• 제목/요약/키워드: oxalate method

검색결과 99건 처리시간 0.029초

Development of HPLC Determination Method for Trace Levels of 1-, 2-Nitropyrenes and 2-Nitrofluoranthene in Airborne Particulates and Its Application to Samples Collected at Noto Peninsula

  • Hayakawa, Kazuichi;Tang, Ning;Sato, Kosuke;Izaki, Akihiko;Tatematsu, Michiya;Hama, Hirotaka;Li, Ying;Kameda, Takayuki;Toriba, Akira
    • Asian Journal of Atmospheric Environment
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    • 제5권3호
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    • pp.146-151
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    • 2011
  • 1-Nitropyrene (1-NP), 2-NP and 2-nitrofluoranthene (2-NFR) are useful markers for studying the atmospheric behaviors of polycyclic aromatic hydrocarbons (PAHs) and nitropolycyclic aromatic hydrocarbons (NPAHs). However, present methods for measuring trace levels of these compounds are lesssensitive and laborious. Here we describe several improvements to a previously reported high-performance liquid chromatography-chemiluminescence detection system that allows it to determine trace levels of 1-, 2-NPs and 2-NFR. The proposed system was equipped with a reducer column packed with Pt/Rh instead of zinc whose life-time was limited. The combination of Cosmosil MS-II (monomeric ODS) and AR-II (polymeric ODS) columns was used instead of polymeric ODS columns as the separator column to improve the separation. An ethanol mixture with acetate buffer (pH 5.5) was used in place of an acetonitrile mixture with the same buffer to activate the reducer column. The same ethanol mixture was used as the mobile phase for the clean-up column. The switching time of the column switching valve was optimized to concentrate the amino-derivatives of above NPAHs quantitatively on the concentrator column. The concentrations of bis(2,4,6-trichlorophenly) oxalate and hydrogen peroxide in the chemiluminescence reagent solution were optimized to 0.4 mM and 30 mM, respectively, to increase the sensitivity. Under the above conditions, the detection limits (S/N=3) of 1-, 2-NPs and 2-NFR were 1 fmol (0.25 pg), 10 fmol (2.5 pg) and 4 fmol (1 pg), respectively. The proposed system was effectively used to determine trace levels of 1-, 2-NPs and 2-NFR in airborne particulates collected at Noto Peninsula. The atmospheric concentrations of 1-, 2-NPs and 2-NFR were not more than sub pg $m^{-3}$ levels. They were higher in winter (January) than in summer (July). In both seasons, the concentrations were in decreasing order, [2-NFR]>[1-NP]>[2-NP].

경사관법(傾斜管法)에 의한 우혈액(牛血液)의 적혈구침강율(赤血球沈降率) 측정(測定) (Angled Tube Method for Determining Erythrocyte Sedimentation Rate of Cattle)

  • 이방환;신종욱
    • 대한수의학회지
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    • 제26권1호
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    • pp.175-185
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    • 1986
  • The measurement of angled erythrocyte sedimentation rate (ESR), as a replacement for perpendicular ESR, for cattle blood was scrutinized since it has been well known that perpendicular ESR in cattle is too slow to be adopted as an effective clinical test. Samples of blood were taken from 186 Korean native cattle over 2 years old. The results obtained in the experiment were summarized as follows. 1. Average values of perpendicular ESR/24hrs in 15 apparently healthy cattle, as measured by Wintrobe, Westergren and capillary tubes, were $5.8{\pm}2.2$, $11.1{\pm}3.7$ and $10.4{\pm}4.5%$ respectively, which were found to be similar to the values of perpendicular ESR/hr of normal blood of human. 2. The ESR was determined in the tubes held at 90, 75, 60, 45, 30 and 15-degree angles, using 3 types of tubes. For the diagnostic purposes, the best results were obtained from the tubes held at 45-degree angle. 3. The angled ESR values increased as the diameters of the tube-bores decreased. 4. The tube length did not affect the angled ESR(%). 5. The angled ESR values increased with the increased environmental temperature during the ESR measurement. 6. The storage temperature at $5^{\circ}C$, $20^{\circ}C$ and $35^{\circ}C$, of the blood for 24 hours did not affect the angled ESR. 7. Samples of blood were treated with 4 kinds of anticoagulants (heparin, $K_2$-EDTA, double oxalate and sodium citrate) and the ESR was determined at 45-degree angle, using capillary hematocrit tubes. The ESR values were higher in the blood samples treated with sodium citrate than in those treated with other anticoagulants. 8. By using the autologous plasma, the PCV was adjusted to be 5, 10, 20, 30, 40 and 50ml/100ml and the ESR was determined in the capillary hematocrit and Wintrobe tubes held at 45 degrees. In both of the methods the ESRs increased as the values of PCV decreased. The regressions of ESR to PCV in both 45-degree-angled capillary and Wintrobe tubes were curvilinear. For the capillary hematocrit tubes the second degree polynomial $Y=61.9779-2.3533x+0.0228x^2$ (r=0.9999) fits the data. And in the case of Wintrobe tubes the second degree polynomial $Y=27.9767-1.1314x-0.0117x^2$ (r=0.9998) fits the data. 9. The 45-degree angled ESR was determined in the blood of 71 healthy Korean native cows using capillary hematocrit tubes. The average PCV was $35.4{\pm}3.6ml/100ml$. The observed ESR/hr averaged $7.2{\pm}2.7%$, while the corrected ESR/hr to a PCV of 36ml/100ml averaged $6.6{\pm}1.3%$. From these results it was concluded that to obtain the best results the ESR/hr of Korean native cattle should be determined at 45-degree angle at room temperature($20^{\circ}C$) using capillary hematocrit tubes.

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산수유(山茱萸)의 기미론(氣味論)적 해석과 내외부형태연구 (The Approach of Properties-Flavours Theory and the Study of Morphological Standard in CORNI FRUCTUS)

  • 최문일;이화정;윤주봉;김자영;강경식;신철균;주영승
    • 대한본초학회지
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    • 제21권2호
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    • pp.109-119
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    • 2006
  • Objectives : This study was performed to approach of properties-flavours theory and the study of morphological standard in CORNI FRUCTUS. Methods : The properties-flavours theory were attempted with bibliographic method and various climate-information. The external-internal morphological standards were determined by using stereoscope and butanol series. Results and conclusion : 1. The significant analysis for the corni fructus as the properties-flavours theory, is a follow-up survey of the effect written in the official oriental medicine book. 2. The other analytic methods according to the gathering time, processing or storing system or especially nature or growth environment(altitude, temperature,. the mean moisture, and the agronomical survey) by way of the explanation of properties-flavours theory appears so many insufficiency at the many cases. 3. The external and internal characteristics according to the shape of original plant or herbal states, entirely correspond to all the literature on this subject. 4. According to the place of production, there are some different points. (l) In the external shapes, it is reasonable that if we make the basic standard of classification by the sharpness of color, the existence of gloss and the size of products. In the case of the Korean products, it shows bright and glossy color totally, but in the case of North Korea products, it shows black and lackluster. And in the case of the foreign products, it has softer body than Korea one and shows white color on the surface. (2) In the internal shapes, the Korea products has a thicker cuticle layer than the foreign one, and has fewer ca-oxalate in the parenchyma cell.

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우리나라 토양(土壤)에 있어서 수종(數種) 분산제(分散劑)의 분산능(分散能)에 관(關)하여 (The Dispersion Capacity of Some Chemical Dispersing Agents in Korean Soils)

  • 임정남;조인상;조성진
    • 한국토양비료학회지
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    • 제13권2호
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    • pp.65-70
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    • 1980
  • 우리나라 토양(土壤)의 입도분석(粒度分析)에 적합(適合)한 분산제(分散劑)를 선정(選定)하기 위하여 대표토양(代表土壤) 18점(点)에 대(對)한 표토(表土) 및 심토(深土)의 입도분석(粒度分析) 결과(結果)는 다음과 같다. 1. 토양입자(土壤粒子)가 작을수록 분산제별(分散劑別) 분산능력(分散能力)의 차이(差異)가 커지는 경향(傾向)으로 점토입자(粘土粒子)(<0.002mm)의 분석치(分析値)에 있어서 분산제(分散劑)에 따라 차이(差異)가 컸었다. 2. 분산율(分散率)은 Sodium Pyrophosphate가 가장 높고 다음으로 Sodium Hexametaphophate, Ammonium Hydroxide, Sodium Hydroxide, Sodium Oxalate 순(順)이었다. 3. Sodium Hexametaphosphate는 Volcanic Ash Soil만을 제외(除外)하고 우리나라 모두 토양(土壤)의 입도분석(粒度分析)에 있어서 분산제(分散劑)로써 사용(使用)할 수 있을 것으로 본다. 4. Volcanic Ash Soil의 분산율(分散率)은 분산제(分散劑)를 사용(使用)하지 않은 경우보다 오히려 감소(減少)되는 경향(傾向)이 있으므로 이의 분산방법(分散方法)의 선정(選定)에는 특별(特別)한 주의(注意)가 요망(要望)된다.

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N2분위기에서 FeC2O4·2H2O의 열분해에 의한 Fe3O4-δ합성 (Synthesis of Fe3O4-δ Using FeC2O4·2H2O by Thermal Decomposition in N2 Atmosphere)

  • 박원식;오경환;안석진;서동수
    • 한국재료학회지
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    • 제22권5호
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    • pp.253-258
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    • 2012
  • Activated magnetite ($Fe_3O_{4-{\delta}}$) was applied to reducing $CO_2$ gas emissions to avoid greenhouse effects. Wet and dry methods were developed as a $CO_2$ removal process. One of the typical dry methods is $CO_2$ decomposition using activated magnetite ($Fe_3O_{4-{\delta}}$). Generally, $Fe_3O_{4-{\delta}}$ is manufactured by reduction of $Fe_3O_4$ by $H_2$ gas. This process has an explosion risk. Therefore, a non-explosive process to make $Fe_3O_{4-{\delta}}$ was studied using $FeC_2O_4{\cdot}2H_2O$ and $N_2$. $FeSO_4{\cdot}7H_2O$ and $(NH_4)_2C_2O_4{\cdot}H_2O$ were used as starting materials. So, ${\alpha}-FeC_2O_4{\cdot}2H_2O$ was synthesized by precipitation method. During the calcination process, $FeC_2O_4{\cdot}2H_2O$ was decomposed to $Fe_3O_4$, CO, and $CO_2$. The specific surface area of the activated magnetite varied with the calcination temperature from 15.43 $m^2/g$ to 9.32 $m^2/g$. The densities of $FeC_2O_4{\cdot}2H_2O$ and $Fe_3O_4$ were 2.28 g/$cm^3$ and 5.2 g/$cm^3$, respectively. Also, the $Fe_3O_4$ was reduced to $Fe_3O_{4-{\delta}}$ by CO. From the TGA results in air of the specimen that was calcined at $450^{\circ}C$ for three hours in $N_2$ atmosphere, the ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was estimated. The ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was 0.3170 when the sample was heat treated at $400^{\circ}C$ for 3 hours and 0.6583 when the sample was heat treated at $450^{\circ}C$ for 3 hours. $Fe_3O_{4-{\delta}}$ was oxidized to $Fe_3O_4$ when $Fe_3O_{4-{\delta}}$ was reacted with $CO_2$ because $CO_2$ is decomposed to C and $O_2$.

강변 여과 취수 지역 퇴적물의 철 화학종 추출 특성 (Iron Extraction Characteristics of Sediment Samples from a River Bank Filtration Site)

  • 현성필;문희선;윤필선;김보아;하규철
    • 한국광물학회지
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    • 제26권2호
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    • pp.129-138
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    • 2013
  • 최근 들어 안정된 수자원 확보를 위해 하천수를 강변의 충적층을 통과시켜 취수하는 강변 여과수 개발이 각광을 받고 있다. 지표수 및 지하수와 반응하는 주변 충적층 퇴적물에 존재하는 철은 강변 여과 후 양수정을 통해 얻어지는 지하수의 수질을 결정하는 데 매우 중요한 요소이다. 본 연구에서는 퇴적물-지하수-지표수의 상호 작용에 의한 철 화학종의 존재 변화를 알아보기 위해 창원시 대산면 낙동강변의 강변여과 부지에서 채취한 대수층 퇴적물 내에 존재하는 철 함유량을 퇴적물 심도 및 입자 크기에 따라 다양한 화학적 철 추출법을 통해 비교하였다. 실험 결과는 전체적으로 지표로부터 20 m 부근까지는 2가철 및 총 철 함량이 전체적으로 감소하다 20 m 깊이 이하에서는 증가하는 경향을 나타내었다. 이러한 결과는 육안으로 관찰되는 퇴적물 색깔이 지시하는 산화/환원 환경 특성과도 일치하였다. 한편, 퇴적물의 모래 부분보다 미사/점토 부분에서 추출법에 따라 2~10배의 철이 추출되었다. 그리고, 다양한 추출법 중 DCB 용액에 의해 가장 많은 철이 추출되었다. 이와 같은 다양한 철 분석법으로 추출되는 철 함량 특성은 퇴적물 내에서 철의 용해 및 침전을 결정짓는 심도에 따른 산화/환원 조건의 좋은 지시자로 활용될 수 있을 것으로 판단된다.

사람의 적혈구에서 용혈성을 이용하여 측정한 음이온 교환특성 (Characteristics of Anion Exchange Measured by the Rate of Hemolysis in Human Erythrocyte)

  • 우재석;김용근;황일용
    • The Korean Journal of Physiology
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    • 제20권2호
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    • pp.218-224
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    • 1986
  • 사람의 적혈구에서 여러 가지 음이온들의 등삼투성 암모늄 염으로 된 용액속에서의 용혈성을 이용하여 이들 음이온들이 $HCO_3\;^-$ 혹은 $OH^-$와 교환되어 이동되는 정도와 몇 가지 억제 물질의 영향, pH 및 온도 변화의 효과를 관찰하여 그 결과를 지금까지 방사성동위원소를 이용한 실험에서 보고된 성적들과 비교하였다. $SITS.\;H_2DIDS$, furosemide등은 농도에 비례하여 등삼투성 $NH_4Cl$ 용액에서의 용혈 시간을 연장시켰으며 $t_{1/2}$를 두배로 연장시킨 농도는 각각 $ 2.3{\times}10^{-7}M,\;3{\times}10^{-7}M,\;2.5{\times}10^{-5}M$이었다. Acetazolamide도 농도에 비례하여 적혈구 용혈 시간을 연장시켰으며 $t_{1/2}$을 2배로 연장시킨 농도는 $2.4{\times}10^{-5}M$이었다. 온도를 $2^{\circ}C$에서 $37^{\circ}C$까지 변화시키며 적혈구 용혈시간을 관찰했을 때 높은 온도 의존성을 보였으며 $1/t_{1/2}$을 Arrhenius plot하였을 때 $20^{\circ}C$에서 회절점을 보였고 activation energy는 $20^{\circ}C{\sim}37^{\circ}C$범위에서 11.2kcal/mol이었다. 여러 가지 무기 음이온의 투과도를 $t_{1/2}$을 기준으로 비교했을 때 $Cl^->NO_3\;^->SCN^->SO_4\;^{2-}>SSO_3\;^{2-}>HPO_4\;^{2-}$의 순이었으며 유기 음이온 중 oxalate는 $Cl^-$보다 높은 투과도를 succinate는 낮은 투과도를 보였다. 이상의 결과를 종합하면 등삼투성 암모늄염 용액에서의 적혈구 용혈성을 이용하여 음이온 이동에 대하여 관찰한 결과들이 지금까지의 동위원소를 이용한 실험 성적들과 유사한 결과를 보여주고 있으며 특히 이동률이 빠르거나, 높은 온도범위에서의 음이온의 이동을 관찰하는데는 동위원소를 이용한 실험의 단점을 보완할 수 있는 장점도 있어 이 방법의 적혈구 막을 통한 음이온의 이동 기전과 이에 영향을 미치는 인자들을 연구하는데 간편하고 유용하게 이용될 수 있을 것으로 사료된다.

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활성화된(Fe1-xMnx)3O4-δ과 (Fe1-xCox)3O4-δ의 이산화탄소 분해 특성 (CO2 Decomposition Characteristics of Activated(Fe1-xMnx)3O4-δ and (Fe1-xCox)3O4-δ)

  • 박원식;오경환;이상인;서동수
    • 한국재료학회지
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    • 제23권4호
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    • pp.219-226
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    • 2013
  • Activated magnetite ($Fe_3O_{4-{\delta}}$) has the capability of decomposing $CO_2$ proportional to the ${\delta}$-value at comparatively low temperature of $300^{\circ}C$. To enhance the $CO_2$ decomposition capability of $Fe_3O_{4-{\delta}}$, $(Fe_{1-x}Co_x)_3O_{4-{\delta}}$ and $(Fe_{1-x}Mn_x)_3O_{4-{\delta}}$ were synthesized and then reacted with $CO_2$. $Fe_{1-x}Co_xC_2O_4{\cdot}2H_2O$ powders having Fe to Co mixing ratios of 9:1, 8:2, 7:3, 6:4, and 5:5 were synthesized by co-precipitation of $FeSO_4{\cdot}7H_2O$ and $CoSO_4{\cdot}7H_2O$ solutions with a $(NH_4)_2C_2O_4{\cdot}H_2O$ solution. The same method was used to synthesize $Fe_{1-x}Mn_xC_2O_4{\cdot}2H_2O$ powders having Fe to Mn mixing ratios of 9:1, 8:2, 7:3, 6:4, 5:5 with a $MnSO_4{\cdot}4H_2O$ solution. The thermal decomposition of synthesized $Fe_{1-x}Co_xC_2O_4{\cdot}2H_2O$ and $Fe_{1-x}Mn_xC_2O_4{\cdot}2H_2O$ was analyzed in an Ar atmosphere with TG/DTA. The synthesized powders were heat-treated for 3 hours in an Ar atmosphere at $450^{\circ}C$ to produce activated powders of $(Fe_{1-x}Co_x)_3O_{4-{\delta}}$ and $(Fe_{1-x}Mn_x)_3O_{4-{\delta}}$. The activated powders were reacted with a mixed gas (Ar : 85 %, $CO_2$ : 15 %) at $300^{\circ}C$ for 12 hours. The exhaust gas was analyzed for $CO_2$ with a $CO_2$ gas analyzer. The decomposition of $CO_2$ was estimated by measuring $CO_2$ content in the exhaust gas after the reaction with $CO_2$. For $(Fe_{1-x}Mn_x)_3O_{4-{\delta}}$, the amount of $Mn^{2+}$ oxidized to $Mn^{3+}$ increased as x increased. The ${\delta}$ value and $CO_2$ decomposition efficiency decreased as x increased. When the ${\delta}$ value was below 0.641, $CO_2$ was not decomposed. For $(Fe_{1-x}Co_x)_3O_{4-{\delta}}$, the ${\delta}$ value and $CO_2$ decomposition efficiency increased as x increased. At a ${\delta}$ value of 0.857, an active state was maintained even after 12 hours of reaction and the amount of decomposed $CO_2$ was $52.844cm^3$ per 1 g of $(Fe_{0.5}Co_{0.5})_3O_{4-{\delta}}$.

경북(慶北) 봉화군(奉化郡) 장군광산산(將軍鑛山産) 신종광물(新種鑛物) 장군석(將軍石)에 대(對)한 광물학적(鑛物學的) 연구(硏究) (Janggunite, a New Mineral from the Janggun Mine, Bonghwa, Korea)

  • 김수진
    • 자원환경지질
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    • 제8권3호
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    • pp.117-124
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    • 1975
  • 경북(慶北) 봉화군(奉化郡) 소재(所在) 장군광산(將軍鑛山)의 표성산화(表成酸化)망간광석중(鑛石中)에서 필자(筆者)에 의(依)하여 발견명명(發見命名)된 신종건물(新種鍵物) 장군석(將軍石)은 국제(國際) 광물학회내연합(鑛物學會內聯合)에 있는 "신종광물(新種鑛物) 및 광물명위원회(鑛物名委員會)"의 공인(公認)을 받았는바 이에 대(對)한 광물학적(鑛物學的)인 연구결과(硏究結果)를 요약(要約)하면 다음과 같다. (1) 장군석(將軍石)은 표성산화(表成酸化)망간 광석중(鑛石中) cementation zone에서 산출(産出)되며, 엔소타이트, 토도로카이트, 방해석(方解石)을 수반(隨伴)한다. 대체로 공동(空洞)에서 수기상(樹技狀) 또는 방사상(放射狀)을 이루는 엽편상(葉片狀) 세립집합체(細粒集合體)(입자(粒子)의 크기 <0.05mm)로 또는 교질상대(膠質狀帶)로 산출(産出)한다. (2) 색(色)은 흑색(黑色)이며 광택(光澤)은 무염(無艶), 조흔(條痕)은 흑갈(黑褐)~암갈(暗褐色)이다. 벽개(劈開)는 한방향(方向)으로 완전(完全)하다. 경도(硬度)(H)=2-3이며 역쇄성(易碎性)이다. 비중(比重)(G)=3.59(실측시(實測植)), 3.58이론치(理論値)이다. (5) 화학분석치(化學分析値)로부터 계산(計算)된 장군석(將軍石)의 화학식(化學式)은 $Mn^{4+}{_{4.85}}(Mn^{2+}{_{0.90}}Fe^{3+}{_{0.30}})_{1.20}O_{8.09}(OH)_{5.91}$이며, 이상식(理想式)은 $Mn^{4+}{_{5-x}}(Mn^{2+},\;Fe^{3+}){_{1+x}}O_8(OH)_6$ ($x{\approx}0.2$)이다. (6) 장군석(將軍石)은 사방정사 속(屬)하며 X선(線) 분말회절분석(粉末廻折分析) 결과(結果), 단위포(單位胞)의 크기는 $a=9.324{\AA}$, $b=14.05{\AA}$, $c=7.956{\AA}$이며, 단위포(單位胞)의 체적(體積)은 $1042.25{\times}10^{-24}cm$이다. 보솔(輔率) a : b : c=0.663 : 1 : 0.566. 단위포함유수(單位胞含有數) (Z)=4. (7) 시차열분석곡선(示差熱分析曲線)은 $250{\sim}370^{\circ}C$$955^{\circ}C$에서 흡열(吸熱)피크를 보여준다. 전자(前者)는 장군석(將軍石)이 탈수(脫水) 및 산화(酸化)를 받아 $(Mn,\;Fe)_2O_3$이 생성(生成)된데 기인(基因)하며 후자(後者)는 hausmannite 형(型)의 구조(構造)를 갖는 $(Mn,\;Fe)_3O_4$의 생성(生成)에 기인(基因)하는 것이다. $(Mn,\;Fe)_2O_3$는 등보정사이고 $a=9.417{\AA}$이었고 $(Mn,\;Fe)_3O_4$는 정방정사이고 $a=5.76{\AA}$, $c=9.51{\AA}$이었다. (6) 장군석(將軍石)의 적외선흡수분광(赤外線吸收分光)스펙트럼은 $515cm^{-1}$$545cm^{-1}$에서 Mn-O stretching 진동(振動)을, $1025cm^{-1}$에서 O-H bending 진동(振動)을 그리고 $3225cm^{-1}$에서 O-H stretching 진동(振動)을 보여준다. (3) 장군석(將軍石)은 불투명광물(不透明鑛物)이며 현미경하(顯微鏡下)에서 반사도(反射度)는 13~15%이고 복반사율(複反射率)은 공기중(空氣中)에서 현저(顯著)하며 침액중(浸液中)에서 강(强)하다. 반사다색성(反射多色性)은 백색(白色)~담회색(淡灰色)이다. 십자(十字)니콜하(下)에서의 편광색(偏光色)은 공기중(空氣中)에서 청색(靑色)을 띈 황갈(黃褐)~회색(灰色)이고 침액중(浸液中)에서는 黃褐(황갈)~청갈(靑褐)~회색(灰色)이다. 내부반사(內部反射)는 없다. (4) 연마면(硏磨面)에 대(對)한 에칭반응(反應)은 HCl(conc.)와 $H_2SO_4+H_2O_2$ 회색(灰色), 퇴색(褪色), SnCl(sat.): 암색(暗色), $HNO_3$ (conc.) : 회색(灰色), $H_2O_2$ : 거품을 내며 퇴색(褪色). (9) 신종광물(新種鑛物) 장군석(將軍石)은 독특(獨特)한 화학조성(化學組成)과 단위포(單位胞)를 가지고 있어서 이의 발견(發見)은 산화(酸化)망간광물(鑛物)의 분류(分類)와 연구(硏究)에 새로운 방향(方向)과 지침(指針)이 되었다.

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