KR0169578B1 - Droplet paper for the density analysis of ci in liquid - Google Patents

Droplet paper for the density analysis of ci in liquid Download PDF

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KR0169578B1
KR0169578B1 KR1019930031672A KR930031672A KR0169578B1 KR 0169578 B1 KR0169578 B1 KR 0169578B1 KR 1019930031672 A KR1019930031672 A KR 1019930031672A KR 930031672 A KR930031672 A KR 930031672A KR 0169578 B1 KR0169578 B1 KR 0169578B1
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sample
drop
concentration
present
liquid
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KR950019726A (en
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소재춘
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김종진
포항종합제철주식회사
신창식
재단법인산업과학기술연구소
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/20—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using microanalysis, e.g. drop reaction
    • 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

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Abstract

본 발명은, 액체시료중에 함유된 Cl의 농도를 정확히 분석할 수 있도록 하기 위한 것으로, 여과지에 AgNO3와 폴리비닐알코올 보호 콜로이드의 혼합용액을 일정량 적하후 건조시켜서된 점적여지에 관한 것으로서, 점적법을 적용함에 있어 Cl이 Cl2로 변하여 휘발되는 것을 방지함으로써 보다 정확한 Cl 농도를 분석할 수 있게 한다.The present invention relates to accurate dropping of Cl contained in a liquid sample, and to a drop filter obtained by dropping a predetermined amount of a mixed solution of AgNO 3 and a polyvinyl alcohol protective colloid onto a filter paper and then drying it. in application to be able to analyze the exact Cl concentration than by preventing the Cl it is changed to a Cl 2 volatilization.

Description

액체시료중에 함유된 Cl 농도 분석용 점적여지Drip spot for analysis of Cl concentration in liquid samples

제1도는 종래 점적법에 의한 시료 조제과정도.1 is a process for preparing a sample by the conventional drip method.

제2도는 종래 점적여지의 구성을 나타낸 평면도 및 단면도.2 is a plan view and a cross-sectional view showing the configuration of a conventional drop filter.

제3도는 본 발명을 이용하여 작성한 순수한(pure)-Zn 도금액중의 Cl 성분에 대한 검량곡선도이다.3 is a calibration curve diagram for the Cl component in the pure-Zn plating solution prepared using the present invention.

본 발명은 액체시료중 Cl 농도 분석용 점적여지에 관한 것으로서, 특히 점적법 및 형광 X-선 분석방법에 의하여 액체시료중의 Cl 농도를 분석함에 있어 사용되는 점적여지에 관한 것이다.The present invention relates to a drop filter for analyzing Cl concentration in a liquid sample, and more particularly, to a drop filter used for analyzing Cl concentration in a liquid sample by a drop method and a fluorescent X-ray analysis method.

종래 형광 X-선 분석방법을 이용하여 액체시료의 Cl 농도를 분석할때 사용되는 시료조제 방법으로는 액체 시료홀더에 시료용액을 넣고 직접 분석하는 직접법과, 이온교환수지등을 이용하여 분석하고자 하는 원소(Cl)만 농축한 후 분석하는 농축법, 그리고 시료용액을 점적하여 건조시켜 분석하는 점적법 등이 사용되어져 왔다.As a sample preparation method used when analyzing Cl concentration of a liquid sample by using a conventional fluorescent X-ray analysis method, a direct method of directly putting a sample solution into a liquid sample holder and analyzing it by using an ion exchange resin, etc. Concentration methods for concentrating and analyzing only element (Cl) and drip methods for dropping and analyzing sample solutions have been used.

상기 시료 조제 방법들중 직접법은 시료용액을 액체시료홀더에 주입하여야하는 불편함이 있을뿐만 아니라, 시료주입량을 적게 하면 용기내부에 기포가 형성되어 부석오차가 발생할 우려가 있으며, 한편 시료주입량을 많이 하면 시료용액이 넘쳐흘러 금속재 시료홀더가 부식되거나 작업자의 피부를 상하게 하는 문제점들이 있었다.Among the sample preparation methods, the direct method is not only inconvenient to inject the sample solution into the liquid sample holder, but also a small amount of sample injection may cause bubbles to form in the container, which may cause pumice errors. When the sample solution overflowed, there was a problem that the metal sample holder was corroded or the worker's skin was damaged.

농축법의 경우에는 시료용액중에 미량함유된, 분석대상의 원소만을 농축시키는 과정이 매우 복잡하여 시료조제시간이 수시간 이상 소요되는 등의 문제점이 있었다.In the case of the concentration method, the process of concentrating only the elements of the analyte to be contained in the sample solution is very complicated, and the sample preparation time takes several hours or more.

직접법 및 농축법이 각각 상기와 같은 문제점을 지니고 있기 때문에 종래에는 점적법에 의한 시료 조제 방법이 널리 이용되어 왔었다.Since the direct method and the concentration method each have the above problems, the method for preparing a sample by the drop method has been widely used.

점적법에 의한 시료 조제과정은 제1도에서 보는 바와 같다.Sample preparation by drip method is as shown in FIG.

여과지 1 위에 스템프 2를 이용하여 일정크기(약 20㎜의 직경)의 파라핀 원형띠 3를 형성시키고, 마이크로 피펫 4을 사용하여 시료용액 5을 파라핀 원형띠 3 안쪽에 일정량(약 50-60μ1) 적하하여 이를 건조시킨후 시료홀더 6의 크기에 맞게 절단하여 분석을 실시하는 것이다.Using a stamp 2 on the filter paper 1 to form a paraffin circular band 3 of a predetermined size (diameter of about 20㎜), using a micro pipette 4 dropping a predetermined amount (about 50-60μ1) of the sample solution 5 inside the paraffin circular band 3 After drying it, it is cut to fit the size of the sample holder 6 and analyzed.

점적법을 이용하여 시료를 조제할 경우에는, 위에서 보듯이 여러가지 과정을 거치도록 되어 있어 시료조제시간이 길기 때문에 신속한 분석이 곤란하다는 결점이 있었다. 이러한 결점을 해소하기 위하여, 최근에는 제2도에서와 같이 중앙부 8가 천공된, 48㎜ 크기의 직경을 가진 프라스틱링 7에 그 안쪽으로 여과지 10를 파라핀 9을 이용하여 고착시킨 점적여지가 상품화되어 널리 사용되고 있다.When the sample is prepared using the drip method, as described above, various processes are required, and thus, the sample analysis is long, and thus, the rapid analysis is difficult. In order to solve this drawback, in recent years, a spot filter in which a filter paper 10 is fixed with paraffin 9 on a plastic ring 7 having a diameter of 48 mm, in which a central portion 8 is drilled, as shown in FIG. It is widely used.

상기와 같은 점적여지는 점적법을 이용한 액체시료조제과정을 단순화하여 신속한 액체 시료분석을 가능케하고, 나아가 프라스틱링 7을 이용하기 때문에 시료조제과정을 자동화시킬수 있다는 장점도 지니고 있으나, 시료용액을 점적한 후 건조시키는 과정에서 일부 Cl 성분들이 Cl2상태로 휘발되어 날아가 버려 Cl 성분의 정확한 분석이 부가능하다는 문제점이 있었다.Simplify the liquid sample preparation process using the dripping method as described above to enable rapid liquid sample analysis, and furthermore, because plastic ring 7 is used, the sample preparation process can be automated. In the drying process, some Cl components are volatilized into the Cl 2 state and fly away, which makes it impossible to accurately analyze the Cl components.

본 발명은 종래 점적법의 결점을 해결하기 위한 것으로서, 본 발명의 목적은 Cl 성분들이 Cl2상태로 휘발되어 날아가지 않도록 하여, 액체시료중에 함유된 Cl 성분의 농도를 정확히 분석할 수 있게 하는 점적여지를 제공하는 것이다.The present invention is to solve the drawbacks of the conventional drip method, an object of the present invention is to prevent the Cl components volatilized in the Cl 2 state to fly, it is possible to accurately analyze the concentration of Cl components contained in the liquid sample To provide room.

본 발명은 특수약품처리된 점적여지로서, 본 발명의 점적여지를 사용하면, 시료용액이 여지위에 적하되자마자 곧바로 화학반응을 일으켜 안정한 상태의 화합물로 변화되기 때문에 Cl의 휘발성이 방지되어진다.The present invention is a special chemically treated drip filter, and when the drip filter of the present invention is used, the volatilization of Cl is prevented because the sample solution immediately changes to a stable state, causing a chemical reaction to change into a stable compound.

본 발명에서 Cl을 안정한 화합물로 만들어주기 위하여 사용하는 약품은 AgNO3와 분산제인 폴리비닐알코올 보호콜로이드(Poly vinyl alcohol protective colloid)이다. 이중 AgNO3는 용액중에 함유되어 있는 Cl과 반응하여, 하기식에서와 같이 안정한 AgCl로 변화된다.In the present invention, a drug used to make Cl a stable compound is AgNO 3 and a polyvinyl alcohol protective colloid which is a dispersant. AgNO 3 reacts with Cl contained in the solution and is converted into stable AgCl as in the following formula.

한편, 분산제인 폴리비닐알코올 보호콜로이드는 생성되는 AgCl의 침전을 미세한 입자로 만들어준다. 이 폴리비닐알코올 보호콜로이드를 사용하지 않으면 점적여지의 표면이 AgCl의 침전에 의하여 거칠어지게 되고, 나아가 X-선의 산란현상을 초래하여 정확한 Cl농도 분석이 어려워지게 된다.On the other hand, polyvinyl alcohol protective colloid as a dispersant makes the precipitate of the resulting AgCl into fine particles. If this polyvinyl alcohol protective colloid is not used, the surface of the drip spot becomes rough due to the precipitation of AgCl, and furthermore, the scattering phenomenon of X-ray becomes difficult, making accurate Cl concentration analysis difficult.

따라서, 이 폴리비닐알코올 보호콜로이드는 AgCl의 침전을 미세한 입자로 형성시킴으로서 형광 X-선의 산란현상을 사전에 방지하여 Cl의 정확한 농도 분석을 가능케하는 것이다.Therefore, this polyvinyl alcohol protective colloid forms AgCl precipitate into fine particles to prevent scattering of fluorescent X-rays in advance, thereby enabling accurate concentration analysis of Cl.

본 발명의 점적여지는, 적정농도의 AgNO3와 0.4%의 폴리비닐알코올 보호콜로이드의 혼합용액을 조제한 후, 이 혼합용액을 일정량 여과지에 적하한후 건조기로 충분히 건조시킴으로써 제조한다. 종래의 프라스틱링에 여과지를 고착시켜 형성된 점적여지를 사용할수도 있다.The present invention is prepared by preparing a mixed solution of AgNO 3 and 0.4% polyvinyl alcohol protective colloid at an appropriate concentration, and then dropping the mixed solution on a predetermined amount of filter paper and drying it sufficiently with a drier. It is also possible to use a drop filter formed by fixing filter paper to a conventional plastic ring.

이하 실시예에 의거 본 발명을 설명한다.The present invention will be described based on the following examples.

[실시예]EXAMPLE

1N-AgNO3용액 1ℓ와 0.4% 폴리비닐알코올 보호콜로이드용액 1ℓ를 조제한 후, 이 두 용액을 혼합하여, 이를 마이크로 디스펜서를 이용하여 종래의 점적여지의 여과지의 소정부위에 50μl 점적한 후 건조기로 충분히 건조시켜 본 발명의 점적여지를 제조하였다.After preparing 1 L of 1N-AgNO 3 solution and 1 L of 0.4% polyvinyl alcohol protective colloidal solution, the two solutions were mixed, and 50 µl of the solution was applied to a predetermined portion of a conventional filter paper using a micro dispenser, followed by a drier. Drying prepared the drip staple of the present invention.

한편, 순수한 -Zn 도금액과 유사한 조성을 가지는 표준용액 12개를 조제한후, 각 표준용액 50μl를 본 발명의 점적여지에 점적한후 건조기로 건조시켰다. 그리고, 형광 X-선 분석기로 강도를 측정하여 검량선을 작성하였다. 제3도는 그 결과를 나타낸 것이다.On the other hand, after preparing 12 standard solutions having a composition similar to that of a pure -Zn plating solution, 50 µl of each standard solution was added to the drop space of the present invention, and then dried by a drier. And the intensity | strength was measured with the fluorescent X-ray analyzer, and the analytical curve was created. 3 shows the result.

측정결과, Cl에 대한 검량곡선의 정확도는 0.214 이었으며, 작성된 검량곡선을 이용하여 미지농도의 도금용액을 측정한 후, 다른 방법에 의한 분석 결과와 비교하여, 그결과를 표 1에 나타내었다.As a result of measurement, the accuracy of the calibration curve for Cl was 0.214. After measuring the plating solution of unknown concentration using the prepared calibration curve, the results are shown in Table 1 in comparison with the analysis results by other methods.

표 1에 나타난 바와같이, 본 발명의 점적여지를 사용한 경우의 분석결과는 종래의 점적법에 의한 경우의 분석결과와 크게 차이가 있었다.As shown in Table 1, the analysis results in the case of using the drop margin of the present invention were significantly different from the analysis results in the case of the conventional drop method.

그러나, 본 발명의 경우가, 보다 정확한 방법인 습식분석에 의한 경우의 분석치와 극히 근접해 있음을 볼때, 본 발명의 점적여지를 사용하는 것이 종래의 점적법에 의하는 경우와 비교하여 훨씬 정확한 것임을 알 수 있었다.However, in the case of the present invention, which is very close to the analysis value obtained by the wet analysis, which is a more accurate method, it is found that the use of the drip spot of the present invention is much more accurate than the case of the conventional drop method. Could.

Claims (3)

여과지에 AgNO3와 폴리비닐알코올 보호 콜로이드 분산제의 혼합용액을 적하한 후 이를 건조시켜서된 점적여지.A drop of mixed solution of AgNO 3 and a polyvinyl alcohol protective colloidal dispersant was added dropwise to the filter paper, followed by drying. 제1항에 있어서, 상기 AgNO3의 양이 분석대상 액체시료중의 예상함유 Cl 보다 많도록 혼합용액을 여과지에 적하시켜서된 점적여지.The drop solution according to claim 1, wherein the mixed solution is added dropwise to the filter paper so that the amount of AgNO 3 is greater than the expected content of Cl in the liquid sample to be analyzed. 제1항에 있어서, 상기 폴리비닐알코올 보호콜로이드 분산제의 양이 분석대상 액체시료중의 예상함유 Cl보다 많도록 혼합용액을 여과지에 적하시켜서 된 점적여지.The drop solution according to claim 1, wherein the mixed solution is added dropwise to the filter paper so that the amount of the polyvinyl alcohol protective colloidal dispersant is larger than the expected Cl in the liquid sample to be analyzed.
KR1019930031672A 1993-12-30 1993-12-30 Droplet paper for the density analysis of ci in liquid KR0169578B1 (en)

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