CN111624077A - 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 PDF

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Publication number
CN111624077A
CN111624077A CN202010714123.7A CN202010714123A CN111624077A CN 111624077 A CN111624077 A CN 111624077A CN 202010714123 A CN202010714123 A CN 202010714123A CN 111624077 A CN111624077 A CN 111624077A
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sample
measured
source
total
screw rod
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CN111624077B (en
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欧频
俞添虹
黄丽芳
李昱丞
郑雪婷
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01TMEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16Measuring radiation intensity
    • G01T1/167Measuring radioactive content of objects, e.g. contamination
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing 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
    • G01N2001/2866Grinding or homogeneising

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Analytical Chemistry (AREA)
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  • Molecular Biology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention relates to a total alpha and total beta radioactivity measurement sample preparation device and a method. Wherein: the sampler comprises a sample disc and a scraping blade, the height between the scraping blade and the sample disc defines the manufacturing thickness of the sample source to be detected, so that the scraping blade can manufacture the sample to be detected into the sample source to be detected with relatively uniform thickness under the condition that the scraping blade and the sample disc rotate relatively to each other.

Description

Total alpha and total beta radioactivity measurement sample preparation device and method
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 device and method.
Background
Total α and total β radioactivity refer to the total radioactivity levels of α and β radionuclides in a sample due to radionuclide contentGenerally, the radioactivity of the total α and the total β is measured by concentrating or processing samples such as water, organisms, aerosol, soil and the like into solid substances, grinding the solid substances into fine ash (an important premise of uniformly spreading the samples), uniformly spreading the solid substances in a sample tray to prepare sample sources (a measurement source and a sample source), sending the sample sources into a low background α and β measuring instrument to measure and record the counting caused by the fact that particles α and β which are emitted by the sample sources, enter a detector through an air layer between the sample sources and the detector and an entrance window of the detector and still have certain energy trigger the detector, and finally comparing the measurement result with the measurement result of a standard source (a reference source) prepared from standard substances under the same measurement condition to obtain the total α and the radioactivity level of the sample, the total β and the radioactivity level of the total α and the total β, which are relative measurements essentially relative measurements2) 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) Since most of the β 0 and β particles are absorbed or have reduced energy due to self-absorption, only a few α and β particles from the sample and standard source surface layers can be emitted and recorded by the low background α, β meterThe uniformity and flatness of the prepared sample source and standard source thickness have great influence on the accuracy of the total α and β radioactivity measurement results because the air layer between the sample source or standard source and the detector and the entrance window of the detector absorb α and β particles or the energy loss of α and β particles is constant and constant.
Disclosure of Invention
Aiming at the defects of the prior art: the sample spreading method of the sample source and the standard source is a dry spreading method and a wet spreading method. The dry spreading method is that the fully ground ash sample in the sample plate is spread evenly by a pin or a clip, and then is pressed by a stainless steel sample presser matched with the sample plate; the wet spreading method is that a small amount of absolute ethyl alcohol or a mixed solution of absolute ethyl alcohol and acetone is dripped into a sample plate, a pin or a clip is used for stirring and spreading the fully ground ash sample in the sample plate, and then the sample plate is placed under an infrared lamp for drying. Both of the two sample spreading methods need to fully grind the sample which is processed and concentrated into solid matter into fine ash in a ceramic evaporating dish or a mortar in advance, which is an important precondition for uniform sample spreading. Grinding of the concentrated or treated solid matter and tiling of the ash sample are completely completed manually by experimenters, which is time-consuming and labor-consuming, and can not ensure sufficient grinding of the sample, and can not ensure even and smooth thickness of the prepared sample source and the standard source. The dry spreading method is easy to cause the spread sample to scatter and deform or even fall off due to slight vibration in the operation process, is not beneficial to 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 paving method is easy to cause the paved sample to be close to or even overflow the plate edge, the sample or the standard substance can climb outside the plate edge in the drying process, the probe is easy to be polluted in the measuring process, and the background of the 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 measurements. This sample preparation facilities, including grinding the appearance ware and spread the appearance ware, wherein: the sampler grinds the solid sample that awaits measuring into and accords with the sample spreading device sample preparation mesh requirement's the grey sample that awaits measuring, the sample spreading device is used for with the grey sample that awaits measuring is prepared into the relatively even sample source that awaits measuring of thickness, the sample spreading device includes sample dish and doctor-bar, the doctor-bar with the sample dish is parallel to each other and makes highly injecing between the two the thickness of making of the sample source that awaits measuring, thereby the doctor-bar with under the relative pivoted condition each other of sample dish, the doctor-bar can with the grey sample that awaits measuring is made the relatively even sample source that awaits measuring of thickness.
In the invention, the manufactured thickness of the sample source to be measured is finely adjusted, on one hand, the thickness of the sample source to be measured is relatively uniform, and on the other hand, the sample source to be measured is infinitely thin. The infinite thin refers to that a sample source to be detected observed by human eyes is a layer of thin film, so that the interaction between alpha particles, beta particles and solid matters is reduced, the absorbed sample is reduced or the energy loss is reduced, the technical problem that the sample source to be detected in the prior art cannot obtain the infinite thin and extremely thin sample source to be detected 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 detected in the prior art has a certain thickness is further solved.
In the invention, the comparison between 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 be detected by the low-background alpha and beta measuring instrument; 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 preparation device provided by the invention, is more scientific and instructive.
According to a preferred embodiment, the scraping blade comprises a rigid scraping wire for making the ash sample to be detected into a sample source to be detected, and the rigid scraping wire is fixedly connected with the height adjuster in a mode that the ash sample to be detected does not 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 screwed to the inner screw rod, the outer screw rod being screwed to an outer fixed cylinder, wherein the rigid scraper is fixedly connected to 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 and the sample plate can be determined at least in a coarse adjustment followed by a fine adjustment.
According to a preferred embodiment, the rigid scraping wire is connected to the inner screw rod through at least two inclined edges, so that the scraping blade can be fixedly connected with the height adjuster relatively smoothly during the contact of the rigid scraping wire and the ash sample to be measured.
According to a preferred embodiment, the sample plate is in a horizontal state so 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 plate in the rotation of the wiper and the sample plate 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 the rotational speed is first slow, then gradually increased and then gradually decreased to a constant speed.
According to a preferred embodiment, the rigid scraping wire is a smooth-surfaced wire with a diameter of 0.2mm to 0.5mm and a length matching the sample disk loading diameter size.
According to a preferred embodiment, the sample plate loading diameter and the measurement probe are matched to each other in size, so that after the preparation of the sample source to be measured is completed, the sample source to be measured laid on the sample plate can be directly used for measurement by the measurement probe after being dried.
According to a preferred embodiment, the invention also discloses a total alpha and total beta radioactivity measurement sample preparation method, which comprises the steps of grinding a sample to be measured into a gray sample to be measured with a mesh number meeting the requirement; preparing a gray sample to be detected into a sample source to be detected with relatively uniform thickness, and enabling a scraping blade and a sample disc to be parallel to each other so that the height between the scraping blade and the sample disc is set according to the thickness requirement of the sample source to be detected, so that under the condition that the scraping blade and the sample disc rotate relatively to each other, the scraping blade can make the gray sample to be detected into the sample source to be detected with relatively uniform thickness.
According to a preferred embodiment, in the method, the rotation speed of the relative rotation of the scraping blade and the sample plate is configured in a manner that the rotation speed is firstly slow, then increased and then decreased to be uniform.
Drawings
FIG. 1 is a schematic representation of a sample applicator of an overall alpha and overall beta radioactivity measuring sample preparation device according to the present invention;
FIG. 2 is a schematic view of a wiper blade of a total alpha and total beta radioactivity measuring sample preparation device according to the present invention; and
FIG. 3 is a schematic diagram of an applicator of a total alpha and total beta radioactivity measuring sample preparation device according to 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 300: infrared lamp
Detailed Description
This is described in detail below with reference to fig. 1-3.
In the present invention, the sample has at least the following three forms, which are included in the order of the processing steps:
the solid sample to be measured is first concentrated or treated into solid matter with water, biological matter, aerosol, soil and other sample.
And (4) fully grinding a sample of the treated and concentrated solid matter into a gray sample to be tested.
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 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
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 thickness of the prepared sample source to be measured is thick and uneven, and the total alpha and total beta radioactivity measurement results have large fluctuation due to the self-absorption effect of alpha particles and beta particles. 2. In the process of manually flattening the sample source to be measured, the sample source easily climbs to the outer edge of the sample plate, the probe is easily polluted in the measuring process, the background of the alpha and beta measuring instrument with low background is increased, and the accuracy of the total alpha and beta radioactivity measuring result is influenced. Therefore, the present embodiment mainly provides a total α and total β radioactivity measurement and preparation apparatus, which is capable of quickly and conveniently preparing a sample source and a standard source with uniform and flat thickness, and the prepared sample source and standard source do not climb out to pollute a probe. Further, the present embodiment provides a preparation apparatus for improving the accuracy of the total α and total β radioactivity detection and the stability of the measured values. Specifically, the method comprises the following steps:
this example discloses a total alpha and total beta radioactivity measurement sample preparation device. The preparation device comprises a sample spreader 200 for preparing the ash sample to be measured into a sample source to be measured with relatively uniform thickness. Specifically, the sample applicator 200 includes a sample tray 200a and a wiper 200 b. As shown in fig. 1 and 2, the sample plate 200a and the wiper blade 200b are arranged in parallel, and the difference in height between them defines the finished thickness of the sample source to be measured. Generally, the thickness of the sample source to be tested is 0.5-50 mg/cm 2. The inventor of the present invention finely adjusts the thickness of the sample source to be measured, so as to ensure that the thickness of the sample source to be measured is relatively uniform, and to make the sample source to be measured infinitely thin. The infinite thin refers to that a sample source to be detected observed by human eyes is a layer of thin film, so that the interaction between alpha particles, beta particles and solid matters is reduced, the absorbed energy is reduced or the energy loss is reduced, the technical problem that the sample source to be detected in the prior art cannot obtain the infinite thin and ultrathin sample source to be detected with uniform thickness 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 detected in the prior art has a certain thickness is further 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 (or the mixed solution of the absolute ethyl alcohol and the acetone) can rotate relative to the scraping blade 200 b. 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 sample source 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 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 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 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 manufacture the sample without spending great energy 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 ash sample to be measured is gradually driven to the part, corresponding to the sample disc 200a, of the sample disc 200a without the ash sample to be measured laid on the sample disc in a manner similar to the linear cutting, the formed surface of 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 rigid scraping wire 200b-1 is substantially matched with the sample loading diameter of the sample tray 200a to prevent the ash sample to be measured from climbing to the outer edge of the sample tray 200a during relative rotation, thereby preventing the increase of background radioactivity.
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 while rotating the outer screw 200c-2 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 while rotating the inner screw 200c-1 until the wiper 200b comes into contact with the sample ash or the standard substance. 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 contacted with the ash sample to be detected, the rigid scraping wire 200b-1 is not easy to shake based on a triangular stable structure, and the linear cutting and the leveling of the sample source to be detected are relatively stably carried out. 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 2
This embodiment may be a further improvement and/or a supplement to embodiment 1, 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.
This example provides a total alpha and total beta radioactivity measuring sample preparation device, the specific required components of which include:
sample laying support 200 c-4: used for supporting the inner and outer spiral rods, the diameter is 10mm, the length is 200mm, the vertical to the bottom plate 200e, the material is 304 stainless steel.
Bottom plate 200 e: 200mm long, wide 200mm, high 10mm, the upper surface center sets up a diameter and is 60mm, highly is the 304 stainless steel cylinder of 5mm, and the material is 304 stainless steel.
Leveling the base 200 f: under the base plate 200e, the rotating disk 200 i/the base plate 200e can be ensured to be in a horizontal state by adjusting the leveling base 200 f.
Turning disc 200 i: rotate around the cylinder on the bottom plate 200e, diameter 100mm, height 10mm, the concave degree of depth in lower surface center 5mm, diameter 60mm, 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;
horizontal bubble instrument 200 g: checking whether the rotary disk 200 i/the base plate 200e is in a horizontal state;
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 of the sample plate 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 part is connected with the inner spiral 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) respectively being 20mm, 30mm, 45mm and 52mm in length can be manufactured according to the sample loading diameters of 20mm, 30mm, 45mm and 52mm of the current commonly-used sample plate 200a, so that the sample preparation requirements of the sample plates 200a with different sample loading diameters can be met.
The infrared lamp 300 is used for drying the paved sample source and standard source, and has the rated power of 50W and adjustable power.
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, has a thread pitch of 1mm, an outer diameter of 5mm and an inner diameter of 2mm, is perpendicular to the rotating disc 200 i/the bottom plate 200e, and is made of 304 stainless steel.
An internal screw rod 200c-1 with a pitch of 0.1mm and a diameter of 2mm, perpendicular to the rotating disc 200 i/the bottom plate 200 e. 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 low background alpha and beta measuring instrument probe of the rigid scraping wire 200b-1, the diameter (sample loading diameter) is 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 measurement 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 gray sample to be measured does not flow to the outer edge of the sample plate 200a in the rotation in which the wiper blade 200b and the sample plate 200a are relatively rotated with respect to each other, thereby preventing it from contaminating the probe and thus from increasing the background.
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, taking a proper amount of ground sample ash or standard substances according to measurement requirements, putting the sample ash or the standard substances into a sample disc 200a, putting the sample disc 200a on a lining supporting plate 200h, fixing the sample disc by a pressing clamp 200d, dropping a small amount of absolute ethyl alcohol or a mixed solution of the absolute ethyl alcohol and acetone, and mixing the sample ash or the standard substances into slime by using a pin and spreading the slime approximately and uniformly.
(2) Rotating the outer screw rod 200c-2 until the scraping blade 200b approaches the sample ash or the standard substance, 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 sample ash or the standard substance, 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 sample ash or the standard substance, repeating the steps for a plurality of times to enable the scraping blade 200b to contact the sample ash or the standard substance, and then scraping until the sample ash or the standard substance is uniformly paved. 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) Finally, the infrared lamp 300 is started to dry the sample ash or the standard substance to prepare a sample source or a standard source with uniform and flat thickness.
Example 3
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. This example discloses that, without causing conflict or contradiction, the whole and/or partial contents of the preferred embodiments of other examples can be supplemented by this example.
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, 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, and then the measurement result is imaged. 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 4
This embodiment may be a further improvement and/or a supplement to embodiments 1, 2, and 3 or a combination thereof, and repeated details are not repeated. This example discloses that, without causing conflict or contradiction, the whole and/or partial contents of the preferred embodiments of other examples can be supplemented by this example.
The preparation apparatus disclosed in this example includes a sample applicator 100 and a sample applicator 200. The sample grinder 100 is used for grinding the solid sample to be measured into 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 fixed sleeve 100b, forms an angle of 30 degrees with the upper part of the fixed sleeve, and is used for supporting the fixed sleeve 100b and fixing and collecting weighing paper of ground ash samples.
Fixed sleeve 100b, adopt 304 stainless steel to make, the upper portion is long 40mm, upper portion internal diameter 20mm, the long 7mm of lower part, lower part internal diameter 12mm, thickness 2mm sets 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 a diameter of 4mm and a length of 38mm, is provided with threads at two ends, has an upper end thread length of 4mm and a lower end 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, and thickness 1mm, internal 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 100 meshes of sieve mesh, the upper end outside sets up length and is 5mm screw thread, links to each other bottom fixed sleeve 100 b.
Grinding ball 100g adopts 304 stainless steel to support, 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 sample of the treated and concentrated solid matter into a U-shaped sieve 100f in a grinder 100, screwing the U-shaped sieve 100f and a fixed sleeve 100b, placing the weighing paper below the U-shaped sieve 100f, pressing 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 way, slightly pulling the U-shaped sieve 100f by fingers for a plurality of times, then pushing the handle 100d by hand to rotate the rotating screw 100c until the grinding ball 100g is completely matched with the U-shaped sieve 100f, repeating the steps, and fully grinding the treated and concentrated solid sample into a gray sample. After the sample is ground, the U-shaped sieve 100f and the hemispherical grinding ball 100g are detached, cleaned by ultrapure water and absolute ethyl alcohol and dried for later use.
Example 5
This example also discloses a method of manufacture that may be carried out by the apparatus of the invention and/or other alternative components. The method of the present invention is carried out, for example, by using various components of the apparatus of the present invention.
The embodiment discloses a total alpha and total beta radioactivity measurement sample preparation method, which comprises the following steps:
s1: grinding the solid of the sample to be detected into a dust sample to be detected with the mesh number meeting the requirement;
s2: preparing the ash sample to be detected into a sample source to be detected with relatively uniform thickness.
Here, in step S2, 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. The wiper blade 200b can make the gray sample to be measured into a sample source to be measured having a relatively uniform thickness in a state where the wiper blade 200b and the sample tray 200a are rotated relative to each other.
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.
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. An apparatus for preparing total alpha and total beta radioactivity measurement samples comprises a sample applicator (200), the sample applicator (200) is used for preparing an ash sample to be measured into a sample source to be measured with relatively uniform thickness,
it is characterized in that the preparation method is characterized in that,
the applicator (200) comprises a sample tray (200a) and a wiper (200b), wherein:
the scraping blade (200b) and the sample tray (200a) are parallel to each other, so that the height between the scraping blade and the sample tray defines the manufacturing thickness of the sample source to be measured, and therefore under the condition that the scraping blade (200b) and the sample tray (200a) rotate relative to each other, the scraping blade (200b) can manufacture the gray sample to be measured into the sample source to be measured with relatively uniform thickness.
2. The device for preparing measurement samples according to claim 1, characterized in that the scraper (200b) comprises a rigid scraper wire (200b-1) for making the ash sample to be measured into a sample source to be measured,
the rigid scraping wire (200b-1) is fixedly connected with the height adjuster (200c) in a mode that the ash sample to be measured cannot climb to the outer edge of the sample tray (200 a).
3. The measurement sample preparation device according to claim 1 or 2, wherein the height adjuster (200c) comprises an inner screw rod (200c-1) and an outer screw rod (200c-2) screw-coupled to the inner screw rod (200c-1), the outer screw rod (200c-2) screw-coupled to an outer fixed cylinder (200c-3),
wherein the rigid scraping wire (200b-1) is fixedly connected with the inner screw rod (200c-1),
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.
4. The measurement sample preparation device according to one of the preceding claims, wherein the rigid scraping wire (200b-1) is connected to the inner screw rod (200c-1) by at least two oblique edges, such that the scraping blade (200b) can be fixedly connected to the increaser (200c) relatively smoothly during contact of the rigid scraping wire (200b-1) with the ash sample to be measured.
5. The measurement sample preparation device according to one of the preceding claims, characterized in that the sample plate (200a) is in a horizontal state, so that the thickness of the finished sample source to be measured is relatively uniform and the liquid phase fraction in the ash sample to be measured does not flow to the outer edge of the sample plate (200a) in the relative rotation of the wiper blade (200b) and the sample plate (200a) with respect to each other.
6. Device for the preparation of samples for measurement according to any one of the preceding claims, characterised in that the rotational speed of the relative rotation of the wiper blade (200b) and the sample plate (200a) is configured in such a way that it is slow first, then gradually increasing and then gradually decreasing to a constant speed.
7. The measurement sample preparation device according to one of the preceding claims, wherein the rigid scraping wire (200b-1) is a smooth-surfaced filament having a diameter of 0.2mm to 0.5mm and a length matching the dimensions of the sample plate (200 a).
8. The measurement sample preparation device according to one of the preceding claims, characterized in that the dimensions of the sample plate (200a) and the measuring probe are matched to one another such that, after the preparation of the sample source to be measured has been completed, the sample source to be measured laid on the sample plate (200a) can be used directly for measuring probe measurements.
9. A total alpha and total beta radioactivity measurement sample preparation method comprising:
grinding the solid of the sample 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 thickness,
it is characterized in that the preparation method is characterized in that,
the scraping blade (200b) and the sample disc (200a) are parallel to each other, so that the height between the scraping blade and the sample disc (200a) is set according to the manufacturing thickness requirement of the sample source to be detected, and therefore under the condition that the scraping blade (200b) and the sample disc (200a) rotate relative to each other, the scraping blade (200b) can manufacture the gray sample to be detected into the sample source to be detected with relatively uniform thickness.
10. The method for preparing a measurement sample according to claim 9, wherein the rotation speed of the wiper (200b) and the sample plate (200a) relative to each other is configured in such a manner that the speed is first slow, then increased, and then decreased to a constant speed.
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