• 분석과학
• /
• 제32권6호
• /
• pp.225-232
• /
• 2019

Traceability establishment in chemical measurements is a like a linkage established through an unbroken chain from the measured results to the international system (SI) of units. The primary process for traceability establishment is the purity assignment of a target material to be measured. In this study, we studied the purity assignment of 17α-hydroxyprogesterone (17-OHP). The presence of 17-OHP is indicative of congenital adrenal hyperplasia (CAH) and it builds up due to the deficiency of 21-hydroxylase and 11β-hydroxylase enzyme in the human blood. The purity assignment of 17-OHP was performed by the mass balance method, in which the impurities are categorized into four classes: total related structural impurities, water, residual organic solvents, and nonvolatiles/inorganics. The total related structural impurities were characterized by HPLC-UV; water content was determined by Karl-Fisher coulometer; and the total residual solvents and nonvolatiles/inorganics were determined by TGA. The purity of 17-OHP from a commercial manufacturer was calculated as 993.30 mg/g, and the expanded uncertainty was 0.58 mg/g. The proposed method was validated by uncertainty evaluation and comparing with the actual value of purity.

• 분석과학
• /
• 제30권5호
• /
• pp.226-233
• /
• 2017

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

• 한국자기공명학회논문지
• /
• 제24권1호
• /
• pp.30-37
• /
• 2020

Quantitative nuclear magnetic resonance (qNMR) has been gaining attention as a purity assessment method. In particular, qNMR is recognized as the primary method to realize the Internal System of Units (SI) in organic analysis. The capability of quantitative analysis is recognized as the beginning of NMR development. NMR signals are proportional to the number of nuclei and qNMR has been used in various fields, such as metabolomics and food and pharmaceutical analysis. However, careful sample preparation and thorough optimization of measurement parameters are required to obtain accurate and reliable results. In this review, quantitative methods used in qNMR are discussed, and the important factors to be considered also introduced. The recent development of qNMR techniques including combination with chromatography and, multidimensional NMR are also presented.

• Imaging Science in Dentistry
• /
• 제53권3호
• /
• pp.217-220
• /
• 2023

Purpose: This pilot study was conducted to evaluate half-value layer (HVL) measurements obtained using a semiconductor dosimeter for intraoral radiography. Materials and Methods: This study included 8 aluminum plates, 4 of which were low-purity (less than 99.9%) and 4 high-purity (greater than 99.9%). Intraoral radiography was performed using an intraoral X-ray unit in accordance with the dental protocol at the authors' affiliated hospital: tube voltage, 60 kVp and 70 kVp; tube current, 7 mA; and exposure time, 0.10 s. The accuracy of HVL measurements for intraoral radiography was assessed using a semiconductor dosimeter. A simple regression analysis was performed to compare the aluminum plate thickness and HVL in relation to the tube voltage (60 kVp and 70 kVp) and aluminum purity (low and high). Results: For the low-purity aluminum plates, the HVL at 60 kVp (Y) and 70 kVp (Y) was significantly correlated with the thickness of the aluminum plate (X), with Y=1.708+0.415X (r=0.999, P<0.05) and Y=1.980+0.484X (r=0.999, P<0.05), respectively. Similarly, for the high-purity aluminum plates, the HVL at 60 kVp (Y) and 70 kVp (Y) was significantly correlated with the plate thickness(X), with Y=1.696+0.454X (r=0.999, P<0.05) and Y=1.968+0.515X (r=0.998, P<0.05), respectively. Conclusion: This pilot study examined the relationship between aluminum plate thickness and HVL measurements using a semiconductor dosimeter for intraoral radiography. Semiconductor dosimeters may prove useful in HVL measurement for purposes such as quality assurance in dental X-ray imaging.

• 한국재료학회지
• /
• 제26권12호
• /
• pp.688-695
• /
• 2016

Recrystallization behavior has been investigated for commercial purity AA1050 (99.5wt%Al) and high purity 3N Al (99.9wt% Al). Samples were cold rolled with 90% of thickness reduction and were annealed isothermally at 290, 315, and 350o C for various times until complete recrystallization was achieved. Hardness measurement and Electron Backscatter Diffraction(EBSD) analyses, combined with Grain Orientation Spread(GOS), were employed to investigate the recrystallization behavior. EBSD analysis combined with GOS were distinctly revealed to be a more useful method to determine the recrystallization fraction and to characterize the recrystallization kinetics. As the annealing temperature increased, recrystallization in AA1050 accelerated more than that process did in Al 3N. Both AA1050 and Al 3N showed the same temperature dependence of the n value of the Johnson-Mehl-Avrami-Kolmogorov equation(JMAK equation), i.e., n values increased as annealing temperature increased. Activation energy of recrystallization in AA1050 is about 176 kJ/mol, which is comparable with the activation energy of grain boundary migration in cold-rolled AA1050. This value is somewhat higher than the activation energy of recrystallization in Al 3N.

• 분석과학
• /
• 제24권5호
• /
• pp.360-367
• /
• 2011

8개의 제약회사에서 제조되어 현재 시판되고 있는 10개의 나프록센에 대한 광학순도를 최적조건의 키랄 HPLC로 조사하였다. Chiralcel OD-H 칼럼과 ChiralHyun-LE(S)-1 칼럼을 키랄정지상으로 사용하였고, hexane:isopropanol:acetic acid 이 100:2.85:0.1로 혼합된 용액을 전개용매로 사용하였다. 대부분 시료의 광학순도는 97% 이상이었고, 하나는 95% 수준으로 나타났다. 이 값들에 대한 상대표준편차 평균은 0.034%로 매우 작게 나타났다.

• 조명전기설비학회논문지
• /
• 제16권6호
• /
• pp.60-65
• /
• 2002

본 연구의 목적은 헬륨의 순도가 셀레늄증기 레이저에서의 출력특성과 광이득에 미치는 영향을 측정, 비교해보는 것이다. 헬륨의 순도는 특수 헬륨필터로써 개선하였다. 본 측정에서는 개개의 선들이 복굴절필터에 의해서 선택 되어졌다. 대부분의 선들이 헬륨필터를 사용한 레이저에서 더 높은 output-coupling 출력과 소신호 이득을 보여 주고, 특히 강력한 선들(497.6 nm, 499.3 nm, 506.9 nm, 517.6 nm, 522.8 nm, 530.5 nm)과 청색선(460.4 nm, 464.8 nm)및 적색선(644.4 nm, 649.1 nm)에서 현저히 더 높은 값을 보여 준다.

• 공업화학
• /
• 제19권1호
• /
• pp.105-110
• /
• 2008

증류-추출의 조합에 의해 접촉분해경유(LCO)로부터 회수한 dimethylnaphthalene (DMN) 이성체 농축액을 원료로 사용하여 결정화조작을 행해 2,6-DMN의 정제를 검토했다. 2,6-DMN의 정제에 적합한 용매의 선정을 위해 13종의 용매(acetone, cyclohexanone, ethanol, ethyl ether, ethyl acetate, isopropyl ether, methanol, n-hexane, n-heptane, pyridine, THF, toluene, methanol과 acetone의 혼합용매)를 사용하여 결정화조작을 행한 결과, 60 vol% methanol과 40 vol% acetone의 혼합용매(M/A = 1.5)가 2,6-DMN의 순도 및 수율의 측면에서 우수한 정제성능을 보였다. 결정화 온도의 상승 및 용매(M/A = 1.5)/원료(농축액)의 체적비의 증가는 2,6-DMN의 순도를 향상시켰으나, 역으로 수율의 저하를 초래시켰다. DMN 이성체 농축액을 원료(10.43 wt% 2,6-DMN)로 사용한 결정화를 통해 회수한 결정(76 wt% 2,6-DMN)을 원료로 사용하여 재차 결정화조작을 행한 결과, 40%의 수율로 99.7 wt% 2,6-DMN의 결정을 얻을 수 있었다.

• 한국대기환경학회지
• /
• 제20권1호
• /
• pp.99-110
• /
• 2004

In order to investigate the performance of carbon dioxide PSA over zeolite adsorbent, the present study showed results of isotherm measurement, cyclic operation of 3-bed apparatus, and the corresponding numerical simulation. The experiment data of bed temperature, purity, recovery were matched well with that of numerical simulation. Purity of both gas and adsorbent phase increased rapidly with rinse rate but the degree of increase was retarded for large rinse rate The total amount of adsorbed increased only 10% even if rinse rate was enlarged to 4 times. Optimal rinse rate was 7N㎥/hr in this study. The heating rinse led to augments in recovery and productivity, possibly thanks to ease of description resulting from increased volumetric rinse rate and temperature rise in the column.

• 한국신재생에너지학회:학술대회논문집
• /
• 한국신재생에너지학회 2009년도 춘계학술대회 논문집
• /
• pp.126-129
• /
• 2009

In this study, it was aimed to develop the re-use technology of ultra-fine silicon powders, by-products during the current production process of high purity poly-Si feedstock. For this goal, the compacts of the silicon powders were tried to fabricate by CIP (Cold Isostatic Pressing) method using silicon rubber mold without chemical binder materials. The density ratio of the silicon powder compacts reached 74%. In order to simulate the actual handling and charging conditions of feedstock material in casting process, a shaking test was carried out and mass loss measured. Finally, the silicon powder compacts were melted using a cold crucible induction melting method and the purity assessment was conducted by Hall effect measurement.