of 77 K, while the walls of the vessel caused by nanodiamonds support at a temperature 290-298, the introduction of gaseous tritium and activation of a tungsten filament within 5-15 seconds, the removal of residual tritium.

Also the problem is solved in that the stage of introduction of the gaseous tritium and its activation is repeated from one to eight times.

A particular variant of this is about of the invention is the above-mentioned method, characterized in that the activation of tritium on the tungsten filament should be performed within 10 seconds.

Also the problem is solved by the provision of tritium-labeled nanodiamonds in which tritium is associated with nanodiamond by C-H-bond, which is characterized by the specific radioactivity of not less than 1 TBq/year

A particular variant of the present invention are mentioned above, tritium-labeled nanodiamonds, which are characterized by specific radioactivity, equal to 2.6 TBq/year

For the introduction of tritium in nanodiamonds their suspension contribute in the reaction vessel of cylindrical form, are distributed uniformly on the walls, quickly frozen and the water removed by lyophilization under vacuum. Further procedures are to remove air from the reaction vessel at a special vacuum unit for operation with gaseous tritium. Gaseous tritium putting into the reaction vessel through a palladium filter, purifying the tritium from helium and other gases. Atomization of tritium carried out by heating a tungsten wire by an electric current of up to 2000 K at a gas pressure of 1-1,5 PA. To increase the radioactivity of nanodiamonds reaction stopped after 5-15 seconds, remove residual gas, putting a new batch of tritium and repeat the procedure label. Processed tritium nanodiamonds extracted from the reaction vessel using water when exposed to the and the walls of ultrasound. The resulting suspension is transferred into a glass flask and the next day the solvent is removed by rotary evaporator. The procedure is repeated 2-3 times, then nanodiamonds suspended in ethanol, transferred into test tubes, centrifuged, take the supernatant and add a new batch of ethanol and centrifugation procedure was repeated once more. These stages of cleaning can completely remove the labile label and radioactive impurities. As a result you can get tritium-labeled nanodiamonds with a specific radioactivity of from 1.0 to 2.6 TBq/year

Implementation of the proposed invention described in the Examples.

The implementation of the invention

Example 1. 0.4 ml of aqueous suspension of nanodiamond concentration of 1.5 mg/ml (0.6 mg) with an average particle diameter of 125 nm were uniformly distributed on the walls of the reaction vessel was frozen and the water removed by lyophilization. The reaction vessel was connected to a vacuum system for operation with gaseous tritium. The air from the reaction vessel was removed to a residual pressure of 0.001 PA. The bottom of the reaction vessel, not containing nanodiamonds, cooled by liquid nitrogen (77 K). The reaction vessel was filled with a mixture of hydrogen and tritium (tritium 27,5%) up to a pressure of 1.3 PA. Heated tungsten wire to 2000 To an electric current for 10 sec. The residual gas was pumped out of the system until the pressure 001 PA, fill the reaction vessel with a new portion of the tritium and repeated the procedure for tagging.

Processed atomic tritium nanodiamond powder suspended in water under the action of ultrasound and was transferred to a glass flask. After 1 day the water kept under vacuum using a rotary evaporator. Added a new portion of water, after 1 day the water drove away. All this procedure was repeated 3 times. Then nanodiamonds suspended in ethanol using ultrasonic treatment, was transferred into a test tube type Eppendorf. After 1 day the suspension was centrifuged for 3 hours, took away the solvent above the sediment and to the residue was added ethanol. After 1 day the procedure was repeated centrifugation. At all stages of the purification of the drug samples were taken suspension and supernatant for measurement of their radioactivity. Following treatment received nanodiamonds, labeled with tritium, which is connected by C-H bond.

The obtained value of the specific radioactivity was 1.0 TBq/g (in terms of 100% tritium), which is 30 times higher than the amount shown in the prototype.

Example 2. The training target of nanodiamonds was performed as in example 1. The tagging procedure was repeated 8 times. Washing of tritium-labeled preparation was carried out as in example 1.

The obtained value of the specific radioactivity was 1.8 TBq/g (in terms of 100% t is iti), in 53 times the amount shown in the prototype.

Example 3. 1 ml of aqueous suspension of nanodiamond concentration of 0.15 mg/ml evenly distributed on the walls of the reaction vessel, froze and was liofilizovane. The procedure for tagging and cleaning of labeled preparation was carried out as in example 2.

The specific radioactivity of tritium-labeled nanodiamonds was 2.6 TBq/g (in terms of 100% content of tritium used in the reaction mixture), which is 76 times higher than the specific radioactivity of the prototype.

1. The method of obtaining tritium-labeled nanodiamonds by the method of thermal activation of tritium, including the preparation of an aqueous suspension of nanodiamonds with an average particle size of not more than 125 nm and the content of the dispersed phase from 0.15 to 0.6 mg, uniform application of the obtained suspension of the vessel wall with subsequent lyophilization and removal of air, and the said vessel contains installed with the possibility of connecting an electric current tungsten filament to activate tritium, the cooling of the bottom of the vessel, not containing nanodiamonds, to a temperature of 77 K, while the walls of the vessel caused by nanodiamonds support at a temperature 290-298, the introduction of gaseous tritium and activation of a tungsten filament within 5-15 seconds, the removal of residual tritium.

2. The method according to p. 1, characterized by the fact that one hundred is the ia injection of gaseous tritium and its activation is repeated from one to eight times.

3. The method according to p. 1, characterized in that the activation of tritium on the tungsten filament should be performed within 10 seconds.

4. Tritium-labeled nanodiamonds in which tritium is associated with nanodiamond by C-H-bond, which is characterized by the specific radioactivity of not less than 1 TBq/year

5. Tritium-labeled nanodiamonds under item 4, characterized by the specific radioactivity, equal to 2.6 TBq/year



 

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