阻抑褪色光度法测定水样中阴离子表面活性剂

在弱酸性的HCl-NaOAC缓冲介质中,溴化十六烷基吡啶(CPB)和曙红Y(EY)染料的混合溶液发生褪色,在该褪色的溶液中分别加入十二烷基硫酸钠(SDS)及十二烷基苯磺酸钠(SDBS)等阴离子表面活性剂(AS),溶液颜色发生改变,最大吸收波长都在514 nm处,并分别在548、546 nm处产生明显褪色。在吸收或褪色波长处,阴离子表面活性剂的浓度与增色或褪色程度呈良好线性关系,从而建立测定阴离子表面活性剂的光度法。在最大吸收波长处,SDBS体系、SDS体系中AS的浓度在0~2.06×10-5mol/L、0~2.63×10-5mol/L范围内遵守比尔定律,表观摩尔吸光系数分别为1.30×104、1.01×104L.mol-1.cm-1,检出限分别为8.14×10-7、9.96×10-7mol/L。若用双波长叠加,表观摩尔吸光系数达2.07×104、1.78×104L.mol-1.cm-1,检出限为4.82×10-7、8.34×10-7mol/L。方法具有较高的灵敏度和良好的选择性,用于水样中AS的测定。     

Spectrophotometric determination of micro amounts of nitrite in water and soil

A spectrophotometric method for determination of micro amounts of nitrite in water and soil with p-aminoacetophenone and resorcinol is described. The interference of foreign ions can be eliminated by masking with complexing agents. Beer's law is obeyed up to 20 mug of NO(2)(-) in 60 ml of solution and the molar absorptivity at 435 nm is 5.27 x 10(4) l.mole(-1).cm(-1). The colour is stable for 10 hr. Results obtained by using the proposed method for water and soil samples agree well with those obtained by the Saltzman standard method.     

Spectrophotometric determination of trace copper in water samples with thiomichlersketone

A simple and sensitive spectrophotometric method for determination of trace copper in water samples is proposed. In the presence of pH 4.6 HAc-NaAc buffer solution and surfactant polyethylene octyl phenyl ether (OP) medium, copper reacts with thiomichlersketone (TMK) to form a stable 1:4 complex. The complex Cu(II)-TMK-OP shows maximum absorbance at 500 nm with a molar absorptivity value of 5.7x10(4) l mol-1 cm-1. Beer's law is obeyed for copper concentrations in the range of 0-15 microg/25 ml. The average recovery of copper is between 95.8 and 106%. The method has been applied for determination of trace copper in different water samples with satisfactory results.     

Spectrophotometric determination of beryllium in water samples after micelle-mediated extraction preconcentration

A new micelle-mediated phase preconcentration method for preconcentration of ultra-trace quantities of beryllium as a prior step to its determination by spectrophotometry has been developed. Chrome Azurol S (CAS) and cetyltrimethylammonium bromide (CTAB) were used as chelating agent and cationic surfactant, respectively. The method evaluates and eliminates the blank bias error present in such procedures using mean centering of ratio spectra. This procedure gives more accurate results than the traditional approach using absorbance values against reagent blank. The optimal extraction and reaction conditions were studied and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration and improvement factors) were obtained. Linearity was obeyed in the range of 0.9-18.0 ng mL⁻¹ (1.00 × 10⁻⁷-2.00 × 10⁻⁶ mol L⁻¹) of beryllium. The detection limit of the method is 0.51 ng mL⁻¹ (5.66 × 10⁻⁸ mol L⁻¹) of beryllium. The interference effect of some anions and cations was also tested. The method was applied to the determination of beryllium in spring water samples.     

Spectrophotometric determination of traces of arsenic

Arsenic(III) is extracted into carbon tetrachloride from 3.5M sulphuric acid that is 0.8M in potassium iodide. 8-Mercaptoquinoline and acetone are added to the organic extract and the absorbance of the arsenic(III)-8-mercaptoquinolinate formed is measured at 380 nm. Repeating the extraction procedure highly increases the selectivity of the method; only tin(II) interferes with the determination.     

Spectrophotometric determination of micro amounts of uranium

Uranium(VI) in the presence of numerous cations and anions is determined by the iron(II)-phosphoric acid-Ferrozine method at concentrations of 8-75,mug/25 ml with a relative precision of 3-1%.     

Spectrophotometric determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction

A simple method for the determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction is described. The procedure is based on the extraction of mercury in the form of a complex and its subsequent determination by spectrophotometry. The complex is formed between Hg(II) and 2-(2-benzothiazolylazo)-p-cresol. The detection at 650 nm is performed directly in the metal-rich phase, which is spread on a triacetylcellulose membrane. The method eliminates the need to use a cuvet or large quantities of samples and reagents. The parameters that influence the preconcentration were studied, and the analytical characteristics were determined. The enrichment factor and the consumptive index for this method were 64 and 0.16 mL, respectively. The LOD (3.3 microg/L) and LOQ (11.1 microg/L) were also determined. The accuracy of the method was tested by the determination of mercury in certified reference materials BCR 397 (Human Hair) and SRM 2781 (Domestic Sludge). The method was applied to the determination of mercury in samples of drinking water, sea water, and river water.     

荧光桃红分光光度法测定微量盐酸异丙嗪

在pH 1.85的HCl-NaAc缓冲溶液中,荧光桃红与盐酸异丙嗪依靠静电引力和疏水作用力相互作用形成离子缔合物,其组成比为1∶2,最大褪色波长537 nm,表观摩尔吸光系数ε=4.07×104L.mol-1.cm-1,研究了体系的光谱特征,适宜的反应条件和影响因素,发现体系的吸光度与盐酸异丙嗪的质量浓度在0.04~3.6μg/mL范围内呈良好的线性关系,线性回归方程A=-0.04991-0.1269ρ(μg/mL),线性相关系数r=0.9998,检出限和RSD分别为0.0177μg/mL和2.2%。本法可用于药物制剂中盐酸异丙嗪含量的快速测定。     

刚果红-溴化十六烷基吡啶光度法测定阴离子表面活性剂

日常生活中常用的表面活性剂多数是阴离子洗涤剂.洗涤剂进入水环境后,其分子聚集在水和其它介质的表面,产生泡沫、乳化和微粒悬浮等现象,隔绝水中氧与空气中氧的交换,影响水体净化,导致水质恶化,由此对水体的环境污染问题越来越严重,引起了人们的重视.因此, 准确快速地测定阴离子表面活性剂的含量, 对于研究其在环境中的转化、迁移及对生理过程的影响, 均具有重要意义.     

Spectrophotometric determination of micro amounts of cadmium in waste water with cadion and triton X-100

A spectrophotometric method for determination of micro amounts of cadmium in waste water with Cadion and Triton X-100 is described. The interference of foreign ions can be eliminated by masking with an ascorbic acid-Rochelle salt-potassium cyanide-potassium fluoride mixture. After demasking with formalin, cadmium is determined directly in aqueous solution without separation. Beer's law is obeyed for 0-8 mug of Cd in 25 ml of solution. The method is more sensitive than the dithizone method, its apparent molar absorptivity at 480 nm being 1.19 x 10(5) 1. mole(-1). cm(-1). Results obtained by using the proposed method on waste water samples agree well with those obtained by atomic-absorption spectrophotometry.     

Spectrophotometric determination of phosphorus and arsenic in pharmaceutical organic compounds

Summary A simple and accurate method is described for the microdeter-mination of phosphorus and arsenic in some pharmaceutical organic compounds. It is based on the conversion of phosphorus and arsenic into phosphate and arsenate ions respectively, followed by precipitation with quinoline and sodium molybdate reagents. The excess quinoline in the supernatant is spectrophotometrically measured at 312.5 nm in an ammonium acetate background of pH 5.5. The results obtained with 24 structurally different phosphorus and arsenic compounds show an average recovery of 99% and a mean standard deviation of ±1%. Excipients and diluents normally used in drug formulations do not interfere.

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Spektrophotometrische Bestimmung von Phosphor und Arsen in organischen Arzneimitteln

Zusammenfassung Eine einfache und genaue Methode zur Mikrobestimmung von Phosphor und Arsen in einigen organischen Arzneimitteln wurde angegeben. Sie beruht auf der Umsetzung des Phosphors zu Phosphat und des Arsens zu Arsenat sowie deren Fällung mit Chinolin und Natriummolybdat. Der Chinolinüberschuß wird spektrophotometrisch bei 312,5 nm in Ammonium-acetat bei pH 5,5 gemessen. Die mit 24 strukturell verschiedenen Phosphorbzw. Arsenverbindungen erhaltenen Resultate ergaben eine durchschnittliche Wiederfindungsrate von 99% und eine rel. Standardabweichung von ±1%. Arzneimittelträger und Verdünnungsmittel stören nicht.

     

Spectrophotometric determination of bismuth in water samples after preconcentration of its thiourea-bromide ternary complex on activated carbon

A simple, accurate, sensitive and reliable method for the selective extraction and spectrophotometric determination of Bi(III) was developed. Bi(III) was collected on activated carbon after complexation with thiourea and bromide ion in acidic media. The complex retained on activated carbon was then desorbed with the bromide solution in N,N-dimethylformamide (DMF) and determined spectrophotometrically at 375 nm. The linear calibration ranges and limit of detection for the proposed method was 1.00×10⁻⁹-1.50×10⁻⁷ and 8.00×10⁻¹⁰ mol l⁻¹, respectively. The influence of the interfering cations and anions on the determination of bismuth was investigated. The method was successfully applied to the extraction and determination of bismuth in natural water samples.     

Spectrophotometric determination of nitrate and nitrite in water and some fruit samples using column preconcentration

A sensitive analytical method for the simultaneous assay of nitrate and nitrite in water and some fruit samples is presented. The method is based on nitrite determination using the diazotization-coupling reaction by column preconcentration and on the reduction of nitrate to nitrite using the Cd-Cu reductor column. Nitrite is diazotized with sulfanilamide (SAM) in the pH range 2.0-5.0, sulfamethizole (SM) in pH 1.8-5.6 and sulfadimidine (SD) in pH 1.8-4.0 in a hydrochloric acid medium to form water-soluble colourless diazonium cations. These cations were coupled with sodium 1-naphthol-4-sulfonate (NS) in the pH range 9.0-12.0 for the SAM-NS system, pH 8.6-12.0 for the SM-NS system and pH 9.4-12.0 for the SD-NS system to be retained on naphthalene-tetradecyldimethylbenzylammonium (TDBA)-iodide (I) adsorbent packed in a column. The solid mass is dissolved out from the column with 5 ml of dimethylformamide (DMF) and the absorbance is measured by a spectrophotometer at 543 nm for SAM-NS, 537 nm for SM-NS and 530 nm for SD-NS. The calibration graph was linear over 30-600 ng NO(2)-N and 22-450 ng NO(3)-N in 15 ml of final aqueous solution (i.e. 2-40 ng NO(2)-N ml(-1) and 1.5-30 ng NO(3)-N ml(-1) in aqueous sample) for three systems. The detection limits were 1.4 ng NO(2)-N ml(-1) and 1.1 ng NO(3)-N ml(-1) for SAM-NS, 1.2 ng NO(2)-N ml(-1) and 0.89 ng NO(3)-N ml(-1) for SM-NS, 1.0 ng NO(2)-N ml(-1) and 0.75 ng NO(3)-N ml(-1) for SD-NS, respectively. The concentration factor is eight for SAM-NS and SM-NS, and 12 for SD-NS. Interferences from various foreign ions have been examined and the method was successfully applied to the determination of low levels of nitrate and nitrite in water and some fruit samples.     

Spectrophotometric determination of lead in biological samples with dibromo-p-methyl-methylsulfonazo

A new highly sensitive and selective chromogenic reagent, dibromo-p-methyl-methylsulfonazo (DBM-MSA), was studied for determination of lead. In 0.24 mol l(-1) phosphoric acid medium, which greatly increases the selectivity, lead reacts with DBM-MSA to form a 1:2 blue complex which has a sensitive absorption peak at 642 nm. Under the optimal conditions, Beer's law was obeyed over the range 0-0.6 mug ml(-1) Pb(II). The molar absorptivity and Sandell's sensitivity are 1.02x10(5) l mol(-1) cm(-1) and 0.00203 mug cm(-2), respectively. The limit of quantification, limit of detection and relative standard deviations were found to be 7.30 and 2.21 ng ml(-1) and 1.1%, respectively. It is found that, except for Ca(II) and Ba(II), all foreign ions studied do not interfere with the determination. The interference caused by Ca(II) and Ba(II) can be easily eliminated by prior extraction with potassium iodide-methylisobutylketone. The method has been applied to the determination of lead in some biological samples with satisfactory results.