• Title/Summary/Keyword: Method detection limits

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Spectrochemical Determination of Impurities in Rutile (金紅石內에 포함된 不純物의 分光化學的 測定)

  • Jae-Young Hwang
    • Journal of the Korean Chemical Society
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    • v.10 no.2
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    • pp.98-102
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    • 1966
  • A spectrochemical method for the determination of the major impurities, such as aluminum, iron, magnesium and silicon, in rutile single crystals and variously doped rutile is presented. By applying higher current (12 amp) and a 1:2 sample-to-graphite dilution by weight, the elaborate sample preparation needed for conventional fusion technique was avoided, and relatively higher detection limits were established. Average deviations are approximately ${\pm}8%$ for iron and magnesium in the concentration ranges of 0.007 to 0.7% and 0.006 to 0.6% respectively, and ${\pm}5%$ for aluminum and silicon in the range of 0.005 to 0.5%.

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Evaluation Technology for the Flaw Sizing of Generator Rotor by Using Phased Array Ultrasonic Technique (위상배열 초음파기법을 이용한 발전기 로터 결점크기 평가)

  • Kim, Jin-Hoi;Park, Cher-Young;Lee, Sang-Hoon
    • Transactions of the Korean Society of Pressure Vessels and Piping
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    • v.5 no.1
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    • pp.14-19
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    • 2009
  • NDE(Nondestructive examination) detects a flaw or discontinuity in materials. Flaws detected by the examination shall be evaluated for the decision basis of the integrity. The internal flaws of forging products can be detected by UT. However, UT has detection limits because of its reflected signal weakness. Normally, a 1mm or less flaw is known as the limit. If a flaw was detected, the size of flaw would be evaluated by AVG(or DGS) technique. To verify the evaluation data, alternative examination methods are needed. But there is no alternative examination methods until now. In this study, Phased array ultrasonic technique can be used to size the flaws in the generator rotor with focused beam of ultrasonic wave as a supplement method of AVG. Also, the phased array ultrasonic technique described enables the shape of flaw to be depicted exactly.

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A Study on Evaluation of Accuracy and Precision on B, T, X Analysis Using Thermal Desorption/Gas Chromatograph/Flams Ionization Detector (열탈착/GC/FID를 이용한 B, T, X 분석의 정확도 및 정밀도 평가)

  • 박정근;유기호
    • Journal of Korean Society for Atmospheric Environment
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    • v.16 no.3
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    • pp.265-275
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    • 2000
  • By using thermal desorption/gas chromatograph/flame ionization detector(TD/GC/FID), this study was carried out to evalute an accuracy and a precision on Benzene(B), Toluene(T), o-Xylene(X) analysis in an industrial hygiene laboratory. Limits of detection of TD/GC/FID on B, T, X were showed 13.75ng/sample or less. For the accuracy of the method by concentration levels, overall bias was showed 7.7% as an absolute value, and the pooled coefficient of variation showed 3.51%. For the precision on repeatability of peak area and retention time between within-run and between-run of analytical system, it is showed the results of within-run gave better than those of between-run. Also the accuracy by sorbents(Tenax TA and Chromosorb 106)was evaluated, and the precision on reproducibility between MDHS72 and this study was compared. It is showed it is possible for TD/GC/FID to evaluate accurately B, T, X concentration levels of less than 1ppm at indoor or outdoor of workplaces in Korea.

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Simultaneous Determination of Plasma Lactate, Pyruvate, and Ketone Bodies following tert-Butyldimethylsilyl Derivatization using GC-MS-SIM

  • Yoon, Hye-Ran
    • Biomedical Science Letters
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    • v.21 no.4
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    • pp.241-247
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    • 2015
  • Lactate and ketone bodies are considered biological markers for ketosis and several inherited metabolic disorders. In the current study, the specific ratios of lactate and ketone bodies as analytical tools for differential diagnosis of various lactic acidosis were devised. The study included a protein precipitation step following tert-butyldimethylsilyl derivatisation. Total run time was approximately 30 min including sample preparation and GS/MS analysis. The limits of detection were below 0.1 pg/mL over the targeted 4 analytes. The calibration curve was linear over the concentration range of $0.001{\sim}250{\mu}g/mL$ for pyruvate, beta-hydroxybutyrate, and acetoacetate ($R^2$ > 0.99). Inter-day accuracy and precision were 87.7~94.8% with RSD of 2.5~5.7% at 2 levels. Absolute recoveries (%) of target analytes were 87.0~98.4%. The method was validated for the quantification of lactate and ketone bodies for differentiation of lactic acidosis.

Microanalysis of Metocurine Iodide in Urine and Blood by HPLC (HPLC를 이용한 뇨 및 혈액중 Metocurine Iodide의 미량분석)

  • Kim, Kyung-Nim;Lee, Jong-Pil;Kim, Hyo-Jin;Kim, Bak-Kwang
    • YAKHAK HOEJI
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    • v.38 no.4
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    • pp.379-388
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    • 1994
  • A new method for the analysis of metocurine iodide in biological fluids was developed. Metocurine iodide was quantitatively extracted with rose bengal from aqueous layer into dichloromethane layer and the amount of metocurine iodide was calculated from the amount of rose bengal which was determined by HPLC with fluorescence detector. It was possible to analyze metocurine iodide without the effect of co-prescribed drugs in the concentration range of $0.09{\sim}9.10\;{\mu}g/ml$. The detection limits of metocurine iodide in urine and blood were 0.8 and 1.2 ng at S/N=3, each respectively.

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Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Jeong Soo;Kim, Do Hwan;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3971-3976
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    • 2012
  • A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

A Novel Phase Extraction for the Detection of Time Parameters in Signal

  • Lee Eun-bang
    • Journal of Navigation and Port Research
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    • v.29 no.4
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    • pp.341-347
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    • 2005
  • A unique technique to extract the phase in time domain is proposed in order to measure the time parameters such as speed and depth by transmitting sound and electric waves. In the signal analysis processing, the phase of pulse signal can be transformed and digitalized with local data in real time without the effect of direct current bias and Nyquist limits. This method is sensitive to base frequency of pulse signal with high spacial resolution and is effective to compare two signals which have different forms. It is expected that the phase analysis technique will be applied to the measurement of the speed and depth accurately by ultrasonic pulse signal in water.

A Study on Detection Method of Sulfonamides Residues in Raw Milk by HPLC (HPLC를 이용한 원유중 잔류 Sulfonamides 분석법 연구)

  • 정동수;윤교복;김종술;신명균;김교승
    • Korean Journal of Veterinary Service
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    • v.16 no.1
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    • pp.11-19
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    • 1993
  • This experiment was carried out to detect the residues of sulfonamides in raw milk. Raw milks which does not contain sulfonamides was collected from one of the farm and fortified with 5 sulfonamides (sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfadimethoxine, sulfaqinoxaline). The sulfonamides in the fortified sample were extracted and detected by High Performance Liquid Chromatography. UV /vis detector was used in this experiment. The results obtained were summarized as follows : 1. Chloroform was good as a extracting solution. 2. 15.5% methanol in PDP as a mobile phase solution was best detective condition for SMR, SMT, SMM. But for SDM and SQN the best condition was 23% methanol. 3. The detectable limits of SMR, SMT, SMM were 2ppb. but SDM and SQN were 20ppb because of delayed retention time and relatively low recovery rate. 4. The peaks of SMR, SMT, SMM and SDM were erected at baseline and the apexes were sharp but SQN was round shape.

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The Simultaneous Analysis of Oxytetracycline, Chloramphenicol and Sulfamethoxazole in Pork by HPLC (HPLC를 이용한 돈육 중의 Oxytetracycline, Chloramphenicol 및 Sulfamethoxazole의 동시검출)

  • 조혜연;조진국;이치호
    • Food Science of Animal Resources
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    • v.21 no.1
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    • pp.64-70
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    • 2001
  • The extraction procedure and HPLC condition were modified to analyze the residues of oxytetracycline, sulfamethoxazole and chloramphenicol in pork, simultaneously. The antibacterial agents in pork were extracted with 0.02M EDTA-Mcilivine buffer:ethanol:acetonitrile (5:3:2). After the removal of fat with n-hexane, the extracts were evaporated and purified with Sep-pak $C_{18}$ cartridge column using 0.01M oxalic acid 0.1% (v/v) triethylamine (TEA) in acetonitrile. The peak of antibacterial agents was detected with $\mu$ Bondapak C18 column, UV detector (280nm) and 0.01M oxalic acid: methanol: acetonitrile (7.5:2.0:0.5). Detection limits for three antibacterial standards were 0.03 ppm. Calibration curves were linear between 0.03 and 2.0 ppm (R$^2$>0.999). When spiked the level of 1.0 ppm of oxytetracycline, sulfamethoxazole and chloramphenicol into meats, the recoveries from meats were 77.3%, 79.7% and 59.3%, respectively. These results showed that the modified extraction method provided good analytical resolution and the recoveries of the above antibacterial agents in meats.

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The Analysis of Common Metabolites of Organophosphorus Pesticides in Urine by Gas Chromatography/Mass Spectrometry

  • 박성수;표희수;이강진;박송자;박택규
    • Bulletin of the Korean Chemical Society
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    • v.19 no.1
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    • pp.45-50
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    • 1998
  • Most organophosphorus pesticides may be metabolized to yield some common phosphates in human or in animals, and these metabolites may be used as the exposure biomarkers to pesticides. In this study, we developed the extraction method of four phosphate metabolites from the spiked human urine in high recovery by the solid phase extraction with a reverse-phase cartridge (cyclohexyl silica) followed by the elution with methanol. The extracted urinary metabolites were derivatized with hexamethyldisilazane/trimethyl-chlorosilane/pyridine (2 : 1 : 10, v/v/v) and identified by gas chromatography/mass spectrometry. Calibration curve obtained from each metabolite standard using by GC/MS/SIM has shown good linearity and detection limits of metabolites were the range of 0.05-0.1 ㎍/㎖ in urine. Phenthoate, one of the organophosphorus pesticides, was orally administrated to rats. Four metabolites were detected in the rat urine. The results of this study may be applied to development of exposure biomarkers for monitoring of environmental pollutants.