Spectrophotometric Determination of Iron with EDDHA (Ethylenediamine N N′ Bis O-Hydroxyphenilacetic Acid) by Derivative Spectroscopy

Abstract

Derivative spectrometry is applied to a spectrophotometric determination of iron with EDDHA. the effect of amount of reagent, acidity, time and temperature have also been studied. the interval of application of the method is increased to 0.16–15.36 μg Fe(III) mL^?1. the reproducibility, precision and potential interferents have been investigated. the interferences due to chlorate, wolframate, molybdate, permanganate, cyanide, cromate, Cu(II), Be(II), Ce(III), Al(III), Hg(II), Sn(II) and Zn(II) are reduced in this new procedure.     

Extraction,Separation and Spectrophotometric Determination of Bismuth(III) Using 1(4′-Bromophenyl) 4,4,6-Trimethyl (1H,4H)-Pyrimidine-2-Thiol

Abstract

The operating conditions for the spectrophotometric determination of bismuth(III) with 1-(4′-bromophenyl)-4,4,6-trimethyl-(1H,4H)-pyrimidine-2-thiol (4′bromo PTPT) as a ligand by a liquid-liquid extraction technique are presented. In acidic conditions bismuth(III) forms a yellow complex with the ligand which can be extracted in chloroform with an absorption maxima at 410 nm. The molar absorptivity is 1.5×10⁴ l mole^?1 cm^?1 and Sandell's sensitivity is 14.3 ng cm^?2. The difference in the absorbance between the chloroform blank and bismuth(III) sample increases linearly in the concentration range 2-14 ppm at 0.3 M hydrochloric acid. The proposed method is extremely sensitive, rapid, reproducible and has been satisfactorily applied to the determination of trace amounts of bismuth(III) in synthetic mixtures, alloys and pharmaceutical formulations and also provides binary separation of bismuth(III) from selenium, tellurium, lead, antimony, copper and gold. The overall process of extraction and determination takes about 15 to 20 min.     

Spectrophotometric determination of acidity constants of 4-(2′-thiazolylazo)-resorcinol (TAR) in water-organic mixtures

<正>The acidity constants of TAR in different water-organic solvent binary mixtures at 25℃have been determined spectrophotometrically. DATa ANalysis(DATAN) program was used for calculations of the acidity constants and pure spectra of all formed species and their concentration distribution diagram in applied pH interval.Results show that there are a fairly inverse relationship between acidity constants and the mole fraction of the organic solvent in the binary mixtures.Effects of solvent composition on the pK_as and pure spectrum of each component are also discussed.     

Spectrophotometric determination of uranium with 5-(2′-carboxyphenyl)azo-8-quinolinol in the non-ionic micellar medium of Triton X-100

Triton X-100, a non-ionic surfactant, has been used to sensitize the reaction of 5-(2-carboxyphenyl)azo-8-quinolinol with uranium in aqueous medium at pH 5.2–6.1 to form a wine red coloured complex. The micellar sensitization results in two and a half-times enhanced molar absorptivity enabling the determination of uranium in rock samples at ppm level, stability of the complex enhanced from 4 hours to at least 72 hours. Extraction of the complex is avoided making the procedure simple, rapid and easy in operation. The molar absorptivity and Sandell's sensitivity of the complex are 1.50·10⁴l·mol^–1·cm^–1 and 15.9 ng·cm^–2, respectively, at _max=568 nm. Beer's law is obeyed over the range 0–3.3 g·ml^–1 of uranium. An amount as low as 0.19 g·ml^–1 of uranium could be determined satisfactorily within a relative standard deviation of ±1.3%. The limits of determination and practical quantitation are 0.29 and 1.80 ppm, respectively. The method was applied to the determination of uranium in soil, stream sediment and rock samples.     

Ternary Complex Nickel(II)/3-(4′,5′-Dimethyl-2′-Thiazolylazo)-2,6-Dihydroxybenzoic Acid/Cyanide. Spectrophotometric Determination of Nickel

Abstract

A spectrophotometric method for nickel has been developed based on the formation of a ternary complex in the system Ni(II)/3-(4′,5′-dimethyl-2′-thiazolylazo)-2,6-dihydroxybenzoic acid/cyanide at pH 9.2 (borate buffer), which allows the determination of 0.05–0.47ppm of nickel (ε = 3.53×10⁴ 1.mol^?1. cm^?1) at 538nm. Interferences have been studied and the method applied to the determination of nickel in low alloy steels.     

β-(4-Nitrophenyl)-α,α′-dichlor-hydracrylsäure

Zusammenfassung Basenkatalysierte Kondensation von 4-Nitrobenzaldehyd mit Dichloracetonitril in Methanol lieferte ein als Methyliminoäther aufgefaßtes Kondensationsprodukt, dessen salzsaure Hydrolyse die im Titel genannte Säure ergab. Sie erwies sich als völlig ident mit einem Präparat, das in einer vorigen Arbeit durch Hydrolyse des 2-[-(4-Nitrophenyl)--oxy-,-dichlormethyl]-oxazolin erhalten wurde.     

5-(2′-Carboxyphnyl) Azo-8-quinolinol as a Sensitive Reagent for Extractive Spectrophotometric Determination of Nickel

Abstract

A new sensitive extractive spectrophotometric method for the determination of nickel in sub-microgram level is discussed. 5-(2′-carboxyphenyl) azo-8-quinolinol reats with nickel at pH 5.2 to 6.1 to produce a wine red complex extractable in isomayl alcohol. The complex is stable for 24 hrs. Beer's law is obeyed in the range 0.04 to 0.60 ug of nickel per ml. The molar absorptivity and Sandell's sensitivity of the method are 5.5 × 10⁴1. mol^?1 cm^?1 and 0.001 μg cm^?2, respectively, at wavelength of maximum absorption (λ max 540 nm). Effects of diverse ions and variables have been studied in detail. The method has been applied to the determination of nickel in alloys like manganin, constantan, german silver, bronze, steel and in geological samples. Features of the method include high sensitivity, excelllent reproducibility and reliability.     

Spectrophotometric Determination of Iron(Ⅱ) Diphosphine Carbonyl Compounds Using Charge-transfer Ban

ＳｐｅｃｔｒｏｐｈｏｔｏｍｅｔｒｉｃＤｅｔｅｒｍｉｎａｔｉｏｎｏｆＩｒｏｎ（Ⅱ）ＤｉｐｈｏｓｐｈｉｎｅＣａｒｂｏｎｙｌＣｏｍｐｏｕｎｄｓＵｓｉｎｇＣｈａｒｇｅ－ｔｒａｎｓｆｅｒＢａｎｄＬＩＳｏｎｇ－ｌａｎ,ＺＨＡＮＧＢａｏ－ｓｈｅｎ,ＷＡＮＧＺｈｉ－...     

Spectrophotometric Determination of Cadmium(II) Using p,p′‐Dinitro‐SYM‐Diphenylcarbazid in Aqueous Solutions

Abstract

A sensitive and selective spectrophotometric method is proposed for the rapid determination of cadmium(II) using, p,p′‐dinitro‐sym‐diphenylcarbazid, directly in aqueous solution. The reaction between cadmium(II) and p,p′‐dinitro‐sym‐diphenylcarbazid occurs immediately in strong basic media (0.02 N sodium hydroxide solution). The complex shows a maximum of absorption at 630–640 nm, and the absorbance remains stable for at least 24 h. The method allows the cadmium determination over the range 0.5–6.0 µg mL^?1, with a molar absortivity of 2.05×10⁴ L mol^?1 cm^?1 and features a detection limit of 0.13 ppm. The interferences caused by several ions [Ca(II), K(I), Ba(II), Al(III), Pb(II), Zn(II), Cl^?1, NO₃ ^?, SO₄ ^2?], which are present in most of environmental samples, were determined. The validation of the spectrophotometric method was done by recovery test of cadmium(II) in tap water and sea water. The results show that the proposed method has been successfully applied to the determination of cadmium(II) in water samples.     

Spectrophotometric Method for the Determination of Cobalt with N,N′-Bis(2-Aminobenzoyl)Ethylenediamine

 A simple and direct spectrophotometric method has been developed for the determination of cobalt(II) using N,N′-Bis(2-aminobenzoyl)ethylenediamine (Baben). The method is based on the colour reaction between Baben and cobalt(II) in borax buffer (pH 9.2). The studies are carried out at 470 nm at which the calculated value of molar absorptivity is found to be 1.102 × 10⁴ L mol⁻¹ cm⁻¹. The system obeys Beer’s law over a wide range of concentration (2–20 μg/ml). The effect of interfering ions has been studied and the method was applied to the determination of cobalt in water, industrial effluents and in alloys and the results were highly satisfactory. Received May 8, 2000. Revision January 30, 2001.     

Spectrophotometric determination of molybdenum(V) by extraction of its 2-(2′-furyl)-3-hydroxychromone complex

A simple method is described for the rapid spectrophotometric determination of molybedenum in synthetic and industrial samples containing 0.1-5% Mo. Molybdenum is reduced with ascorbic acid at room temperature in 1 mol dm^–3 H₂SO₄ and extracted with chloroform after adding 2-(2-furyl)-3-hydroxychromone (FHC). The yellow colour of the 1 2 Mo-FHC complex is measured at 414 nm against a reagent blank. Beer's law is obeyed over the range 0-2.7 g Mo cm^–3 of solvent phase. The molar absorptivity and Sandell's sensitivity are 5.18 × 10⁴ dm³ mol^–1 cm^–1 and 0.0018 g Mo cm^–2, respectively. Relative standard deviations are 0.2% for solutions and 0.5–1.5% for solid samples. Interference from tungsten and tin is removed by adding citrate and EDTA, respectively, while niobium and tantalum are masked by fluoride. Many elements such as V, Fe, Ti, U, Mn, Cr, Co, Ni, Re, Ru, Pt, Rh, Se, Au, Bi, Zr, Th, Ce, As and Al do not interfere even in large amounts, but antimony always interferes. Among the anions and complexing agents, only thiocyanate interferes seriously.     

A Spectrophotometric Study of Complexation Between Nickel(II) and 4-(5′-Methyl-3′-Isoxazolylazo)Resorcinol

Abstract

The complexation equilibria between Ni(II) and 4-(5′-methyl-3′-isoxazolylazo)resorcinol have been spec-trophotometrically studied in a 20% (v/v) ethanol-water medium at 0.1M NaCIO₄ ionic strength and species NiHR (log β₁₁₁ = 14.83 ± 0.05), NiR (log β₁₀₁ = 9.32 ± 0.04) and NiR₂ (log β₁₀₂ = 17.84 ± 0.05) are established.     

Synthesis and Structure Determination of (2S, 2′S)-3-Phenyl-2-(pyrrolidin-2′-yl)- propionic Acid

Abstract

Aβ²,β³-homoproline derivative, (2S, 2′S)-3-phenyl-2-(pyrrolidin-2′-yl)propionic acid, was synthesized starting from l-proline. After preparation of the (4S, 4aS)-4-benzyl-4a,5,6,7-tetrahydro-pyrrolo-[1,2-c]pyrimidine-1,3-dione under a mild condition, the absolute configuration of target compound was assigned using 2D H-H COSY and H-H NOESY technologies.     

Determination of Mn(Ⅱ) Using l-(2-pyridylazo)-2-naphthol Solid Liquid Extraction Spectrophotometry

A procedure is described for the spectrophotometric determination of Mn(Ⅱ) after extraction with molten paraffin. The complex of Mn(Ⅱ) with l-(2-pyridylazo)-2-naphthol can be extracted quantitatively into paraffin in the range of PH=8.5~10.0. After solidified paraffin is dissolved in CHC1₃, the absorbance is determined at 570nm. Beer's law is obeyed in the range of 0 to lOug Mn/lOml. The linear regression equation is A=0.0032+0.0486C, the relative coefficient r=0.9997.     

Synthesis of Sucrose 4′-(L-Arabinose-2-YL Phosphate) (Agrocinopihe A) Using an Arabinose 2-H-Phosphonate Intermediate

Abstract

The first completed chemical synthesis of Agrocinopine A (5) is presented. The key step in the synthesis was the pivaloyl chloride promoted condensation of a blocked arabinose 2-H-phosphonate derivative 3 with a protected sucrose derivative 1 having a free hydroxyl at 4′-OH. The resulting H-phosphonic acid diester was oxidised in situ with iodine to produce the corresponding phosphodiester 4, which was subsequently deblocked to give Agrocinopine A.     

Indirect Spectrophotometric Determination of Sulphide with the Complex of Cd(Ⅱ)-5-Br-PADAP-CPB

ampornoNTh6SpetemofCd-&Br-PADAPis~SenSitbo(s=l.4Xlotl.mol-l.CIn-'),ltwaSuSUaIly~todet6rInintal-[1],butitedotodboboeofitsWatertheOlUbuny,italSocanbeodtodetermineodboinwater8oforbobytheuseOfnthe8ufor[2J.Intthework,catiOnisuthetantwasedinCd-5Br-PADAPsy8tem,itssensitivityndthenduzn~tionwavelengthhaofthecomplexcanbeincred2O%and2onInreSpeivelybycom-P8tisonwithliteratureL2J.TheapplicaiOnOfdsterwicomplexspstemtosperOPhOtomethedeterminaiOnofsulPhidefromitseboOfdecreaseinabeorPtboonth…     

Spectrophotometric Determination of Trace Chromium(VI) in Mass Chromium(III)

There is little conclusive evidence of the toxic effects of Cr(III) so far, but Cr(VI) has carcinogenic activity, so the analysis of the chromine ions is very important in environmental research and the quality control of industry products. Usually Cr(III) and Cr(VI) interfere with each other in the species analysis, the measurement of Cr(VI) of numerous previous papers is related to the Cr(VI) samples, which contain a little Cr(III). When the amount of trivalent chromine exceeds ten …     

Determination of the enantiomeric purity of 2-(2′-carboxy-3′-phenylcyclopropyl)glycines by chiral capillary electrophoresis

Summary A fast and practical chiral capillary electrophoretic method has been developed for determination of the enantiomeric purity of 2-(2′-carboxy-3′-phenylcyclopropyl)glycine (PCCG) compounds. In particular, the isomer PCCG-13, a potent selective and competitive antagonist at phospholipaseD-coupled metabotropic glutamate receptors (mGluRs), was completely resolved from its enantiomer PCCG-15 by use of dimethyl-β-cyclodextrin (DMCD) as chiral selector. pH 9.0 running buffer containing 2-amino-2-methyl-1,3-propanediol (AMPD; 100mM) was a suitable medium enabling resolution of the enantiomers in a short (32.5 cm total length) poly(vinyl alcohol) (PVA)-coated capillary. Because of the suppression of the electroosmotic flow and the good peak shape, baseline resolution of the enantiomers was obtained by use of the optimum concentration of chiral selector. For quantitative purposes at impurity levels, high sample loading was required and adequate separation was obtained in the presence of 80 mM DMCD. This CE method enabled quantification of 0.3% m/m of undesired enantiomer in PCCG-13; the samples analyzed, obtained from enantioselective synthesis, proved to be of high enantiomeric purity.     

Spectrophotometric Simultaneous Determination of Zinc(II), Manganese(II) and Iron(II) in Pharmaceutical Preparations Using OSC-PLS

The purpose of this paper is to develop a fast and sensitive spectrophotometric method for the simultaneous determination of zinc(II), manganese(II) and iron(II) in pharmaceutical preparations. The method presented in this work is based on the well-known reaction of these ions with 4-(pyridylazo)resorcinol (PAR)1. The application of quantitative chemometric methods, particularly PLS to multivariate chemical data is becoming more widespread owing to the availability of digitized spectroscop…     

Spectrophotometric study of the complexation equilibria of cobalt(II) with 4-(5′-methyl-3′-isoxazolylazo)-resorcinol and determination of cobalt(II)

The reaction of cobalt(II) with 4-(5′-methyl-3′-isoxazolylazo)-resorcinol (MIAR) in 4% v/v ethanol-water medium at I = 0.1 M (NaClO₄) was investigated spectrophotometrically. Graphical and numerical calculation methods were used to establish the equilibria in solution and to evaluate the stability constant of the complexes formed (log β₁₀₁ = 7.48±0.06, log β₁₁₁ = 12.77 max 12.99, log β₁₀₂ = 16.41±0.07). The optimum conditions for the spectrophotometric determination of Co(II) with MIAR were established and the method applied to its determination in some low alloy steels and hydrofining catalysts.