• Title/Summary/Keyword: titration method

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Evaluation of Drainage by Near Infrared Spectroscopy

  • Takamura, Hitoshi;Miyamoto, Hiroko;Mori, Yoshikuni;Matoba, Teruyoshi
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1271-1271
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    • 2001
  • Water pollutants in drainage mainly consist of organic compounds. Hence, total organic carbon (TOC), chemical oxygen demand (COD), and biochemical oxygen demand (BOD) were generally used as the indices of pollution. However, these values are determined by special analyzer (TOC), titration method (COD), or microbe culture (BOD). Therefore, the development of simple and easy methods for the determination of water pollution is required. The authors reported the evaluation of water pollution by near infrared (NIR) spectroscopy in a model system with food components (Takamura et al. (200) Near Infrared Spectroscopy: Proceedings of 9th International Conference, pp. 503-507). In this study, the relationship between NIR spectra and drainage was investigated in order to develop a method for evaluation of drainage by NIR. Drainage was obtained in Nara Purification Center. The ranges of TOC, COD, and BOD were 0-130, 0-100 and 0-200, respectively. NIR transmittance spectra were recorded on NIR Systems Model 6250 Research Composition Analyzer in the wavelength range of 680-1235 and 1100-2500 nm with a quartz cell (light path: 0.5, 1, 2, 4 and 10mm) at 10-40. Statistical analysis was performed using NSAS program. A partial least squares (PLS) regression analysis was used for calibration. As the result, a good correlation between the raw NIR spectra and OC was obtained in the calibration. The best light path was 10 and 0.5mm in the wavelength range of 680-1235 and 110-2500nm, respectively. In the calibration, correlation coefficients(R) were 096-0.97 in the both range. In the prediction, however, a good correlation (R=0.89-0.96) was obtained only in the range of 6801235 nm, Similar results were obtained in the cases of COD and BOD. These results suggest the possibility that NIR spectroscopy can be used to evaluate drainage.

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Optimization of Immunosasay Procedures for the measurement of Progesterone (Progesterone 측정을 위한 면역분석법의 최적조건에 관한 연구)

  • 강원준;고대환;이경광;김종배;정길생
    • Korean Journal of Animal Reproduction
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    • v.9 no.2
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    • pp.105-112
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    • 1985
  • This research was carried out to investigate the optimal conditions ssociated with the RIA procedures such as a bridging phenomena, prozone effects and a new separation methods etc. The results obtained were summarized as follows: 1. The lgG fractions of donkey anti-rabbit IgG sera were purified by Protein-A-Sepharose affinity column, which indicates that Protein-A an affinity for IgG class of donkey antiserum. 2. In coating the IgG fraction on polystryene tubes, incubation conditions made no differences between 2 hr at room temperature and overnight at 4$^{\circ}C$. 3. There were no significant differences between 1st antibody-coated tube and 2nd antibody-coated tube as a separation method when compared in terms of reproducbility. A better reproducibility may be expected if the titers of 1st antibody for the progesterone to be assayed and of corresponding 2nd antibody are reasonably high. 4. The titers of anti-progesterone antibody for 3H-progesterone and progesterone-11HS-125I were 1:300 and 1:700 in liquid-phase, and 1:100 and 1:300 in solid-phse for the separation methods. 5. A bridging phenomena in which a standard curve is long and shallow were observed when progesterone-11HS-125I was used for the tracer, but not in 3H-progesterone. 6. A prozone effect in a solid-phase system, especially 1st antibody-coated tube method was observed which the degree of inhibition was significantly different although zero bindings look the same. In this case, the titration curve should be made both in the absence and in the presence of a, pp.opriate amount of competiter, standard, respectively.

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Crystallization and high purification of aluminium chloride hexahydrate from kaolin leaching solution (고령토 침출용액으로부터 고순도 염화알루미늄 결정화 분리)

  • 김우식;장희동
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.6 no.4
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    • pp.584-594
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    • 1996
  • For the separation and purification of aluminium chloride hexahydrate crystals from kaolin leaching solution the effects of crystallization conditions, such as crystallization temperature, concentration of aluminium chloride concentration in the leaching solutin and gas flow rate of HCl into the leaching solution, on purity of the aluminium chloride hexahydrate crystals were investigated. The supersaturation level of aluminium chloride in the leaching solution gave great influence on the purity of the crystals. When supersaturated concentration of the aluminium chloride in the leaching solution was generated in low level, the aluminium chloride hexahydrate crystals were produced with high purity ; that is, the crystals hving a low Fe-ion concentration. The supersaturation level of aluminium chloride in the leaching solution was mainly determined by crystallization temperature, concentrations of aluminium chloride and hydrochloric acid in the solution. However, in spite of changes of the above crystallization coditions, a needle shape morphology of aluminium chloride hexahydrate crystals did not modified. To measure hydrochloric acid concentration in the kaolin leaching solution, we applied the oxalate titration method, which was suggested by shank [9] and it was prove that this method could titrate hydrochloroic acid concentration in multi-component ionic solution such as kaolin leaching solution.

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Determination of Neutron Absorption Fraction Factor in Manganese Sulfate Bath System (황산망간 용액조 장치의 중성자 흡수분율 보정인자 결정)

  • Lee, Kyung-Ju;Park, Kil-Oung;Hwang, Sun-Tae;Lee, Kun-Jai
    • Nuclear Engineering and Technology
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    • v.21 no.1
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    • pp.12-17
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    • 1989
  • The correction factor of neutron fraction absorbed by $^{55}$ Mn in the MnSO$_4$ bath was determined for the absolute measurement of neutron emission rate by using the solution circulation-type manganese sulfate bath system. For the determination of this correction factor, I/f, the atomic number desnsity and the effective neutron capture cross section data of Mn, S and impurity elements in the MnSO$_4$ solution were determined. For the atomic number density determination, the MnSO$_4$ solution concentration was determined by using the volumetric EDTA titration and gravimetric method. The impurity contents were analyzed by using the ICP method. For the calculation of effective neutron capture cross sections, a FORTRAN computer program EASCAL was developed in this study. in which Westcott's parameters and Axton's empirical relations are used.

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Changes in CO2 Absorption Efficiency of NaOH Solution Trap with Temperature

  • Park, Se-In;Park, Hyun-Jin;Yang, Hye In;Choi, Woo-Jung
    • Korean Journal of Soil Science and Fertilizer
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    • v.50 no.6
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    • pp.554-561
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    • 2017
  • Under the projected global warming, release of carbon as $CO_2$ through soil organic matter decomposition is expected to increase. Therefore, accurate measurement of $CO_2$ released from soil is crucial in understanding the soil carbon dynamics under increased temperature conditions. Sodium hydroxide (NaOH) traps are frequently used in laboratory soil incubation studies to measure soil respiration rate, but decreasing $CO_2$ gas solubility with increasing temperature may render the reliability of the method questionable. In this study, the influences of increasing temperature on the $CO_2$ capture capacity of NaOH traps were evaluated under $5{\sim}35^{\circ}C$ temperature range at $10^{\circ}C$ interval. Two closed-chamber experiments were performed where NaOH traps were used to capture $CO_2$ either released from acidified $Na_2CO_3$ solution or directly injected into the chamber. The sorption of ambient $CO_2$ within the incubators into NaOH traps was also measured. The amount $CO_2$ captured increased as temperature increased within 2 days of incubation, suggesting that increased diffusion rate of $CO_2$ at higher temperatures led to increases in $CO_2$ captured by the NaOH traps. However, after 2 days, over 95% of $CO_2$ emitted in the emission-absorption experiment was captured regardless of temperature, demonstrating high $CO_2$ absorption efficiency of the NaOH traps. Thus, we conclude that the influence of decreased $CO_2$ solubility by increased temperatures is negligible on the $CO_2$ capture capacity of NaOH traps, supporting that the use of NaOH traps in the study of temperature effect on soil respiration is a valid method.

Cobalt Recovery by Oxalic Acid and Hydroxide Precipitation from Waste Cemented Carbide Scrap Cobalt Leaching Solution (폐초경 스크랩 코발트 침출용액으로부터 옥살산 및 수산화물 침전에 의한 코발트 분말 회수)

  • Lee, Jaesung;Kim, Mingoo;Kim, Seulgi;Lee, Dongju
    • Journal of Powder Materials
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    • v.28 no.6
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    • pp.497-501
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    • 2021
  • Cobalt (Co) is mainly used to prepare cathode materials for lithium-ion batteries (LIBs) and binder metals for WC-Co hard metals. Developing an effective method for recovering Co from WC-Co waste sludge is of immense significance. In this study, Co is extracted from waste cemented carbide soft scrap via mechanochemical milling. The leaching ratio of Co reaches approximately 93%, and the leached solution, from which impurities except nickel are removed by pH titration, exhibits a purity of approximately 97%. The titrated aqueous Co salts are precipitated using oxalic acid and hydroxide precipitation, and the effects of the precipitating agent (oxalic acid and hydroxide) on the cobalt microstructure are investigated. It is confirmed that the type of Co compound and the crystal growth direction change according to the precipitation method, both of which affect the microstructure of the cobalt powders. This novel mechanochemical process is of significant importance for the recovery of Co from waste WC-Co hard metal. The recycled Co can be applied as a cemented carbide binder or a cathode material for lithium secondary batteries.

Analysis of Chloride Content in Aqueous Solution and Mortar using Laser Induced Breakdown Spectroscopy (LIBS를 활용한 수용액과 모르타르 내 염화물량 분석)

  • Ryu, Hwa-Sung;Park, Won-Jun
    • Journal of the Korea Institute of Building Construction
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    • v.21 no.3
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    • pp.189-194
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    • 2021
  • LIBS has been attracting attention as an analytical method capable of real-time measurement without sample preparation. In this study, a Lab. scale LIBS device was fabricated to examine the applicability and reproducibility of LIBS in the analysis of chloride contents in mortar. The existing analysis method and LIBS analysis were performed simultaneously on the mortar test specimen with the chloride content adjusted. Compared to the chloride content condition of the mortar, the XRF and Potentiometric Titration results also showed a similar trend. As a result of LIBS analysis, chlorine ions were detected at a wavelength of 837.59 nm according to the chloride content condition. In order to improve the precision in various concentration ranges, the LIBS signal amplification of about 50 times through the electric field enhancement was implemented. Through the verification of the aqueous solution-based reproducibility, a high correlation between the LIBS signal strength and the Cl concentration was confirmed, and the possibility of applying LIBS to the durability diagnosis of concrete damage by chloride was confirmed.

Comparison of the Methods to Analyze Freshwater Sediments (담수 퇴적물의 분석법간 비교 분석)

  • Yoon, Byeng-Seok;Kim, Eun-Mi;Kim, Hak-Chul;Lee, Jae-Hee;Jung, Sang-Gi;Lee, Sang-Tae
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.11
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    • pp.1207-1212
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    • 2006
  • In this study, Chemical Oxygen Demand(COD) which is the measure of organic substances, Total nitrogen(T-N), Total phosphorous(T-P), Fe and Mn were analyzed in the sediments of dam reservoir. The purpose of this study were to understand the relevances among the analytical methods adopted and the applicabilities of those methods. For the determination of COD, Standard Method for the Examination of Marine Environment(SMEME) and Standard Method for the Examination of Sanitary(SMES) was used. Both method had wide dynamic range and the deviations of the values obtained by two methods were small because $KMnO_4$ method closely reflected BOD and organic substances. For the determination of T-N and T-P, Standard Method for the Examination of Food(SMEF) and Standard Method for the Examination of Sanitary(SMES) were used. Two methods for T-N were both the acid-base titration but SMES gave less T-N values than SMEF because of the differences in digestion and distillation steps. Two methods for T-P gave the comparable values after acid digestion of $HNO_3$ and $HClO_4$. The determination of heavy metals as a Fe, Mn was mainly divided to the leaching method and acid digestion method. The values obtained by leaching method were less than those by digestion method. It is thought that the condition of acid digestion was more severe than that of leaching method.

Evaluation of CODsed Analytical Methods for Domestic Freshwater Sediments: Comparison of Reliability and Correlationship between CODMn and CODCr Methods (국내 담수퇴적물의 CODsed 분석방법 평가: CODMn법과 CODCr법의 신뢰성 및 상관성 비교)

  • Choi, Jiyeon;Oh, Sanghwa;Park, Jeong-Hun;Hwang, Inseong;Oh, Jeong-Eun;Hur, Jin;Shin, Hyun-Sang;Huh, In-Ae;Kim, Young-Hoon;Shin, Won Sik
    • Journal of Environmental Science International
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    • v.23 no.2
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    • pp.181-192
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    • 2014
  • In Korea, the chemical oxygen demand($COD_{sed}$) in freshwater sediments has been measured by the potassium permanganate method used for marine sediment because of the absence of authorized analytical method. However, this method has not been fully verified for the freshwater sediment. Therefore, the use or modification of the potassium permanganate method or the development of the new $COD_{sed}$ analytical method may be necessary. In this study, two modified $COD_{sed}$ analytical methods such as the modified potassium permanganate method for $COD_{Mn}$ and the modified closed reflux method using potassium dichromate for $COD_{Cr}$ were compared. In the preliminary experiment to estimate the capability of the two oxidants for glucose oxidation, $COD_{Mn}$ and $COD_{Cr}$ were about 70% and 100% of theoretical oxygen demand(ThOD), respectively, indicating that $COD_{Cr}$ was very close to the ThOD. The effective titration ranges in $COD_{Mn}$ and $COD_{Cr}$ were 3.2 to 7.5 mL and 1.0 to 5.0 mL for glucose, 4.3 to 7.5 mL and 1.4 to 4.3 mL for lake sediment, and 2.5 to 5.8 mL and 3.6 to 4.5 mL for river sediment, respectively, within 10% errors. For estimating $COD_{sed}$ recovery(%) in glucose-spiked sediment after aging for 1 day, the mass balances of the $COD_{Mn}$ and $COD_{Cr}$ among glucose, sediments and glucose-spiked sediments were compared. The recoveries of $COD_{Mn}$ and $COD_{Cr}$ were 78% and 78% in glucose-spiked river sediments, 91% and 86% in glucose-spiked lake sediments, 97% and 104% in glucose-spiked sand, and 134% and 107% in glucose-spiked clay, respectively. In conclusion, both methods have high confidence levels in terms of analytical methodology but show significant different $COD_{sed}$ concentrations due to difference in the oxidation powers of the oxidants.

Simultaneous Spectrophotometric Determination of Cr(Ⅲ) and Cr(Ⅳ) in Chromium Plating Solution via Flow-Through Analysis (흐름계를 이용한 크롬도금 용액의 Cr(Ⅲ)와 Cr(Ⅵ)의 분광학적 동시 분석 방법)

  • Kim, Sun Kwan;Nam, Hakhyun;So, Jae Chun;Lee, Won;Cha, Geun Sig;Han, Sang Hyun
    • Journal of the Korean Chemical Society
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    • v.39 no.2
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    • pp.87-93
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    • 1995
  • The amount of Cr(Ⅲ) and Cr(Ⅵ) in a chromium plating solution could be determined simultaneously within five minutes using UV/VIS spectrophotometer coupled with a flow-through analysis(FTA) setup. The λmax's at 580 nm and 440 nm which correspond to Cr(Ⅲ) and Cr(Ⅵ), respectively, well obey the Beer-Lambert law in the range over 0.05 g/L for Cr(Ⅲ) and 0.005 g/L for Cr(Ⅵ). when the pH of the sample is less than 4.0, the absorption extinction coefficients of those peaks are not much dependent on the proton concentration. The amount of Cr(Ⅲ) and Cr(Ⅵ), and the total chromium in post treatment chromium plating solution, which normally has few g/L of Cr concentration, could be easily measured using UV/VIS spectrophotometry after the sample had been diluted with sulfuric acid of pH=1.0 in the flow-through analysis setup; this method is far more convenient and faster than the common redox titration (which requires at least 40 min/sample) method, while the accuracy of the method is highly comparable to conventional titrimetric method. Since the implementation of an PTA-UV/VIS setup in any plating industry is cost effective and easy to operate, the analytic method described in this paper may be applied directly for in situ analysis of plating solutions.

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