Reduction of Sulfur Dioxide to Sulfur Monoxide by Ferrous Porphyrin**

The reduction of SO₂ to fixed forms of sulfur can address the growing concerns regarding its detrimental effect on health and the environment as well as enable its valorization into valuable chemicals. The naturally occurring heme enzyme sulfite reductase (SiR) is known to reduce SO₂ to H₂S and is an integral part of the global sulfur cycle. However, its action has not yet been mimicked in artificial systems outside of the protein matrix even after several decades of structural elucidation of the enzyme. While the coordination of SO₂ to transition metals is documented, its reduction using molecular catalysts has remained elusive. Herein reduction of SO₂ by iron(II) tetraphenylporphyrin is demonstrated. A combination of spectroscopic data backed up by theoretical calculations indicate that Fe^IITPP reduces SO₂ by 2e⁻/2H⁺ to form an intermediate [Fe^III−SO]⁺ species, also proposed for SiR, which releases SO. The SO obtained from the chemical reduction of SO₂ could be evidenced in the form of a cheletropic adduct of butadiene resulting in an organic sulfoxide.     

Decoloring Spectrophotometric Method for the Determination of Sulfur Dioxide

The discharge of sulfur dioxide (SO₂) is one of the most important reasons of resulting in the environmental pollution. Current method for determination SO₂ is fuchsine-formaldehyde spectrophotometry. This paper describes a decoloring spectrophotometry, which is based on azo dye being reduced in the presence of manganese (Ⅱ) as inducer and in weak acidic medium. It is shown that the result has better selectivity and higher sensitivity. This method was used to measure the content of SO₂ in the air of northern china with satisfactory results.     

New Spectrophotometric Method for the Determination of Titanium in Soil and Standard Geochemical Samples

Abstract

In the present communication a simple and rapid spectrophotometric method for the determination of titanium is described. The method is based on the reaction of Ti(IV) with a newly synthesized reagent, 6-(4-nitrophenylazo)-3,4,5-trihydroxy benzoic acid (NATHB), in ethanol medium at pH 3.2 to 4.2. The complex exhibits an absorption maximum at 495 nm and Beer's law is valid over the range of 0.04 – 1.00 μg.ml^?1 Ti. The molar absorptivity is 3.48 × 10⁴ dm³.mole^?1. cm^?1. Most of the foreign metal ions and anions do not produce any colorations with NATHB at selected conditions. Based on these results, a simple and direct spectrophotometric method with high selectivity and sensitivity was proposed. The method has been successfully applied for the determination of titanium in 5 soil and 3 standard geochemical samples.     

一种用于食品中二氧化硫快速测定的样品前处理方法

提出了一种采用半微量蒸馏-半导体制冷技术的食品中二氧化硫快速提取的新方法, 研制出了可在15 min内完成二氧化硫提取的食品检测快速蒸馏提取装置. 采用本装置,  无需冷凝水和含汞吸收剂即可实现对样品中二氧化硫的蒸馏提取. 考察了蒸馏液酸度、   蒸馏液体积、 馏分收集体积和蒸馏提取时间对二氧化硫提取效率的影响. 研究结果表明,  采用该方法在30 min内即可完成对食品中二氧化硫的快速定量测定.     

Spectrophotometric Determination of Hydrazine

Abstract

A simple sensitive and selective method is described for the determination of trace amounts of hydrazine. The method is based on the reduction of nitrate to nitrite. Hydrazine in ammoniacal condition is used as reducing agent with copper(II) as catalyst. The nitrite prepared is determined based on the diazo coupling reaction between p‐nitroaniline and N‐(1‐naphthyl)ethylenediammine dihydrochloride(NEDA). The method obeys Beer's law in the concentration range of 0–15 µg of hydrazine in a sample volume of 10 ml at 545 nm and the colour is stable for 3 h. The molar absorptivity is calculated to be 3.83×10⁴ l/mol/cm with a correlation coefficient of 0.999. The relative standard deviation is 1.8% (n=10) at 12 µg of hydrazine. Interferences due to foreign ions have been studied and the method has been applied for the determination of hydrazine in boiler feed water.     

褪色分光光度法间接测定草甘膦

在ｐＨ＝５．６的醋酸－醋酸钠冲溶液中，草甘膦与微量过量的溴反应，剩余的溴能使罗丹明Ｂ褪色，以此建立了一种分光光度法测定甘甘膦的新方法，在最佳条件下，草甘膦浓度与吸光度呈良好的线性关系，当加入溴的浓度分别为１．４４×１０＾－５ｍｏｌ／Ｌ和２．７２×１０＾－５ｍｏｌ／Ｌ时，测定范围分别为０～０．５ｍｇ／Ｌ和０．４～０．９ｍｇ／Ｌ，干扰试验表明Ｆｅ＾２＋，Ｆｅ＾３＋和三乙胺有严重干扰，但可被阳离子交换权     

褪色光度法测定SO_3~(2-)的研究

本文研究了ＳＯ２－３褪色碱蓝６Ｂ的反应，在ｐＨ５．２ＨＡｃ－ＮａＡｃ缓冲介质中，ＳＯ２－３浓度在０．３９～１２ｍｇ／Ｌ范围内符合比尔定律，仅Ｆｅ３＋、Ｎｉ２＋、Ｃｒ３＋干扰测定，用于食品中ＳＯ２－３的测定，结果令人满意。     

A Systematic Approach for the Evaluation of Triethanolamine as a Possible Sulfur Dioxide Sorption Detector Coating

Abstract

A change in the vibrating frequency of a quartz crystal can be an accurate measurement of the mass change on the surface of the crystal. When coated with an absorbing compound, the subsequent frequency change indicates the sorption of a chemical species by the coating. An approach is proposed for evaluating potential crystal coatings and is. applied to the evaluation of Triethanolamine as a possible sulfur dioxide sorption detector coating.     

Indirect Catalytic Spectrophotometric Determination of Metamizol Following Oxidation by Lead Dioxide Immobilized in A Polyester Resin Bed

Abstract

A spectrophotometric-indirect procedure for the determination of metamizol is described. The method is based on the reaction of the drug in a solid-phase (lead dioxide immobilized in a polyester resin bed) in acidic media (perchloric acid 0.01 M as carrier). The lead dioxide reactor provides simultaneously an effective oxidation of the drug and a controlled liberation of Pb(II) which acts as catalyst on the reaction pyrogallol red-potassium persulphate; the oxidation of the red pyrogallol results in a less coloured solution. The decreased red colour (negative FIA peaks) is monitored at 520 nm. The calibration graph is linear in the interval 2–16 ppm in metamizol. The relative standard deviation for the determination of 10.4 ppm of metamizol is 2.9% (n=23) and the sample throughput is 72 h^?1.     

Detection of Sulfur Dioxide Using a Piezoelectric Quartz Crystal Microbalance

Abstract

Sulfur dioxide was detected and determined in air by a piezoelectric quartz crystal sensor coated with 4-aminoantipyrine 1-hydroxyetil-2-heptadecenyl imidazol (amine 220) solution (1:1 v/v in chloroform). The analytical response curve is linear over the concentration range from 0.70 to 5.0 ppm of SO₂. Good linearities (r = 0.9990, 0.9995 and 0.9968) and sensitivities (18.0, 33.4 and 50.7 Hz/ppm) were found, respectively for exposure times of 30, 60 and 90 seconds. The sensor can be used for more than six months without loss in sensitivity and presented good reversibility and reproducibility. Among some possible interferents tested, only nitrogen dioxide and moisture caused major frequency changes.     

2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚-BrO_3~--SCN-三元离子缔合物测定微量BrO_3~-的研究

本文研究了5-Br-PADAP在酸性介质中质子化,与BrO_3~-和SCN~-形成三元离子缔合物的最佳条件,其表观摩尔吸光系数ε_(540)=4.3×10~4L·mol~(-1)·cm~(-1),缔合物组成比为:5-Br-PADAP:BrO_(3-)SCN~-=1:1·1。提供了测定微量BrO_(3-)的新方法,可应用于化学试剂中微量BrO~(3-)的测定。此外,本文还探讨了反应机理。     

Spectrophotometric Determination of Sulphathiazole

Abstract

A new, rapid, simple, selective and sensitive method for the spectrophotometric determination of sulphathiazole is described. The drug forms a yellow coloured complex with Pd(II) in alkaline medium (1 M NaOH). The drug complex exhibits maximum absorbance at 410 nm, with a molar absorptivity of 1.9 × 10³ 1 mol^?1 cm^?1. Effects of molarity of NaOH, reagent concentration on the proper complex formation are discussed. The system obeys Beer's law in the concentration range of 10-160 ppm of sulphathiazole.     

新显色剂2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸光度法测定钒的研究

研究了新显色剂 2 -( 5-羧基 -1 ,3 ,4-三氮唑偶氮 ) -5-二乙氨基苯甲酸 ( CTZD-BA)与钒的显色反应的条件。在 p H 3 .0的 HAc-Na Ac介质中 ,CTZDBA与 V( )形成稳定的摩尔比为 2∶ 1的紫红色络合物 ,最大吸收波长在 583 nm处 ,表观摩尔吸光系数为 4.0 6× 1 0 4 L·mol- 1·cm- 1,V( )在 0～ 0 .8mg/L范围内遵守比耳定律。方法可不经分离直接测定铝合金样品中的钒 ,结果满意     

Spectrophotometric Determination of Piroxicam via Chelation with Fe(III) in Commercial Dosage Forms

The objective of this work is to develop and validate spectrophotometric method for the determination of piroxicam in commercial dosage forms. The method is based on the chelation of the drug with Fe(III) to form pink coloured metal chelate at room temperature which absorbs maximally at 504 nm. Beer's law is obeyed over the concentration range of 8–160 μg mL^?1 (A = 1.07 × 10^?3 + 7.75 × 10^?3 C). Under the optimized experimental conditions, proposed method is validated as per the International Conference on Harmonisation guidelines. The limits of detection and quantitation for the proposed method are 0.775 and 2.348 μg mL^?1, respectively. The proposed method has been successfully applied to the determination of piroxicam in commercial dosage forms. The results are compared with the reference El‐Ries et al. spectrophotometric method.     

卟啉试剂光度法间接测定硫离子的研究（1）

本文以ＴＰＰＳ４、Ｔ（４－ＭＯＰ）ＰＳ４和Ｔ（４－ＭＰ）ＰＳ４为例，研究了Ａｇ·ｐｈｅｎ·ＰＰ光度法间接测定废水中痕量硫离子的有关条件。同时用上述三种卟啉试剂试验了Ｃｕ￣（２＋）、Ｈｇ￣（２＋）、Ｃｄ￣（２＋）、Ｐｂ￣（２＋）等软酸和交界酸间接测定Ｓ￣（２－）的可能性，结果表明，Ｈｇ－ＰＰ也可用于间接测定Ｓ（２－）。最后，对Ｈ＿２Ｓ的吸收液进行了筛选。     

在阳离子表面活性剂存在下锇与对硝基苯基荧光酮显色反应的研究

本文研究了在CTMAB存在下锇的分光光度测定新方法。络合物最大吸收峰位于570nm,摩尔吸光系数ε_(570)=1.0×10~5L·mol~(-1)·cm~(-1)。反应的pH为7.2～7.8。锇含量在0～7.0μg/10mL范围内服从比尔定律。锇在络合物中与p-NPF的摩尔比有1:1、1:2两种。采用蒸馏法锇能与所有金属离子分离,使该测定锇的方法具有专一性。用于人工合成样及矿样的分析结果满意。对显色反应机理进行了初步探讨。     

显色剂2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸与钯(Ⅱ)的显色反应研究

研究了显色剂2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸(CTZDBA)与钯(Ⅱ)的显色反应。结果表明,Pd(Ⅱ)与CTZDBA生成稳定的1∶2的紫红色配合物,其最大吸收波长为548 nm,配合物的表观摩尔吸光系数为9.32×104L.mol-1.cm-1,Pd(Ⅱ)质量浓度在0.08~0.8 mg/L范围内符合比耳定律。该方法可不经分离直接测定钯碳催化剂和钯纳米碳催化剂中的微量钯,测定结果与原子吸收法(AAS)基本相符。     

常见饮料中痕量铝的分光光度法研究

新试剂5-溴水杨基荧光酮可在pH5.5～6.8的六次甲基四胺缓冲溶液中,与铝,溴化十六烷基吡啶形成稳定的红色三元配合物。最大吸收波长约为568nm,摩尔吸光系数高达1.7×10~5L mol~(-1)·cm~1,常见金属离子很少干扰。据此,建立了测定微量铝的方法。其线性范围为0～6μg/25ml回收率在96％～103％之间。本文测定了常见饮茶,饮料及饮水中的微量铝。