• Title/Summary/Keyword: Purity analysis #3

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Development of analysis method for high purity nitrogen using GC-FID/Methanizer (GC-FID/Methanizer를 이용한 고순도 질소의 순도분석법 개발)

  • Jei, You;Jin Bok, Lee;Jin Seog, Kim;Woonjung, Kim;Kiryong, Hong
    • Analytical Science and Technology
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    • v.35 no.6
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    • pp.249-255
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    • 2022
  • In this study, a new method for the analysis of high-purity nitrogen was developed. A gas chromatography-flame ionization detector (GC-FID) was used for purity analysis. Certified reference materials (CRMs) at a level of 3 µmol/mol of carbon monoxide (CO), carbon dioxide (CO2), and methane (CH4), which may exist in high-purity nitrogen, were prepared using the gravimetric method, and these CRMs were used for purity analysis. In this new method, ultra-high-purity and high-purity nitrogen were used as carrier gases. The impurities in high-purity nitrogen were quantitatively analyzed by comparing the differences in the area values of the GC chromatograms of the prepared CRMs. We purchased liquid nitrogen and three bottles of nitrogen gas, which were produced by three different manufacturers, using high-purity nitrogen. Furthermore, to validate the developed purity analysis method, the fraction of impurities in high-purity nitrogen was compared with the results of the typical purity analysis method. The comparison results were consistent within the expanded uncertainties (k = 2).

Seed Purity Test and Genetic Diversity Evaluation Using RAPD Markers in Radish (Raphanus sativus L.)

  • Huh, Man-Kyu;Choi, Joo-Soo
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.54 no.4
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    • pp.346-350
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    • 2009
  • The cultivated radish (Raphanus sativus L.) is a major vegetable crop in the world wide and fast-growing species that grows inhabitats of six continents. It is very important to determine hybrid seed purity in the production of hybrid Brassica vegetable seeds to avoid unacceptable contamination with self-inbred (sib) seeds. The use of random amplified polymorphic DNA (RAPD) markers for evaluating seed purity in $F_2$-hybrid radish cultivars demonstrated. One hundred eighty seeds from the F1 male and female harvest were subsequently screened for seed purity using 13 primers. The 13 primers result in 17 cultivar-specific bands and 23 variable RAPD bands scored for cultivar. RAPD analysis of hybrid seeds from the harvest revealed 128 seeds tested except underdevelopment and decayed seeds were sibs. Especially, $F_2$ hybrids of radish, OPC13, OPD20 were presented clear hybrid bands. It maintains higher than average level of genetic diversity compared with their correspondent parents. RAPD amplification of DNA extracted from germinated individuals from the female harvest reveal that 10 of 208 seeds tested were self-inbred (4.8%). RAPD analysis of hybrid seeds from the male harvest revealed 7 of the 208 seeds tested were sibs (3.4%). The RAPD may lead to a better insight in to the hybrid seed purity.

Assessment of the Purity of Emodin by Quantitative Nuclear Magnetic Resonance Spectroscopy and Mass Balance

  • Park, Sojung;Choi, Yu-Jin;Do, Giang Hoang;Seo, Eun Kyoung;Hyun, Seunghun;Lee, Dongho
    • Natural Product Sciences
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    • v.25 no.3
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    • pp.222-227
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    • 2019
  • Quantitative nuclear magnetic resonance (qNMR) is a well-established method adopted by international pharmacopoeia for quantitative and purity analyses. Emodin is a type of anthraquinone, well known as the main active component of Fabaceae, Polygonaceae and Rhamnaceae. Purity analysis of emodin is usually performed by using the high-performance liquid chromatography (HPLC)-UV method. However, it cannot detect impurities such as salts, volatile matter, and trace elements. Using the qNMR method, it is possible to determine the compound content as well as the nature of the impurities. Several experimental parameters were optimized for the quantification, such as relaxation delay, spectral width, number of scans, temperature, pulse width, and acquisition time. The method was validated, and the results of the qNMR method were compared with those obtained by the HPLC and mass balance analysis methods. The qNMR method is specific, rapid, simple, and therefore, a valuable and reliable method for the purity analysis of emodin.

1Determination of optical purity of N-acetyl-1-naphthylethylamine by chiral chromatography and NMR spectroscopy (키랄 크로마토그래피와 NMR 분광법에 의한 N-acetyl-1-naphthylethylamine의 광학순도 측정)

  • Jeong, Young-Han;Ryoo, Jae-Jeong
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.97-101
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    • 2010
  • (R)-N-3,5-dinitrobenzoyl (DNB) phenylglycinol derived chiral selector was used as a HPLC chiral stationary phase (CSP) for the resolution of racemic N-acylnaphthylalkylamines. In this study, determination of optical purity was performed by both chiral chromatography and NMR spectroscopy by using the (R)-phenylglycinol derived chiral selector. The data of accuracy and precision of each optical purity value are calculated from the results of NMR and HPLC experiments by comparing with true value. Average error of the NMR method was +2.2% with average RSD of 4.54%, while that of HPLC method was -3.5% with average RSD of 3.23%.

A Study on the Formation of Spinel Pigment(Green Pigment based on Magnesium-Chrome) (Spinel Pigment의 생성반응에 관한 연구)

  • 이응상;박철원;황성연
    • Journal of the Korean Ceramic Society
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    • v.12 no.1
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    • pp.29-36
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    • 1975
  • This study was conducted to research the formation, color development and application for colored glazes of the spinel solid solutions of the green pigment. On specimens prepared by calcining the oxide and basic carbonate mixture at 1250℃ for 1.5 hour, the x-ray analysis, measurement of reflectance and the test of their stabiality as a glaze pigment were carried out. The results are summarized as follows 1) Each sample is composed of single spinel and not of mixture of spinel. 2) Formation of continuous soild solution, except for a few instances, pertaining to Vegard's law was confirmed by means of the x-ray analysis. 3) The more difference between absorption and reflectance lies, the lighter colors are. When the absorption occurs at the high-reflectance, the excitation purity becomes low. On the contrary when the absorption takes place at the low-reflectance, the excitation purity becomes low. On the contrary when the absorption takes place at the low-reflectance, the excitation purity is higher. 4) Colors obtained in the CdO-MgO-Cr2O3-Al2O3 system, as the amounts of Al3+ increased, change from green through brown to pink, and the absorption peak shifts towards violet region. 5) An increase in Co2+ in the CoO-MgO-Cr2O3-Al2O3 system, changes the color from blue green to dark blue. The excitation purity is higher, and the absorption peak shifts toward regions. 6) Colors are green in the NiO-MgO-Cr2O3 and CdO-MgO-Cr2O3 systems in general, but in the ZnO-MgO-Cr2O3 system brillant hue is not obtained. 70 According to the results of the colored glaze test, the spinels turn outto be stable as brilliant glaze pigment in the calcium-magnesia glaze.

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Development of analytical method for the isotope purity of pure D2 gas using high-precision magnetic sector mass spectrometer

  • Chang, Jinwoo;Lee, Jin Bok;Kim, Jin Seog;Lee, Jin-Hong;Hong, Kiryong
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.205-211
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    • 2022
  • Deuterium (D) is an isotope with one more neutron number than hydrogen (H). Heavy elements rarely change their chemical properties with little effect even if the number of neutrons increases, but low-mass elements change their vibration energy, diffusion rate, and reaction rate because the effect cannot be ignored, which is called an isotope effect. Recently, in the semiconductor and display industries, there is a trend to replace hydrogen gas (H2) with deuterium gas (D2) in order to improve process stability and product quality by using the isotope effect. In addition, as the demand for D2 in industries increases, domestic gas producers are making efforts to produce and supply D2 on their own. In the case of high purity D2, most of them are produced by electrolysis of heavy water (D2O), and among D2, hydrogen deuteride (HD) molecules are present as isotope impurities. Therefore, in order to maximize the isotope effect of hydrogen in the electronic industry, HD, which is an isotope impurity of D2 used in the process, should be small amount. To this end, purity analysis of D2 for industrial processing is essential. In this study, HD quantitative analysis of D2 for high purity D2 purity analysis was established and hydrogen isotope RM (Reference material) was developed. Since hydrogen isotopes are difficult to analyze with general gas analysis instrument, they were analyzed using a high-precision mass spectrometer (Gas/MS, Finnigan MAT271). High purity HD gas was injected into Gas/MS, sensitivity was determined by a signal according to pressure, and HD concentrations in two bottles of D2 were quantified using the corresponding sensitivity. The amount fraction of HD in each D2 was (4518 ± 275) μmol/mol, (2282 ± 144) μmol/mol. D2, which quantifies HD amount using the developed quantitative analysis method, will be manufactured with hydrogen isotope RM and distributed for quality management and maintenance of electronic industries and gas producers in the future.

Synthesis of Phospholene Oxide Catalysts for Hydrolysis Stabilizers (가수분해 방지제 제조용 Phospholene Oxide 촉매의 합성)

  • Lee, Jin-Ha;Lee, Chang-Young
    • Applied Chemistry for Engineering
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    • v.26 no.1
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    • pp.86-91
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    • 2015
  • The MPPO (3-methyl-1-phenyl-2-phospholene-1-oxide) was prepared by using various polymerization inhibitors such as BHT (2,6-di-tert-butyl-4-methylphenol), TBC (4-tert-butylcatechol), and copper stearate. The MPPO was confirmed by the analysis using FTIR, $^1H$-NMR, and GC/MS regardless of the type of inhibitors. The yield of MPPO increased with the increase of reaction time, whereas the purity of MPPO decreased slightly. The yield and purity of MPPO increased with temperature, but the MPPO prepared by using copper stearate as a polymerization inhibitor exhibited no changes in the purity. The amount of inhibitors had no effect on the yield of MPPO. The purity of MPPOs increased with the amount of inhibitors, but the MPPO prepared by using BHT showed no changes of the purity. We found that the MPPO prepared by using copper stearate exhibited the highest catalytic activity for diphenylcarbodiimide synthesis.

Analysis of 3-Dimensional Magnetic Field Distribution in C.P.M Considering Magnetization Vector Distribution (자화 벡터 분포를 고려한 C.P.M(Convergence Purity Magnet)의 3차원 자계 분포 해석)

  • Lee, Chol-Gyu;Kwon, Byung-Il;Park, Seung-Chan;Yoon, Tae-Ho
    • Proceedings of the KIEE Conference
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    • 2000.11b
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    • pp.241-243
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    • 2000
  • In this paper, we analyze three-dimensional magnetic field distribution of a convergence purity maget(C.P.M) which is used for a cathode ray tube. The magnetization vector distribution of the C.P.M is obtained from the result of magnetization process analysis using the 2D F.E.M. Then the motion of electron beam passing through the inner space of the C.P.M is determined and compared with experimental result.

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Fabrication and Characterization of High Purity Al2O3 by Decomposition of Selicite (세리사이드 분해에 의한 고순도 Al2O3의 제조 및 특성에 관한 연구)

  • 이경희;박한수;송명신
    • Journal of the Korean Ceramic Society
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    • v.24 no.5
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    • pp.431-436
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    • 1987
  • High purity Al2O3 has been extracted from serlcite of clayminerals, selicite was treated by H2SO4(2N∼18N) solution, NH4OH treatment(PH8.5∼10.0) and metallic impurities such as Fe were removed by NaOH treatment. The tendency of extraction yield of ${\alpha}$-Al2O3 have been investigated by relating reaction time, acid concentration. Reaction products were analyzed by DT-TGA, chemical analysis and X-ray diffractometer. Prepared ${\alpha}$-Al2O3 power is fired in air at 1400$^{\circ}C$, 1600$^{\circ}C$ 2hr. The results are as follows; 1. The most suitable extracting conditions of ${\alpha}$-Al2O3 from Selicite were N-H2SO4, 120 min acidtreating time. 2. The optimum pH condition was 9.0. 3. Physical properties of sintered Al2O3 bodies were as follows. Relative density is 99%. Water absorption is 0.26%. Rock well hardness is 89.

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Extraction Chromatograph Separation Spark Source Mass Spectrometric Analysis of 14 Rare Earth Impurities in High Purity Rare Earth Oxide

  • Sui, Xiyun;Wang, Zishu;Shao, Baohai
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.553-559
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    • 1995
  • An extraction chromatographic method of separating rare earth impurities from high purity $Nd_2O_3$, $Sm_2O_3$, $Gd_2O_3$, $Er_2O_3$, $Dy_2O_3$ and $Yb_2O_3$ was studied by using $HCl-NH_4Cl$ as moving phase and P507 as stationary phase. After the impurities were enriched from the eluate by chelant-activated carbon, the active carbon was ashed and the ignited residue was used to prepare the sample electrode for spark source mass spectrometric determination. The impurities in 99.9999% rare earth oxide can be determined by the proposed method with recovery over 80%.

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