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.     

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％。     

Chemiluminometric determination of vanillin in commercial vanillin products

Vanillin, ethylvanillin and 4-hydroxy-3-methoxy-benzylalcohol have been found to chemiluminesce by the action of potassium permanganate in sulphuric or polyphosphoric acid media. Both acid media have been compared and sulphuric acid allows the sensitive determination of 0.15-10.0, 0.010-1.0 and 0.0030-0.30 μg mL⁻¹ of vanillin, ethylvanillin and 4-hydroxy-3-methoxy-benzylalcohol with limits of detection equal to 0.045, 0.0030 and 0.00090 μg mL⁻¹, respectively. Recoveries of vanillin from commercial vanillin products are within the range of 95-109%. Comparison with results from the official method shows differences within the range of 0.5-3.0%. The chemiluminogenic reaction mechanism is also discussed.     

火焰原子吸收测定泥炭中三种形态钾的方法研究

本文研究了原子吸收法测定泥炭中全量钾、缓效钾和速效钾的溶解，提取方法和测定条件，获得满意结果，钾的平均回收率为９７％－１０２％，相对标准偏差小于３％。     

Study on the initiation step of vinyloxirane and 3-butenyloxirane polymerization by alkalide K, K(15-crown-5)2

Transfer of one electron from potassium anion of alkalide K⁻, K⁺(15-crown-5)₂ to the double bond of vinyloxirane results in the oxirane ring opening exclusively in the α-position. K⁰ and radical anions are formed in the process. The former transfers the second electron mainly to the next monomer molecule. The latter dimerize to potassium glycoxides, which initiate the polymerization of vinyloxirane. The introduction of two CH₂ groups between the double bond and the oxirane ring changes the way of electron transfer. The oxirane ring of 3-butenyloxirane becomes the electron acceptor and its opening occurs in the β-position. In this case K⁰ transfers the second electron to the primarily formed radical anion giving an organopotassium intermediate. It reacts with crown ether. Potassium alkoxides are the reaction products. They become the real initiators of 3-butenyloxirane polymerization.     

间接原子吸收光谱法测定氢溴酸山莨菪碱

研究了原子吸收光谱法间接测定氢溴酸山莨菪碱。在溶液pH为 5 1～ 5 3,当四苯硼钠过量时可完全沉淀氢溴酸山莨菪碱 ;加入过量的氯化钾沉淀滤液中剩余的四苯硼钠 ;干过滤 ,用原子吸收分光光度计在76 6 5nm波长下测定滤液中过量的钾 ,因四苯硼钠与氢溴酸山莨菪碱和氯化钾均按 1∶1的计量关系生成沉淀 ,可以直接计算得到氢溴酸山莨菪碱的含量。对氢溴酸山莨菪碱注射液进行了测定 ,测定结果准确。方法简单快速 ,回收率在 96 %～ 10 3%之间 ,相对标准偏差为 1 4 %。该方法可进一步推广原子吸收光谱法在其他相关药物测定方面的应用。     

高碘酸钾催化光度法测定痕量铑

在磷酸和热水浴中 ,Rh( )催化高碘酸钾氧化二甲基黄褪色 ,由此建立了测定铑的新催化光度法。本方法的线性范围为 0— 4 .0 μg/ 2 5 m L,检出限为 4 .71× 10 -10 g/ m L。对 2 .0 μg/ 2 5 m L Rh( )测定的相对标准偏差为 1.4 3% (n=11) ,催化反应的表观活化能为 12 5 .8k J/ mol。此法已用于某些催化剂和冶金产品中痕量铑的测定 ,结果令人满意。