KR970006680Y1 - Liquid sample holder in x-ray analysis method - Google Patents

Liquid sample holder in x-ray analysis method Download PDF

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Publication number
KR970006680Y1
KR970006680Y1 KR2019930030066U KR930030066U KR970006680Y1 KR 970006680 Y1 KR970006680 Y1 KR 970006680Y1 KR 2019930030066 U KR2019930030066 U KR 2019930030066U KR 930030066 U KR930030066 U KR 930030066U KR 970006680 Y1 KR970006680 Y1 KR 970006680Y1
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sample
holder
sample holder
liquid sample
analysis
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KR2019930030066U
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KR950020387U (en
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소재춘
조용호
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포항종합제철 주식회사
조말수
재단법인 산업과학기술연구소
백덕현
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025—Sample holders or supports therefor

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

없음.none.

Description

형광 엑스(X)-선 분석법을 이용한 액체시료 분석용 시료홀더Sample holder for liquid sample analysis using fluorescence X-ray analysis

제1도는 종래의 점적법에 의한 시료조에 과정을 도시한 구성도1 is a block diagram showing a process in a sample tank by a conventional drip method

제2도는 종래의 시료홀더를 도시한 분해사시도2 is an exploded perspective view showing a conventional sample holder

제3도(A) 및 (B)는 본 고안에 따른 액 시료분석용 점적여지 장착구의 평면도3 (A) and (B) is a plan view of the drip holding device for analyzing a liquid sample according to the present invention

제4도는 제3도(A)의 A-A선 단면도4 is a cross-sectional view taken along the line A-A of FIG.

제5도는 본 고안의 시료홀더에 점적여지 장착구를 결합하는 상태를 도시한 사시도5 is a perspective view showing a state in which the drip stop mounting device is coupled to the sample holder of the present invention

*도면의 주요 부분에 대한 부호의 설명** Description of the symbols for the main parts of the drawings *

1 : 프라스틱 링2 : 원형천공1: plastic ring 2: round hole

3 : 파라핀4 : 점적여지3: paraffin 4: drip hold

5 : 스틸링6 : 점적여지 장착구5: steel ring 6: drop opening

7 : 홀더마개8 : 홀더시료몸체7: holder stopper 8: holder sample body

9 : 알루미늄판10 : 시료홀더9: aluminum plate 10: sample holder

11 : 자석11: magnet

본 고안은 형광 X-선 분석법을 이용하여 점적법에 의한 시료조제과정을 거쳐 액체 시료중에 함유되어 있는 각종 성분 원소들을 정량 분석하는 경우, 이에 사용되는 점적여지를 시료홀더에 자동으로 장입 시킬 수 있도록 한 형광 X-선 분석법을 이용한 액체 시료 분석용 홀더에 관한 것이다.The present invention uses a fluorescent X-ray method to quantitatively analyze various component elements contained in a liquid sample through a dropwise sample preparation process, so that the drop space used for this can be automatically loaded into the sample holder. A holder for analyzing a liquid sample using a fluorescent X-ray analysis method.

일반적으로 형광 X-선 분리법을 이용하여 액체시료를 분석할 때 사용되는 사료조제 방법에 있어서는, 액체시료 홀더에 시료용액을 직접 넣고 분석을 실시하는 직접법과, 이온교환수지등을 이용하여 분석하고져 하는 원소들을 농축시킨 후 이를 분석하는 농축법과, 시료용액을 건조시켜 시료 홀더의 크기에 맞게 절단하여 분석을 실시하는 점적법등이 알려져 있다.In general, the feed preparation method used when analyzing a liquid sample by using a fluorescent X-ray separation method, the direct method to put the sample solution directly into the liquid sample holder for analysis and the analysis using ion exchange resin, etc. Concentration methods for concentrating elements and analyzing them, and drip methods, in which a sample solution is dried and cut to fit the size of a sample holder, are analyzed.

그러나 이러한 시료제조방법들중 직접법은 시료용액을 액체시료 홀더에 시료용액을 주입하는 것이 불편하게 되어 있을 뿐만 아니라 시료 주입량을 적제하면 용기내부에 기포가 형성되어 분석오차가 발생할 우려가 있으며, 이를 방지하기 위하여 시료주입량을 많이 하면 시료용액이 넘쳐 흘러 금속재 시료홀더가 부식되거나 작업자의 피부를 상하게 하는 문제점들이 있었으며, 농축법의 경우에도 시료 용액중에 미량 함유된 일부 분석하고자 하는 원소들만을 농축시키는 과정이 복잡하고 시료조제시간이 수시간 이상 소용되는 등의 문제점들을 갖고 있어 액체 시료를 분석할때는 주로 점적법에 의한 시료제조방법이 널리 이용되고 있는 실정인 것이다.However, the direct method among these sample manufacturing methods is not only inconvenient to inject the sample solution into the liquid sample holder, but also the amount of sample injection may cause bubbles to form inside the container, which may cause an analysis error. In order to increase the amount of sample injection, the sample solution overflows and the metal sample holder is corroded or the skin of the worker is damaged.In the case of the concentration method, only a part of the sample to be analyzed is concentrated in the sample solution. It is complicated and has a problem such that the sample preparation time is used for several hours or more, and when analyzing a liquid sample, the sample preparation method by the drip method is widely used.

이와 같은 점적법에 의한 시료용액의 분석은 제1도에 도시한 바와 같이, 여과지(31)위에 스탬프(32)를 이용하여 일정크기(약 20㎝의 지경)의 파라핀원형띠(33)를 형성한 후 마이크로 피펫(34)를 사용하여 시료 용액(35)을 파라핀 원형띠(33)내에 일정량(약 50-60㎕) 적하하고, 이를 건조시킨 다음 시료홀더(36)의 크기에 맞게 절단하여 분석을 실시하는 것이다.As shown in FIG. 1, the analysis of the sample solution by the dropping method was performed by using a stamp 32 on the filter paper 31 to form a paraffin circular band 33 having a predetermined size (about 20 cm diameter). After the sample solution 35 was dropped into the paraffin circular band 33 by using a micro pipette 34, a predetermined amount (about 50-60 μl) was dropped, dried, and cut to fit the size of the sample holder 36. Will be carried out.

그러나, 상기와 같은 점적법을 이용하여 시료를 분석할 경우에는, 제2도에 도시한 바와 같이, 시료조제를 완료한 점적여지(37)를 시료홀더에 넣어 이를 분석하기 위해 나사식으로 결합되는 시료홀더 마개를 완전히 열고, 스프링(39)위에 위치된 시료지지판(40)상측에 점적여지(37)를 올려놓은 다음, 재차 시료홀더 마개(38)를 완전히 결합시킨 후 분석하도록 함으로써, 이와 같은 시료홀더에 점적 여지를 장입하는 과정이 복잡하게 되어 액체 시료 분석자동화 시스템을 개발하기 위한 시도가 있음에도 불구하고 자동화 작업에 많은 문제점이 있었던 것이다.However, in the case of analyzing the sample using the above dropping method, as shown in FIG. 2, the drop stop 37, which has completed the sample preparation, is screwed to the sample holder for analysis. By opening the sample holder stopper completely, placing the drop stop 37 on the upper side of the sample support plate 40 positioned on the spring 39, and then again combining the sample holder stopper 38 to analyze the sample. Although the process of loading drip space into the holder is complicated, there have been many problems in the automation work despite the attempt to develop an automated liquid sample analysis system.

본 고안은 상기한 바와 같은 종래의 여러 문제점들을 개선시키기 위하여 안출된 것으로서, 그 목적은, 점적여지의 장착과정을 용이하게 수행할 수 있고, 이로 인한 시료분석의 자동화 시스템에 적용가능하도록 하여, 별도의 말루미늄판등을 준비할 필요없이 손쉽게 시료 분석작업을 수행할 수 있는 형광 X-선 분석법을 이용한 액체시료 분석용 시료 홀더를 제공하는데 있다.The present invention has been made in order to improve the various problems of the prior art as described above, the object of which is to facilitate the mounting process of drip spot, thereby making it applicable to the automated system of sample analysis, thereby The present invention provides a sample holder for analyzing a liquid sample using fluorescence X-ray analysis that can easily perform sample analysis without the need to prepare aluminum plates.

이하, 첨부된 도면에 의거하여 본 고안의 실시예를 상세하게 설명하면 다음과 같다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

제3도(A)(B)는 본 고안에 따른 액체시료 분석용 점적여지 장착구의 평면도 및 저면도이며, 제4도는 제3도의 A-A선 단면도이고, 제5도는 본 고안의 시료홀더에 점적여지를 결합하는 상태를 도시한 사시도로서, 본 고안은 시료홀더(10)와 그 상측에 위치되는 점적여지 장착구(6)로서 구성된다.3 (A) and (B) are a plan view and a bottom view of a drop filter mounting fixture for analyzing a liquid sample according to the present invention, and FIG. 4 is a cross-sectional view taken along line AA of FIG. 3, and FIG. As a perspective view showing a state that combines, the subject innovation is configured as a sample holder 10 and the drop opening mounting hole 6 located above.

상기 점적여지 장착구(6)는, 프라스틱 링(1)의 상측에 4개의 원형천공(2)이 형성되고, 천공되지 않은 4방향에는 파라핀(3)이 부착된 점적여지(4)를 고착하며, 상기 프라스틱링(1)의 하단으로 스틸링(5)이 착설된다.The drip stop mounting hole 6, four circular perforations (2) are formed on the upper side of the plastic ring (1), and in the non-perforated four directions to secure the drip stop (4) attached to the paraffin (3) The steel ring 5 is installed at the lower end of the plastic ring 1.

또한, 상기 시료홀더(10)에 있어서는 홀더마개(7)와 홀더시료 몸체(8)가 일체로 형성토록 되며, 상기 홀더마개(7)의 상측에는 고순도 알루미늄판(9)이 착설되는 한편, 상기 알루미늄판(9)의 주변에는 상기 점적여지 장착구(6) 하단의 스틸링(5)과 상호 일치되어 결합토록 자석(11)이 설치되는 구성으로 이루어진다.In addition, in the sample holder 10, the holder stopper 7 and the holder sample body 8 are integrally formed, and a high purity aluminum plate 9 is installed on the holder stopper 7, The periphery of the aluminum plate 9 is made of a configuration in which the magnet 11 is installed so as to coincide with the steel ring 5 at the lower end of the drip stop mounting hole 6.

이와 같은 구조로 구성된 본 고안의 작용 및 효과를 설명하면 다음과 같다.Referring to the operation and effects of the present invention composed of such a structure as follows.

즉, 제3도 내지 제5도에 도시한 바와 같이, 종래의 같은 방법으로 점적여지 장착구(6)상에 점적여지(4)에 시료용액을 일정량 적하하여 이를 건조시킨 후, 상기 점적여지 장착구(6)를 시료홀더(10)위에 올려놓게 되면 점적여지 장착구(6)의 플라스틱링(1) 하단에 착설된 스틸링(5)이 시료홀더(10)의 상단에 설치된 자석(11)의 자력에 의해 시료홀더(10)에 고정되어 손쉽게 점적여지 장착구(6)를 시료홀더(10)에 부착시킬 수 있게 된다.That is, as shown in Figs. 3 to 5, a predetermined amount of sample solution is added dropwise to the drip sheet 4 on the drip sheet mounting hole 6 in the same manner as the conventional method, and then dried. When the sphere 6 is placed on the sample holder 10, the magnet 11 installed on the top of the sample holder 10 is a steel ring 5 installed at the bottom of the plastic ring 1. It is fixed to the sample holder 10 by the magnetic force of the drip-mounted mounting hole 6 can be easily attached to the sample holder 10.

또한, 상기 시료홀더(10)의 중앙에 착설된 알루미늄판(9)은, 점적여지 장착구(6)의 점적여지(4)상의 시료용액을 형광 X-선 분석하는 경우, 형광 X-선 분석기의 X-레이(Ray)튜브로부터 발생되는 X-선을 점적여지(4)의 시료용액으로 조사하면, X-선이 상기 점적여지(4)를 투과하여 시료홀더(10)의 안쪽까지 도달되어 산란, 여기되는 현상을 방지함으로서 효과적인 분석작업이 이루어지도록 한다. 이는 알루미늄판(9)이 없으면, X-선의 산란이 발생하게 되어 동일시료의 경우에도 반복하여 분석할 수 없을 정도로 형광 X-선의 강도가 심하게 흔들리는 현상이 발생되지만, 고순도의 알루미늄판(9)을 점적여지(4)에 받치고 분석을 하면 이러한 현상이 방지된다. 따라서 시료홀더(10) 상단에 알루미늄판(9)을 일체형으로 형성시킴으로써, 별도의 알루미늄판을 준비할 필요가 없게 된다.In addition, the aluminum plate 9 installed in the center of the sample holder 10 is a fluorescent X-ray analyzer when the sample solution on the drop holder 4 of the drop holder is mounted. When the X-rays emitted from the X-ray tube of the sample solution of the drop stop (4) is irradiated, the X-rays penetrate the drop stop (4) to reach the inside of the sample holder 10 By preventing scattering and excitation, effective analysis can be performed. This is because without the aluminum plate 9, the scattering of X-rays occurs, so that the intensity of the fluorescence X-rays is severely shaken so that it cannot be repeatedly analyzed even in the same sample. This phenomenon can be prevented by supporting the spot stop (4). Therefore, by forming the aluminum plate 9 integrally on the upper end of the sample holder 10, there is no need to prepare a separate aluminum plate.

이상과 같이, 본 고안에 따른 형광 X-선 분석법을 이용한 액체시료 분석용 시료홀더에 의하며, 시료홀더의 상단에 자석을 설치하여 상기 자석의 자력에 의해 점적 여지의 분리 및 결합이 용이하게 수행될 수 있도록 구성함은 물론, 이로 인한 시료분석의 자동화 시스템에 적용이 가능하게 될 수 있으며, 시료 홀더의 중앙에 고순도 알루미늄판을 일체로 착설함으로 인하여 별도의 알루미늄을 준비할 필요없이 손쉽게 시료분석작업을 수행할 수 있는 우수한 효과가 있다.As described above, by the liquid sample analysis sample holder using the fluorescent X-ray analysis method according to the present invention, by installing a magnet on the upper end of the sample holder can be easily separated and combined by the magnetic force of the magnet In addition, it can be applied to the automated system for analyzing the sample, and the high purity aluminum plate is installed at the center of the sample holder. There is an excellent effect that can be performed.

Claims (1)

프라스틱 링(1)의 상측에 4개의 원형천공(2)이 형성되고, 천공되지 않은 4방향으로 파라핀(3)이 착설된 점적여지(4)를 고정복귀하며, 상기 프라스틱링(1)의 하단에는 스틸링(5)이 착설되는 점적여지 장착구(6):Four circular perforations (2) are formed on the upper side of the plastic ring (1), and fixed return to the drip stop (4) in which the paraffin (3) is installed in four unperforated directions, the lower end of the plastic ring (1) On the drip stop mounting hole (6) where the steel ring (5) is mounted: 홀더마개(7)와 홀더시료 몸체(8)가 일체로 형성되며, 상기 홀더마개(7)의 상부면에는 상기 점적여지(6) 하단의 스틸링(5)이 상호 일치되어 결합하도록 자석(11)이 설치되는 시료홀더(10)를 구비한 형광 X-선 분석법을 이용한 액체시료 분석용 시료홀더에 있어서, 상기 홀더마개(7)의 상측중앙에는 형광 X-선의 산란 및 여기 현상을 방지하는 알루미늄판(9)이 부착됨을 특징으로 하는 형광 X-선 분석법을 이용한 액체시료분석용 시료홀더.The holder stopper 7 and the holder sample body 8 are integrally formed, and the magnet ring 11 is formed on the upper surface of the holder stopper 7 so that the steel rings 5 at the bottom of the drop stop 6 coincide with each other. In the sample holder for liquid sample analysis using the fluorescent X-ray analysis method provided with a sample holder 10 is installed, the upper center of the holder stopper (7) to prevent the scattering and excitation of the fluorescent X-rays aluminum Sample holder for liquid sample analysis using a fluorescence X-ray analysis characterized in that the plate (9) is attached.
KR2019930030066U 1993-12-28 1993-12-28 Liquid sample holder in x-ray analysis method KR970006680Y1 (en)

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KR950020387U KR950020387U (en) 1995-07-26
KR970006680Y1 true KR970006680Y1 (en) 1997-07-01

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