• 제목/요약/키워드: Determination of Fe(II)

검색결과 61건 처리시간 0.025초

Spectrophotometric Determination of Palladium after Solid-liquid Extraction with 4-(2-Pyridylazo)-resorcinol at 90°C

  • Dong, Yanjie;Gai, Ke
    • Bulletin of the Korean Chemical Society
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    • 제26권6호
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    • pp.943-946
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    • 2005
  • An effective spectrophotometric determination of palladium with 4-(2-pyridylazo)-resorcinol (PAR) using molten naphthalene as a diluent has been studied. A red complex of palladium with PAR is formed at 90 ${^{\circ}C}$. In the range of pH 9.0-11.0, the complex is quantitatively extracted into molten naphthalene. The organic phase is anhydrously dissolved in $CHCl_3$ to be determined spectrophotometrically at 520 nm against the reagent blank. Beer’s law is obeyed over the concentration range of 0.1-2 ${\mu}g{\cdot}mL^{-1}$. The molar absorptivity and Sandell’s sensitivity are 8.0 ${\times}\;10^5\;L{\cdot}mol^{-1}{\cdot}cm^{-}1\;and\;0.49\;{\mu}g{\cdot}cm^{-2}$ respectively. From the results of tolerance limits, it was found that there was no interferences were observed for most of the ions examined and those somewhat high interferences by Co(II), Fe(II) and Bi(III) could be effectively masked by EDTA.

2-(5-브로모-2-피리딜아조)-5-(N-프로필-N-슬포프로필아미노)아닐린을 사용하여 흐름주입법에 의한 코발트의 분광광도법적 정량 (Flow Injection Spectrophotometric Determination of Cobalt with 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)aniline)

  • 강삼우;김인영;한흥석;이승석
    • 분석과학
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    • 제6권1호
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    • pp.57-63
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    • 1993
  • 흐름주입법에 의하여 분광광도 방법으로 코발트를 정량하였다. $NH_3-NH_4Cl$ 완충용액(pH 10.5)에서 2-(5-bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)aniline은 코발트와 수용성 착물을 형성한다. 이 착물의 최대흡수 파장은 545nm이고, 몰흡광계수는 $58000L\;mol^{-1}\;cm^{-1}$이다. 코발트의 검정곡선은 0.1~0.6ppm 범위에서 직선관계를 보였고, 검출한계는 25ppb였다. 상대표준편차는 0.5ppm에 대하여 ${\pm}0.72%$였고, 시료의 채취속도는 $60samples\;hr^{-1}$였다. 여러 가지 양이온과 음이온의 방해효과를 조사한 결과, NI(II), Cu(II), Fe(III) 및 $CN^-$이 많은 방해를 하였다. 그러나 운반체흐름에 $1.0{\times}10^{-3}M$ EDTA 용액을 넣음으로써 금속이온들의 방해를 감소시킬 수 있었다.

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Novel Solid Phase Extraction Procedure for Some Trace Elements in Various Samples Prior to Their Determinations by FAAS

  • Sacmaci, Srife;Kartal, Senol;Sacmaci, Mustafa;Soykan, Cengiz
    • Bulletin of the Korean Chemical Society
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    • 제32권2호
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    • pp.444-450
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    • 2011
  • A novel method that utilizes poly(5-methyl-2-thiozyl methacrylamide-co-2-acrylamido-2-methyl-1-propanesulfonic acid-co-divinylbenzene) [MTMAAm/AMPS/DVB] as a solid-phase extractant was developed for simultaneous preconcentration of trace Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Ni(II), Pb(II), and Zn(II) prior to the measurement by flame atomic absorpiton spectrometry (FAAS). Experimental conditions for effective adsorption of the metal ions were optimized using column procedures. The optimum pH value for the simultaneously separation of the metal ions on the new adsorbent was 2.5. Effects of concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of the analytes were investigated. A high preconcentration factor, 100, and low relative standard deviation values, $\leq$1.5% (n = 10), were obtained. The detection limits (${\mu}gL^{-1}$) based on the 3s criterion were 0.18 for Cd(II), 0.11 for Co(II), 0.07 for Cr(III), 0.12 for Cu(II), 0.18 for Fe(III), 0.67 for Mn(II), 0.13 for Ni(II), 0.06 for Pb(II), and 0.09 for Zn(II). The validation of the procedure was performed by the analysis of two certified reference materials. The presented method was applied to the determination of the analytes in various environmental samples with satisfactory results.

A STUDY ON THE STELLAR PHYSICAL PARAMETERS

  • Lee, Sank-Gak;Kim, Ke-Young
    • 천문학논총
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    • 제8권1호
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    • pp.243-263
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    • 1993
  • One hundred forty two digital spectra of 110 standard stars with 1 A resolution in ${\lambda}{\lambda}\;3000\;A\;{\sim}4150\;A$ region were analyzed to determine the spectral indices sensitive to the atmospheric parameters. The standard stars cover the temperature in the range of $T_eff$ from ${\sim}4000^{\circ}$ to ${\sim}7000^{\circ}\;K$ and the surface gravity in the range of log g from 0 to 5 and the metal abundance [Fe/H] from -2.7 to 0.4. We have derived physical parameters, theta(=T/5040), log g, and [Fe/H] for the standard stars using indices, P(38/93), Fe I(A), Fe I(B), SrII, and $H{\delta}$, with overall accuracies of 0.067, 0.617, and 0.466, respectively. However for some region of spectral type and metallicity, those can be obtained with better accuracies. Those indices are found to be useful especially for stellar gravity determination.

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납-티오황산 착물생성과 구리치환에 의한 미량 납(II)의 비색분석에 관한 연구 (Spectrophotometric Determination of Trace Lead(II) After Extraction of Lead-Thiosulfate Complex into Aliquat336-CHCl$_3$ and Replacement by Cu)

  • Lee, Seok-Ki;Joung, Chang-Ung
    • 한국환경보건학회지
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    • 제24권3호
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    • pp.1-5
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    • 1998
  • A spectrophotometric method was developed for the acidic solution stripped after an extraction of 0.5 to 2.5 ppm of Lead(II) from 50 mL of $Na_2S_2O_3$ solution into chloroform as the ion-pairs formed between their thiosulfate complexes and alkylamine, Aliquat336. Pb(II) in the stripped solution forms an complex with DDTC in pH 7.3 buffer solution, and was developed in yellow by copper replacement. The ydlow-colored solution have the maximum absorbance at 435 nm in the measurement of absorbance by UV-Visible spectrophotometer. The interference ions such as Fe(III), Hg (II), Al(III), Co, Cu, Ni, Zn, Ca, Sn, have great effects on the extraction, but they were overcomed by the usage of adequate masking agents before an extraction. At last, a good result was obtained in applying this method to synthetic water.

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Development of Photo-Fenton Method for Gaseous Peroxides Determination and Field Observations in Gwangju, South Korea

  • Chang, Won-Il;Shim, Jae-Bum;Hong, Sang-Bum;Lee, Jai H.
    • Journal of Korean Society for Atmospheric Environment
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    • 제23권E1호
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    • pp.16-28
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    • 2007
  • An improved method was developed to determine gas-phase hydrogen peroxide($H_2O_2$) and organic hydro-peroxides (ROOH) in real-time, The analytical system for $H_2O_2$ is based on formation of hydroxybenzoic acid (OHBA), a strong fluorescent compound. OHBA is formed by a sequence of reactions, photoreduction of Fe(III)-EDTA to Fe(II)-EDTA, the Fenton reaction of Fe(II)-EDTA with $H_2O_2$, and hydroxylation of benzoic acid. By use of this analytical method rather than a previous similar method, Fenton reaction time was reduced from 2 min. to 30s. Air samples were collected by a surfaceless inlet to prevent inlet line losses. With a special arrangement of the sampling apparatus, sample delivery time was drastically reduced from ${\sim}5\;min\;to\;{\sim}20\;s$. The automated system was found to be sensitive, capable of continuous monitoring, and affordable to operate. A comparison of this method with a well-established one showed an excellent linear correlation, validating applicability of this technique to $H_2O_2$ determination. The system was applied to field measurements conducted during summertime of 2004 in Gwangju, South Korea. $H_2O_2$ was found to be a predominant species of peroxides. The diurnal variation of $H_2O_2$ displayed the maximum in early afternoon and the broad minimum throughout night. $H_2O_2$ was correlated positively with ozone, photochemical age, and temperature, however, negatively with $NO_x$ and relative humidity.

호소내 퇴적물의 수질오염물질 분석(II) - 중금속 - (Determination of Heavy Metals for Sediment Proximated to Water in Lake(II))

  • 박선구;김성수;고오석
    • 분석과학
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    • 제14권2호
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    • pp.140-146
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    • 2001
  • K 수계 5개 지점의 3종류 퇴적물에 대해 Fe, Cu, Cr, Zn, Cd를 측정분석하였다. 물과 근접된 퇴적물(5cm)이 다른 퇴적물(5-10cm, 10cm)보다 Fe, Cu, Cr, Zn, Cd 모두 높은 값을 나타내었다. 물과 근접된 퇴적물의 중금속 결과는 34.9-39.8mg Fe/L, 34.5-44.8mg Cu/L, 68.0-79.2mg Cr/L, 147.4-126.0mg Zn/L, 2.2-1.0mg Cd/L를 나타내었다. 이상의 결과로부터 퇴적물이 호소내 수질오염에 영향을 미치는 요인임을 알 수 있었다.

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$P^{32}$ 추적자법(追跡子法)에 의(依)한 토양(土壤)의 유효인산정량법(有動燐畿定量法)에 관(關)한 연구(硏究) (II) (Studies with $P^{32}$ Tracer on Laboratory Index of Available Phosphorus in Paddy Soil, Korea (II))

  • 이춘영;박훈
    • Applied Biological Chemistry
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    • 제13권1호
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    • pp.73-79
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    • 1970
  • 한국답토양십종(韓國畓土壤十種)을 시료(試料)로하여 유효인산정량(有動燐酸定量)에 적합한 화학적(化學的) 추출방법(油出方法)을 찾고저 A-value인(燐)-32 추적자법(追跡子淪)에 의한 유효인산정량치(有效燐酸定量値)를 표준으로 하여 시험한 결과 다음과 같은 결과(讀果)를 얻었다. 1 A·value는 Fe-P(인산철(燐酸鐵))와만 1%수준(水準)의 유의상관(有意相鬪)이 있으므로 답토양(畓土壤)의 유효인산(有刻燐酸)은 Fe·p계(系)에 의하여 지배(支配)되고 있다고 볼 수 있다. 2. 본(本) 실험(實驗)에 사용(使用)한 6개침출법(個浸出法)은 Fe-P와 상안(相關)이 없으므로 답토양유효인산정량법(容土壤有效燐酸定量法)으로 적합하지 않다. 3. 답토양유효인산(容土壤有效燐酸)에 적합한 침출법(浸出法)은 Fe-P계(系)의 환원강도(還元强度)를 측정(測定)할 수 있는 것이어야 하며 침출강도(浸出强度)는 평균(平均) 270 ppm 으로 추정(推定)된다. 4. Bray No. 2-p는 Lancaster-p, Spurway-p, Truog-p 및 (Ca+Al)-p와 5% 수준(水準) 이상(以上)에서 유의상관(有意相關)이 있고 Al-P는 Olsen-P 및 Lancaster-p와, Ca-p는 Spurway-p와 1% 수준(水準)에서 유의상관(有意相關)이 있다.

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Ce(OH)$_3$의 공침부선에 의한 해주중 몇 가지 미량원소의 동시 농축 및 정량 (Simultaneous Concentration and Determination of Several Trace Elements in Sea Water by Ce(OH)$_3$ Coprecipitation)

  • 성우식;최희선;김영상
    • 대한화학회지
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    • 제37권3호
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    • pp.327-333
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    • 1993
  • 침전부선법에 의한 해수중 몇 가지 미량원소이 예비농축에 관하여 연구하였으며, 농축된 원소들을 불꽃 원자흡수분광법으로 정량하였다. Cd(II), Cu(II), Fe(III), Mn(II), Pb(II) 및 Pd(II) 등의 미량원소를 정량적으로 농축하기 위하여, 해수 1.0l에 1.0M Ce(III)용액 2.0 ml를 가하고 자석젓개로 저어주면서 5.0M NaOH 용액으로 pH 를 9.5로 조정하여 침전시켰다. 부선용기에서 계면활성제인 0.3% sodium oleate 용액 1.0 ml 가하고 다공성(porosity No.4) 유리판을 통하여 질소기체를 통과시켜 침전들을 용액 표면으로 띄웠다. 부선된 침전들을 모아서 거르고 씻은 다음 8.0M HNO$_3$으로 녹여 탈이온수로 10.0ml되게 만들었다. 원자흡광도를 측정하여 농축된 원소들을 정량하였다. 동해안 강릉지역과 서해안 강화도지역의 해수 중 상기 분석원소들의 농도는 이 방법의 검출한계 이하였다. 그러나 이 방법의 응용성을 보기 위하여 해수시료에 일정량의 원소들을 첨가하여 분석한 회수율이 92% 이상이었다.

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유도결합 플라즈마 원자방출 분광법에 의한 아연광 중 Ga 및 In의 분석에 관한 연구 (Studies on Analysis of Gallium and Indium in Zinc Ores by Inductively Coupled Plasma Atomic Emission Spectrometry)

  • 황윤옥;심상권;성학제;양명권
    • 분석과학
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    • 제6권1호
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    • pp.131-139
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    • 1993
  • 아연광 중 미량으로 존재하는 갈륨 및 인듐을 유도결합 플라스마 원자방출분광법(ICP-AES)으로 분석할 때 간섭하는 아연 및 다른 이온들과 특히 Fe(III) 이온으로부터 이들을 분리하는 방법에 대해 연구하였다. 갈륨과 인듐을 tributyl phosphate(TBP)로 용매추출하였는데 이때 영향을 주는 산농도, 다른 이온들의 간섭, 수용액상/유기상의 비율, TBP의 농도 및 탈거율 등에 대하여 조사하였다. 갈륨과 인듐이 함유되어 있는 아연광을 녹인 5N 염산용액에서 100% TBP로 추출하여 아연 및 기타 간섭이온들로부터 분리하였으며, 이때 철(III)이온은 hydroxylamine hydrochloride를 사용하여 Fe(II)로 환원시켜 coetraction되는 것을 방지하였다. 유기상으로부터 갈륨과 인듐의 탈거는 0.02N 염산용액으로 역추출하여 이루어졌으며 이 용액을 ICP-AES로 측정하여 이들을 정량하였다. 전체적으로 추출률이 95% 이상으로 정량적이었다.

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