FTIR과 XRD를 이용한 a.-Quartz 분석법 비교

김부욱(Boo Wook Kim),이종성(Jong Seong Lee),최병순(Byung-Soon Choi) 한국환경보건학회 2009 한국환경보건학회지 Vol.35 No.2

This study compared FTIR with XRD method for the anysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coεfficient of determination (r2) was 0.9998 in a calibration curve of 695 cm-1, and the limit of detection was 4.9 μg/sample. 2. The highest recovery was 799 cm-1 (98.2%). 3. πle CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for qutz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve,and the limit of detection was 5.9 μg/sample. 6. The recovery and CV pooled were 104.3%, and 11 %, rζ, spective1y. 7. In mufflε fumace asng, the quartz weight decrled to 34% when the maximum weit of the iron 0dε was more than eight times. In conclusion, the accuracy (% recovery) and pr떠sion (CV) of FTIR and XRD method for analyzing a.-qutz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of inκrference. However, XRD method dis디ng버shed specific crystalline forms of silica, and the majority of silicatε minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

FTIR과 XRD를 이용한 α-Quartz 분석법 비교

김부욱,이종성,최병순,Kim, Boo-Wook,Lee, Jong-Seong,Choi, Byung-Soon 한국환경보건학회 2009 한국환경보건학회지 Vol.35 No.2

This study compared FTIR with XRD method for the analysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coefficient of determination ($r^2$) was 0.9998 in a calibration curve of $695\;cm^{-1}$, and the limit of detection was $4.9{\mu}g/sample$. 2. The highest recovery was $799\;cm^{-1}$ (98.2%). 3. The CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for quartz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve, and the limit of detection was $5.9{\mu}g/sample$. 6. The recovery and CV pooled were 104.3%, and 11 %, respectively. 7. In muffle furnace ashing, the quartz weight decreased to 34% when the maximum weight of the iron oxide was more than eight times. In conclusion, the accuracy (% recovery) and precision (CV) of FTIR and XRD method for analyzing $\alpha$-quartz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of interference. However, XRD method distinguished specific crystalline forms of silica, and the majority of silicate minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

FTIR과 XRD를 이용한 α-Quartz 분석법 비교

김부욱,이종성,최병순 한국환경보건학회 2009 한국환경보건학회지 Vol.35 No.2

This study compared FTIR with XRD method for the analysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coefficient of determination (r2) was 0.9998 in a calibration curve of 695㎝−1, and the limit of detection was 4.9 ㎍/sample. 2. The highest recovery was 799㎝−1 (98.2%). 3. The CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for quartz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve, and the limit of detection was 5.9 ㎍/sample. 6. The recovery and CV pooled were 104.3%, and 11%, respectively. 7. In muffle furnace ashing, the quartz weight decreased to 34% when the maximum weight of the iron oxide was more than eight times. In conclusion, the accuracy (% recovery) and precision (CV) of FTIR and XRD method for analyzing α-quartz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of interference. However, XRD method distinguished specific crystalline forms of silica, and the majority of silicate minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

XRD와 XAS에 의한 TiO₂ 분말의 상분율 결정

나사균,이연승,Rha, Sa-Kyun,Lee, Youn Seoung 한국세라믹학회 2012 한국세라믹학회지 Vol.49 No.5

The crystallinity and phase ratio of anatase to rutile in $TiO_2$ were estimated by x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS). Traditionally, the structural characterization of $TiO_2$ powders has been carried out by XRD techniques, which are comparatively easy in use and analysis. However, materials with amorphous phase, nano-sized or nano-structured crystallinities cannot be fully characterized by XRD because XRD analysis has a limit for abnormal contributions of the nano-crystal such as the surface contribution. From the comparison with the experimental and calculated Ti K-edge XAS spectra, we found the possibility of efficient estimation in the crystalinites and the phase ratio of anatase to rutile for nano-sized $TiO_2$ mixture.

XRD와 XAS에 의한 TiO2 분말의 상분율 결정

나사균,이연승 한국세라믹학회 2012 한국세라믹학회지 Vol.49 No.5

The crystallinity and phase ratio of anatase to rutile in TiO2 were estimated by x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS). Traditionally, the structural characterization of TiO2 powders has been carried out by XRD techniques, which are comparatively easy in use and analysis. However, materials with amorphous phase, nano-sized or nano-structured crystallinities cannot be fully characterized by XRD because XRD analysis has a limit for abnormal contributions of the nano-crystal such as the surface contribution. From the comparison with the experimental and calculated Ti K-edge XAS spectra, we found the possibility of efficient estimation in the crystalinites and the phase ratio of anatase to rutile for nano-sized TiO2 mixture.

산화반응에 의한 이방성 메조페이스 탄소섬유의 구조 변화(I) - TEM 및 XRD를 이용한 분석

노재승,Roh, J.S. 한국재료학회 2003 한국재료학회지 Vol.13 No.12

Structural changes during oxidation of anisotopic mesophase carbon fiber(AMCFs) have been observed with TEM and XRD. It was shown that the AMCFs are three dimensionally stacked structure of turbostratic layers, and are non-homogeneous structure which consist of the highly ordered areas and the random areas. The $d_{ 002}$, Lc, and La of AMCFs which were measured by XRD were 3.44, 146, and $135\AA$, respectively. It was observed that the oxidation initiated at the random areas, because the $d_{002}$ / decreased to the value of 3.41 $\AA$ during initial oxidation stage. It was also observed that the La of the oxidized AMCFs increased up to 182 $\AA$ during the whole oxidation process, and the $d_{002}$ of that increases up to 9.44 $\AA$ when the burn-off is over the degree of 20%. Therefore, it was suggested that the micro-crystalline grew up by heat treatment effects during the fibers were oxidized, In addition, it was shown that there was difference in the measured value of La by XRD and TEM, in case of 39% oxidized fibers for example, the measured La was $ 165\AA$ by XRD and in the range of 180∼220 $\AA$ by TEM.

해산 이매패류 패각의 CaCO₃ 결정 구조에 대한 X-ray 회절 분석

남기웅,이승우,송재희,정희도,박경일,Nam, Ki-Woong,Lee, Seng-Woo,Song, Jae-Hee,Jeung, Hee-Do,Park, Kyung-Il 한국패류학회 2015 The Korean Journal of Malacology Vol.31 No.4

본 연구는 해산 이매패 8종에 대해 패각 결정 (結晶)에 대한 분광학적 특성을 XRD 기법을 이용하여 조사하고 종간 근연관계에 대해 기존의 조사와 비교하였다. XRD분석을 수행한 결과, 바지락, 백합, 꼬막, 새조개의 패각은 $CaCO_3$의 orthorhombic 결정형인 aragonite였으며, 가리비와 굴의 패각은 trigonal-rhombohedral 결정형인 calcite였다. 담치와 키조개의 경우 aragonite와 calcite가 혼합된 결정으로 분석되었다. XRD를 이용하여 측정된 패각의 x-선 회절정보는 패류별 특이성을 나타내었으며, 이러한 특성을 이용한 과 (Family) 간 근연관계를 조사한 결과 현재 알려진 분류체계를 잘 대변하고 있었다. 결론적으로 패각 결정 (結晶)에 대한 분광학적 특성은 조사된 패류의 과 (Family) 수준에서 특이성을 잘 나타내며, 향후 종수준의 연구를 통한 종 동정을 위한 추가 연구가 필요함을 시사하였다. 또한 이러한 기술은 소량의 패각을 이용하므로 미확인 소량 절편의 패류 종 파악에 유용하게 이용될 수 있을 것으로 기대된다. This study investigated spectroscopic characteristics of shell crystals of eight marine bivalve species using X-ray diffraction (XRD) analysis; moreover, the Family level relatedness of shellfish was investigated. In XRD analysis, the shells of Ruditapes philippinarum, Meretrix lusoria, Anadara granosa, and Fulvia mutica were found to have orthorhombic aragonite $CaCO_3$ crystals, while shells of Patinopecten yessoensis and Crassostrea gigas had trigonal-rhombohedral calcite crystals. The shells of Mytilus coruscus and Atrina pectinata were determined to have a mixture of aragonite and calcite crystals. XRD information revealed the Family level-specific characteristics of shellfish; the results agreed with the current taxonomic system. In conclusion, spectroscopic characteristics of shell crystals indicated Family-level characteristics of shellfish and suggested a more intense species-level investigation; this technology may be useful in identifying shellfish species using small quantities of shells.

$BaTiO_3$의 입도와 분체특성과의 상관 관계 연구

전명표,조정호,김병익,Chun, M.P.,Cho, J.H.,Kim, B.I. 한국결정성장학회 2005 한국결정성장학회지 Vol.15 No.6

수열합성법에 의해 제조된 티탄산바륨 (BT01, BT02, BT03, BT04, BT05)의 입자크기와 분체특성과의 상관관계를 비표면적, 제타전위, XPS, XRD 및 SEM에 의해 조사하였다. 레이져광산법에 의해 측정된 입자의 크기는 비표면적과 XRD를 통해 결정된 격자이방성과 밀접한 관계가 있음을 보였다. 분말의 비표면적은 입자의 크기가 증가함에 따라 감소하였으며, BT03 시료는 동일한 입자크기의 BT04에 비하여 큰 비표면적을 보였으며, 이는 입자들의 응집에 기인하는 것으로 SEM사진 및 XRD 분석을 통하여 밝혀졌다. 입자의 크기가 증가함에 따라 제타전위는 증가하는 경향을 보였으며, BT02와 BT03 분말은 다른 분말에 비하여 제타전위가 큰 음의 값을 나타내었다. XPS 분석결과 분쇄시 티탄산바륨과 물 사이의 반응에 의한 $Ba^{2+}$ 이온의 용출과 관련이 있는 것으로 분석되었다. The relationship between particle size of hydro-thermally synthesized barium titanate powders (BT01, BT02, BT03, BT04, BT05) and the powder properties was investigated by means of particle size, specific surface area, zeta potential, XPS, XRD and SEM. Particle size determined by laser light scattering is closely related with specific surface area and the tetragonality (c/a) obtained from XRD. The specific surface area of the samples inversely decreased with increasing particle size except BT03 powder. BT03 sample showed higher surface area than BT04 sample of equivalent particle size, which was attributed mostly to the agglomeration of particles in terms of SEM image and XRD analysis. Zeta potential increased with increasing particle size with the exception of BT02 and BT03 which showed larger minus value of zeta potential in comparison with other BT powders. Beta potential results of BT02 and BT03 are considered to be related with the dissolution of $Ba^{2+}$ ion in these powers which was examined by XPS.

XRD 피크 면적을 이용한 탄산칼슘 결정 형태의 정량분석

박영철 ( Young-cheol Bak ) 한국화학공학회 2022 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.60 No.4

Calcium carbonate (CaCO₃) exhibits three polymorphs: calcite with arhombohedral, vaterite with a spherical, and aragonite with a needle-like structure. Qualitative and quantitative analyses of the morphology of CaCO₃ are very important to investigate the synthesis of single-crystal vaterite and aragonite. In this work, the polymorphs of calcium carbonate were quantitatively analyzed using XRD. Pure vaterite and pure aragonite were synthesized and the peak distribution of a single phase was analyzed. The vaterite fraction of a mixture of calcite and vaterite was calculated based on the intensity of a specific diffraction peak, and compared to the results based on the peak area. The mean value of f_sV (the correction factor for the peak area of vaterite) was 0.654. The phase analysis of calcite-aragonite mixtures was performed, and the mean value of f_sA (the correction factor for the peak area of aragonite) was obtained as 0.6713. Using these factors, Eq. (24)~Eq. (32) for the quantitative analysis based on the total peak area of XRD were derived to calculate the phase contents of ternary phase CaCO₃. And three-component XRD section was defined considering overlapping sections.

Structural Study of the Oxidized High Modulus Carbon Fiber using Laser Raman Spectroscopy

Jae-Seung Roh,Suk-Hwan Kim 한국탄소학회 2009 Carbon Letters Vol.10 No.1

This study aims to find a correlation between XRD and Raman result of the oxidized high modulus carbon fibers as a function of its oxidation degrees, and compare with the isotropic carbon fiber reported early. La of the high modulus carbon fiber prepared by oxidation in carbon dioxide gas have been observed using laser Raman spectroscopy. The basic structural parameters of the fibers were evaluated by XRD as well. The La of the original high modulus carbon fibers were measured to be 144 a from Raman analysis and 135 a from XRD analysis. La of the 92% oxidized fiber were 168 a by using Raman and 182 a by using XRD. There was some correlation between the La value obtained from Raman and XRD. However the La value changes of the high modulus carbon fiber through whole oxidation process showed opposite tendency compare with the isotropic carbon fiber because of the fiber structure basically.