Synthesis and characterization of graft copolymer (alginate-g-poly(N,N-dimethylacrylamide))

<正>The graft copolymerization of N,N-dimethylacrylamide onto alginate by free radical polymerization using potassium peroxymonosulphate-sarbose as a redox pair in an inert atmosphere was investigated.The reaction conditions for maximum grafting have been optimized by varying the reaction variables,including the concentration of N,N-dimethylacrylamide(7×10~(-2) mol/L to 23×10~(-2) mol/L),potassium peroxymonosulphate(2×10~(-3) mol/L to 18×10~(-3) mol/L),sarbose(0.4×10~(-3) mol/L to 3.4×10~(-3) mol/L),sulphuric acid(1×10~(-3) mol/L to 8×10~(-3) mol/L) and alginic acid(0.4 g/L to 1.8 g/L) along with time duration(60 min to 180 min) and temperature(25℃to 45℃).Water swelling capacity,metal ion sorption and flocculation studies of the synthesized graft copolymer have been performed.The graft copolymer has been characterized by FTIR spectroscopy and thermogravimetric analysis.     

甲基绿-高碘酸钾系统催化动力学光度法测定痕量铱(Ⅳ)

基于以H3PO4为反应介质,用HAc-NaAc(1+8)(pH5.7)作缓冲溶液,在沸水浴中加热条件下,痕量铱(Ⅳ)能灵敏地催化高碘酸钾氧化甲基绿的褪色反应,建立了一种测定痕量铱(Ⅳ)的新催化光度法。研究了反应的最佳条件。催化反应吸光度A与非催化反应吸光度A0的差值ΔA与铱(Ⅳ)的质量浓度ρ在0～2.0μg/25mL范围内呈良好的线性关系。检出限为2.97×10-10g/mL。对1μg/25mL铱(Ⅳ)测定的相对标准偏差为1.7%(n=11)。测定了动力学参数。该催化反应对铱(Ⅳ)为一级反应,总反应为准一级反应。反应的表观速率常数为4.613×10-4/s,表观活化能为40.56kJ/mol。该方法用于分子筛样品和活性炭中痕量铱(Ⅳ)的测定,回收率97.9%～104.4%。     

离子色谱分离-亚铁氰化钾-钙黄绿素偶合化学发光测定NO_2~-

利用NO2-在酸性介质中氧化亚铁氰化钾为铁氰化钾,然后在碱性条件下和钙黄绿素化学发光反应相偶合,结合离子色谱分离和流动注射技术间接测定了NO2-。结果发现当钙黄绿素浓度为1.0×10-4mol/L,亚铁氰化钾浓度为2.0×10-4mol/L时,NO2-在1.0×10-5～1.0×10-7g/L范围内,化学发光强度与NO2-浓度成良好的线性关系(R=0.9958),检出限(3σ)为5.1×10-8g/L,对质量浓度为1.0×10-6g/LNO2-溶液进行11次平行测定,相对标准偏差为1.4%。将该方法用于蒸馏水和自来水中NO2-的测定,加标回收率分别为94.2%和107.1%。     

钼(Ⅵ)-2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚-溴酸钾体系的催化吸附波

在0.046mol/L HAc-NaAc(pH4.84)支持电解质中,Mo(Ⅵ)-2-(5-溴-2-吡啶偶氮-5-二乙氨基苯酚-溴酸钾)[Mo(Ⅵ)-5-Br-PADAP-KBrO3]络合物于-0.72V(vs.SCE)左右产生一个灵敏的络合吸附波,该波的二阶导数峰峰电流与1.5×10-8-2.0×10 -5 mol/...     

流动注射化学发光法测定山奈酚

采用流动注射技术,研究了高锰酸钾-山奈酚-过氧化氢体系的化学发光行为,对影响化学发光强度的因素进行了试验,建立了流动注射化学发光法测定山奈酚的新方法.方法检出限为1×10-10g·mL-1,线性范围为1.0×10-7-1.0×10-4g·mL-1.对1.0×10-6g·mL-1的山奈酚平行测定11次,其RSD为2.1%...     

Measurement of water activities of alanine + tri-potassium citrate + water system at temperatures between 293.15 and 313 K—Experimental and modeling

Water activity measurements by isopiestic method have been carried out on the aqueous solutions of alanine + tri-potassium citrate (K₃Cit) over a range of temperatures at atmospheric pressure. From these measurements, values of the vapor pressure of solutions were determined. The effect of temperature on the vapor–liquid equilibrium of alanine + K₃Cit + H₂O systems has been studied. The experimental water activities have been correlated successfully with the segment-based local composition Wilson and NRTL models. The agreement between the correlations and the experimental data is good.     

Potassium bromide catalyzed NS bond formation via oxidative dehydrogenation

N-Substituted benzo[d]isothiazol-3(2H)-ones are a family of compounds with extremely important application. Recently, we have developed a new green pathway to synthesize these compounds via potassium bromide-catalyzed intramolecular oxidative dehydrogenative cyclization. This reaction has high functional group tolerance and affords excellent yield even in gram scale.     

Markovnikov addition of vinyl acetate with azoles catalyzed by potassium tert-butoxide

A simple and efficient methodology for Markovnikov addition of azoles with vinyl acetate catalyzed by potassium tert-butoxide is described.N-heterocyclic compounds are synthesized from simple and commercially available starting materials under mild conditions in high yields.     

Mild and efficient oxy-iodination of alkynes and phenols with potassium iodide and tert-butyl hydroperoxide

An efficient synthesis of 1-iodoalkynes and iodophenols was easily achieved by employing simple KI and TBHP. The reaction does not involve the use of a metal and base combination. A variety of substituted alkynes and phenols were prepared with good to excellent yield.     

ICP－AES法测定钨酸钇钾激光晶体中的Er和Nd

应用ＩＣＰ－ＡＥＳ法测定钨酸钇钾［ｋＹ（ＷＯ４）２］激光晶体中的Ｅｒ和Ｎｄ。试样用磷酸分解，Ｔｍ被选作内标元素。Ｅｒ和Ｎｄ的回收率分别为９８．６％－１０５．３％和９６．５％－１０５．８％，相对标准偏差分别为１．９０％和１．６０％。