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1.
文章以水溶性碘化四对(4-三甲氨基苯基)铁卟啉和钒取代杂多酸H5PMo10V2O40为原料,采用离子交换方法在水溶液中合成了一种铁卟啉/钒取代杂多酸新型无机-有机复合催化剂,并使用红外和紫外光谱技术对其结构进行了表征,结果表明,这种新型复合催化剂仍然保持着卟啉的大环共轭结构和杂多酸的笼状多电子结构.同时研究了以30%过氧化氢水溶液为绿色氧化剂,初步探讨了这种铁卟啉杂多酸催化剂对苯的羟基化反应的的影响,考察了催化剂的催化活性.催化氧化实验表明,制备的铁卟啉/杂多酸配合物可用作苯直接氧化羟基化成苯酚的催化剂,并且表现出较高的催化活性.  相似文献   

2.
锰卟啉/钒取代杂多酸配合物的合成、表征和性能研究   总被引:1,自引:0,他引:1  
利用碘化四对(4-三甲氨基苯基)锰卟啉与钒取代杂多酸H5 PMo10 V2O40,在水溶液中,室温下反应合成了锰卟啉/钒取代杂多酸配合物,用红外和紫外光谱技术对其结构进行了表征,发现该配合物中包含着金属卟啉的环状结构与杂多酸的笼状结构,并且二者以化学键的形式键合在一起.以该化合物作为催化剂,以过氧化氢水溶液为氧化剂,在温和的条件下研究了锰卟啉/钒杂多酸配合物对苯的羟基化反应的影响,考察了催化剂的催化活性,探讨了催化剂对苯羟基化反应的活性中心.研究结果表明,杂多酸中的钒原子是其主要的催化活性中心,锰卟啉的存在可以有效地提高其催化活性.  相似文献   

3.
在应用火焰原子吸收光谱法测定铬和钼时,加入浓度为0.5%和0.5%以上的阴离子表面活性剂十二烷基硫酸钠(SLS)可使铬和钼的吸光度增高几乎为原来的两倍。同时能够克服盐酸、硝酸和钒(Ⅴ)硅(Ⅳ)、铝(Ⅲ)、铁(Ⅲ)、锰(Ⅱ)、钙(Ⅱ)、钾(Ⅰ)、和钠(Ⅰ)等十多种金属离子的干扰。进而讨论了测定铬时应用0.25%的非离子表面活性剂乙二醇辛基苯酚(OP-10)或triton X-100以及测定钼时应用0.6%的阳离子表面活性剂溴化十四烷基吡啶的增感效应及其克服干扰的情况,并与应用十二烷基硫酸钠作了比较。  相似文献   

4.
硅钼蓝光度法测定沸石分子筛中的硅   总被引:6,自引:0,他引:6  
提出沸石分子筛中硅含量测定的硅钼蓝光度法。方法基于盐酸介质中Si(Ⅳ)与钼酸铵形成硅钼黄杂多酸后,用抗坏血酸还原硅钼黄形成硅钼蓝的原理进行硅的测定。本文实验条件下,体系的λmax位于770nm,表观摩尔吸光系数εmax=1.92×10^4L·mol^-1·cm^-1,硅量在0-0.60μg/mL范围内遵守比耳定律。本文提出的新方法已成功地用于某些沸石分子筛中的硅测定。  相似文献   

5.
利用拉曼光谱研究了钼、钒单一及混合溶液在pH=10.0~1.0时的离子分布行为. 钼、钒离子在存在形式上存在着差异:当pH=9.0~7.5时钒主要以(VO3)nn-形式存在,而钼主要为MoO42-. 这一差异是目前现有的许多钼钒分离方法的基本原理. 通过将混合溶液体系的拉曼光谱与单一体系进行对比,分析得出了混合体系中离子的存在形式. 当pH低于6.5时,部分V-O-V基团中的V原子会被Mo原子取代,从而形成了钼钒杂多酸离子. 当pH=6.0~2.0时,钒主要以十聚钒酸盐形式存在;当pH=2.0~1.0时,混合溶液中的钼主要以具有七钼酸盐结构的杂多酸离子存在,而在相同pH的单一溶液中,钼的存在形式主要为Mo8O264-和Mo36O1128-.  相似文献   

6.
间接原子吸收光谱法测定四氧化三钴中的微量硅   总被引:7,自引:0,他引:7  
以盐酸、甲醛溶解试样,在pH1~2的盐酸介质中,硅、磷与钼酸铵生成硅钼及磷钼杂多酸。以乙酸丁酯萃取磷钼酸分离除去磷,再用MIBK萃取硅钼酸,因硅与钼原子数之比为112,利用原子吸收光谱法测定有机相中的钼,即可间接测定硅。本法测定高纯四氧化三钴中的硅有很高的灵敏度,检测限达0.2μg/mL,并可避免基体钴及其他共存元素的干扰。与分光光度法对照,结果满意。  相似文献   

7.
在非离子(O/W)型微乳液(OP/n-C5H11OH/n-C7H16/H2O)存在下,磷钼钒杂多酸与乙基紫在0.7-1.0mol/L硝酸介质中形成蓝色的离子缔合物,缔合物的最大吸收波长为612nm,表观摩尔吸光系数ε612为1.58×105L·mol-1·cm-1,磷含量在0.03-0.4μg/mL范围内符合比耳定律,...  相似文献   

8.
杂多阴离子的NMR和ESR研究:Ⅱ磷钼钒杂多酸及其镧盐的NMR   总被引:1,自引:0,他引:1  
具有Keggin结构的磷钼钒杂多酸及其盐是有效的氧化剂.本文通过磷钼钒杂多酸及其镧盐的~(31)p,~(51)V,~(139)La,~(17)O及~1H的NMR测定,并结合红外和差热分析,说明镧的引入对Keggin结构没有影响,但镧对水分子有强的作用力,使阴离子之间存在更多的水分子,从而对催化氧化活性产生了影响.  相似文献   

9.
分光光度法测定磷矿石中五氧化二磷及二氧化硅的含量   总被引:6,自引:0,他引:6  
试样经碱熔,酸化后,以磷-钼-钒黄分光光度法测定五气化二磷;在草酸存在下,以抗坏血酸为还原剂,硅钼蓝法测定二氧化硅。本方法操作简单、快速,具有较好的精密度和准确度。  相似文献   

10.
磷钼杂多酸-结晶紫分光光度法测定高纯氯化铯中微量磷   总被引:1,自引:0,他引:1  
张毅  汪明礼 《光谱实验室》2004,21(3):501-503
以 4 -叔丁基 - 2 (α-甲苄基 )苯酚 (t- BAMBP)萃取分离基体铯 ,磷钼杂多酸与结晶紫染料生成离子缔合物 ,在聚乙烯醇存在下 ,在水溶液中显色。在波长 5 45 nm处 ,其摩尔吸光系数可达 2 .0 1× 10 5L· mol-1·cm-1。方法的回收率为 97%— 10 1% ,相对标准偏差为 0 .8%— 2 .7%。  相似文献   

11.
韦莉 《光谱实验室》2012,29(1):423-426
采用微波消解-电感耦合等离子体-原子发射光谱法(ICP-AES),通过分析回收率,着重研究消解用无机酸(盐酸、硝酸和过氧化氢)对油墨中铅含量测定的影响.盐酸的加入对ICP-AES分析影响较小,但会与铅形成二氯化铅,造成微量损失,回收率下降.硝酸对ICP-AES分析有酸效应,过量硝酸会影响仪器精准性.当过氧化氢用量为1.0-2.0mL时,对回收率基本没有影响.结果表明,6mL硝酸和1mL过氧化氢就可使1.5g油墨消解完全,此时铅的加标回收率为100.7%.实验优化了前处理方法,使结果更加准确可靠.  相似文献   

12.
Most products especially metallic surfaces require cleaning treatment to remove surface contaminations that remain after processing or usage. Lead fouling is a general problem which arises from lead fouling on the chromium surfaces of bores and other interior parts of systems which have interaction with metallic lead in high temperatures and pressures. In this study, a novel chemical solution was introduced as a cleaner reagent for removing metallic lead pollution, as a fouling metal, from chromium surfaces. The cleaner aqueous solution contains hydrogen peroxide (H2O2) as oxidizing agent of lead layer on the chromium surface and acetic acid (CH3COOH) as chelating agent of lead ions. The effect of some experimental parameters such as acetic acid concentration, hydrogen peroxide concentration and temperature of the cleaner solution during the operation on the efficiency of lead cleaning procedure was investigated. The results of scanning electron microscopy (SEM) showed that using this procedure, the lead pollution layer could be completely removed from real chromium surfaces without corrosion of the original surface. Finally, the optimum conditions for the complete and fast removing of lead pollution layer from chromium surfaces were proposed. The experimental results showed that at the optimum condition (acetic acid concentration 28% (V/V), hydrogen peroxide 8% (V/V) and temperature 35 °C), only 15-min time is needed for complete removal of 3 g fouling lead from a chromium surface.  相似文献   

13.
Abstract

Using supercritical water oxidation, the cation exchange resin was decomposed fast and completely to water, carbon dioxide and sulfuric acid. While the resin decomposition yield increased with the reaction time and the amount of hydrogen peroxide added as oxidizing agent, it was constant in the resin concentration from 0.14 to 1.9 dry resin weight percent to water. More than 99% of the cation exchange resin was decomposed with hydrogen peroxide added in the amount of 7 times the stoichiometric value at 673 K and 30MPa for 30 minutes of the reaction time. The cation exchange resin is decomposed through two main reaction pathways. One has a rate controlling intermediate such as acetic acid whose decomposition rate was very slow, and the other does not have stable intermediates. The decomposition of the acetic acid is a significant factor for the complete decomposition of the resin, although it does not dominate the whole resin decomposition. A simple kinetic model that estimates the resin decomposition yield was developed.  相似文献   

14.
以ZSM-5为原料,采用浸渍法将其交换成HZSM-5,以HZSM-5为催化剂,对以冰乙酸和正戊醇为原料合成乙酸戊酯的反应条件进行了研究。研究表明,以1.0m ol/L硫酸浸渍后的ZSM-5催化活性最高,当醇酸摩尔比为1.1∶1,催化剂用量为0.4g,反应时间为90m in,反应温度为125—135℃,酯化率可达82.5%。  相似文献   

15.
Epoxy resins made from vegetable oils are an alternative to synthesize epoxy resins from renewable sources. Tung oil is rich in α -eleostearic fatty acid, which contains three double bonds producing epoxy resins with up to three epoxy groups per fatty acid. This work studied the production of tung oil epoxy resin using hydrogen peroxide as an oxidizing agent and acetic and formic acid as percarboxylic acid precursors, applying low frequency high power ultrasound. This study evaluated the effects of ultrasound power density, hydrogen peroxide concentration, acetic acid concentration, and formic acid concentration on the yield into epoxy resin, selectivity, and by-products formation. Application of ultrasound was carried out using a 19 kHz probe ultrasound (horn ultrasound) with a 1.3 cm diameter titanium probe, 500 W nominal power, 2940 W L−1 maximum effective power density applied to the reaction mixture. Ultrasound technology yielded up to 85% of epoxy resin in 3 h of reaction. The use of formic acid resulted in a slightly lower oil conversion than acetic acid but with a much higher selectivity towards epoxidized tung oil. However, using acetic acid resulted in the production of high-value by-products, such as 2-heptenal and 2,4-nonadienal. The ultrasound-assisted epoxidation showed to be particularly efficient when applied to oils containing conjugated double-bonds.  相似文献   

16.
Effect of coal ash on sonochemical degradation of phenol in water   总被引:1,自引:0,他引:1  
The influences of coal ash on the degradation of phenol in water were investigated under the stirring or ultrasonic irradiation conditions. Phenol solution (10mg/L, 100mL) was sonicated at 200 kHz and 200 W with or without coal ash (53-106 microm in particle size and concentration of 0.0-1.5 wt%). It was found that the sonochemical degradation of phenol in the presence of coal ash was faster than that in the absence of coal ash, and the optimum amount of coal ash was a maximum at 0.4-0.6 wt%. It was confirmed that the phenol degradation did not occur by the addition of hydrogen peroxide and nitric acid under the stirring conditions. The sonochemical degradation with coal ash was depressed by the addition of tertiary butyl alcohol as a radical scavenger. These results indicated that the coal ash accelerated the phenol degradation due to the increase in the amount of hydroxyl radicals under the ultrasonic irradiation. Since the coal ash used had a porous and uneven surface, which was observed by SEM, it was assumed that the coal ash led to the increase in the nucleation site for cavitation bubble due to its surface roughness.  相似文献   

17.
陈张好  刘小娟 《光谱实验室》2012,29(2):1046-1049
建立了高效液相色谱法测定祛痘类化妆品中禁用组分苯海拉明的含量。采用Inertsil CN-3色谱柱,流动相为乙腈-水-三乙胺(50∶50∶0.5,用冰醋酸调节pH至6.5),检测波长258nm,流速1.0mL/min,柱温25℃。苯海拉明在0.05—2.00mg/mL内呈良好线性(r=1.0000),平均回收率103.2%(RSD=0.70%,n=6);方法检出限(S/N=3)为50μg/g。该法操作简便,准确可靠,稳定性好,可用于祛痘类化妆品中苯海拉明的检测。  相似文献   

18.
过氧化氢-邻氨基酚体系催化显色分光光度法测定痕量铁   总被引:1,自引:0,他引:1  
在乙酸-乙酸钠缓冲溶液(pH=5.6)介质中.Fe(Ⅲ)催化H2O2氧化邻氨基酚显色,建立了催化显色分光光度法测定痕量铁的新方法.在冰水浴中反应10min,Fe(Ⅲ)线性范围为0-1.2μg/mL,回归方程为△4=0.4923C+0.0258,摩尔吸光系数为2.9×104L·mol-1·cm-1.方法用于广西东兰县产墨...  相似文献   

19.
Abstract

An inductively coupled plasma mass spectrometer method for estimating trace elements in tree nut oils has been developed which employs microwave digestion equipped with high pressure subassembly. Residual carbon content and residual acidity were determined to evaluate the efficiency of digestion. The best digestion efficiency was obtained using Easyprep? system with 0.5?g of oil, 4?mL concentrated nitric acid, and 2?mL hydrogen peroxide, and a final temperature of 235?°C. Residual carbon content and residual acidity were estimated as 1.7% (corresponding to 852?mg L?1 of carbon in sample solution) and 7.5%, respectively, and recovery values ranged from 90.7% to 107.7%. Whereas, only 0.2?g of oil could be digested through conventional microwave system with 5?mL concentrated nitric acid and 2?mL hydrogen peroxide at 205?°C (residual carbon content?=?3.2%). The developed method has been applied to determine nine trace elements (Cr, Mn, Fe, Ni, Cu, As, Zn, Cd, and Pb) in different categories of tree nut oils, and high content of Fe, Mn, and Zn were found in some of those oils. To the best of our knowledge, the present investigation is the first attempt to analyze trace elements in different categories of tree nut oils consumed in China.  相似文献   

20.
微波溶样—ICP/MS法测定稻中15种痕量稀土元素   总被引:3,自引:0,他引:3  
本文报道采用HNO3+H2O2微波溶样,ICP-MS直接测定稻中15种稀土元素,对微波溶样和等离子体质谱测定条件进行了优化选择。选用Re作内标可补偿基体效应。方法检出限为7.0-25.8pg/mL,稻壳加标回收率为95-105%,RSD为2.3-4.2%,方法快速、灵敏、准确。  相似文献   

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