KR102126606B1 - Method for analyzing contents of k in la compounds - Google Patents
Method for analyzing contents of k in la compounds Download PDFInfo
- Publication number
- KR102126606B1 KR102126606B1 KR1020170084252A KR20170084252A KR102126606B1 KR 102126606 B1 KR102126606 B1 KR 102126606B1 KR 1020170084252 A KR1020170084252 A KR 1020170084252A KR 20170084252 A KR20170084252 A KR 20170084252A KR 102126606 B1 KR102126606 B1 KR 102126606B1
- Authority
- KR
- South Korea
- Prior art keywords
- lscf
- acid
- content
- solution
- present
- Prior art date
Links
Images
Classifications
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4083—Concentrating samples by other techniques involving separation of suspended solids sedimentation
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4088—Concentrating samples by other techniques involving separation of suspended solids filtration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N2021/258—Surface plasmon spectroscopy, e.g. micro- or nanoparticles in suspension
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
본 발명은 LSCF 내의 K 함량의 분석방법에 관한 것으로, LSCF를 질산(HNO3)과 염산(HCl)에 용해시킨 후 불산(HF)을 첨가하여 La만을 선택적으로 침전시킴으로써 La에 의한 분광 간섭을 제거하여 K의 함량을 유도결합 플라즈마 분광광도계(ICP-OES)를 이용하여 정확히 분석할 수 있다. The present invention relates to a method for analyzing the K content in LSCF, by dissolving LSCF in nitric acid (HNO 3 ) and hydrochloric acid (HCl) and adding hydrofluoric acid (HF) to selectively precipitate only La to eliminate spectral interference caused by La. Therefore, the content of K can be accurately analyzed using an inductively coupled plasma spectrophotometer (ICP-OES).
Description
본 발명은 고체 산화물 연료 전지(Solid Oxide Fuel Cell, SOFC)의 캐소드(cathode, 환원전극) 물질, 구체적으로 LSCF(La0.6Sr0.4Co0.2Fe0.8O3) 내에 존재하는 K 함량의 분석방법에 관한 것이다.The present invention relates to a cathode oxide (cathode, cathode) material of a solid oxide fuel cell (SOFC), specifically, a method for analyzing the K content present in LSCF (La0.6Sr0.4Co0.2Fe0.8O3). .
종래 고체 산화물 연료 전지(SOFC)의 캐소드 물질인 LSCF(La0.6Sr0.4Co0.2Fe0.8O3)를 합성하기 위해서는 La 니트레이트(nitrate), Sr 니트레이트, Co 니트레이트 및 Fe 니트레이트를 물에 용해시킨 후 침전제로서 KOH를 이용하여 공침시켰다. 이에 따라 LaSrCoFe-하이드록사이드가 만들어지는데, 이때 침전제로 사용된 KOH에서 기인한 K가 매트릭스(matrix)로 존재하게 되며, K를 제거하기 위한 세척공정을 확립하기 위해 유도결합 플라즈마 분광광도계(ICP-OES)를 이용한 K의 정확한 정량분석이 필요했다. 종래 기술 중 한 가지는 LSCF를 질산, 염산 또는 이들의 혼합산에 녹인 후 용출된 K를 ICP-OES를 이용하여 정량분석하는 것이었는데, LSCF가 이들 산에 잘 녹기는 하나, 이들 산은 LSCF를 모두 녹이기 때문에 이로부터 ICP-OES를 이용하여 K의 함량을 측정할 경우 무기물에 의한 분광 간섭으로 인하여 K의 정확한 측정값을 얻기가 어려웠다. 또 다른 방법은, LSCF에 초순수와 산을 넣고 K를 용출시킨 후 LSCF를 여과하여 분석하는 것이었는데, K를 1,000℃에서 소성한 후 세척하는 것이어서 K가 산화칼륨을 형성하여 쉽게 녹아 나오지 않았다. 이에, 실제 측정값보다 낮은 K 값이 측정되었다. 실제로 상기 측정 과정을 2회 반복하더라도 서로 다른 측정값을 보여서 K가 모두 녹아 나오지 않음을 확인할 수 있었다.In order to synthesize LSCF (La0.6Sr0.4Co0.2Fe0.8O3), a cathode material of a conventional solid oxide fuel cell (SOFC), La nitrate, Sr nitrate, Co nitrate, and Fe nitrate are dissolved in water. After precipitation, coprecipitation was performed using KOH as a precipitating agent. As a result, LaSrCoFe-hydroxide is produced. At this time, K derived from KOH used as a precipitating agent exists as a matrix, and an inductively coupled plasma spectrophotometer (ICP-) is used to establish a washing process for removing K. OES) required accurate quantitative analysis of K. One of the prior arts was to dissolve LSCF in nitric acid, hydrochloric acid, or a mixed acid thereof, and then quantitatively analyze the eluted K using ICP-OES. LSCF dissolves well in these acids, but these acids dissolve all LSCF. Therefore, when measuring the content of K using ICP-OES, it was difficult to obtain an accurate measurement of K due to spectral interference caused by inorganic substances. Another method was to add ultrapure water and acid to the LSCF, elute K, and then analyze the LSCF by filtration. K was calcined at 1,000°C and washed, so that K did not readily dissolve by forming potassium oxide. Thus, a K value lower than the actual measured value was measured. In fact, even if the above measurement process was repeated twice, it was confirmed that K was not melted by showing different measurement values.
따라서, 위와 같은 단점들을 나타내지 않으면서, 무기물에 의한 분광 간섭 없이 LSCF 내의 K의 함량을 ICP-OES를 이용하여 정확히 분석하기 위한 새로운 방법을 개발할 필요가 있었다.Therefore, it is necessary to develop a new method for accurately analyzing the content of K in LSCF using ICP-OES without spectral interference by inorganic substances without exhibiting the above-described disadvantages.
본 발명은 LSCF 내에 매트릭스로 존재하는 K의 함량을 ICP-OES를 이용하여 정확히 분석하는 방법을 제공하는 것을 목적으로 한다.An object of the present invention is to provide a method for accurately analyzing the content of K present as a matrix in LSCF using ICP-OES.
본 발명에서는 선행 기술의 단점을 극복하고자 연구한 결과 LSCF에서 La만을 선택적으로 제거함으로써 La에 의한 K의 분광 간섭이 나타나지 않는 방법을 제공하게 되었다.In the present invention, as a result of studying to overcome the disadvantages of the prior art, by selectively removing only La from the LSCF, a method in which spectral interference of K by La does not appear is provided.
즉, 본 발명은 LSCF를 질산(HNO3)과 염산(HCl)에 용해시킨 후 불산(HF)을 첨가하여 La만을 선택적으로 침전시키는 것을 특징으로 한다.That is, the present invention is characterized in that only LS is selectively precipitated by adding hydrofluoric acid (HF) after dissolving LSCF in nitric acid (HNO 3 ) and hydrochloric acid (HCl).
구체적으로 본 발명은,Specifically, the present invention,
LSCF를 칭량하는 단계;Weighing the LSCF;
상기 LSCF에 질산(HNO3), 염산(HCl) 및 과산화수소를 첨가하여 상기 LSCF를 용해시키는 단계;Dissolving the LSCF by adding nitric acid (HNO 3 ), hydrochloric acid (HCl) and hydrogen peroxide to the LSCF;
상기 용액을 물 중탕으로 가열하고 산을 소량만 남기고 제거하는 단계;Heating the solution with a water bath and removing only a small amount of acid;
상기 용액에 초순수를 첨가하여 희석시키는 단계;Diluting the solution by adding ultrapure water;
상기 희석액에 불산(HF)을 첨가하여 La만을 선택적으로 침전시키는 단계; 및Selectively precipitating only La by adding hydrofluoric acid (HF) to the diluent; And
상기 용액을 여과하여 La만을 선택적으로 제거하는 단계를 포함하는, K 함량의 분석방법을 제공한다.It provides a method for analyzing the K content, including the step of selectively removing only La by filtering the solution.
본 발명의 한 실시양태에서, LSCF에 대한 불산의 사용 비율은 중량비로 1:0.1 내지 1:10이다.In one embodiment of the invention, the ratio of use of hydrofluoric acid to LSCF is 1:0.1 to 1:10 by weight.
본 발명의 한 실시양태에서, 상기 불산의 사용량은 0.02mL 내지 2mL이다.In one embodiment of the invention, the amount of hydrofluoric acid used is from 0.02 mL to 2 mL.
본 발명의 한 실시양태에서, 상기 물 중탕으로 10분 내지 12시간 동안 가열할 수 있다.In one embodiment of the invention, the water bath may be heated for 10 minutes to 12 hours.
본 발명의 한 실시양태에서, 상기 여과는 필터, 예를 들어, 시린지 필터(PTFE Syringe Filter)를 사용하여 수행할 수 있다.In one embodiment of the present invention, the filtration can be performed using a filter, for example, a PTFE Syringe Filter.
본 발명의 한 실시양태에서, K의 정량분석은 유도결합 플라즈마 분광광도계(ICP-OES)를 이용한다.In one embodiment of the present invention, the quantitative analysis of K uses an inductively coupled plasma spectrophotometer (ICP-OES).
본 발명의 K 함량의 분석방법은 질산과 염산에 용해시킨 LSCF에 불산을 첨가하여 La만을 선택적으로 침전시킴으로써 La에 의한 분광 간섭을 제거하여 K의 함량을 정확히 분석할 수 있다.The method for analyzing the K content of the present invention can accurately analyze the content of K by removing spectral interference caused by La by selectively precipitating only La by adding hydrofluoric acid to the LSCF dissolved in nitric acid and hydrochloric acid.
도 1은 선행 기술의 K 함량의 분석방법에 따른 La에 의한 분광 간섭을 보여 주는 분광광도계 스펙트럼이다(비교예).
도 2는 본 발명의 K 함량의 분석방법에 따라 La를 제거한 후의 분광광도계 스펙트럼이다(실시예).Figure 1 is a spectrophotometer spectrum showing the spectral interference by La according to the analysis method of the K content of the prior art (comparative example).
2 is a spectrophotometer spectrum after removing La according to the analysis method of the K content of the present invention (Example).
이하에서는, 본 발명을 보다 구체적으로 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
본 명세서 및 청구범위에 사용된 용어나 단어는 통상적이거나 사전적인 의미로 한정해서 해석되어서는 안 되며, 발명자는 그 자신의 발명을 가장 최선의 방법으로 설명하기 위해 용어의 개념을 적절하게 정의할 수 있다는 원칙에 입각하여 본 발명의 기술적 사상에 부합하는 의미와 개념으로 해석되어야만 한다.The terms or words used in the specification and claims should not be interpreted as being limited to the ordinary or dictionary meanings, and the inventor can appropriately define the concept of terms in order to best describe his or her invention. Based on the principle that it should be interpreted as meanings and concepts consistent with the technical spirit of the present invention.
본 발명에 따른 K 함량의 분석방법은 Analysis method of the K content according to the present invention
LSCF를 칭량하는 단계;Weighing the LSCF;
상기 LSCF에 질산, 염산 및 과산화수소를 첨가하여 상기 LSCF를 용해시키는 단계;Dissolving the LSCF by adding nitric acid, hydrochloric acid and hydrogen peroxide to the LSCF;
상기 용액을 물 중탕으로 가열하고 산을 소량만 남기고 제거하는 단계;Heating the solution with a water bath and removing only a small amount of acid;
상기 용액에 초순수를 첨가하여 희석시키는 단계;Diluting the solution by adding ultrapure water;
상기 희석액에 불산을 첨가하여 La만을 선택적으로 침전시키는 단계; 및Selectively precipitating only La by adding hydrofluoric acid to the diluent; And
상기 용액을 여과하여 La만을 선택적으로 제거하는 단계를 포함한다. And selectively removing only La by filtering the solution.
상기 방법에서, LSCF 용액에 불산을 첨가하면 F-와 La3 +가 착물을 형성하여 La 착물이 침전됨으로써, LSCF로부터 La를 선택적으로 제거할 수 있다.In the above method, when hydrofluoric acid is added to the LSCF solution, F − and La 3 + form a complex, and the La complex precipitates, so that La can be selectively removed from the LSCF.
지금까지는 LSCF로부터 K를 제거하기 위해 LSCF를 질산, 염산 또는 이들의 혼합산에 녹이는 과정을 사용하였다. 그러나, 이들 산은 LSCF를 모두 녹이기 때문에 무기물에 의한 분광 간섭으로 인하여 K의 정확한 측정값을 얻기가 어려웠다. 그러나, 본 발명에 따른 분석방법에 따르면, LSCF를 질산과 염산의 혼합산에 녹인 후 불산을 첨가하여 La를 제거함으로써 K의 함량을 정확하게 측정하는 것이 가능해졌다.So far, in order to remove K from LSCF, the process of dissolving LSCF in nitric acid, hydrochloric acid or a mixed acid thereof has been used. However, since these acids dissolve all LSCF, it is difficult to obtain an accurate measurement of K due to spectral interference by inorganic substances. However, according to the analysis method according to the present invention, it was possible to accurately measure the content of K by dissolving LSCF in a mixed acid of nitric acid and hydrochloric acid and then removing La by adding hydrofluoric acid.
본 발명의 한 실시양태에서, 질산과 염산의 혼합산에 녹은 LSCF에 불산을 첨가하여 F-와 La3 +의 착물을 형성시킴으로써 La에 의한 K의 분광 간섭 없이 LSCF 내의 K의 함량을 정확히 정량분석할 수 있다.In one embodiment of the present invention, hydrofluoric acid is added to LSCF dissolved in a mixed acid of nitric acid and hydrochloric acid to form a complex of F - and La 3 + to accurately quantify the content of K in LSCF without spectral interference of K by La. can do.
본 발명의 한 실시양태에서, LSCF에 대한 불산의 사용 비율은 1:0.1 내지 1:10 이다.In one embodiment of the present invention, the ratio of use of hydrofluoric acid to LSCF is 1:0.1 to 1:10.
본 발명의 한 실시양태에서, 상기 불산의 사용량은 0.02mL 내지 2mL, 바람직하게는 0.05mL 내지 1mL이다.In one embodiment of the invention, the amount of hydrofluoric acid used is from 0.02 mL to 2 mL, preferably from 0.05 mL to 1 mL.
본 발명의 한 실시양태에서, 상기 물 중탕으로 10분 내지 12시간, 바람직하게는 30분 내지 5시간 동안 가열할 수 있다.In one embodiment of the present invention, the water bath may be heated for 10 minutes to 12 hours, preferably 30 minutes to 5 hours.
본 발명의 한 실시양태에서, 상기 여과는 필터, 예를 들어, 시린지 필터(PTFE Syringe Filter)를 사용하여 수행하고, 여과가 어려울 경우에는 원심분리기를 사용하여 층을 분리한 후 시린지 필터를 사용하여 여과할 수 있다. In one embodiment of the present invention, the filtration is performed using a filter, for example, a PTFE Syringe Filter, and if filtration is difficult, the layer is separated using a centrifuge and then a syringe filter is used. Can be filtered.
본 발명의 한 실시양태에서, K의 정량분석은 ICP-OES를 이용한다.In one embodiment of the present invention, the quantitative analysis of K uses ICP-OES.
상술한 바와 같이, LSCF를 질산과 염산의 혼합산에 녹인 후 불산을 첨가하는 본 발명의 K의 정량분석으로 기존의 방법으로는 불가능했던 K의 정확한 함량을 측정할 수 있다. 본 발명의 정량분석 방법에 의하여, La의 침전에 의해 분광 간섭이 제거됨으로써 K 정량분석의 정확도가 개선되었다. As described above, by quantitative analysis of K of the present invention in which hydrochloric acid is added after dissolving LSCF in a mixed acid of nitric acid and hydrochloric acid, it is possible to measure the exact content of K that was not possible with the conventional method. By the quantitative analysis method of the present invention, spectral interference is removed by precipitation of La, thereby improving the accuracy of K quantitative analysis.
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 아래에 기재한 실시예는 오로지 본 발명을 보다 구체적으로 설명하기 위한 것으로, 본 발명의 요지에 따라 본 발명의 범위가 이들 실시예에 의해 제한되지 않는다는 것은 당업계에서 통상의 지식을 가진 자에 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail through examples. The examples described below are only for explaining the present invention in more detail, and it is to those skilled in the art that the scope of the present invention is not limited by these examples according to the gist of the present invention. It will be self-evident.
실시예Example
LSCF 시료 0.1g을 PET 튜브, 예를 들어, 코닝 튜브(Corning™ tube)에 분취하여 정확히 무게를 측정하였다. 상기 시료에 질산 1mL, 염산 1mL 및 과산화수소 0.05mL를 가하여 상기 시료를 용해시켰다. 상기 용액을 180℃로 세팅된 핫 플레이트(hot plate) 상에서 물 중탕으로 5시간 동안 가열하며 상기 용액을 소량(대략 0.1mL)만 남기고 제거하였다. 상기 용액에 초순수 약 10mL를 첨가하고 불산 0.1mL를 첨가하여 La 착물을 침전시켰으며, 초순수를 더 첨가하여 용액의 전체 용적이 15mL가 되도록 희석하였다. 이 용액을 시린지 필터(PTFE Syringe Filter 13㎜×0.45㎛/100)로 여과하여 La 착물을 제거하였다. 이로부터 수득된 4개의 시료 케이크를 ICP-OES로 분석하여 얻은 각각의 K의 함량을 아래 표에 나타냈다.0.1 g of LSCF sample was aliquoted into a PET tube, for example, a Corning™ tube, to accurately weigh. The sample was dissolved by adding 1 mL of nitric acid, 1 mL of hydrochloric acid and 0.05 mL of hydrogen peroxide. The solution was heated on a hot plate set at 180° C. with a water bath for 5 hours and the solution was removed leaving only a small amount (approximately 0.1 mL). About 10 mL of ultrapure water was added to the solution, and 0.1 mL of hydrofluoric acid was added to precipitate the La complex, and further ultrapure water was added to dilute the total volume of the solution to 15 mL. The solution was filtered through a syringe filter (PTFE Syringe Filter 13 mm×0.45 μm/100) to remove the La complex. The four sample cakes obtained therefrom were analyzed by ICP-OES to show the contents of each K obtained in the table below.
위와 같은 결과는, 도 2에서 볼 수 있듯이, La에 의한 분광 간섭이 제거된 후 K의 함량이 정확히 측정될 수 있다는 것을 시사한다.The above results, as can be seen in Figure 2, suggests that the content of K can be accurately measured after spectral interference caused by La is removed.
비교예Comparative example
LSCF 시료 0.1g을 PET 튜브, 예를 들어, 코닝 튜브(Corning™ tube)에 분취하여 정확히 무게를 측정하였다. 상기 시료에 질산 1mL, 염산 1mL 및 과산화수소 0.05mL를 가하여 상기 시료를 용해시켰다. 상기 용액을 180℃로 세팅된 핫 플레이트 상에서 물 중탕으로 5시간 동안 가열하며 상기 용액을 소량(대략 0.1mL)만 남기고 제거하였다. 상기 용액에 초순수를 첨가하여 전체 용액의 용적이 15mL가 되도록 희석하였다. 이 희석액을 시린지 필터(PTFE Syringe Filter 13㎜×0.45㎛/100)로 여과한 후 시료를 ICP-OES를 이용하여 분석하였다. 그 결과, 도 1에 나타낸 바와 같이, La에 의한 분광 간섭으로 K 함량이 정확하게 분석되지 않았다.0.1 g of LSCF sample was aliquoted into a PET tube, for example, a Corning™ tube, to accurately weigh. The sample was dissolved by adding 1 mL of nitric acid, 1 mL of hydrochloric acid and 0.05 mL of hydrogen peroxide. The solution was heated on a hot plate set at 180° C. with a water bath for 5 hours and the solution was removed leaving only a small amount (approximately 0.1 mL). Ultrapure water was added to the solution, and the total solution was diluted to a volume of 15 mL. After filtering this dilution with a syringe filter (PTFE Syringe Filter 13 mm×0.45 μm/100), the sample was analyzed using ICP-OES. As a result, as shown in FIG. 1, the K content was not accurately analyzed due to spectral interference caused by La.
따라서, 상기 실시예 및 비교예를 근거로, 본원 발명에 따른 방법은 무기물에 의한 분광 간섭 없이 LSCF 내의 K의 함량을 ICP-OES를 이용하여 정확히 분석할 수 있다는 것을 확인할 수 있다.Accordingly, it can be seen that based on the above examples and comparative examples, the method according to the present invention can accurately analyze the content of K in LSCF using ICP-OES without spectral interference by inorganic substances.
이상에서는 도면 및 실시예를 참조하여 본 발명에 따른 바람직한 실시양태를 기술하였으나, 이는 예시적인 것이며 당업계의 통상의 지식을 가진 자라면 이에 의해 본 발명의 범위가 제한되는 것이 아니고 이로부터 다양한 변형 및 균등한 다른 실시양태가 가능하다는 점을 이해할 수 있을 것이다. 따라서, 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의하여 정의된다고 할 것이다.In the above, preferred embodiments according to the present invention have been described with reference to the drawings and examples, but these are exemplary and those of ordinary skill in the art are not limited by this, and various modifications and variations therefrom. It will be understood that other equivalent embodiments are possible. Accordingly, the substantial scope of the present invention will be defined by the appended claims and their equivalents.
Claims (4)
LSCF를 칭량하는 단계;
상기 LSCF에 질산(HNO3), 염산(HCl) 및 과산화수소를 첨가하여 상기 LSCF가 용해된 용액을 수득하는 단계;
상기 LSCF 용액을 물 중탕으로 가열하고 산을 소량만 남기고 제거하는 단계;
상기 산이 제거된 용액에 초순수를 첨가하여 희석시키는 단계;
상기 희석액에 불산(HF)을 첨가하여 La만을 선택적으로 침전시키는 단계; 및
상기 침전 용액을 여과하여 La만을 선택적으로 제거하는 단계를 포함하고,
상기 LSCF에 대한 불산의 사용 비율이 1:0.1 내지 1:10인 것을 특징으로 하는, K 함량의 분석방법.As a method for analyzing the K content present in LSCF (La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3 ),
Weighing the LSCF;
Adding nitric acid (HNO 3 ), hydrochloric acid (HCl) and hydrogen peroxide to the LSCF to obtain a solution in which the LSCF is dissolved;
Heating the LSCF solution with a water bath and removing only a small amount of acid;
Diluting the acid-removed solution by adding ultrapure water;
Selectively precipitating only La by adding hydrofluoric acid (HF) to the diluent; And
Filtering the precipitation solution to selectively remove only La,
Method of analyzing the K content, characterized in that the ratio of the use of hydrofluoric acid to the LSCF is 1:0.1 to 1:10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020170084252A KR102126606B1 (en) | 2017-07-03 | 2017-07-03 | Method for analyzing contents of k in la compounds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020170084252A KR102126606B1 (en) | 2017-07-03 | 2017-07-03 | Method for analyzing contents of k in la compounds |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20190004105A KR20190004105A (en) | 2019-01-11 |
| KR102126606B1 true KR102126606B1 (en) | 2020-06-24 |
Family
ID=65028239
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020170084252A KR102126606B1 (en) | 2017-07-03 | 2017-07-03 | Method for analyzing contents of k in la compounds |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR102126606B1 (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008002916A (en) * | 2006-06-21 | 2008-01-10 | Okayama Univ | Component removing system for in-line removing specific component in sample liquid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102054465B1 (en) * | 2015-06-15 | 2019-12-11 | 주식회사 엘지화학 | Method for analyzing phosphorus content in cathode materials and composition used in the same |
-
2017
- 2017-07-03 KR KR1020170084252A patent/KR102126606B1/en active IP Right Grant
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008002916A (en) * | 2006-06-21 | 2008-01-10 | Okayama Univ | Component removing system for in-line removing specific component in sample liquid |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20190004105A (en) | 2019-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8222038B2 (en) | Method for analyzing metal specimen | |
| CN103364426A (en) | Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry | |
| CN102680470B (en) | Method for determining content of arsenic and antimony in copper electrolyte | |
| CN103412034A (en) | Measuring method for quickly measuring contents of heavy metals in tobacco by using microwave digestion/ICP-MS method | |
| CN104764704B (en) | Copper thing molybdenum determination method in flash blowing clinker | |
| CN102192967A (en) | Grain production place discriminating method utilizing heavy element isotope ratio composition | |
| CN105203475A (en) | Method of determining chemical oxygen demand in chlorine-containing water sample | |
| CN109374599A (en) | The rapid assay methods of 20 kinds of impurity elements in a kind of ingot casting bronze | |
| CN103454131A (en) | High-efficiency measuring method of content of cobalt, nickel and aluminum in natural microalloy iron powder | |
| CN105300961A (en) | Separation and enrichment determination method for Ir, Rh, Pt, Pd and Au in secondary resource material | |
| CN103901018A (en) | Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers | |
| KR102126606B1 (en) | Method for analyzing contents of k in la compounds | |
| CN106404515A (en) | Detection method for determining multiple elements in solid cosmetic powder | |
| CN104215634A (en) | Method for determining content of tin in tungsten concentrate | |
| JP7020447B2 (en) | A method for analyzing inclusions and / or precipitates in a metal sample, and a method for collecting inclusions and / or precipitates in a metal sample. | |
| CN104502179A (en) | Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP | |
| JP2011158326A (en) | Method for quantifying very small amount of chlorine in silver powder | |
| CN106706603A (en) | Method for detecting content of elements in pig iron | |
| JP2020085894A (en) | Evaluation methods for tungsten and element | |
| CN106404991A (en) | Method for determination of iron in copper alloy | |
| CN109612954A (en) | A kind of test method and its application method of copper simple substance content | |
| CN104155267A (en) | Method for chemically analyzing content of boron nitride in nickel-based powder material | |
| CN109520948A (en) | A kind of method of quick detection low-grade copper polymetallic ore copper object phase | |
| CN104165848A (en) | Method for measuring antimony content of polyester slice | |
| CN104215541A (en) | Method for high efficiently and precisely measuring contents of high purity alumina and impurities |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E902 | Notification of reason for refusal | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant |