CN111624076A - Total alpha and total beta radioactivity measurement sample preparation method and device - Google Patents
Total alpha and total beta radioactivity measurement sample preparation method and device Download PDFInfo
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- CN111624076A CN111624076A CN202010714122.2A CN202010714122A CN111624076A CN 111624076 A CN111624076 A CN 111624076A CN 202010714122 A CN202010714122 A CN 202010714122A CN 111624076 A CN111624076 A CN 111624076A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/167—Measuring radioactive content of objects, e.g. contamination
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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Abstract
The invention relates to a total alpha and total beta radioactivity measurement sample preparation method and a device, comprising the following steps: step S1: in the U-shaped sieve, grinding balls and the U-shaped sieve are matched with each other and can rotate relatively to apply grinding pressure to the concentrated or processed solid sample to be detected, and the concentrated or processed solid sample to be detected is ground into an ash sample to be detected based on the grinding pressure; step S2: adding absolute ethyl alcohol into the ash sample to be detected, stirring the ash sample in a sample plate to form paste, and performing step S3: and rotating the sample disc, and making the ash sample to be detected into the sample source to be detected with uniform and flat thickness by the scraping blades parallel to the sample disc according to the height of the sample disc and the scraping blades capable of limiting the manufacturing thickness of the sample source to be detected.
Description
Technical Field
The invention relates to the technical field of radioactivity measurement, in particular to a total alpha and total beta radioactivity measurement sample preparation method and device.
Background
The radioactivity of the total α and the total β refers to the total radioactivity level of β radionuclide and β 1 radionuclide in the sample, because the content of the radionuclide is usually very low, the radioactivity of the total β and the total β is usually measured by previously concentrating or processing the sample such as water, biology, aerosol, soil and the like into solid substances, grinding the solid substances into fine ash (important premise of uniformly spreading the sample), uniformly spreading the solid substances in a sample tray to prepare a sample source (measuring source and sample source), sending the sample source into a low-background α and β measuring instrument to measure and record particles which are emitted by the sample source, enter a detector through an air layer between the sample source and the detector and still have certain energy and trigger the detector by α particles and β particles to be measured, and count the particles, finally comparing the measurement result with the measurement result of a standard source (reference source) prepared by using a standard substance under the same conditions under the same measurement conditions, obtaining the total α and the radioactivity level of the sample, the total α and the radioactivity of the total β, the radioactivity of the total α and the total 6854 is almost the radioactivity of the total α and the total 465, the total 465 is more completely consistent with the total radioactive concentration or almost the infinite solid substances of the total 465, the total α and the total 465 is ensured by the total radioactive concentration and the total concentration of the sample can be completely consistent with the total or almost even concentration and the total radioactive concentration of the sample, and the sample concentration of the sample2) The sample source and the standard source of (1).
For example, chinese patent publication No. CN1103200072A discloses a sample source preparation device and method for total α and total β measurement in water, which includes a suction pump, a filter flask connected to the suction pump, and a filter device inserted into the filter flask, wherein the filter device has filter paper therein. The filter device comprises a filter cylinder and a filter head, wherein the filter head is inserted into the filter flask, the filter cylinder is detachably connected above the filter head, a sieve plate and filter paper are arranged in the filter head, and the filter paper is placed on the sieve plate. The invention aims to provide a sample source preparation device and a sample source preparation method for measuring total alpha and total beta radioactivity in water, which aim to solve the problem that the uniformity preparation of a sample source spreading disc for measuring the total alpha and total beta radioactivity in water in the prior art is greatly interfered by human subjective factors, and realize the purposes of ensuring the uniformity and the flatness of the sample source spreading disc and improving the quality of the sample source for measuring a water sample. However, this device is only used for samples in which the sample is liquid, and cannot be used for preparing samples in which the sample is solid.
Compared with nuclide analysis, total alpha and total beta radioactivity measurement has the advantages of short period, low cost, simplicity, feasibility and the like, and the level of radioactive nuclides in the environment is very low in most cases, so that the health hazard is extremely limited, and the nuclide analysis is not needed generally. Therefore, total alpha and total beta radioactivity are widely used for radioactive contamination screening, i.e., total alpha and total beta radioactivity of a sample are determined, and nuclide analysis is performed when the total alpha and total beta radioactivity level exceeds a screening level or a preset operation level. The world health organization and a plurality of countries use total alpha radioactivity and total beta radioactivity as radioactive screening indexes of drinking water, and the international atomic energy organization uses the total alpha radioactivity and the total beta radioactivity as radioactive screening indexes of food, milk and drinking water under nuclear and radiation accident emergency situations. The total alpha and beta radioactivity levels of the sample are accurately measured, and unnecessary nuclide analysis can be avoided. At present, many technicians have carried out a great deal of research work on various factors affecting the accurate measurement of total alpha and total beta radioactivity and have provided corresponding solutions, but no feasible method is provided for how to prepare a sample source with uniform and flat thickness and a standard source so as to reduce the counting error.
In a solid material, the α particles and the low energy β particles have a short range, e.g., are not infinitely thin (e.g., 0.5 mg/cm)2) The emitted α particles and low-energy β particles are easy to be absorbed or energy loss due to interaction with solid substances, namely α particles and β particles are self-absorbed, for total α and total β radioactivity measurement, in order to ensure measurement sensitivity and sample preparation convenience, a sample source and a standard source generally have certain thicknesses (generally 10-20 mg/cm)2) Because of the self-absorption, most α and β particles are absorbed or have reduced energy, and only a few α and β particles from the sample source and standard source surface layers can be ejected and provide a low background α, β meterGenerally, the thicker the solid matter is, the more serious the α particles and β particles are self-absorbed, the uneven thickness distribution of the sample source and the standard source is, the self-absorption of β 1 particles and β 0 particles at all positions of the sample source and the standard source is inconsistent, so the even flatness of the thickness of the sample source and the standard source seriously affects the counting efficiency of α particles and β 4 particles (particularly α particles) by the low background β 3 and β 2 measuring instrument, and the even flatness of the thickness of the prepared sample source and the standard source has a great influence on the accuracy of the total α and total β radioactivity measuring results because the air layer between the sample source or the standard source and the detector and the incident window of the detector absorb α particles and β particles or lead α particles and β particles to be constant and invariable.
Disclosure of Invention
Aiming at the defects of the prior art: a total alpha and total beta radioactivity measurement sampling method, comprising: grinding the concentrated or processed sample solid to be detected into a sample to be detected with the mesh number meeting the requirement, preparing the sample to be detected into a sample source to be detected with relatively uniform and flat thickness, and performing S1: in the U-shaped sieve, grinding balls and the U-shaped sieve are matched with each other and can rotate relatively to apply grinding pressure to the concentrated or processed solid sample to be detected, and the concentrated or processed solid sample to be detected is ground into an ash sample to be detected based on the grinding pressure; step S2: adding absolute ethyl alcohol into the ash sample to be detected, stirring the ash sample in a sample plate to form paste, and performing step S3: and rotating the sample disc, and manufacturing the ash sample to be detected into the sample source to be detected according to the mode that the scraping blades parallel to the sample disc can limit the manufacturing thickness of the sample source to be detected according to the heights of the sample disc and the scraping blades.
According to a preferred embodiment, the ash sample to be measured is intensively placed in the middle area of the sample tray in a large number, so that when the sample tray rotates, the ash sample to be measured can be driven to rotate by the wire scraping thickening area of the rigid scraping wire, so that the ash sample to be measured is driven by the wire scraping thickening area to creep towards two sides of the wire scraping wing area based on the centrifugal force and the scraping action of the wire scraping thickening area.
According to a preferred embodiment, as the sample disk rotates, the ash sample to be measured in the middle area of the sample disk gradually creeps to the side wing area of the scraping wire under the action of centrifugal force and scraping gear of the wire scraping thickening area, and is gradually and uniformly spread under the action of leveling of the scraping bottom.
According to a preferred embodiment, both ends of the rigid scraping wire are respectively connected to the inner screw rod via at least two oblique wires, wherein the torsional rigidity of the oblique wires is greater than that of the rigid scraping wire, so that the rigid scraping wire can flatten the ash sample to be measured in a controllable shaking manner during the rotation of the rotating disc.
According to a preferred embodiment, the inner screw is screwed to an outer screw, which is screwed to the outer fixed cylinder, wherein the pitch of the inner screw is smaller than the pitch of the outer screw, so that the height between the wiper blade and the sample plate can be determined at least in a coarse and then fine adjustment manner.
According to a preferred embodiment, the inner screw is provided with a sensor, the rotational speed of the sample plate being determinable on the basis of a measurement signal of the sensor.
According to a preferred embodiment, in step S3, the sample tray is checked for being horizontal using a horizontal bubble vial.
According to a preferred embodiment, the method comprises: and step S4, turning on an infrared lamp to dry the prepared sample source to be tested with uniform and smooth thickness.
According to a preferred embodiment, the invention also provides a total alpha and total beta radioactivity measurement sample preparation device, which at least comprises a U-shaped sieve, grinding balls, a sample tray and a scraping blade, wherein in the U-shaped sieve, the grinding balls and the U-shaped sieve are matched with each other and can rotate relatively to apply a grinding pressure on concentrated or processed sample solids to be detected, and the concentrated or processed sample solids to be detected are ground into ash samples to be detected based on the grinding pressure; and adding absolute ethyl alcohol into the to-be-detected ash sample, stirring the to-be-detected ash sample in a sample disc to form paste, rotating the sample disc, and making the to-be-detected ash sample into the to-be-detected sample source by using scraping blades parallel to the sample disc according to the height of the sample disc and the scraping blades, wherein the scraping blades can limit the making thickness of the to-be-detected sample source.
According to a preferred embodiment, the wiper blade comprises a rigid wiper blade comprising a wiper blade thickened region and wiper blade flank regions, wherein the wiper blade thickened region is located in the middle of the wiper blade flank regions on both sides in such a way that it increases in the thickness direction from the bottom to the top of the wiper blade and decreases in the thickness direction from the bottom to the top of the wiper blade after reaching a maximum at the axis of symmetry of the wiper blade.
Drawings
FIG. 1 is a schematic diagram of a sample applicator of an overall alpha and overall beta measurement sample preparation device provided by the present invention;
FIG. 2 is a schematic view of the wiper blade of a total alpha and total beta measurement sample preparation device provided by the present invention; and
FIG. 3 is a schematic diagram of a sample grinder of an overall alpha and overall beta measurement sample preparation device provided by the present invention; and
FIG. 4 is a preferred rigid scraping wire provided by the present invention;
FIG. 5 is a schematic flow chart of the method of the present invention.
List of reference numerals
100: sample grinder 200 f: leveling base
200: sample applicator 200 g: horizontal bubble instrument
200 a: sample tray 200 h: lining supporting plate
200 b: blade 200 i: rotary disc
200 c: height adjuster 200 b-1: rigid scraping wire
200 c-1: inner screw rod 100 a: sample grinder support
200 c-2: outer screw rod 100 b: fixing sleeve
200 c-3: outer fixed cylinder 100 c: rotary screw
200 c-4: sample laying support 100 d: handle (CN)
200 c-5: inner screw fixing knob 100 e: connecting rod
200 c-6: outer screw rod fixing knob 100 f: u-shaped sieve
200 d: 100g of a sheet pressing clip: grinding ball
200 e: bottom plate 200 b-2: inclined wire drawing
200b-1 a: bottom scraping 200b-1 c: scraping roof
200b-1 b: filament-scraping flank region 200b-1 d: thickened area for scraping wire
300: infrared lamp
Detailed Description
This is described in detail below with reference to fig. 1-5.
In the present invention, the sample has at least the following three forms, which are included in the order of the processing steps:
the sample solid to be detected is obtained by concentrating or processing samples such as water, organisms, aerosol, soil and the like into the sample solid to be detected.
And (3) fully grinding the concentrated or processed sample solid to be detected into the ash sample to be detected.
And (3) dripping a small amount of absolute ethyl alcohol into the to-be-measured ash sample, stirring the to-be-measured ash sample into paste, uniformly spreading the paste, and drying the paste to form the sample source which can be measured by the measuring probe.
In the present invention, since total α and total β are relative measurement values, a reference sample is required for measurement. Thus, the sample source to be tested includes a sample source) and a standard source (made of a reference sample).
Example 1
This example discloses a total alpha and total beta radioactivity measurement wear method.
The sample preparation device comprises a sample grinding device 100 and a sample spreading device 200. The sample grinder 100 is used for grinding the concentrated or processed sample solids to form an ash sample to be measured which meets the sample preparation mesh requirement of the sample spreader 200. Specifically, the sample grinder 100 includes the following components:
the sample grinder support 100a is made of 304 stainless steel, has the diameter of 4mm and the length of 70mm, is welded in the middle of the upper part of the fixing sleeve 100b, forms an angle of 30 degrees with the upper part of the fixing sleeve, and is used for supporting the fixing sleeve 100b and fixing and collecting weighing paper of a ground ash sample to be measured.
Fixed sleeve 100b adopts 304 stainless steel to make, and the upper portion is long 40mm, upper portion internal diameter 20mm, and the long 7mm of lower part, lower part internal diameter 12mm, thickness 2mm set up the screw thread in the section of thick bamboo, and pitch 0.1mm for fixed connection rotates hob 100c and U type sieve 100 f.
The screw rod 100c is rotated and made of 304 stainless steel, the diameter is 20mm, the length is 50mm, the thread pitch is 0.1mm, the side edge of the upper end is connected with the handle 100d, and the middle part of the bottom end is provided with a screw hole with the diameter of 4mm and the depth of 4mm and is connected with the connecting rod 100 e.
The handle 100d, made of 304 stainless steel, has a length of 40mm and a diameter of 4mm, and is connected to the rotary screw 100 c.
The connecting rod 100e is made of 304 stainless steel, has the diameter of 4mm and the length of 38mm, is provided with threads at two ends, has the length of 4mm at the upper end and the length of 3mm at the lower end, and is respectively connected with the rotating screw rod 100c and the grinding ball 100 g.
Grinding ball 100g adopts 304 stainless steel to make, is the hemisphere, and the diameter is 10mm, and the sphere is smooth, and the upper portion center sets up the screw that the diameter is 4mm, the degree of depth is 3mm, links to each other with connecting rod 100e, and when rotating screw 100c and rotating to fixed cylinder 100b upper portion bottom, grinding ball 100g and U type sieve 100f bottom coincide completely.
At least one optional workflow of the sample grinder 100 is: transferring the concentrated or processed solid sample to be tested into a U-shaped sieve 100f in a grinder 100, screwing the U-shaped sieve 100f and a fixed sleeve 100b to be connected, placing weighing paper below the U-shaped sieve 100f, pressing the weighing paper tightly by a sample grinder support 100a, pushing a handle 100d by hand to rotate a rotating screw 100c until a grinding ball 100g is completely matched with the U-shaped sieve 100f, rotating the screw 100c in a rotating manner, slightly pulling the U-shaped sieve 100f by fingers for a plurality of times, then rotating the rotating screw 100c by hand pushing the handle 100d until the grinding ball 100g is completely matched with the U-shaped sieve 100f, repeating the steps for a plurality of times, and fully grinding the concentrated or processed solid sample to be tested into an ash sample to be tested. After the sample is ground, the U-shaped sieve 100f and the grinding ball 100g are detached, cleaned by ultrapure water and absolute ethyl alcohol and dried for later use.
Example 2
This example discloses a total alpha and total beta radioactivity measurement sampling method.
After long-term research and study on the existing devices and processes, the inventor of the present invention mainly has the following problems in the existing manual manufacturing: 1. the uniform and flat thickness of the prepared sample source and the standard source can not be ensured, and especially the infinite thin or extremely thin (0.5-5 mg/cm) thickness can be prepared under the condition of needing or little ash sample quantity to be detected2) The uniform and flat sample source is extremely difficult, due to the self-absorption effect of α particles and β particles, the thickness of the sample source to be measured is not uniform and flat after preparation, so that the total β and total β radioactivity measurement results have great influence, 2, in the process of manually flattening the sample source to be measured, the sample source easily climbs to the outer edge of a sample disc, the probe is easily polluted in the measurement process, the background of low background α and β measuring instruments is increased, and the accuracy of the total α and total β radioactivity measurement results is influenced, therefore, the total α and total β radioactivity measurement sample preparation device is mainly provided in the embodiment, the sample source and the standard source with uniform and flat thickness can be quickly and conveniently prepared, and the prepared sample source and the standard source cannot climb outwards to pollute the probe.
The sample preparation device 200 comprises a sample disc 200a and a scraping blade 200b, as shown in figures 1 and 2, the sample disc 200a and the scraping blade 200b are arranged in parallel, and the height difference between the two defines the preparation thickness of the sample source to be detected, and the preparation thickness of the sample source to be detected is generally 0.5-50 mg/cm2. The inventor of the invention finely adjusts the thickness of the sample source to be measured, on one hand, to ensure that the thickness of the sample source to be measured is relatively uniform and flat, and on the other hand, to ensure that the sample source can be manufactured to a thickness even when the thickness is infinitely thin or extremely thinThe infinite thin is that the sample source to be detected observed by human eyes is a layer of thin film, so that the interaction between α particles and β particles and solid matters is reduced, the absorbed energy loss is reduced, and the technical problem that the sample source to be detected in the prior art cannot obtain the infinite thin or extremely thin uniform and flat sample source to be detected due to manual manufacturing is solved, so that the technical problem that the sample source to be detected in the prior art is excessively absorbed by α particles and β particles due to the fact that the sample source to be detected has larger thickness is solved.
In this embodiment, the scraping blade 200b and the sample tray 200a can rotate relative to each other, so that the ash sample to be measured on the sample tray 200a after being stirred by the absolute ethyl alcohol can rotate relative to the scraping blade 200 b. The scraping blade 200b contacts with the ash sample to be measured in the process that the sample disc 200a rotates relative to the sample disc, the ash sample to be measured is gradually spread and flattened based on the centrifugal force and the contact force of the scraping blade 200b, the heights of the scraping blade 200b and the ash sample to be measured are gradually adjusted, and the rotating disc 200i is rotated to drive the sample disc 200a to rotate until the sample disc 200a forms a sample source to be measured with relatively uniform and flat thickness. At this time, the maximum thickness that the sample source to be measured can reach is the height difference between the sample pan 200a and the wiper 200b, and the sample source to be measured is made to be a substantially pie-shaped sheet (similar to a thin film). The comparison of the sample source to be tested (sample source No. 1) prepared by the method and the sample source to be tested (sample source No. 2) prepared by hand is carried out under the same experimental conditions, and the results show that: the No. 1 sample source is thinner, so that the No. 1 sample source is easier to detect by the low-background alpha and beta measuring instrument, and the measured value of the No. 1 sample source is closer to the true value and has higher reference value; as the sample source No. 1 is more uniform, the total alpha and total beta radioactivity values of the sample source No. 1 show higher stability (namely, the standard deviation is smaller) when the sample preparation and measurement are carried out on the solid sample to be measured in the same batch, and the measured value of the sample source to be measured, which is prepared by the sample preparation device provided by the invention, is more scientific and instructive.
Furthermore, in addition to the above considerations of measurement accuracy and stability, the present invention minimizes the labor and effort of the experimenter (or measurer). On one hand, the more accurate and stable the measured value, the experimenter (or measurer) can make and measure the sample without repetition; on the other hand, with this apparatus, the flattening process of the sample source to be measured is almost completely performed by the apparatus, so that the experimenter (or the measuring person) can prepare the sample without spending much effort and time.
Preferably, as shown in FIG. 2, the blade 200b includes a rigid scraping wire 200b-1 for forming the sample to be tested into a sample source to be tested. The air passages in the rigid scraping wire 200b-1 during rotation of the sample tray 200a relative thereto act like "wire cutting" and "flattening" the ash sample to be measured. In the early stage of the relative rotation, the ash sample to be measured is uneven, the part of the rigid scraping wire 200b-1 higher than the rigid scraping wire is gradually driven to the part, corresponding to the sample disc 200a, of the sample disc 200a where the ash sample to be measured is not laid in a manner similar to the linear cutting, the surface formed by the ash sample to be measured is gradually just contacted with the rigid scraping wire 200b-1, and then the ash sample to be measured is gradually flattened until the ash sample to be measured is relatively uniformly spread out based on the centrifugal force and the contact of the rigid scraping wire 200 b-1. In the present invention, the rigid scraping wire 200b-1 is fixedly connected to the height adjuster 200c, the height adjuster 200c adjusts the rigid scraping wire 200b-1 to the thickness requirement according to the thickness requirement of the sample source to be measured, and the stirred ash sample to be measured is approximately uniformly placed at the center of the sample pan 200 a. The length of the rigid scraping wire 200b-1 is matched with the sample carrying diameter of the sample tray 200a, so that the ash sample to be detected cannot climb to the outer edge of the sample tray 200a in the relative rotation process, and the increase of the radioactivity of the background is prevented.
Preferably, as shown in FIG. 1, the height adjuster 200c includes an inner screw rod 200c-1 and an outer screw rod 200 c-2. The inner screw bar 200c-1 is screw-coupled to the outer screw bar 200 c-2. The external screw rod 200c-2 is screw-coupled to the external fixing cylinder 200 c-3. As shown in FIG. 2, the rigid scraping wire 200b-1 is fixedly connected to the inner screw rod 200 c-1. Preferably, the pitch of the inner screw bar 200c-1 is smaller than the pitch of the outer screw bar 200 c-2. Thus, the outer screw 200c-2 is fixed by the outer screw fixing knob 200c-6 when the outer screw 200c-2 is rotated until the wiper 200b approaches the ash sample or the standard substance to be measured, and then the inner screw 200c-1 is fixed by the inner screw fixing knob 200c-5 when the inner screw 200c-1 is rotated until the wiper 200b contacts the ash sample or the standard substance to be measured. Thus, the height between the wiper blade 200b and the sample plate 200a can be fine-tuned, with a coarse tuning followed by a fine tuning, thereby ensuring that the sample source to be measured can be as thin as possible.
Preferably, the rigid scraping wire 200b-1 is connected to the inner screw rod 200c-1 by at least two oblique edges. As shown in FIGS. 1 and 2, the rigid scraping wire 200b-1 is connected to the inner screw bar 200c-1 by two oblique sides, so that the scraping blade 200b forms a stable triangular mechanism. The two beveled edges are also made of stainless steel wire of comparable size. In the process that the rigid scraping wire 200b-1 is in contact with the ash sample to be tested, based on the stable structure of the triangle, the rigid scraping wire 200b-1 performs linear cutting and leveling on the ash sample to be tested relatively stably (some shaking can occur, especially at the early stage of sample laying). Through careful measurement results, it was found that: if the rigid scraping wire 200b-1 is not connected to the inner screw 200c-1 by a bevel but is connected to the inner screw 200c-1 by a T-shape, the flatness of the sample source to be measured is low (but still higher than manually made) and the stability of the measured value is low (but still higher than manually made).
Example 3
This embodiment may be a further improvement and/or a supplement to embodiments 1 and 2, and repeated contents are not described again. The preferred embodiments of the present invention are described in whole and/or in part in the context of other embodiments, which can supplement the present embodiment, without resulting in conflict or inconsistency.
The embodiment provides a total alpha and total beta radioactivity measurement sample preparation device, and the specific required components comprise:
Leveling the base 200 f: under the base plate 200e, the leveling base 200f can be adjusted to ensure that the rotating disk 200 i/the base plate 200e is in a horizontal state.
Turning disc 200 i: the sample tray 200a is driven to rotate relative to the scraping blade 200b by rotating around a cylinder on the bottom plate 200e, the diameter is 100mm, the height is 10mm, the concave depth of the center of the lower surface is 5mm, the diameter is 60mm, and the material is 304 stainless steel.
The pressing clip 200 d: on the rotating disk 200i, for holding the sample disk 200 a.
Lining and supporting plate 200 h: the sample tray 200a is positioned on the rotating disc 200i, and the outer diameter of the sample tray is 60mm and is recessed by 1mm compared with the upper surface of the rotating disc 200 i; the inner diameter is 54mm, and is recessed 3mm compared with the upper surface of the rotating disc 200 i;
the rigid scraping wire 200b-1 is a thin wire with a smooth surface. And has a diameter of 0.2mm to 0.5mm and a length matching the loading diameter size of the sample tray 200 a. Preferably, the scraping blade 200b is a regular triangle made of 316 stainless steel wire with a diameter of 0.3mm, the bottom side (rigid scraping wire 200b-1) is parallel to the rotating disk 200i, the length of the bottom side (rigid scraping wire 200b-1) matches the sample loading diameter of the sample disk 200a, and the top side is connected with the inner screw rod 200c-1 through a nut by the 316 stainless steel wire with a diameter of 0.3 mm. The scraping blades with the bottom edges (the rigid scraping wires 200b-1) being 20mm, 30mm, 45mm and 52mm long can be manufactured according to the sample loading diameter sizes of 20mm, 30mm, 45mm and 52mm of the sample loading plate 200a commonly used at present so as to meet the sample preparation requirements of the sample loading plates 200a with different sample loading diameters.
The infrared lamp 300 is used for drying the paved sample source and the standard source, the rated power is 50W, the power is adjustable, the lamp cap emits parallel infrared light, the cross section area of the parallel infrared light is slightly larger than that of the sample disc 200a, and the heating temperature in the heating area range is relatively uniform and stable.
Internal screw rod fixing knob 200 c-5: made of plastic, for fixing the inner screw rod 200c-1, and fixing the inner screw rod 200c-1 not to rotate when the rotating disk 200i is rotated to lay the sample source or the standard source.
External screw rod fixing knob 200 c-6: and plastic for fixing the outer screw rod 200c-2, and fixing the outer screw rod 200c-2 not to rotate when the rotating disk 200i is rotated to lay the sample source or the standard source.
The outer screw rod 200c-2 is hollow, is internally and externally provided with threads, has the thread pitch of 1mm, the outer diameter of 5mm and the inner diameter of 2mm, is perpendicular to the rotating disc 200 i/the bottom plate 200e, and is made of 304 stainless steel.
The inner screw rod 200c-1 is provided with threads, the thread pitch is 0.1mm, the diameter is 2mm, the inner screw rod is perpendicular to the rotating disc 200 i/the bottom plate 200e, and the material is 304 stainless steel.
The diameter of the outer edge of the sample plate 200a is 60mm, the thickness is 0.7mm, the diameter (sample loading diameter) of the sample plate is matched with the size of the rigid scraping wire 200b-1 and the low background alpha and beta measuring instrument probes, the diameters are usually 20mm, 30mm, 45mm and 52mm, the clear depth is 1.5mm, the surface is flat and uniform, the surface is polished, and the material is 304 stainless steel. After the preparation of the sample source to be measured is completed, the sample source to be measured laid on the sample tray 200a can be directly used for measurement by the measuring probe after being dried by the infrared lamp. The sample tray 200a is in a horizontal state. The thickness of the manufactured sample source to be measured is relatively uniform and flat, and the liquid phase part in the ash sample to be measured does not flow to the outer edge of the sample plate 200a in the rotation of the scraping blade 200b and the sample plate 200a relative to each other, thereby preventing the probe from being contaminated, and further preventing the background from being increased.
In use of the device:
(1) the method comprises the steps of checking a horizontal bubble instrument 200g, adjusting a leveling base 200f to ensure that a rotating disc 200 i/a bottom plate 200e is in a horizontal state, then taking a proper amount of an ash sample or a standard substance to be measured according to measurement requirements and placing the ash sample or the standard substance into a sample disc 200a, placing the sample disc 200a on a lining supporting plate 200h and fixing the sample disc by a pressing clamp 200d, dropping a small amount of absolute ethyl alcohol, and blending the ash sample or the standard substance to be measured into paste (thin mud) by using a pin and spreading the paste substantially uniformly.
(2) Rotating the outer screw rod 200c-2 until the scraping blade 200b approaches the ash sample or the standard substance to be measured, fixing the outer screw rod 200c-2 by using the outer screw rod fixing knob 200c-6, then rotating the inner screw rod 200c-1 until the scraping blade 200b contacts the ash sample or the standard substance to be measured, fixing the inner screw rod 200c-1 by using the inner screw rod fixing knob 200c-5, slowly rotating the rotating disc 200i to scrape the ash sample or the standard substance to be measured flat, repeating the steps for a plurality of times to enable the scraping blade 200b to contact the ash sample or the standard substance to be measured, and then scraping the ash sample or the standard substance to be measured until the ash sample or the standard substance to be measured is laid uniformly. Preferably, the rotating disc 200i is rotated manually by an experimenter to rotate the sample disc 200a relative to the scraping blade 200 b.
(3) And finally, the infrared lamp 300 is started to dry the ash sample or the standard substance to be detected in the sample tray to prepare a sample source or a standard source with uniform and flat thickness.
Example 4
This embodiment may be a further improvement and/or a supplement to embodiments 1, 2 or a combination thereof, and repeated contents are not described again. The preferred embodiments of the present invention are described in whole and/or in part in the context of other embodiments, which can supplement the present embodiment, without resulting in conflict or inconsistency.
Preferably, the rotation speed of the relative rotation of the wiper blade 200b and the sample tray 200a is configured in such a manner that the rotation speed is first slow, then gradually increased and then gradually decreased to a constant speed. The rotary disk 200i of the present embodiment is driven by a motor. The speed of the motor is first set by laboratory personnel in a controller, such as a PLC controller. The inventor finds that in the research of the rotating speed to the measured value: in the process of carrying out 'linear cutting' on the ash sample to be measured by the rigid scraping wire 200b-1, the rotation speed is as slow as possible, and if the rotation speed is too fast, a liquid phase in a sample source to be measured is easy to separate from a solid phase, so that the measurement result is influenced. After the ash sample to be measured is gradually and uniformly spread, the rotating speed can be properly increased so as to improve the centrifugal force and make the ash sample to be measured spread as thin as possible. Subsequently, the purpose of reducing the rotation speed of the sample tray 200a and keeping the sample tray rotating at a constant speed is to make the flatness of the sample source to be measured higher, that is, the thickness of the sample source to be measured is as uniform as possible in the process of constant speed.
Example 5
This embodiment may be a further improvement and/or a supplement to any one or a combination of embodiments 1, 2, and 3, and repeated details are not repeated. The preferred embodiments of the present invention are described in whole and/or in part in the context of other embodiments, which can supplement the present embodiment, without resulting in conflict or inconsistency.
The present embodiment discloses a preferred wiper blade 200 b. The wiper blade 200b includes a rigid wiper wire 200b-1 and an inclined wire 200b-2 (i.e., an inclined edge) for fastening the rigid wiper wire 200 b-1.
Preferably, the rigid scratch 200b-1 includes a scratch thickening region 200b-1d and a scratch wing region 200b-1 b. As shown in FIG. 4, the filament scraping thickened region 200b-1d is located in the middle of the filament scraping wing regions 200b-1b at both sides in such a manner that it increases in the thickness direction of the blade bottom 200b-1a to the blade top 200b-1c and decreases in the thickness direction of the blade bottom 200b-1a to the blade top 200b-1c after reaching the maximum value at the symmetry axis of the blade 200 b. Also, the areas of increased and decreased thickness are formed only in the vicinity of the symmetry axis of the blade 200 b. Also, preferably, as shown in fig. 4, the scratch thickening regions 200b-1d are formed as follows: the height of the blade base 200b-1a relative to the sample plate 200a in the direction from the one-side blade wing region 200b-1b to the other-side blade wing region 200b-1b is constant, while the height of the blade tip 200b-1c relative to the sample plate 200a increases in the direction from the one-side blade wing region 200b-1b to the other-side blade wing region 200b-1b and reaches a maximum value at the axis of symmetry of the blade 200b and then decreases. Preferably, the scraping tip 200b-1c is streamlined. The scraping bottom 200b-1a is used as an important part for flattening the ash sample to be measured and is always relatively parallel to the sample disc 200a, so that the scraping bottom 200b-1a is in a straight line in the front projection direction. Preferably, the trend of increase or decrease is smooth rather than abrupt.
In sample placement, the ash sample to be tested is placed in the middle area of the sample pan 200a, i.e., nearly corresponding to the scraped thickening area 200b-1 d. When the sample disc 200a rotates, a large amount of ash samples to be measured are concentrated in the scraping thickening area 200b-1d and stacked, at this time, the scraping thickening area 200b-1d plays a role of a baffle to drive more ash samples to be measured in the middle area to rotate, based on the centrifugal force and the scraping action of the scraping thickening area 200b-1d, the ash samples to be measured driven by the scraping thickening area 200b-1d creep to both sides of the scraping wing area 200b-1b, and along with the rotation of the sample disc 200a, the ash samples to be measured in the middle area of the sample disc 200a gradually creep to the scraping wing area 200b-1b under the centrifugal force and the scraping action of the scraping thickening area 200b-1d, and gradually and uniformly (relatively uniformly) under the flattening action of the scraping bottom 200b-1 a. This structure of the scraping wire 200 b-1: on one hand, in order to improve the product efficiency of the sample source to be detected, the wire scraping thickening area 200b-1d can pull more ash samples to be detected to rotate relative to the wire scraping thickening area, so that the ash samples to be detected can creep towards two sides by centrifugal force, the time for the ash samples to be detected to move towards two sides is reduced, and the efficiency is improved; on the other hand, although the rigid scraping wire 200b-1 is a piece made of steel, since it is slender and flexible in nature, the provision of the scraping wire thickening region 200b-1d increases the rigidity coefficient of the rigid scraping wire, and can keep the vibration thereof at a reasonable amplitude and frequency as much as possible to urge the dust sample to be measured to move to both sides.
Example 6
This embodiment may be a further improvement and/or a supplement to any one or a combination of embodiments 1, 2, 3, 4, and 5, and repeated details are not repeated. The preferred embodiments of the present invention are described in whole and/or in part in the context of other embodiments, which can supplement the present embodiment, without resulting in conflict or inconsistency.
The present embodiment discloses a preferred wiper blade 200 b. The wiper blade 200b includes a rigid wiper wire 200b-1 and an inclined wire 200b-2 (i.e., an inclined edge) for fastening the rigid wiper wire 200 b-1.
The rigid scraping wire 200b-1, as the name implies, is a filament made of a rigid material, such as 304 stainless steel. However, since the length of the rigid scraping wire 200b-1 is 20mm or more, which corresponds to a beam structure with both ends fixed, it shows "flexibility" during contact with the ash sample to be measured, and further, it may be shaken. According to research, the shaking of the rigid scraping wire 200b-1 is greatly influenced by the rotating speed, the flexibility of the inclined pulling wire 200b-2 and the suspension point height of the inclined pulling wire 200 b-2. Further, the inventors of the present invention found in their studies that: compared with the situation that the torsional rigidity of the inclined drawing wire 200b-2 is less than or equal to that of the rigid scraping wire 200b-1, when the torsional rigidity of the inclined drawing wire 200b-2 is greater than that of the rigid scraping wire 200b-1, the shaking of the rigid scraping wire 200b-1 is controllable, and the speed of flattening the ash sample to be measured is accelerated. Controllable means that: at the initial stage of contact between the rigid scraping wire 200b-1 and the ash sample to be measured, the shaking amplitude and shaking frequency of the rigid scraping wire 200b-1 are large, but the creeping speed of the ash sample to be measured towards two sides is increased, and then in the process of gradually flattening the ash sample to be measured, the shaking amplitude and shaking frequency of the rigid scraping wire 200b-1 are obviously reduced until the ash sample to be measured does not shake. The sample source to be measured accelerates the flattening speed under the controllable shaking action of the rigid scraping wire 200b-1 and is measured by a measuring instrument, and the thickness of the sample source obtained by the method can meet the requirement of infinite thinness or extremely thin.
Preferably, a sensor capable of measuring the vibration of the inner screw 200c-1, such as a displacement sensor, a velocity sensor, or an acceleration sensor, is provided on the inner screw 200 c-1. The thickness of the sample source to be measured can be appropriately (qualitatively or semi-quantitatively) reflected by the measurement signal of the sensor. Under the condition that the measured signals of the sensor are irregular to regular, the thickness of the sample source to be measured almost meets the measurement requirement. In this case, the speed of the rotating disk 200i may start to be reduced and uniform at the time of the measured signal of the sensor to improve the quality of the sample source to be measured. Therefore, the invention can measure the thickness of the sample source to be measured without setting excessive image monitoring equipment and microscopic monitoring equipment, thereby saving the thickness detection process, improving the radioactivity detection rate and efficiency, and being particularly beneficial to the detection of the heavy-spot nuclear area such as a nuclear test area, a nuclear leakage area and the like.
Example 7
This embodiment also discloses a sample preparation device, which may be a further improvement and/or supplement to one or a combination of embodiments 1, 2, 3, 4, 5, and 6, and repeated contents are not repeated. The preferred embodiments of the present invention are described in whole and/or in part in the context of other embodiments, which can supplement the present embodiment, without resulting in conflict or inconsistency.
The embodiment discloses a total alpha and total beta radioactivity measurement sample preparation device, including:
the sample grinding device 100 is used for grinding the concentrated or processed sample solid to be detected into a dust sample to be detected with the mesh number meeting the requirement;
and the sample spreader 200 is used for preparing the ash sample to be detected into a sample source to be detected with relatively uniform and smooth thickness. The sample applicator includes a wiper 200b and a sample tray 200 a. Wherein the wiper blade 200b and the sample tray 200a are parallel to each other. At this time, the height between the two is set according to the requirement of the manufactured thickness of the sample source to be measured. Under the condition that the scraping blade 200b and the sample tray 200a rotate relative to each other, the scraping blade 200b can make the gray sample to be measured into a sample source to be measured with a relatively uniform and flat thickness.
Preferably, the rotation speed of the scraper 200b and the sample tray 200a relative to each other is configured in such a manner that the rotation speed is first slow, then increased and then decreased to a constant speed.
Example 8
The present embodiment further discloses a sample grinder, which may be a further improvement and/or a supplement to one or a combination of embodiments 1, 2, 3, 4, 5, 6, and 7, and repeated contents are not repeated. The preferred embodiments of the present invention are described in whole and/or in part in the context of other embodiments, which can supplement the present embodiment, without resulting in conflict or inconsistency.
The sample grinder includes a U-shaped screen 100f and grinding balls 100 g. In the U-shaped sieve 100f, the grinding balls 100g and the U-shaped sieve 100f are engaged with each other and can rotate relatively to apply a grinding force to the concentrated or processed solid sample to be tested, and the concentrated or processed solid sample to be tested is ground into an ash sample to be tested based on the grinding force.
The ash sample to be tested after being ground by the sample grinder is added with absolute ethyl alcohol and stirred in the sample tray 200a to form paste. The sample plate 200a is rotated, and the scraper 200b parallel to the sample plate 200a makes the ash sample to be measured into the sample source to be measured according to the height of the two in a way of limiting the thickness of the sample source to be measured.
It should be noted that the above-mentioned embodiments are exemplary, and that those skilled in the art, having benefit of the present disclosure, may devise various arrangements that are within the scope of the present disclosure and that fall within the scope of the invention. It should be understood by those skilled in the art that the present specification and figures are illustrative only and are not limiting upon the claims. The scope of the invention is defined by the claims and their equivalents.
Claims (10)
1. A total alpha and total beta radioactivity measurement sampling method, comprising:
grinding the concentrated or processed sample solid to be detected into a dust sample to be detected with the mesh number meeting the requirement,
preparing the ash sample to be measured into a sample source to be measured with relatively uniform and flat thickness,
it is characterized in that the preparation method is characterized in that,
step S1: in the U-shaped sieve (100f), grinding balls (100g) and the U-shaped sieve (100f) are matched with each other and can rotate relatively to apply grinding pressure to the concentrated or processed solid sample to be detected, and the concentrated or processed solid sample to be detected is ground into an ash sample to be detected based on the grinding pressure;
step S2: adding absolute ethyl alcohol into the ash sample to be detected, stirring the ash sample in a sample tray (200a) to form paste,
step S3: rotating a sample plate (200a), and manufacturing the ash sample to be detected into the sample source to be detected according to the mode that the heights of the rotating sample plate and the sample plate (200a) are parallel to each other and a scraping blade (200b) can limit the manufacturing thickness of the sample source to be detected.
2. The sample preparation method according to claim 1, wherein the ash sample to be measured is intensively placed in the middle region of the sample tray (200a) in a large amount, so that the ash sample to be measured can be rotated by the wire scraping thickening region (200b-1d) of the rigid wire scraper (200b-1) when the sample tray (200a) rotates, so that the ash sample to be measured is moved by the wire scraping thickening region (200b-1d) to creep towards both sides of the wire scraping wing region (200b-1b) based on the centrifugal force and the scraping action of the wire scraping thickening region (200b-1 d).
3. The sample preparation method according to claim 1 or 2, wherein as the sample plate (200a) rotates, the ash sample to be measured in the central region of the sample plate (200a) gradually crawls to the side wing region (200b-1b) of the scraping wire under the centrifugal force and the scraping action of the scraping thickening region (200b-1d) and gradually spreads uniformly under the flattening action of the scraping bottom (200b-1 a).
4. The sample preparation method according to claim 2, wherein both ends of the rigid scraping wire (200b-1) are connected to an inner screw rod (200c-1) via at least two inclined drawing wires (200b-2), respectively,
wherein the torsional rigidity of the inclined wire (200b-2) is greater than that of the rigid scraping wire (200b-1), so that the rigid scraping wire (200b-1) can lay the ash sample to be measured in a controllable shaking manner during the rotation of the sample tray (200 a).
5. The sample preparation method according to claim 4, wherein the inner screw rod (200c-1) is screw-coupled to the outer screw rod (200c-2), the outer screw rod (200c-2) is screw-coupled to the outer fixed cylinder (200c-3),
wherein the pitch of the inner screw rod (200c-1) is smaller than the pitch of the outer screw rod (200c-2) so that the height between the wiper blade (200b) and the sample plate (200a) can be determined at least in a coarse adjustment followed by a fine adjustment.
6. A sample preparation method as claimed in claim 5, characterized in that said inner screw (200c-1) is provided with a sensor, the rotational speed of said sample plate (200a) being determinable on the basis of a measurement signal of said sensor.
7. The sample preparation method according to claim 6, wherein in step S3, it is checked whether the sample plate (200a) is in a horizontal state using a horizontal bubble meter (200 g).
8. The sample preparation method according to claim 7, wherein the method comprises:
and step S4, starting an infrared lamp (300) to dry the to-be-detected sample source with uniform and flat thickness.
9. A total alpha and total beta radioactivity measurement sample preparation device at least comprises a U-shaped sieve (100f), a grinding ball (100g), a sample tray (200a) and a scraping blade (200b),
it is characterized in that the preparation method is characterized in that,
in the U-shaped sieve (100f), grinding balls (100g) and the U-shaped sieve (100f) are matched with each other and can rotate relatively to apply grinding pressure to the concentrated or processed solid sample to be detected, and the concentrated or processed solid sample to be detected is ground into an ash sample to be detected based on the grinding pressure;
adding absolute ethyl alcohol into the ash sample to be detected, stirring the ash sample in a sample tray (200a) to form paste,
rotating a sample plate (200a), and manufacturing the ash sample to be detected into the sample source to be detected according to the mode that the heights of the rotating sample plate and the sample plate (200a) are parallel to each other and a scraping blade (200b) can limit the manufacturing thickness of the sample source to be detected.
10. The sample preparation device according to claim 9, wherein the ash sample to be measured is intensively placed in the middle region of the sample tray (200a) in a large amount, so that the ash sample to be measured can be rotated by the wire scraping thickening region (200b-1d) of the rigid wire scraper (200b-1) when the sample tray (200a) rotates, so that the ash sample to be measured is moved by the wire scraping thickening region (200b-1d) to creep towards both sides of the wire scraping wing region (200b-1b) based on the centrifugal force and the scraping action of the wire scraping thickening region (200b-1 d).
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