Promethazine hydrochloride as a new redox indicator in vanadametry

Promethazine hydrochloride is proposed as a new redox indicator in vanadametry. It has been tested rigorously in the titration of iron(II), hydroquinone, uranium(IV) and antimony(III) with sodium vanadate. The indicator gives a very sharp reversible colour change from green to violet at the equivalence point. It has advantages over all the proposed redox indicators in vanadametry. Its redox and transition potentials are reported.     

Chlorpromazine hydrochloride as a new redox indicator in vanadametry

Chlorpromazine hydrochloride is proposed as an indicator in the vanadametric titration of iron(II) and molybdenum(V). It gives a sharp, reversible colour change from green to violet at the equivalence point. It has advantages over the diphenylamine class of indicators. Its redox and transition potentials are reported.     

The use of vanadium-sulphosalicylic acid complex as a redox indicator

In a previous communication it was reported that vanadium^V gives an intense turquoise-blue colour with sulphosalicylic acid in concentrated sulphuric acid and that the colour reaction is specific and very sensitive for the detection of vanadium^V. During our studies on the nature of the complex, it was found that vanadium^IV gives a negative colour test and that the blue colour developed by the reagent with vanadium^V is discharged on the addition of a reducing agent like iron^II, uranium^IV or hydroquinone. It was also observed that the blue colour is restored by the addition cerium^IV solution. This reversible property of the complex has been further investigated to see if the complex can be used as a redox indicator.     

Nickel phthalocyanine sulphonic acid as a redox indicator in cerimetry

Summary The use of nickel phthalocyanine sulphonic acid (Ni-PS) as an internal indicator in the cerimetric titration of iron(II) has been investigated. 0.2 ml of a 0.05% solution of the dye serves well as a redox indicator in 50 ml of the titration mixture. The colour change at the end point is from blue to violet. The addition of about 2.5 ml of syrupy phosphoric acid to 50 ml of the titration mixture has been found to be advantageous as it increases the life period of the violet coloured transitory oxidation product of Ni-PS. The Ni-PS indicator is superior to the Cu-PTS indicator previously reported, in that the intermediate violet oxidation product obtained with the former at the equivalence point has a longer life period.It has been observed that in the cerimetric titration of 3–8 ml of about 0.1 N uranium(IV) diluted to 50 ml, the equivalence point is marked by a colour change from turquois blue to colourless, without the appearance of any intermediate violet colour. However, the intermediate violet colour appears, if 3 ml of syrupy phosphoric acid is added before the start of the titration. In the titration of more dilute solutions of uranium(IV) the indicator gives premature and hazy end points. How-ever, in the presence of phosphoric acid, correct equivalence points are obtained.The cerimetric titration of molybdenum(V) using Ni-PS as indicator is recommended to be carried out in 2 N sulphuric acid medium. The addition of phosphoric acid is not necessary. The colour change at the equivalence point is from turquois blue to violet which is stable for 10–15 sec.

---

Zusammenfassung Nickel-phthalocyanin-sulfonsäure (NPS) kann als Indicator bei der cerimetrischen Titration von Eisen(II), Uran(IV) und Molybdän(V) mit gutem Erfolg verwendet werden. Auf 50 ml Titrationslösung benötigt man 0,2 ml einer 0,05%igen Lösung des Indicators. Der Farbumschlag am Endpunkt erfolgt von Blau nach Violett. Ein Zusatz von 2,5 ml sirupöser Phosphorsäure auf 50 ml Lösung ist vorteilhaft, da er die Lebensdauer des violett gefärbten Zwischenproduktes der Oxydation von NPS erhöht. Der NPS-Indicator ist wegen der längeren Beständigkeit des erwähnten Zwischenproduktes der früher beschriebenen Kupferphthalocyanin-tetrasulfonsäure überlegen.Bei der cerimetrischen Titration von 3–8 ml ungefähr 0,1 n Uran (IV)-lösung, die auf 50 ml verdünnt wurde, erhält man einen Farbumschlag von Türkisblau nach Farblos, ohne daß das Violett gefärbte Zwischen-produkt auftritt. Wenn man jedoch vor der Titration 3 ml sirupöse Phosphorsäure zusetzt, so erscheint die violette Farbe. Bei der Titration verdünnterer Lösungen ergeben sich vorzeitige und unklare Farbum-schläge. Doch führt auch hier ein Zusatz von Phosphorsäure zu richtigen Werten.Die Titration von Molybdän (V) mit dem beschriebenen Indicator wird am besten in 2n schwefelsaurer Lösung ausgeführt, wobei ein Phosphorsäurezusatz nicht erforderlich ist. Der Farbumschlag erfolgt von Türkisblau nach Violett (Beständigkeit 10–15 sec).

     

Optochemical sensor for an ornidazole assay using 1-amino-4-allyloxyanthraquinone as a fluorescent indicator.

To improve the stability of optochemical sensors (optodes), the fluorescence indicator 1-amino-4-allyloxyanthraquinone (AAA), which was synthesized by reacting allyl bromide with 1-amino-4-hydroxyanthraquinone, was covalently immobilized on surface-modified glass slides. The resulting sensor was used to determine the content of ornidazole based on fluorescence quenching. It showed a linear response toward ornidazole in the concentration range of 9.0 x 10(-6) to 1.0 x 10(-3) mol L(-1) with a detection limit of 8 x 10(-6) mol L(-1) at pH 7.5. This AAA-immobilized sensor has a rapid response, high stability and good selectivity to ornidazole.     

Use of nickel phthalocyanine sulphonic acid as redox indicator in cerimetry

Summary In part II of this series the titrations of ferrocyanide, hydroquinone and arsenic(III) with cerium(IV) using the indicator nickel phthalocyanine sulphonic acid are studied. The conditions and the limits of reactions are determined.

---

Zusammenfassung Im II. Teil dieser Reihe werden die Titrationen von Hexacyanoferrat(II), Hydrochinon und Arsen(III) mit Cer(IV)-Lösung unter Verwendung als Indicators Nickel-phthalocyanin-sulfonsäure studiert. Die Reaktionsbedingungen und ihre Grenzen werden festgelegt.

---

---

Part I: Z. analyt. Chem. 190, 213 (1962).     

Some new applications of ferroin as redox indicator in titrations with dichromate

Working conditions for the titration of arsenic(III), hydroquinone, ferrocyanide, uranium(IV) and molybdenum(V) with dichromate in sulphuric acid and hydrochloric acid media have been established, with ferroin as the redox indicator.     

Use of diethazine hydrochloride for the extractive spectrophotometric determination of uranium and as a redox indicator

Optimum conditions have been established for the formation and extraction of the complex formed from diethazine, thiocyanate and uranium(VI). An extractive spectrophotometric method for the determination of uranium(VI) is described. Experimental conditions have been also established for the direct titrimetric determination of uranium(IV) with potassium dichromate, using diethazine hydrochloride as redox indicator. Interferences have been considered.     

Methyl orange as a redox indicator in titrations with ceric ammonium nitrate in perchloric acid

Summary Conditions for the use of methyl orange as a redox indicator for the titration of iron(II), hydroquinone and oxalate with cerio ammonium nitrate dissolved in perchloric acid, have been established. It is found that methyl orange behaves as a reversible indicator with a transition potential of 955±10 mV. Nitric acid as a medium of titration is not satisfactory.

---

Zusammenfassung Methylorange kann als Redoxindicator bei der Titration von Eisen(II), Hydrochinon und Oxalat mit Cer(IV)-ammoniumnitrat in perchlorsaurer Lösung verwendet werden. Der Indicator hat ein Umschlagspotential von 955±10 mV. In salptersaurem Medium erhält man keine befriedigenden Werte.

     

Binding of 2-amino-4-chloro-m-benzenedisulfonamide as a metabolite of hydrochlorothiazide to erythrocytes

2-Amino-4-chloro-m-benzenedisulfonamide (ACBS) is a metabolite of hydrochlorothiazide. We reported that the ACBS concentration in erythrocytes was higher than in plasma in a patient. Therefore the binding of ACBS to rabbit erythrocyte was studied. The Scatchard plot showed the nonlinear plot and the horizontal asymptote. Curvature in this plot indicated the existence of 2 classes of binding. One class was at a specific site, probably at carbonic anhydrase. Chromatographic data seemed to support the possibility.     

Aqueous acetic acid as a medium for the facile use of ferroin as redox indicator in the presence of perchloric acid

Ferroin cannot be used as an indicator in perchloric acid medium because of precipitation of ferroin perchlorate. There is no precipitation, however, if the solution contains 30%(v/v) of acetic acid.     

2,7-二溴-4-氨基芴的合成及其光学性质

以芴(1)为原料,通过溴代、硝化、还原反应合成了2,7-二溴-4-氨基芴(4),其结构经1H NMR,13C NMR,IR和ESI-MS确证。分别对溴化、硝化和还原反应条件进行优化。结果表明:在最佳溴化反应条件[CHCl3为溶剂,Cu Br2为催化剂,1 90 mmol,n(1)∶n(Cu Br2)∶n(Br2)=1.0∶0.025∶2.89,于0℃反应24 h]下,溴化产物2,7-二溴芴(2)的产率93.8%;在最佳硝化反应条件[2 30 mmol,混合酸(85%硝酸+96%硫酸)为硝化试剂,n(2)∶n(HNO3)=1.0∶4.6,于70℃反应1 h]下,硝化产物2,7-二溴-4-硝基芴(3)的产率94.7%;在最佳还原反应条件(3 30 mmol,Zn/Ca Cl2为还原剂,回流反应4 h)下,4的产率89.5%。运用UV-Vis和荧光光谱初步研究了4的光学性质。结果表明:4的λmax为352.4 nm;在352.4 nm波长激发下,4的λem位于388.4 nm和412.2 nm,光带隙低至2.66 e V。     

Stereoisomers of 4-amino-3-hydroxy-1-cyclohexanecarboxylic acid and 4-amino-3-oxo-1-cyclohexanecarboxylic acid as mimetics of a twisted cis-amide bond

Stereoselective synthesis of the title compounds was performed. The relative configuration of methyl t-4-(tert-butoxycarbonylamino)-c-3-hydroxy-r-1-cyclohexanecarboxylate and methyl trans-4-(tert-butoxycarbonylamino)-3-oxo-r-1-cyclohexanecarboxylate was confirmed by X-ray diffraction methods. Analogues of cyclolinopeptide A (CLA) containing these twisted cis-amide bond mimetics were then synthesised.     

1-烷基-4-氨基-1,2,4-三唑类含能离子液体的溶解性能

基于NO3-、ClO4-、N(CN)2-、[2,4,5-TNI]^-和[3,5-DNTZ]^-阴离子,以及1-烷基-4-氨基-1,2,4-三唑阳离子合成了系列环境友好型含能离子液体,通过¹H NMR对其进行了结构表征;采用ab initio结合MP2/6-311G++(2d,p)方法计算了1-烷基-4-氨基-1,2,4-三唑类含能离子液体和溶剂之间的分子间作用能以及含能离子液体的偶极距;系统研究了分子结构、极性以及分子间作用能对该系列含能离子液体的溶解性能的影响。 结果表明:当阳离子不同时,[BATZ]NO₃与水的ΔE绝对值最大为40.7 kJ/mol,当阴离子不同时,[BATZ][3,5-DNTZ]与水的ΔE绝对值最大为45.1 kJ/mol;上述含能离子液体的极性大小顺序为[BATZ][3,5-DNTZ]>[BATZ][2,4,5-TNI]>[BATZ]N(CN)₂>[BATZ]ClO₄>[RATZ]NO₃;最后,1-烷基-4-氨基-1,2,4-三唑类含能离子液体的溶解度随着溶剂介电常数ε的减小、取代烷基链长的增加、阴离子体积的增大以及分子间作用能的减小而降低,即含能离子液体在溶剂中的溶解度大小顺序为[BATZ][3,5-DNTZ]>[BATZ][2,4,5-TNI]>[BATZ]NO₃>[BATZ]ClO₄>[BATZ]N(CN)₂>[PATZ]NO₃>[HATZ]NO₃>[DATZ]NO₃,其中,[BATZ][2,4,5-TNI]在水中溶解度最大为10.0327 g/10 g。