SU1626114A1 - Method of sampling chemically active plastic material and sampling apparatus - Google Patents

Abstract

The invention relates to metallurgy and research methods. The invention allows sampling of mimically active plastic materials while ensuring surface cleanliness while maintaining it for a long time taking a sample from a chilled chemically inert cryogenic ingot liquid by a sampler cooled to a cryogenic temperature. Cooling the sampler can be done by pouring refrigerant as a channel , and in the cavity between the walls of the sampler. After forming a sample in the channel, its ends are cut off by two or more moving blades. and located in the body of the sampler perpendicular or under some distance to the axis of the probe. 2 sec. and 2 z. p. f-ly, 2 ill.

Description

The invention relates to metallurgy and can be used in laboratory and research practice in the selection for the analysis of samples of plastic chemically active materials-metals, alloys, etc.

The purpose of the invention is to increase the representativeness of the sample by ensuring the purity and subsequent protection of the sample surface from oxidation and gaseous media active to the sample.

FIG. 1 shows a device for carrying out the proposed method; in fig. 2 is a section A-A in FIG. one.

The essence of the method is as follows.

Additional cooling of the sampler before sampling is carried out by pouring refrigerant directly into the sampler channel, with the lower opening of the channel covered by the surface of the material from which the sample is taken. This

operation prevents freezing of water, carbon dioxide, etc. on the inner surface of the sampler channel using a chemically inert cryogenic liquid (e.g., liquid apion, nitrogen) both for placing an ingot of the analyzed material, and for cooling the sampler when sampling, and subsequently, prior to its removal, the probe channel leads (as the calculations show) to slowing down the reaction rate, for example, oxygen of the air with the test material L – N) 4 times. Moreover, the specified preparative refrigerant It facilitates the access of aggressive substances (media) directly to the surface (in the Schwessm process, water washes the sample I, which also excludes the possibility of oxidation of both IK fir and sample Hoc.uuiiet, for example, for alkali and alkaline earth metals, such as as their lazy surface, not noi p / kenn n

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inert coolant, vapor and gaseous vapor may precipitate, which after thawing react with it

Cutting off the ends of the sample in the injection channel (the strain allows to completely exclude the possibility of the diffusion contamination of the sample volume from impurities that could be adsorbed or formed on the surface of the spit after preparation before immersion in the refrigerant and remain on the ends of the rod-like sample

The device contains a sampler 1 i a cryostat 2 located under it. Sampler 1 consists of a body 3, having a conical shape below with qi 1 intricate cutting ring and double (forming a cavity 4 with flux 4 to fill the refrigerant, a piston 5 to eject the dust and 3 located in the grooves movable knives 6 The latter are worn out in the form of plates with holes, the pate and which are identical to the cross section and the shape of the through channel 7, and the outer edges of the plates do not protrude beyond the edges of the casing 3 Pusher 8, made in the i, p ". dense plate, one Known with knives thickness, designed for pulling out the i-blades of knives 6 from the slots of the channel 3 Arrows to the sheath are shown the holes in the housing 3 for cooling the coolant

In the cryostat 2 with a metal case

9 and a lid with a passage for the passage of the probe 1 placed an ingot

10 of which a sample is taken. The device operates as follows: Ingot 0 after being removed from the container

the feathers are cooled with a refrigerant and placed in a chemically inert refrigerant 2 filled in. Sampling peak 1 in cavity 4 is also filled in with refrigerant until it is completely cooled.

In the environment, when the environment has a sufficiently high concentration of chemically active gases for sample, the freezing temperature of which is higher than the coolant charge temperature, to prevent these gases from freezing to the inner surface of channel 7, it is advisable to perform the operation Before cooling the sampler, it is placed with a cutting edge. 3 on the ingot 10, pour the channel 7 with a cryogenic liquid and only then cool the refrigerant into the cavity 4 The presence of cryo-liquid in the channel 7 during the selection prevents the freezing of water vapor and gases After complete cooling of Ltitka 10 and sampler 1, the latter is moved down and pushed with the necessary force through the ingot. At the same time, the cytindrical cutting part of the body 3 prevents deformation of the specimen, and the horse a clear surface 3 contributes to the separation of the outer part of the ingot 10 from the central part which penetrates 7 P (i.e., and SB 1), the blades 6, driven by the pusher 8, cut the lower and upper parts of the sample, completely forming a sample with a clean surface bounded by the walls of the channel 7 and n. Jamie 6

If it is necessary to obtain several samples at the same time, the number of knives 6 in the housing 3 can be increased, and the size of the samples can be dosed out by the distance between the planes of the knives 6

In this case, if the blade plane is located at a certain angle to the axis of the sampler, the force applied to cut the sample decreases due to the fact that the cutting edge of the knife has an angle less than 90 ° After the blades 6 return to the initial position, the sample (and sample) from the channel 7, the piston 5 is pushed out directly into the chemically inert cryogenic liquid filling the cryostat 2, or simply onto a cooled metal surface

After being removed from channel 7, the sample is not oxidized for some time in air that has been pre-dried, for example, calcined with calcium oxide. Even the most active metal, cesium, does not oxidize after being removed from the channel of the sampler for 30 seconds. The sample dispensed in volume was analyzed, for example, into a chamber for further investigation.

The tests confirm the reliability of the device in operation and the possibility of preparing samples with high purity of their surface for various classes of materials, including active alkali and alkaline earth metals, the plasticity of which with deep cooling is practically preserved sufficiently

Claims (1)

Invention Formula  The method of sampling from a chemically active plastic material, including the formation of a sample in the sampler channel when pushing it through an ingot, cooling and removing the sampler from the channel, characterized in that, in order to increase the representativeness of the sample by ensuring the surface of the sample is clean and then protecting this surface from gaseous media that interact with it chemically, the ingot of the material under study is placed in a medium of chemically inert cryogenic liquid, and the sampler is cooled temperature 2 The method according to claim 1, characterized in that, in order to prevent chemically active gaseous media from freezing, immediately before pushing through a ingot, a chemically inert cryogenic liquid is poured into the sampler. 3 A device for sampling from a chemically active plastic material, comprising a sampling body with a through channel and a cylindrical cutting edge at the end, characterized in that the sampling body is made with double walls for filling the cavity with cryogenic liquid and through holes on the lateral surface and is provided with openings with movable knives, and the device is equipped with a cryostat installed under the cutting edge of the housing 4 A device according to claim 3, characterized in that the planes of the movable knives are angled to the axis of the sampler body. A / 2i FIG. 7 31-9 A-l