Dibenzazepin hydrochloride as a new spectrophotometric reagent for determination of hydrogen peroxide in plant extracts

A rapid, simple, accurate, and sensitive visible spectrophotometric method for the determination of trace amounts of hydrogen peroxide in acidic buffer medium is reported. The proposed method is based on the oxidative coupling of Ampyrone with dibenzazepin hydrochloride by hydrogen peroxide in the buffer medium of pH?4.0 which is catalyzed by ferrous iron. The blue-colored product formed with maximum absorption at 620?nm was found to be stable for 2?h. Beer's law is obeyed for hydrogen peroxide concentration in the range of 0.03-0.42?μg?ml(-1). The optimum reaction conditions and other important optical parameters are reported. The molar absorptive and Sandell's sensitivity are found to be 5.89?×?10(4)?mol(-1)?cm(-1) and 0.57?g/cm(2), respectively. The interference due to diverse ions and complexing agents was studied. The method is successfully applied to the determination of hydrogen peroxide in green plants satisfactorily.     

Evolution of water chemistry in natural acidic environments in Yangmingshan,Taiwan

In Yangmingshan National Park, located in the northern part of the Taiwan Island, there is a very rare area where fish (Channa asiatica) live in spite of acid environments. The origin of the acid in local acid ponds and rivers and the evolution of the water chemistry are discussed on the basis of sulfur stable isotope ratios and chemical equilibria. One of the sources of the acid is sulfuric acid, which is derived from the oxidation of hydrogen sulfide in volcanic gas gushing out from fumaroles around the area and from acid deposition supplied from Taipei City. It is also derived from the oxidation of pyrite: the sulfur stable isotope ratios of delta 34S of +1@1000 to +4@1000 (relative to CDT) of sulfate in acid pond waters (pH 3-4) could be related to those of hydrogen sulfide in volcanic gas, pyrite in local pond sediments and soils, and sulfate in rain water. One acid source is sulfuric and hydrochloric acids arising in springs from geothermal activity: the delta 34S values were characterised by +13@1000 to +17@1000 sulfate-S, which was provided by a disproportionation reaction of sulfur dioxide in the depths. Another acid source could be the oxidation of iron(II). Under acidic conditions, the water-rock reaction gives rise to high concentrations of aluminium and iron. While flowing down surface streams, iron(II) is oxidised to iron(III) and then hydrolysed to cause further acidification under oxic conditions. The concentrations of iron and aluminium are controlled by redox and dissolution equilibria.     

硫酸雾测试方法若干问题思考

简述了我国硫酸雾测试方法的发展历史,分析和总结了《固定污染源废气硫酸雾的测定离子色谱法》(HJ 544—2016)存在的一些争议和问题,包括硫酸雾的定义、测试方法的干扰控制等。分析认为,相比《硫酸工业污染物排放标准》(GB 26132—2010),HJ 544—2016对硫酸雾的定义更加合理。实验结果表明:硫酸盐是测试方法条件下的目标物,滤筒可以显著地捕捉硫酸盐。9组样品滤筒中,被测目标物所占比例为7.9%~69.1%;滤筒和前吸收液中,被测目标物所占比例为93.7%~97.8%。HJ 544—2016新增加的两级串联碱液吸收瓶可以较完全地捕集穿透滤筒后的硫酸雾,同时也会捕集SO2。SO2会对硫酸雾测试产生正干扰,约42.9%的SO2在被吸收后转化为硫酸雾。     

Workplace monitoring of hydrogen peroxide using titanyl-coated sorbents

The current methods of sampling hydrogen peroxide, based on bubbling in acid solutions (titanium tetrachloride or titanium oxysulfate), are unsuitable for personal sampling. An alternative medium has been developed: silica gel coated with titanium oxysulfate. Sample tubes of this new sampling medium are suitable for personal sampling. The sampling performance is the same as that of the methods based on bubbling, but the tubes must be desorbed as soon as possible, even if the spectrophotometric analysis can be postponed. Special emphasis has been placed on the possible interference by peracetic acid, which is currently used in conjunction with hydrogen peroxide in the food industry.     

Optimization of pulp mill effluent treatment with catalytic adsorbent using orthogonal second-order (Box-Behnken) experimental design

Novel catalytic adsorbent (ruthenium on carbon) was employed for the treatment of pulp mill effluent in the presence of hydrogen peroxide. Mathematical model and optimization of the process regarding the most favorable COD (%), TOC (%) and color (%) removal rates was developed and performed with experimental design taking into account catalytic adsorption process kinetics. As the initial experimental design, 3(3-1) half-fractional factorial design (H-FFD) was accomplished at two levels to study the significance of the main effects, such as catalytic adsorbent (g l(-1)) and hydrogen peroxide (ppm) concentrations using the response surface methodology (RSM). Finally, a four factor-three coded level central composite design (CCD) with 28 runs was performed in order to fit a second-order polynomial model. Validation of the model was accomplished by different criteria including coefficient of determination and the corresponding analysis of variance. The achieved removal rates for TOC (up to 75%), COD (up to 73%) and color (up to 68%) were observed for the defined optimal conditions: 1g l(-1) of ruthenium on carbon, 7 ppm of hydrogen peroxide, pH = 4 and ambient temperature. The proposed method benefited significantly improved TOC, COD and color removal efficiency, regenerability and reusability of the catalytic adsorbent and unaltered initial pH of an effluent in comparison to traditional adsorption or oxidation processes.     

Determination of antimony in human blood with inductively coupled plasma-mass spectrometry

A method is presented for the determination of antimony in whole human blood samples with an ICP-MS instrument using a quadrupole mass analyzer. A nitric acid/hydrogen peroxide open digestion procedure was employed for the blood sample treatment and preparation for analysis. The precision and accuracy of the method were evaluated by analyzing several Seronorm trace elements whole blood reference materials. The precision of the method at various antimony levels was better than 4% RSD and the recovery was greater than 92% at all levels. The detection limit, calculated as three times the standard deviation of the blank (3sigma, n= 12), was 0.03 microg L(-1). The method was successfully applied for the determination of antimony in blood samples from school children in rural areas of Kwazulu/Natal, South Africa and adults from Dearborn, Michigan. Blood antimony levels ranged from <0.03 to 3.82 microg L(-1) in children and 1.40 to 4.35 microg L(-1) for adults.     

Sulfuric acid at workplaces--applicability of the new Indicative Occupational Exposure Limit Value (IOELV) to thoracic particles

Until 2009, the limit values for airborne sulfuric acid in Europe were based on the inhalable particle fraction (e.g. MAK (Maximum allowed concentration at workplace) value 0.1 mg m(-3) as the inhalable fraction). With the publication of the Commission Directive 2009/161/EU, an Indicative Occupational Exposure Limit Value (IOELV) of 0.05 mg m(-3) for sulfuric acid aerosols was based for the first time on the thoracic particle fraction. To permit a comparison of the measured values for the inhalable fraction with those of the thoracic fraction and to quantify the thoracic fraction, a cyclone was fabricated out of sulfuric-acid-resistant stainless steel that achieves suitable collection characteristics (PM(10)) at a flow rate of 5.34 L min(-1). 49 measurements were carried out in parallel in 21 companies. At concentrations well below the IOELV, there is little difference between the thoracic and inhalable particle concentrations. At higher concentrations (>0.1 mg m(-3) inhalable aerosol), larger droplets have a marked effect on the measured values and the thoracic fraction accounts for only 32.1 ± 12.5% of the inhalable fraction. The EU's IOELV and the proposal of the MAK Commission therefore provide a comparable level of protection. In the transposition of the IOELV into national law, an air limit of 0.1 mg m(-3) could therefore be implemented for the inhalable fraction.     

Development of a field method for measuring manganese in welding fume

Workers who perform routine welding tasks are potentially exposed to fume that may contain manganese. Manganese may cause respiratory problems and is implicated in causing the occurrence of Parkinson-like symptoms. In this study, a field colorimetric method for extracting and measuring manganese in welding fume was developed. The method uses ultrasonic extraction with an acidic hydrogen peroxide solution to extract welding fume collected on polyvinyl chloride filters. Commercially available pre-packaged reagents are used to produce a colored solution, created by a reaction of manganese(ii) with 1-(2-pyridylazo)-2-naphthol. Absorbance measurements are then made using a portable spectrophotometer. The method detection limit and limit of quantification (LOQ) were 5.2 microg filter(-1) and 17 microg filter(-1), respectively, with a dynamic range up to 400 microg filter(-1). When the results are above the LOQ for the colorimetric method, the manganese masses are equivalent to those measured by the International Organization for Standardization Method 15202-2, which employs a strong acid digestion and analysis using inductively coupled plasma-optical emission spectrometry.     

垃圾渗滤液中微塑料分析的消解方法评价

微塑料(MPs)是近年来国内外关注度极高的新兴污染物,建立实际环境样品中MPs的分析方法是开展相关研究的基础.对于复杂污水样品而言,样品的消解过程至关重要,将极大地影响MPs的准确分析.选择垃圾渗滤液为典型复杂污水样品,采用样品浊度和色度变化、残余悬浮固体量、MPs在颗粒物中的占比为评价指标,对盐酸消解、30％过氧化氢...     

Appropriate Preservation of Dairy Wastewater Samples for Environmental Analysis

Thousands of gallons of water are used in dairies to wash cows before milking and for cleaning equipment. The wastewater generated contains elevated levels of organic matter and pollutants, including nitrogen that once converted, may contaminate groundwater with nitrate. This study was conducted to determine the amount of sulfuric acid needed to preserve wastewater samples from a New Mexico dairy in the southwestern U.S. Titrations of wastewater from a local dairy using full strength (18 M) sulfuric acid were performed to determine the amount of acid needed to bring the pH of the sample to below two, the recommended pH for sample preservation. An average of 0.33 mL of acid was required for every 100 mL of wastewater. Due to sample variability, we recommend that 0.4 mL sulfuric acid be added for every 100 mL dairy wastewater sample to ensure adequate acidification. This quantity is twice the amount currently recommended in U.S. Environmental Protection Agency guidelines.     

A rapid and sensitive analytical method for the quantification of residues of endosulfan in blood

A new sensitive analytical procedure has been developed for the determination of residues of endosulfan in human blood samples. The method involves the extraction of residues of endosulfan from blood samples by the addition of 60% sulfuric acid at 10 degrees C, liquid/liquid partitioning by using hexane and acetone mixture (9:1) and quantification by using GC-ECD. Residues of endosulfan in blood samples were quantified as the sum of alpha-endosulfan, beta-endosulfan, endosulfan sulfate and endosulfandiol. The influence of temperature during the extraction has been studied. Recovery experiments were conducted over the concentration range 1.0-50 ng ml(-1) and the relative standard deviation calculated. The method was found to be sufficiently sensitive to quantify the residue of total endosulfan up to the 1.0 ng ml(-1) level. The recovery was 92% with a calculated relative standard deviation of 1.96%. Conversion of endosulfan to endosulfandiol is found to be less than 0.5% under the defined conditions. The method was applied to the analysis of residue contents of endosulfan and its metabolites in blood samples collected from the exposed population. The data obtained has been confirmed by GC-MS-EI in selective ion monitoring (SIM) mode.     

Optimizing the removal of carbon phases in soils and sediments for sequential chemical extractions by coulometry

We have developed a coulometric technique to optimize the removal of the carbonate and organic fractions for sequential chemical extractions of soils and sediments. The coulometric system facilitates optimizing these two fractions by direct real-time measurement of carbon dioxide (CO2) evolved during the removal of these two fractions. Further analyses by ICP-MS and alpha-spectrometry aided in interpreting the results of coulometry experiments. The effects of time, temperature, ionic strength and pH were investigated. The sensitivity of the coulometric reaction vessel/detection system was sufficient even at very low total carbon content (< 0.1 mol kg-1). The efficiency of the system is estimated to be 96% with a standard deviation of 8%. Experiments were carried out using NIST Standard Reference Materials 4357 Ocean Sediment (OS), 2704 Buffalo River Sediment (BRS), and pure calcium carbonate. Carbonate minerals were dissolved selectively using an ammonium acetate-acetic acid buffer. Organic matter was then oxidized to CO2 using hydrogen peroxide (H2O2) in nitric acid. The carbonate fraction was completely dissolved within 120 min under all conditions examined (literature suggests up to 8 h). For the OS standard, the oxidation of organic matter self-perpetuates between 45 and 50 degrees C, a factor of two less than commonly suggested, while organic carbon in the BRS standard required 80 degrees C for the reaction to proceed to completion. For complete oxidation of organic matter, we find that at least three additions of H2O2 are required (popular methods suggest one or two).     

New kinetic-spectrophotometric method for monitoring the concentration of iodine in river and city water samples

A new kinetic method has been developed for the determination of iodine in water samples. The method is based on the catalytic effect of I^? with the oxidation of Indigo Carmine (IC) by KBrO₃ in the sulfuric acid medium. The optimum conditions obtained are 0.16 M sulfuric acid, 1?×?10^?3 M of IC, 1?×?10^?2 M KBrO₃, reaction temperature of 35°C, and reaction time of 80 s at 612 nm. Under the optimized conditions, the method allowed the quantification of I^? in a range of 12–375 ng/mL with a detection limit of 0.46 ng/mL. The method was applied to the determination of iodine in river and city water samples with the satisfactorily results.     

溴酸钾—酸性铬蓝K体系催化分光光度法测定水样中痕量NO -2

介绍了一种在稀硫酸介质中,应用NO2^-对溴酸钾-酸性铬蓝K褪色反应的催化作用,测定环境水样中痕量NO2^-的方法。方法检测限为0.0028mg/L,相对标准差（n=6)小于2.6%,加标回收率在91%-105%之间。     

A new catalytic-spectrophotometric method for quantification of trace amounts of nitrite in fruit juice samples

A new kinetic method has been developed for the determination of nitrite in fruit juice samples. The method is based on the catalytic effect of nitrite with the oxidation of Nile Blue A (NBA) by KBrO₃ in the sulfuric acid medium. The optimum conditions obtained are 1.2 mM sulfuric acid, 0.034 mM of NBA, 2.8?×?10^?3 M KBrO₃, reaction temperature of 20 °C, and reaction time of 100 s at 595.5 nm. Under the optimized conditions, the method allowed the quantification of nitrite in a range of 0.2–800 μg/mL with a detection limit of 0.02 μg/mL. The method was applied to the determination of nitrite in 15 brands of fruit juice samples.     

底质样品微波消解总磷测定研究

使用硫酸_高氯酸在微波消解系统消解 ,以钼锑抗比色法测定底质中的总磷 ,通过实验确定最佳消解及分析条件。结果表明 ,该方法快速简便并有较高准确度、精密度和较低的检测限 ,值得推广和应用。     

土壤和沉积物中多氯联苯单体测定的净化方法研究

对浓硫酸净化、铜粉脱硫、氟罗里硅土柱、硅胶柱、石墨碳柱等净化方法在土壤和沉积物多氮联苯单体测定中的应用进行了研究.浓硫酸对多氯联苯单体的净化回收率达92.4％～109％;氟罗里硅土柱用正己烷/丙酮混合溶液淋洗,净化洗脱液体积为8 mL～10 mL时,回收率达85.7％ ～ 108％;硅胶柱用正己烷淋洗,净化洗脱液体积为...     

Sampling and analytical methodology development for the determination of primary and secondary low molecular weight amines in ambient air

In this project, a sampling device and an analytical method have been developed to simultaneously analyse the most frequently found low molecular weight amines, including aliphatic, aromatic and alcohol amines. These amines are diethanolamine, ethanolamine, methylamine, isopropylamine, morpholine, dimethylamine, and aniline. A sampling device was developed using a 37 mm cassette with glass fibre filters impregnated with sulfuric acid. Immediately after sampling, the filter was transferred to vials containing a solution of dansyl chloride. Dansyl chloride was used for derivatisation because it forms aromatic sulfonamides that are fluorescent and easy to protonate for MS detection. The effect of using an internal standard made with the dansylated derivative of 1-(2-methoxyphenyl)piperazine (MOPIP) on the uncertainty and efficiency of the method was also evaluated. This internal standard was spiked directly onto filters. The coupling of HPLC/ESI-MS was used for the simultaneous analysis of all the derivatives. This method showed detection limits of about 0.03 microg mL(-1) to 0.3 microg mL(-1) of amine with an average expanded uncertainty of 3% to 6% depending on the amine. The methodology recoveries are close to 100% for all the amines, and the overall estimated expanded uncertainties vary between 10% and 13% depending on the amine. This new strategy will be useful in evaluating workplace air since a unique sampling system will be used, independent of the amine to be quantified.     

High-performance liquid chromatography method for determination of hydrogen peroxide in aqueous solution and application to simulated Martian soil and related materials

A new method for determination of hydrogen peroxide (H₂O₂) is described. H₂O₂ reacts with iodide in the presence of ammonium molybdate and vanillic acid resulting in the formation of iodovanillic acid which is quantified by reversed-phase high-performance liquid chromatography (HPLC) and detected by UV absorption at 280 nm. The method provides a detection limit of ～0.1 μM and is easy to implement. Iodovanillic acid is stable, allowing multiple measurements of the same sample, and the separation power of the HPLC yields high selectivity against potential interferences. This method will be useful for many environmental applications. The method has been applied to quantify the photochemical production of H₂O₂ by aqueous suspensions of various minerals and soils.     

SO_2浓度对双通道自动荧光过氧化氢在线监测的影响研究

为验证大气中SO2的浓度对气态H2O2自动荧光法监测的影响,设置了SO2与H2O2在自动荧光过氧化氢分析仪中的反应实验;同时,利用SO2和H2O2的反应速率公式进行了模拟计算,模拟计算结果与仪器的监测结果基本相符.证明了在大气SO2浓度较高的情况下,气态SO2对H2O2的自动荧光法测定确实会有显著影响,通过模拟计算的方法可对在线监测的H2O2浓度数据进行校正.