• Title/Summary/Keyword: oxalate method

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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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    • v.5 no.3
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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].

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

  • Lee, Bang-whan;Shin, Jong-uk
    • Korean Journal of Veterinary Research
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    • v.26 no.1
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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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The Approach of Properties-Flavours Theory and the Study of Morphological Standard in CORNI FRUCTUS (산수유(山茱萸)의 기미론(氣味論)적 해석과 내외부형태연구)

  • Choi, Mun-Il;Lee, Hwa-Jung;Yun, Ju-Bong;Kim, Ja-Young;Kang, Kyoung-Sik;Shin, Chol-Gyun;Ju, Young-Sung
    • The Korea Journal of Herbology
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    • v.21 no.2
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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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The Dispersion Capacity of Some Chemical Dispersing Agents in Korean Soils (우리나라 토양(土壤)에 있어서 수종(數種) 분산제(分散劑)의 분산능(分散能)에 관(關)하여)

  • Im, Jeong-Nan;Cho, In-Sang;Cho, Seong-Jin
    • Korean Journal of Soil Science and Fertilizer
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    • v.13 no.2
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    • pp.65-70
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    • 1980
  • This experiment was aimed at selecting the most suitable dispersing agent to the Korean soils. The particle size distribution of 18 soil samples representing the great soil groups in Korea was analysed with 5 different dispersing agents by pipette-method. Passing percent of 0.05, 0.02 and 0.002mm in diameter was used for the comparision of the dispersion capacity of chemical agents. The results obtained are as follows; 1. The influence of chemical agents on dispersion seemed to be greater to finer soil particles. The passing percents of 0.002mm showed a great differences according to the chemical agents used, while little differences was observed in those of 0.05mm. 2. It was showed that sodium pyrophosphate had the highest dispersion capacity for the most of Korean soils, the dispersion capacity of sodium hexametaphosphate was also high enough except for volcanic ash soils. 3. It was recommendable that sodium hexametaphosphate could widely be used as a dispersing agent in the routine analysis of soil particle size distribution except for the Volcanic ash soils. 4. The dispersion of Volcanic ash soils was rather poor when chemical agents used. Therefore, special care should be taken for the dispersion of allophane soils.

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

  • Park, Won-Shik;Oh, Kyoung-Hwan;An, Suk-Jin;Suhr, Dong-Soo
    • Korean Journal of Materials Research
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    • v.22 no.5
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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 $O_2$.

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

  • Hyun, Sung Pil;Moon, Hee Sun;Yoon, Pilsun;Kim, BoA;Ha, Kyoochul
    • Journal of the Mineralogical Society of Korea
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    • v.26 no.2
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    • pp.129-138
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    • 2013
  • River bank filtration has been considered as a promising alternative water management scheme, in which groundwater is extracted from an aquifer near a river after infiltration of the river water into the aquifer, thereby improving and maintaining the quality of water recovered. Iron (Fe) associated with sediment in contact with groundwater and infiltrating surface water is an important factor in determining the quality of water recovered from the pumping wells in river bank filtration. This study reports the results of Fe speciation in the aquifer sediment samples collected from different depths at the river bank filtration site in Changwon, studied using four different chemical extraction methods, namely, ferrozine, oxalate, HCl, and DCB methods. Overall, the results show that Fe(II) as well as the total Fe content decreases with depth down to ~20 m and then increases further below. This trend is consistent with the redox characteristics suggested by visual observation. The silt/clay size fraction (${\phi}$ < 62.5 ${\mu}M$) has up to 2~10 times more Fe compared with the sand size fraction (62.5 ${\mu}M$ < ${\phi}$ < 2 mm), depending on the extraction method. Of the four extraction methods, DCB solution extracted the most Fe from the sediment samples. The amounts of Fe extracted by the different extraction methods can be a good indicator of the redox conditions along the depth of the aquifer.

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

  • Woo, Jae-Suk;Kim, Yong-Keun;Hwang, Il-Yong
    • The Korean Journal of Physiology
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    • v.20 no.2
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    • pp.218-224
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    • 1986
  • The characteristics of anion exchange with internal $HCO_3\;^{-}\;(or\;OH^-)$ was studied by determining the time course of hemolysis in isoosmotic ammonium salt solution in human erythrocytes. The effects of inhibitors, pH and temperature on the exchange between internal $HCO_3\;^-\;(or\;OH^-)$ and external $Cl^-$ were observed and the permeabilities of various organic and inorganic anions were also measured. The results were compared with data previously reported from the experiments using radioisotopes. The results are as follows; 1) SITS $H_2DIDS$ and furosemide inhibited the hemolysis of erythrocytes in isoosmotic $NH_4Cl$ solution in a dose·dependent manner, and the concentrations for lengthening twice the time for $half-hemloysis(t_{1/2})\;were\;2.3{\times}10^{-7},\;1.3{\times}10^{-7}\;and\;2.5{\times}10^{-5}M$, respectively. 2) Acetazolamide also shifted the time-dependent hemolytic curve to the right in a dose-dependent manner, and the concentrations for lengthening twice $t_{1/2}\;was\;2.4{\times}10^{-5}M$. 3) The time-dependent hemolysis was delayed by decreasing pH from 7.0 to 6.2, but w·as not affected by the change of pH in the range of 7.0 to 8.2. 4) The time for $half-hemloysis(t_{1/2})$ showed a temperature-dependency and Arrhenius plot exhibited a break point at $20^{\circ}C$. The apparent activation energy calculated from this plot was 18.1 kcal/mol between $2^{\circ}C-20^{\circ}C$ and 11.2 kcal/mol between $20^{\circ}C-37^{\circ}C$, respectively. 5) The apparent permeabilities of various inorganic anions based on $t_{1/2}$ were in the order of $Cl^->NO_{3}\;^->SCN^->SO_4\;^{2-}>SSO_3\;^{2-}>HPO_4\;^{2-}$. which was similar with the previous reports based on the experiment using radioisotopes. The results Obtained from this study are comparable with the previous data reported from the experiments using radioisotopes. This indicates that the hemolysis of erythrocytes in isoosmotic ammonium salt solution can be used as a simple and good method for the study of anion exchange in erythrocyte membrane.

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

  • Park, Won-Shik;Oh, Kyoung-Hwan;Rhee, Sang-In;Suhr, Dong-Soo
    • Korean Journal of Materials Research
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    • v.23 no.4
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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 $(Fe_{0.5}Co_{0.5})_3O_{4-{\delta}}$.

Janggunite, a New Mineral from the Janggun Mine, Bonghwa, Korea (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))

  • Kim, Soo Jin
    • Economic and Environmental Geology
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    • v.8 no.3
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    • pp.117-124
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    • 1975
  • Wet chemical analysis (for $MnO_2$, MnO, and $H_2O$(+)) and electron microprobe analysis (for $Fe_2O_3$ and PbO) give $MnO_2$ 74.91, MnO 11.33, $Fe_2O_3$ (total Fe) 4.19, PbO 0.03, $H_2O$ (+) 9.46, sum 99.92%. 'Available oxygen determined by oxalate titration method is allotted to $MnO_2$ from total Mn, and the remaining Mn is calculated as MnO. Traces of Ba, Ca, Mg, K, Cu, Zn, and Al were found. Li and Na were not found. The existence of (OH) is verified from the infrared absorption spectra. The analysis corresponds to the formula $Mn^{4+}{_{4.85}}(Mn^{2+}{_{0.90}}Fe^{3+}{_{0.30}})_{1.20}O_{8.09}(OH)_{5.91}$, on the basis of O=14, 'or ideally $Mn^{4+}{_{5-x}}(Mn^{2+},Fe^{3+})_{1+x}O_{8}(OH)_{6}$ ($x{\approx}0.2$). X-ray single crystal study could not be made because of the distortion of single crystals. But the x-ray powder pattern is satisfactorily indexed by an orthorhombic cell with a 9.324, b 14.05, c $7.956{\AA}$., Z=4. The indexed powder diffraction lines are 9.34(s) (100), 7.09(s) (020), 4.62(m) (200, 121), 4.17(m) (130), 3.547(s) (112), 3.212(vw) (041), 3.101(s) (300), 2.597(w) (013), 2.469(m) (331), 2.214(vw)(420), 2.098(vw) (260), 2.014 (vw) (402), 1.863(w) (500), 1.664(w) (314), 1.554(vw) (600), 1.525(m) (601), 1.405(m) (0.10.0). DTA curve shows the endothermic peaks at $250-370^{\circ}C$ and $955^{\circ}C$. The former is due to the dehydration: and oxidation forming$(Mn,\;Fe)_2O_3$(cubic, a $9.417{\AA}$), and the latter is interpreted as the formation of a hausmannite-type oxide (tetragonal, a 5.76, c $9.51{\AA}$) from $(Mn,\;Fe)_2O_3$. Infrared absorption spectral curve shows Mn-O stretching vibrations at $515cm^{-1}$ and $545cm^{-1}$, O-H bending vibration at $1025cm^{-1}$ and O-H stretching vibration at $3225cm^{-1}$. Opaque. Reflectance 13-15%. Bireflectance distinct in air and strong in oil. Reflection pleochroism changes from whitish to light grey. Between crossed nicols, color changes from yellowish brown with bluish tint to grey in air and yellowish brown to grey through bluish brown in oil. No internal reflections. Etching reactions: HCl(conc.) and $H_2SO_4+H_2O_2$-grey tarnish; $SnCl_2$(sat.)-dark color; $HNO_3$(conc.)-grey color; $H_2O_2$-tarnish with effervescence. It is black in color. Luster dull. Cleavage one direction perfect. Streak brownish black to dark brown. H. (Mohs) 2-3, very fragile. Specific gravity 3.59(obs.), 3.57(calc.). It occurs as radiating groups of flakes, flower-like aggregates, colloform bands, dendritic or arborescent masses composed of fine grains in the cementation zone of the supergene manganese oxide deposits of the Janggun mine, Bonghwa-gun, southeastern Korea. Associated minerals are calcite, nsutite, todorokite, and some undetermined manganese dioxide minerals. The name is for the mine, the first locality. The mineral and name were approved before publication by the Commission on New Minerals and Mineral Names, I.M.A.

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