Dual-wavelength beta-correction spectrophotometric determination of arsenic in wastewater with ethyl violet

Arsenic has been determined by beta-correction spectrophotometry with ethyl violet (EV) in the presence of sodium nitrite which is an oxidant and effective for removing absorption spectra and increasing analytical sensitivity. Extraction with benzene can separate most other metals ions and concentrate arsenic in wastewater. The beta-correction method can eliminate completely the effect of excess EV in its As colored solution to give the real absorbance of the chelate produced. Sensitivity, precision and accuracy are all increased. Beer's law is obeyed over the range 0-2.0 mg l(-1) at 630 nm and the detection limit of arsenic is 0.02 mg l(-1). The results show that the relative standard deviation was less than 12% with the recovery between 91.0 and 114%.     

Improved determination of mercury complex with Thiomicher's ketone by beta-correction spectrophotometry

Determination of the mercury complex formed with Thiomicher's ketone (TMK) was improved by beta-correction spectrophotometry in the presence of a nonionic surfactant at pH 5. The complex formed was Hg(TMK)2, and its true molar absorptivity is reported for the first time: epsilon Hg(TMK)2(560) = 1.04 x 10(5) L/mol.cm. In addition, the stability constant of Hg(TMK)2 was equal to 3.64 x 10(10) at an ion strength of 0.01 at 20 degrees C. Results from analyses of wastewater samples showed that the relative standard deviations were < or = 8.3%, and the recoveries of mercury ranged from 90 to 110%.     

Sources of error in beta-correction spectrophotometry

The paper applies equilibrium analysis to the Gao method. This approach is particularly convenient for evaluation of absorbances involved with complexes formed in the system tested.     

溴酸钾氧化孔雀石绿和甲基橙褪色光度法测定水中亚硝酸根

在H3PO4介质中,利用痕量NO2-催化KBrO3氧化孔雀石绿和甲基橙褪色的反应,建立了双波长双指示剂催化动力学光度法测定痕量NO2-的新方法。该反应在最大吸收峰505nm和615nm处,催化和非催化体系吸光度的变化与NO2-浓度呈线性关系,线性范围为0.01～0.80μg/mL,检出限为1.3×10-3μg/mL,该方法用于环境水样(自来水、雨水、延安卷烟厂废水)中痕量NO2-的测定,加标回收率为97%～110.2%.     

Simultaneous determination of antimony and bismuth by beta-correction spectrophotometry and an artificial neural network algorithm

Simultaneous determinations of antimony and bismuth were done by β-correction spectrophotometry and a feed forward neural network algorithm with back propagation of error. The sensitivity was improved using β-correction spectrophotometry. The determination of trace amounts of mixtures of Sb and Bi in various matrices (river, tap and industrial wastewater) were investigated by neural network and β-correction spectrophotometry using the complexes formed between pyrogallol red, Sb and Bi. The results showed that measurement is possible in the ranges of 0.05-5.0 and 0.2-3.2 μg ml⁻¹ for Sb(III) and Bi(III), respectively. The results also show very good agreement between true and predicted concentration values and have the ability to use in routine analysis.     

Dual-wavelength spectrophotometric determination of cadmium with cadion

Cadmium has been determined by dual-wavelength spectrophotometry with cadion, p-nitrobenzenediazoaminobenzene-p-azobenzene, and a non-ionic surfactant, Triton X-100. Cadion and its cadmium chelate are dissolved in a micellar solution of the surfactant. The absorbance difference at the wavelength of maximum absorption of the cadmium chelate (477 nm) and that of cadion (566 nm) is measured. A combination of triethanolamine, iminodiacetate and citrate is very effective for masking other ions. Cadmium in zinc metal can be determined without prior separation.     

双波长双指示剂催化光度法测定铜的研究

研究了在pH 4.0的HAc～NaAc缓冲介质中,利用痕量铜(Ⅱ)催化过氧化氢氧化罗丹明B和亚甲基蓝褪色的指示反应,通过测量540 nm和660 nm下,催化体系和非催化体系吸光度的变化,建立了双波长双指示剂催化动力学光度法测定痕量铜的新方法.方法的线性范围为0.00080～0.048μg/mL,检出限为4.0×10~(-11) g/mL.方法可用于水中铜的测定.     

A green analytical procedure for sensitive and selective determination of iron in water samples by flow-injection solid-phase spectrophotometry

A greener analytical procedure based on flow-injection solid-phase spectrophotometry is proposed for iron determination. Iron(II) is reversibly retained on 1-(2-thiazolylazo)-2-naphthol immobilized on C18-bonded silica, yielding a brown complex. The metal ion is eluted as iron(II) with a small volume of a diluted acid solution without removing the immobilized reagent, which can be used for at least 100 determinations. Other chemicals (buffer and reducing agent) were carefully selected taking into account the analytical performance and toxicity. The developed procedure is 10-fold more sensitive in comparison to the analogous procedure based on measurements in solution, being suitable for the determination of iron in water samples with good accuracy and precision. The detection limit (99.7% confidence level), sampling rate and coefficient of variation (n = 10) were estimated as 15 μg L⁻¹, 25 measurements per hour and 4.0%, respectively. The proposed procedure involves a reduced effluent generation (3.6 mL per determination) and consumes micro amounts of reagents.     

流动注射催化光度法测定NO2-的研究

以流动注射分光光度法,基于NO-2在酸性条件中对溴酸钾氧化胭脂红酸有催化作用这一原理测定NO-2。对实验条件进行了优化。实验结果表明,室温下,当cKBrO3=0.14mol L,c胭脂红酸=3.5×10-4mol L,cH2SO4=1.2mol L时,方法的线性范围为0.005～0.3μg mL,检出限为0.002μg mL。利用该方法对几种河水水样进行了测定。     

阻抑动力学光度法测定痕量铅

在氨水介质中, 痕量Cu(Ⅱ)对H2O2 氧化茜素红S的褪色反应具有催化作用, 而Pb(Ⅱ)对此褪色反应具有明显的阻抑作用, 由此建立了测定痕量Pb(Ⅱ)的新催化动力学光度法. 应用正交试验法确定了反应的最佳条件, 测定了有关动力学参数. 方法的检出限为7.5 ng/mL, 线性范围为0.0～0.35 μg/mL, 并应用于皮蛋和茶叶样品中Pb(Ⅱ)含量的测定, 同时还探讨了阻抑反应机理.     

双波长双指示剂-催化动力学光度法测定奶粉中的锌

研究发现在HCl介质中,痕量锌对H2O2氧化甲基紫和亚甲基蓝褪色具有强烈的催化作用,通过测量580 nm和668 nm处催化反应体系和非催化反应体系吸光度的变化,建立了双波长双指示剂催化动力学光度法测定痕量锌的新方法。在最佳实验条件下,线性范围为1.5~60μg/L,线性方程为ΔA=0.0169ρZn2+(μg/mL)+0.0019,r=0.9982,方法检出限为0.84μg/L。该方法可用于奶粉痕量锌的测定。     

Dual-wavelength spectrophotometry: Part VI. Qualitative and quantitative analysis by means of first-derivative spectra

Derivative spectrophotometry has many important applications, e.g. detecting trace chemicals in mixture and analyzing isomers or turbid samples, but such measurements have been difficult instrumentally. The first-derivative spectrum can be recorded easily by using dual-wavelength measurements, if the two wavelengths λ₃ and λ₂ are set very close to each other (usually 1–2 nm apart) and scanned simultaneously. Practical applications of derivative spectra in the analysis of rare earths and phenol mixtures are described.     

Indirect determination of arsenic by flotation spectrophotometry

An indirect method of arsenic determination in the submicrogram range via the determination of molybdenum is presented here. High sensitivity is achieved by combination of the chemical amplification during formation of dodecamolybdoarsenic acid (arsenic: molybdenum ratio 1 12) with multiplication due to the formation of ion-association complexes during flotation-spectrophotometric molybdenum determination with crystal violet (molar ratio 1 2). Thus, the amplification factor relating to arsenic is 24.Dodecamolybdoarsenic acid is formed in a weakly acidic medium and is quantitatively extracted byn-butanol. Back extraction of the heteropoly acid to the aqueous phase and its simultaneous destruction provides the basis for the reaction of released molybdate ions with thiocyanate ions. The molybdenum-thiocyanate complex forms a sparingly soluble ion-association complex with crystal violet which can be floated with toluene on the phase boundary (film flotation). After separation of the aqueous phase the floated molybdenum compound is dissolved in acetone and the resulting free crystal violet ions are subjected to photometric determination at 590 nm as equivalent of the concentration of arsenic. The molar absorptivity of crystal violet is 3.2 · 10⁵1 · mol^–1 · cm^–1. Beer's law is obeyed in a concentration range from 0.01 to 1 g Mo · ml^–1 (0.001–0.1 g As · ml^–1). The resulting detection limit for arsenic is 1 ng · ml^–1.     

Indirect determination of iodate by atomic-absorption spectrophotometry

An indirect method for determination of trace iodate in certain high-purity chemicals by atomic-absorption spectrophotometry (AAS) is described. Iodate forms a stable ion-association complex [Hg(dipy)(2)](IO(3))(2) in neutral medium, which can be extracted into methyl isobutyl ketone with 99% efficiency. The extract can be analysed for mercury (and hence indirectly for iodate) by flameless AAS. The limit of detection for iodate by this method is 7.5 ng. Apparent recoveries of 92-112% have been obtained for spikes of 0.25-0.70 mug of iodate.     

A sensitive determination of paraquat by spectrophotometry

A sensitive spectrophotometric method for the determination of a widely used herbicide, paraquat using a versatile reducing agent sodium borohydride is described. Paraquat is reduced with sodium borohydride in an alkaline medium to give a blue radical ion with an absorbance maxima at 600 nm. Beer's law is obeyed in the range of 0.05-0.5 mug ml(-1) of paraquat. The molar absorptivity and Sandell's sensitivity are found to be 2.9 x 10(5) l mol(-1) cm(-1) and 0.0006 mug cm(-2) respectively. The important analytical parameters and the optimum reaction conditions were evaluated. The method is free from the interference of other commonly used pesticides and metal ions. The method was applied successfully to the determination of paraquat in human samples, such as blood, urine and mother's milk compared to food and environmental samples.     

分光光度法定量测定柠檬酸及其盐的含量

酸性介质中,柠檬酸(或盐)与Fe3+形成的黄色络合物在光照条件下发生光致变色现象,生成紫红色络合物,采用分光光度法可定量测定柠檬酸及其盐的含量.在冰水浴中,日光照射20 min,阴凉处静置30 min,检测波长为490nm.线性范围为(0～300)mg/L,相对标准偏差(RSD)为0.46％(n=6),检测限为3.46...     

催化褪色光度法测定粉煤灰中痕量钼

在pH11.0的Na2CO3 NaHCO3缓冲溶液中,痕量钼(Ⅵ)对H2O2氧化偶氮胭脂红B的褪色反应具有强烈的催化作用,据此建立了一种测定痕量钼(Ⅵ)的催化光度法的新方法。方法的检出限为2.04×10-2μg/L,线性范围为0～6.0μg/L,该法已应用于粉煤灰中痕量钼的测定。     

荧光光谱法测定氨基酸的新方法

在醋酸 醋酸钠缓冲介质中 ,氨基酸能猝灭壳聚糖 茚三酮体系的荧光。基于此 ,建立了一种新的荧光光谱测定氨基酸的方法 ,探讨了其反应机理及测定条件。方法的线性范围为 0mol·L- 1 ～ 1 2× 1 0 - 4 mol·L- 1 ,已应用于测定果汁饮料