CN111624077B - Total alpha and total beta radioactivity measurement sample preparation device and method - Google Patents
Total alpha and total beta radioactivity measurement sample preparation device and method Download PDFInfo
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Classifications
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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
-
- 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
- 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
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention relates to a sample preparation device and method for total alpha and total beta radioactivity measurement, wherein the device comprises a sample grinder and a sample spreader. Wherein: the sample grinder is used for grinding a solid sample to be measured into a sample to be measured, which meets the requirement of the sample preparation number of the sample spreader, the sample spreader is used for preparing the sample to be measured into a sample source to be measured with relatively uniform thickness, the sample spreader comprises a sample tray and a scraping blade, the height between the scraping blade and the sample tray limits the preparation thickness of the sample source to be measured, and therefore the scraping blade can prepare the sample to be measured into the sample source to be measured with relatively uniform thickness under the condition that the scraping blade and the sample tray rotate relatively to each other.
Description
Technical Field
The invention relates to the technical field of radioactivity measurement, in particular to a device and a method for preparing a total alpha and total beta radioactivity measurement sample.
Background
Total alpha, total beta radioactivity refers to the total level of radioactivity of the beta 0 radionuclide and beta 1 radionuclide in the sample. Because the content of the radionuclide is usually very low, the measurement of the total beta 2 and total beta 3 radioactivity usually needs to concentrate or process samples such as water, biology, aerosol, soil and the like into solid substances in advance, grind the samples into fine ash (an important premise of uniform sample spreading), uniformly spread the samples into a sample tray to prepare sample sources (measuring sources and sample sources), then send the sample sources into a low background alpha and beta measuring instrument to measure and record the count caused by alpha particles and beta particles which are emitted by the sample sources, enter the detector after passing through an air layer between the sample sources and the detector and a detector incident window and still have certain energy, trigger the detector, and finally compare the measurement result with the measurement result of a standard source (reference source) prepared by standard substances under the same measurement condition to obtain the total alpha and total beta radioactivity level of the sample. The total alpha, total beta radioactivity measurement is essentially a relative measurement. At present, grinding of solid of sample to be tested, which is concentrated or processed, and tiling of ash sample to be testedThe method is completely completed manually by experimenters, which is time-consuming and labor-consuming, can not ensure that the solid of the sample to be detected which is concentrated or processed is sufficiently ground, and can not ensure that the thickness of the prepared sample source and the standard source is even and smooth, especially the thickness is infinitely thin or extremely thin (0.5-5 mg/cm) 2 ) A sample source and a standard source.
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 suction bottle, and a filter device, wherein the suction bottle is in communication with the suction pump, the filter device is inserted into the suction bottle, and the filter device has filter paper therein. The filtering device comprises a filtering cylinder and a filtering head, wherein the filtering head is inserted into the suction filtering bottle, the filtering cylinder is detachably connected above the filtering head, a sieve plate and filter paper are arranged in the filtering head, and the filter paper is placed on the sieve plate. The invention aims to provide a sample source preparation device and method for measuring total alpha and total beta radioactivity in water, which are used for solving the problem that the sample source tray paving uniformity for measuring the total alpha and total beta radioactivity in water in the prior art is greatly interfered by human subjective factors, and achieving the purposes of ensuring the uniformity and flatness of the sample source tray paving and improving the sample source quality for measuring the water sample. However, this device is only used for samples where the sample is liquid, but cannot be used for preparing samples where the sample is solid. Compared with nuclide analysis, the total alpha and total beta radioactive measurement has the advantages of short period, low cost, simplicity, practicability and the like, and the radionuclide level in the environment is very low in most cases, has extremely limited health hazard, and generally does not need to be subjected to nuclide analysis. Therefore, the total alpha and total beta radioactivity is widely used for radioactive pollution screening, namely, the total alpha and total beta radioactivity of a sample is firstly measured, and when the total alpha and total beta radioactivity level exceeds the screening level or the preset operation level, the nuclide analysis is carried out. The world health organization and a plurality of countries take the total alpha and total beta radioactivity as the radioactivity screening index of the drinking water, and the international atomic energy organization takes the total alpha and total beta radioactivity as the radioactivity screening index of the food, milk and the drinking water under the emergency situation of nuclear and radiation accidents. The total alpha and total beta radioactivity level of the sample is accurately measured, and unnecessary nuclide analysis can be avoided. At present, many technicians have conducted a great deal of research work on various factors that affect the accurate measurement of total α, total β radioactivity and have given corresponding solutions, but no viable method has been given for how to prepare sample sources and standard sources of uniform and flat thickness to reduce counting errors.
In solid materials, the alpha particles and low energy beta particles are of very short range, e.g. not infinitely thin (e.g. 0.5mg/cm 2 ) The emitted alpha particles and low energy beta particles are easily absorbed or lost in energy due to interaction with the solid matter itself, which is the self-absorption of the alpha particles and beta particles. For total alpha and total beta radioactivity measurement, a certain thickness (usually 10-20 mg/cm) 2 ) Its self-absorption of alpha particles, low energy beta particles is even more non-negligible. Due to the self-absorption, most of the beta 0 particles and beta 1 particles are absorbed or energy is reduced, and only a few beta 2 particles and beta 3 particles on the surface layers of the sample source and the standard source can be emitted and recorded by the low-background beta 4 and beta 5 measuring instrument. Generally, the thicker the solid material, the more severe the self-absorption of the beta 6 particles and beta 8 particles. The thickness distribution of the sample source and the standard source is uneven and flat, and the self absorption of beta 7 particles and alpha 0 particles of the sample source and the standard source is inconsistent, so that the even flatness of the thickness of the sample source and the standard source seriously affects the counting efficiency of the low background beta 9 and alpha 2 measuring instrument on the alpha particles and the beta particles (especially alpha 1 particles). Because the air layer between the sample source or the standard source and the detector and the incident window of the detector absorb alpha particles and beta particles or cause the energy loss of the alpha particles and the beta particles to be constant, whether the thicknesses of the prepared sample source and the standard source are uniform and flat has great influence on the accuracy of the total alpha and total beta radioactivity measurement results.
Disclosure of Invention
Aiming at the defects in the prior art: sample spreading methods of the sample source and the standard source are a dry spreading method and a wet spreading method. The dry laying method is to firstly and uniformly spread out fully ground ash samples in a sample tray by using a pin or paperclip, and then to flatten the ash samples by using a stainless steel sample presser matched with the sample tray; the wet spreading method is to drop a small amount of absolute ethyl alcohol or a mixed solution of absolute ethyl alcohol and acetone into a sample tray, stir and spread the fully ground ash sample in the sample tray by using a pin or paperclip, and then dry the ash sample under an infrared lamp. Both methods require that the sample which has been processed and concentrated to solid substances is sufficiently ground into fine ash in a porcelain evaporation dish or transferred into a mortar in advance, which is an important precondition for uniform sample spreading. The grinding of the concentrated or treated solid substances and the spreading of the ash samples are completely finished manually by experimenters, so that the time and the labor are wasted, the sample cannot be sufficiently ground, and even and flat thickness of the prepared sample source and standard source cannot be ensured. The dry laying method is extremely easy to cause the spread sample to scatter, deform and even fall off due to slight vibration in the operation process, is unfavorable for long-term storage, and is easy to pollute the probe in the measurement process, so that the background of the low-background alpha and beta measuring instrument is increased. The wet-laying method is very easy to cause the laid sample to be close to or even overflow out of the tray edge, the sample or standard substance can climb outwards to the outer side of the tray edge in the drying process, the probe is easy to pollute in the measuring process, and the background of the low-background alpha and beta measuring instrument is increased.
To this end, the present invention provides a sample preparation device for total alpha and total beta radioactivity measurement. The sample preparation device comprises a sample grinder and a sample spreader, wherein: the sample grinder is used for grinding a solid sample to be measured into a sample to be measured, which meets the sample preparation mesh requirement of the sample spreader, the sample spreader is used for preparing the sample to be measured into a sample source to be measured with relatively uniform thickness, the sample spreader comprises a sample tray and a scraping blade, the scraping blade is parallel to the sample tray, so that the height between the scraping blade and the sample tray is used for limiting the thickness of the sample source to be measured, and the scraping blade can be used for preparing the sample to be measured into the sample source to be measured with relatively uniform thickness under the condition that the scraping blade and the sample tray rotate relatively to each other.
In the invention, the thickness of the sample source to be measured is finely adjusted, so that the thickness of the sample source to be measured is relatively uniform, and the sample source to be measured is infinitely thin. The infinite thin is that the sample source to be measured observed by human eyes is a layer of film, so that the interaction of alpha particles and beta particles with solid substances is reduced, and the absorption or the energy loss is reduced, so that the technical problem that the sample source to be measured cannot be obtained in infinite thin and extremely thin due to manual manufacturing in the prior art is solved, and the technical problem that the alpha particles and the beta particles are absorbed due to the fact that the sample source to be measured is made in the prior art has a certain thickness is further solved.
In the invention, the comparison of the sample source to be detected (sample source No. 1) and the sample source to be detected (sample source No. 2) which are prepared by hand in the invention under the same experimental conditions shows that: because the sample source No. 1 is thinner, the sample source No. 1 is easier to detect by the low background alpha and beta measuring instrument; because the sample source No. 1 is more uniform, the sample is prepared and measured on the solid samples to be measured in the same batch, and the total alpha and total beta radioactivity values of the sample source No. 1 show higher stability (namely smaller standard deviation), so that the measurement value of the sample source to be measured prepared by the preparation device provided by the invention is more scientific in value and guiding significance.
According to a preferred embodiment, the scraping blade comprises a rigid scraping wire for manufacturing the ash sample to be measured into a sample source to be measured, and the rigid scraping wire is fixedly connected with the height adjuster in a mode that the ash sample to be measured cannot climb to the outer edge of the sample tray.
According to a preferred embodiment, the height adjuster comprises an inner screw rod and an outer screw rod which is in screw connection with the inner screw rod, the outer screw rod being in screw connection with an outer fixed cylinder, wherein the rigid scraper wire is fixedly connected with the inner screw rod, wherein the pitch of the inner screw rod is smaller than the pitch of the outer screw rod, so that the height between the scraper blade and the sample disk can be determined at least in a coarse-tuning and then fine-tuning manner.
According to a preferred embodiment, the rigid scraping wire is connected to the inner screw rod by at least two oblique sides, so that the scraping blade can be fixedly connected with the height adjuster relatively smoothly in the process of contacting the rigid scraping wire with the ash sample to be measured.
According to a preferred embodiment, the sample tray is in a horizontal state so that the thickness of the sample source to be measured is made relatively uniform and the liquid phase portion in the ash sample to be measured does not flow to the outer edge of the sample tray in the rotation of the wiper blade and the sample tray relative to each other.
According to a preferred embodiment, the rotational speed of the relative rotation of the wiper blade and the sample plate is configured in such a way that it is slow, then gradually increases and then gradually decreases to a uniform speed.
According to a preferred embodiment, the rigid scraper is a smooth-surfaced filament with a diameter of 0.2mm to 0.5mm, the length of which matches the sample tray loading diameter size.
According to a preferred embodiment, the sample loading diameter of the sample tray and the size of the measuring probe are matched with each other, so that after the preparation of the sample source to be measured is completed, the sample source to be measured laid on the sample tray can be directly used for measuring by the measuring probe after being dried.
According to a preferred embodiment, the invention also discloses a preparation method of the total alpha and total beta radioactivity measurement sample, which comprises the steps of grinding the solid of the sample to be measured into a gray sample to be measured with the mesh number meeting the requirement; the method comprises the steps of preparing a to-be-measured ash sample into a to-be-measured sample source with relatively uniform thickness, setting a doctor blade and a sample tray in parallel to each other so that the height between the doctor blade and the sample tray is set according to the requirement of the to-be-measured sample source for preparing the thickness, so that the doctor blade can prepare the to-be-measured ash sample into the to-be-measured sample source with relatively uniform thickness under the condition that the doctor blade and the sample tray rotate relatively to each other.
According to a preferred embodiment, in the method, the rotational speed of the relative rotation of the wiper blade and the sample plate is configured in such a way that the rotational speed is increased first slowly and then decreased to a uniform speed.
Drawings
FIG. 1 is a schematic diagram of a sample spreader of a total alpha and beta radiometric sample preparation device provided by the present invention;
FIG. 2 is a schematic illustration of a wiper blade of a total alpha and total beta radiometric sample preparation device provided by the present invention; and
FIG. 3 is a schematic diagram of a sample grinder for a total alpha and beta radioactivity measuring sample preparation device according to the present invention.
List of reference numerals
100: sample grinder 200f: leveling base
200: sample spreader 200g: horizontal bubble instrument
200a: sample tray 200h: lining support plate
200b: wiper blade 200i: rotary disk
200c: height adjuster 200b-1: rigid scraping wire
200c-1: inner screw rod 100a: sample grinder support
200c-2: outer screw rod 100b: fixing sleeve
200c-3: outer fixed cylinder 100c: rotary screw
200c-4: sample laying rack 100d: handle
200c-5: inner screw fixation knob 100e: connecting rod
200c-6: outer screw rod fixing knob 100f: u-shaped sieve
200d: tablet press 100g: grinding ball
200e: base plate 300: infrared lamp
Detailed Description
The following is a detailed description with reference to fig. 1-3.
In the invention, the sample has at least the following three forms, which comprise the following steps according to the sequence of processing steps:
the solid sample to be measured is obtained by concentrating or processing water, organism, aerosol, soil and other samples into solid substances.
And (3) testing the ash sample, and fully grinding the sample of the solid substance processed and concentrated into the ash sample.
And (3) dripping a small amount of absolute ethyl alcohol or a mixed solution of absolute ethyl alcohol and acetone into the sample source to be measured, stirring, and uniformly spreading to form the sample source which can be measured by the measuring probe.
In the present invention, since the total α and the total β are relative measured values, a reference sample is required for measurement. Thus, the sample source to be tested includes a sample source) and a standard source (made with reference to the sample).
Example 1
The inventor of the present invention has conducted long-term investigation and research on the existing devices and processes, and the existing manual production mainly has at least the following problems: 1. the sample source to be measured is thicker and uneven after being prepared, and the total alpha and total beta radioactivity measurement results have larger fluctuation due to the self-absorption effect of alpha particles and beta particles. 2. In the process of artificially flattening the sample source to be measured, the sample source is easy to climb to the outer edge of a sample tray, and the probe is easy to pollute in the measuring process, so that the background of the low-background alpha and beta measuring instrument is increased, and the accuracy of the total alpha and beta radioactivity measuring result is affected. Therefore, the embodiment mainly provides a total alpha and total beta radioactivity measurement preparation device, which aims to rapidly and conveniently prepare a sample source and a standard source with uniform and flat thickness, and the prepared sample source and standard source cannot climb outwards to pollute a probe. Further, the preparation device provided in this embodiment is for improving the accuracy of the total α and total β radioactivity detection and the stability of the measured values. Specifically:
the present example discloses a total alpha and total beta radioactivity measuring sample preparation device. The preparation device comprises a sample spreading device 200 for preparing the ash sample to be tested into a sample source to be tested with relatively uniform thickness. Specifically, the spreader 200 includes a sample tray 200a and a wiper blade 200b. As shown in fig. 1 and 2, the sample tray 200a and the wiper blade 200b are disposed in parallel, and the difference in height between the two defines the resulting thickness of the sample source to be tested. In general, the sample source to be measured is prepared to have a thickness of 0.5 to 50mg/cm2. The inventor of the present invention finely adjusts the thickness of the sample source to be measured, on one hand, in order to ensure that the thickness of the sample source to be measured is relatively uniform, and on the other hand, in order to make the sample source to be measured infinitely thin. The infinite thin is that the sample source to be measured observed by human eyes is a layer of film, so that the interaction of alpha particles and beta particles with solid substances is reduced, and the absorption of the alpha particles and the beta particles is reduced or the energy loss is reduced, so that the technical problem that the sample source to be measured in the prior art cannot be obtained in an infinite thin and extremely thin manner due to manual manufacturing is solved, and the technical problem that the alpha particles and the beta particles are absorbed due to the fact that the sample source to be measured is made in the prior art has a certain thickness is further solved.
In this embodiment, the wiper 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 alcohol (or the mixture of the absolute alcohol and the acetone) can rotate relative to the wiper blade 200b. The wiper blade 200b contacts the ash sample to be measured during the rotation of the sample tray 200a relative thereto, and the ash sample to be measured is gradually spread out and flattened based on the centrifugal force and the contact force of the wiper blade 200b until it forms a source of the sample to be measured having a relatively uniform thickness. At this time, the maximum thickness that the sample source to be measured can reach is the difference in height between the sample tray 200a and the wiper blade 200b, and the sample source to be measured is made to have a substantially cake-shaped sheet (similar to a film). The comparison of the sample source to be tested (sample source No. 1) and the sample source to be tested (sample source No. 2) which are prepared by hand in the invention under the same experimental conditions shows that: because the sample source No. 1 is thinner, the sample source No. 1 is easier to detect by the low background alpha and beta measuring instrument, so that the measured value of the sample source No. 1 is closer to the true value and has more reference value; because the sample source No. 1 is more uniform, the sample is prepared and measured on the solid samples to be measured in the same batch, and the total alpha and total beta radioactivity values of the sample source No. 1 show higher stability (namely smaller standard deviation), so that the measurement value of the sample source to be measured prepared by the preparation device provided by the invention is more scientific in value and guiding significance.
In addition, in addition to the above considerations of measurement accuracy and stability, the present invention minimizes the effort and effort of the experimenter (or measurer). On the one hand, the more accurate and stable the measurement value is, the more the experimenter (or measuring staff) can do not need to repeatedly manufacture and measure the sample; on the other hand, by using the device, the flattening manufacturing process of the sample source to be measured is completely completed by the device, so that an experimenter (or a measuring person) can not spend great effort and time in the sample manufacturing process.
Preferably, as shown in FIG. 2, the wiper blade 200b includes a rigid wiper wire 200b-1 for producing a gray sample to be tested into a source of the sample to be tested. The air channel of the rigid scraper 200b-1 acts like a "wire-cut" and "flat" ash sample to be measured during rotation of the sample tray 200a relative thereto. In the early stage of the relative rotation, the rigid scraping wire 200b-1 gradually drives the portion above it to the portion of the sample tray 200a corresponding to the sample tray 200a, which is not laid with the ash sample to be measured or below it, in a manner similar to "wire cutting", gradually brings the formed surface of the ash sample to be measured into just contact with the rigid scraping wire 200b-1, and then the ash sample to be measured is gradually flattened until relatively uniformly spread out based on the contact of the centrifugal force and the rigid scraping wire 200b-1. In the invention, the rigid scraping wire 200b-1 is fixedly connected with 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 a sample source to be detected, and the stirred ash sample to be detected is approximately uniformly placed in the central position of the sample tray 200a. The rigid scraping wire 200b-1 is approximately matched with the sample loading diameter of the sample tray 200a, so that ash samples to be tested are prevented from climbing to the outer edge of the sample tray 200a in the relative rotation process, and the background radioactivity is prevented from being increased.
Preferably, as shown in FIG. 1, the height adjuster 200c includes an inner screw 200c-1 and an outer screw 200c-2. 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 with the outer fixing cylinder 200 c-3. As shown in FIG. 2, the rigid wiper wire 200b-1 is fixedly coupled to the inner screw rod 200c-1. Preferably, the pitch of the inner screw rod 200c-1 is smaller than the pitch of the outer screw rod 200c-2. In this way, 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 sample ash or the standard substance, 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 sample ash or the standard substance. Thus, the height between the wiper blade 200b and the sample tray 200a may be fine tuned by coarse and then fine tuning to ensure that the sample source to be measured is as thin as possible.
Preferably, the rigid wiper wire 200b-1 is connected to the inner spiral bar 200c-1 by at least two beveled edges. As shown in fig. 1 and 2, the rigid wiper wire 200b-1 is connected to the inner screw 200c-1 by two hypotenuses, so that the wiper blade 200b forms a stable triangle mechanism. The two bevel edges are also made of stainless steel wires with the same size. In the process that the rigid scraping wire 200b-1 is contacted with the ash sample to be detected, the rigid scraping wire 200b-1 is not easy to shake based on the triangle-shaped stable structure, and the sample source to be detected is relatively and stably subjected to linear cutting and leveling. By carefully measuring the junction results, it was found that: if the rigid wiper blade 200b-1 is not connected by a beveled edge to the inner screw 200c-1 but is connected by a T-shape to the inner screw 200c-1, the flatness of the resulting sample source to be tested is lower (but still higher than that produced by hand), the stability of the measurement is also lower (but still higher than that produced by hand).
Example 2
This embodiment may be a further improvement and/or addition to embodiment 1, and the repeated description is omitted. In addition to this embodiment, the preferred implementation of the other embodiment may be provided in whole and/or in part without conflict or contradiction.
This example provides a total alpha and total beta radioactivity measuring sample preparation device, which specifically requires components including:
sample laying rack 200c-4: the screw rod is used for supporting the inner screw rod and the outer screw rod, has the diameter of 10mm and the length of 200mm, is perpendicular to the bottom plate 200e, and is made of 304 stainless steel.
Base plate 200e: the stainless steel cylinder 304 with the diameter of 60mm and the height of 5mm is arranged in the center of the upper surface, and is made of 304 stainless steel, wherein the length of the stainless steel cylinder is 200mm, the width of the stainless steel cylinder is 200mm, and the height of the stainless steel cylinder is 10 mm.
Leveling base 200f: below the base plate 200e, the leveling base 200f can be adjusted to ensure that the rotating disc 200 i/base plate 200e is in a horizontal position.
Rotating disc 200i: the stainless steel plate rotates 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 stainless steel plate is made of 304 stainless steel.
Compression clip 200d: is positioned on the rotating disk 200i for securing the sample disk 200a.
The susceptor plate 200h: is positioned on the rotating disk 200i for supporting the sample disk 200a, and has an outer diameter of 60mm, which is 1mm inward from the upper surface of the rotating disk 200 i; the inner diameter is 54mm, which is 3mm concave compared with the upper surface of the rotating disc 200 i;
horizontal bubble meter 200g: checking whether the rotating disc 200 i/the bottom plate 200e is in a horizontal state;
rigid doctor blade 200b-1 is a smooth surfaced filament. And has a diameter of 0.2mm to 0.5mm, and a length thereof and a size of the sample loading diameter of the sample tray 200a are matched with each other. Preferably, the wiper blade 200b is a regular triangle made of 316 stainless steel wire with a diameter of 0.3mm, the bottom side (the rigid wiper wire 200 b-1) is parallel to the rotating disk 200i, the length of the bottom side (the rigid wiper wire 200 b-1) is matched with the diameter of the sample disk 200a, the sample loading diameter is matched with the diameter size of the sample disk, and the top part of the wiper blade is connected with the inner screw rod 200c-1 through a nut by 316 stainless steel wire with a diameter of 0.3 mm. The scraping blades with the bottom edges (the rigid scraping wires 200 b-1) respectively 20mm, 30mm, 45mm and 52mm can be manufactured according to the sample loading diameters of 20mm, 30mm, 45mm and 52mm of the conventional sample tray 200a so as to meet the sample preparation requirements of sample trays 200a with different sample loading diameters.
The infrared lamp 300 is used for drying paved sample sources and standard sources, and has 50W rated power and adjustable power.
Inner screw fixation knob 200c-5: made of plastic, for fixing the inner screw rod 200c-1, the inner screw rod 200c-1 is fixed not to rotate while the rotating disc 200i is rotated to lay the sample source or the standard source.
Outer screw fixation knob 200c-6: made of plastic, for fixing the outer screw rod 200c-2, the outer screw rod 200c-2 is fixed from rotation while the rotating disc 200i is rotated to lay the sample source or the standard source.
The outer screw rod 200c-2 has a pitch of 1mm, is hollow, has an outer diameter of 5mm and an inner diameter of 2mm, is perpendicular to the rotating disc 200 i/bottom plate 200e, and is made of 304 stainless steel.
The inner screw 200c-1 has a pitch of 0.1mm and a diameter of 2mm, perpendicular to the rotating disk 200 i/base plate 200e. The material is 304 stainless steel.
The diameter of the outer edge of the sample disc 200a is 60mm, the thickness of the sample disc is 0.7mm, the diameter (sample loading diameter) of the sample disc is matched with the probe size of the low-background alpha and beta measuring instrument of the rigid scraping wire 200b-1, the sample disc is usually 20mm, 30mm, 45mm and 52mm, the clean depth is 1.5mm, the surface is smooth, the thickness is even, and the surface polishing treatment is performed, 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. The sample tray 200a is in a horizontal state. The thickness of the manufactured sample source to be measured is relatively uniform and the liquid phase portion in the ash sample to be measured does not flow to the outer edge of the sample tray 200a in the rotation of the wiper 200b and the sample tray 200a with respect to each other, thereby preventing it from contaminating the probe and thus preventing it from increasing the background.
When the device is in use:
(1) Firstly, checking a horizontal bubble meter 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 ground sample ash or standard substances according to measurement requirements, placing the sample disc 200a on a lining support plate 200h, fixing the sample disc by a tabletting clamp 200d, dripping a small amount of absolute ethyl alcohol or a mixed solution of absolute ethyl alcohol and acetone, mixing the sample ash or standard substances with the obtained slurry by using a pin, and spreading the mixture approximately uniformly.
(2) The outer screw rod 200c-2 is fixed by the outer screw rod fixing knob 200c-6 when the outer screw rod 200c-2 is rotated until the scraping blade 200b approaches the sample ash or the standard substance, then the inner screw rod 200c-1 is fixed by the inner screw rod fixing knob 200c-5 when the inner screw rod 200c-1 is rotated until the scraping blade 200b contacts the sample ash or the standard substance, the sample ash or the standard substance is scraped by slowly rotating the rotating disc 200i, and the operation is repeated for a plurality of times to make the scraping blade 200b contact the sample ash or the standard substance and then be scraped until the sample ash or the standard substance is uniformly paved. Preferably, the rotating disc 200i can be manually rotated by an experimenter to rotate the sample disc 200a relative to the wiper blade 200b.
(3) And finally, starting the infrared lamp 300 to dry the sample ash or the standard substance to prepare a sample source or a standard source with uniform and even thickness.
Example 3
This embodiment may be a further improvement and/or addition to embodiments 1, 2 or a combination thereof, and the repeated description is omitted. This example discloses that the whole and/or part of the contents of the preferred implementation of other examples can be complemented by this example without causing conflict or contradiction.
Preferably, the rotational speeds of the relative rotation of the wiper blade 200b and the sample tray 200a are configured in such a manner that they are slowly increased in speed and then gradually decreased to a uniform speed. The rotating disc 200i of the present embodiment is driven by a motor. The speed of the motor is first set by a laboratory person to a controller, such as a PLC controller. The inventors found in the study of the rotation speed versus the measured value that: in the process of performing '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, the liquid phase in the sample source to be measured is easily separated from the solid phase, so that the measurement result is imaged. After the ash sample to be measured is gradually and uniformly spread, the rotation speed can be properly increased so as to improve the centrifugal force and make the ash sample to be measured thinner as much as possible. Then, the rotation speed of the sample tray 200a is reduced to maintain constant rotation, so that the flatness of the sample source to be measured is higher, that is, the thickness of the sample source to be measured is as uniform as possible in the constant speed process.
Example 4
This embodiment may be a further improvement and/or addition to embodiments 1, 2, 3 or a combination thereof, and the repeated description is omitted. This example discloses that the whole and/or part of the contents of the preferred implementation of other examples can be complemented by this example without causing conflict or contradiction.
The preparation device disclosed in this embodiment includes a sample grinder 100 and a sample spreader 200. The sample grinder 100 is used for grinding a solid sample to be measured into an ash sample to be measured which meets the requirement of the sample preparation number 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 a diameter of 4mm and a length of 70mm, is welded in the middle of the upper part of the fixed sleeve 100b, forms an angle of 30 degrees with the fixed sleeve, and is used for supporting the fixed sleeve 100b and fixedly collecting the ground ash sample weighing paper.
The fixed sleeve 100b is made of 304 stainless steel, the upper part is 40mm long, the upper part is 20mm in inner diameter, the lower part is 7mm long, the lower part is 12mm in inner diameter and 2mm in thickness, threads are arranged in the cylinder, and the thread pitch is 0.1mm and is used for fixedly connecting the rotary screw 100c and the U-shaped sieve 100f.
The rotating screw 100c is made of 304 stainless steel, has a diameter of 20mm, a length of 50mm and a screw pitch of 0.1mm, the side edge of the upper end is connected with the handle 100d, and a screw hole with a diameter of 4mm and a depth of 4mm is arranged in the middle of the bottom end and is connected with the connecting rod 100 e.
The handle 100d, which is made of 304 stainless steel and has a length of 40mm and a diameter of 4mm, is connected to the rotary screw 100 c.
The connecting rod 100e is made of 304 stainless steel, has a diameter of 4mm and a length of 38mm, is provided with threads at two ends, has an upper thread length of 4mm and a lower thread length of 3mm, and is respectively connected with the rotating screw 100c and the grinding ball 100g
U type sieve 100f adopts 304 stainless steel to make, thickness 1mm, inside diameter 10mm, long 35mm, and the inner wall is smooth, and the bottom is the hemisphere, and the sieve mesh is located hemisphere bottom, and the sieve mesh is 100 mesh, and the upper end outside sets up length and is 5mm screw thread, links to each other with fixed sleeve 100b bottom.
The grinding ball 100g is supported by 304 stainless steel and is hemispherical, the diameter is 10mm, the spherical surface is smooth, the center of the upper part is provided with a screw hole with the diameter of 4mm and the depth of 3mm, the screw hole is connected with the connecting rod 100e, and when the rotating screw 100c rotates to the bottom end of the upper part of the fixed sleeve 100b, the grinding ball 100g is completely matched with the bottom end of the U-shaped sieve 100f.
At least one optional workflow of the sample grinder 100 is: transferring the sample of the solid matters processed and concentrated into a U-shaped sieve 100f in a grinder 100, screwing the U-shaped sieve 100f with a fixed sleeve 100b, placing weighing paper below the U-shaped sieve 100f, compacting by using a sample grinder bracket 100a, pushing a handle 100d by hand to rotate a rotary screw 100c until a grinding ball 100g is completely matched with the U-shaped sieve 100f, rotating the rotary screw 100c, slightly shifting the U-shaped sieve 100f for a plurality of times by fingers, pushing the handle 100d by hand to rotate the rotary screw 100c until the grinding ball 100g is completely matched with the U-shaped sieve 100f, repeating for a plurality of times, and fully grinding the solid samples processed and concentrated into ash samples. After the sample is ground, the U-shaped sieve 100f and the hemispherical grinding ball 100g are removed, cleaned with ultrapure water and absolute ethyl alcohol and dried for later use.
Example 5
The present embodiment also discloses a method of manufacture that may be carried out by the apparatus of the present invention and/or other alternative components. The method of the invention is implemented, for example, by using the various components of the device of the invention.
The embodiment discloses a preparation method of total alpha and total beta radioactivity measurement samples, which comprises the following steps:
s1: grinding the solid of the sample to be measured into a dust sample to be measured with the mesh number meeting the requirement;
s2: and preparing the ash sample to be measured into a sample source to be measured with relatively uniform thickness.
Wherein, in step S2, the wiper 200b and the sample tray 200a are parallel to each other. At this time, the height between the two is set according to the requirements of the thickness of the sample source to be measured. In the case that the wiper blade 200b and the sample tray 200a are rotated relative to each other, the wiper blade 200b can make the ash sample to be measured into a sample source to be measured having a relatively uniform thickness.
Preferably, the rotational speeds of the relative rotation of the wiper blade 200b and the sample tray 200a are configured in such a manner that they are slowly increased in speed and then decreased to a uniform speed.
It should be noted that the above-described embodiments are exemplary, and that a person skilled in the art, in light of the present disclosure, may devise various solutions that fall within the scope of the present disclosure and fall within the scope of the present disclosure. It should be understood by those skilled in the art that the present description and drawings are illustrative and not limiting to the claims. The scope of the invention is defined by the claims and their equivalents.
Claims (6)
1. A method of preparing a total α and total β radiometric sample, comprising:
grinding the solid of the sample to be measured into a dust sample to be measured with the mesh number meeting the requirement;
preparing a to-be-measured ash sample into a to-be-measured sample source with relatively uniform thickness;
the method is characterized in that:
the preparation device comprises a sample spreading device (200), wherein the sample spreading device (200) is used for preparing a to-be-detected ash sample into a to-be-detected sample source with relatively uniform thickness;
the sample spreading device (200) comprises a sample tray (200 a) and a scraping blade (200 b), wherein the scraping blade (200 b) comprises a rigid scraping wire (200 b-1) for manufacturing the ash sample to be tested into a sample source to be tested in a linear cutting mode, and the diameter of the rigid scraping wire (200 b-1) is 0.2 mm-0.5 mm;
the scraping blade (200 b) and the sample disc (200 a) can rotate relative to each other, so that the ash sample to be tested on the sample disc (200 a) after being stirred by absolute ethyl alcohol or mixed liquid of absolute ethyl alcohol and acetone can rotate relative to the scraping blade (200 b), and the scraping blade (200 b) is contacted with the ash sample to be tested in the process of rotating the sample disc (200 a) relative to the scraping blade;
the scraping blade (200 b) and the sample disc (200 a) are parallel to each other, so that the height between the scraping blade and the sample disc (200 a) limits the manufacturing thickness of the sample source to be tested, and therefore, under the condition that the scraping blade (200 b) and the sample disc (200 a) rotate relative to each other, the scraping blade (200 b) can manufacture the ash sample to be tested in a solid-liquid mixed state into the sample source to be tested with relatively uniform thickness;
the rigid scraping wire (200 b-1) is fixedly connected with the height adjuster (200 c) in a mode that the ash sample to be detected cannot climb to the outer edge of the sample tray (200 a), the height adjuster (200 c) adjusts the rigid scraping wire (200 b-1) to the thickness requirement according to the thickness requirement of the sample source to be detected, the stirred ash sample to be detected is uniformly placed in the central position of the sample tray (200 a), and the rotating speed of relative rotation of the scraping blade (200 b) and the sample tray (200 a) is configured in a mode that the rotating speed is increased gradually after being increased gradually at a first slow speed and then reduced gradually to a uniform speed.
2. The method for preparing a measurement sample according to claim 1, wherein the height adjuster (200 c) comprises an inner screw rod (200 c-1) and an outer screw rod (200 c-2) screw-coupled to the inner screw rod (200 c-1), the outer screw rod (200 c-2) screw-coupled to an outer fixing cylinder (200 c-3),
wherein the rigid scraping wire (200 b-1) is fixedly connected with the inner screw rod (200 c-1),
wherein the pitch of the inner screw (200 c-1) is smaller than the pitch of the outer screw (200 c-2) such that the height between the wiper blade (200 b) and the sample plate (200 a) can be determined at least in a coarse-and-fine-tuning manner.
3. The method of preparing a measurement sample according to claim 2, characterized in that the rigid wiper wire (200 b-1) is connected to the inner screw (200 c-1) by at least two oblique sides, such that the wiper blade (200 b) can be fixedly connected to the height adjuster (200 c) relatively smoothly during the contact of the rigid wiper wire (200 b-1) with the ash sample to be measured.
4. The method of preparing a measurement sample according to claim 1, characterized in that the sample tray (200 a) is in a horizontal state such that the thickness of the manufactured sample source to be measured is relatively uniform and the liquid phase portion in the ash sample to be measured does not flow to the outer edge of the sample tray (200 a) in rotation of the wiper blade (200 b) and the sample tray (200 a) relative to each other.
5. The method of preparing a measurement sample according to claim 1, characterized in that the rigid wiper wire (200 b-1) is a smooth surfaced filament, the length of which matches the size of the sample tray (200 a).
6. The method for preparing a measurement sample according to claim 1,
it is characterized in that the method comprises the steps of,
the dimensions of the sample tray (200 a) and the measurement probe are matched to each other, so that after the preparation of the sample source to be measured is completed, the sample source to be measured laid on the sample tray (200 a) can be directly used for measurement by the measurement probe.
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