炔基苯基高碘盐的合成与应用

芳基乙炔与羟基对甲苯磺酰氧基碘苯在分子筛催化下反应,生成苯乙炔基对甲苯磺酰氧基碘苯,产率44%-49%。1-三甲基硅基炔与亚碘酰苯在三氟化硼乙醚溶液中反应,经对甲苯磺酸钠水溶液处理后,得炔基对甲苯磺酰氧基碘苯,产率46%-65%。     

制备碘甲磺隆的新工艺

专利WO03/912228公开了如下高收率制备碘甲磺隆的新工艺,其中磺酰基异氰酸酯的制备不用光气及其替代品,而是用无机盐氰酸钠。(LCL)制备碘甲磺隆的新工艺     

全氟磺酰树脂的分析表征

采用DSC、TGA等仪器对本文制备的质子交换膜燃料电池用全氟碘酰树脂进行了分析表征，同时测定了全氟磺酰树脂的力学性能与交换容量。研究结果表明，本文所制备的全氟磺酰树脂的热性能、力学性能以及交换容量基本符合实际使用的要求。     

二乙酸亚碘酰苯及羟基对甲苯磺酰氧碘基苯的合成研究

通过碘化苯直接与 2 6 %～ 30 %的过氧化氢溶液和醋酸酐反应 ,合成了二乙酸亚碘酰苯 ,该反应避免直接使用较高浓度的过乙酸 ,且操作简单方便 ,产物收率较好 ,纯度高。同时也可不必分离出二乙酸亚碘酰苯直接加入对甲苯磺酸反应 ,得到羟基对甲苯磺酰氧碘基苯。     

韦氏溶液中卤素比例的快速测定方法

韦氏溶液是化学分析上的一种试剂，它用来测定油脂、脂肪酸的碘值。其制备方法，通常是通氯于0.1N碘的冰乙醛溶液。韦氏溶液中的卤素总量一般常用Na_2S_2O_3滴定，其游离碘可在盐酸溶液中，用KIo_3溶液直接滴定，碘和氯的比例应保持在1.1（即I/Cl=1.1）本文介绍的就是碘和氯比例的快速测定方法。     

1.2%二磺·甲碘隆油悬浮剂的高效液相色谱分析

[方法]采用反相高效液相色谱法,使用C18柱和紫外检测器,以乙腈和磷酸溶液(体积比50∶50)为流动相,流速为1.0 mL/min,在233 nm波长下,对甲基二磺隆和甲基碘磺隆钠盐同时进行定量测定。[结果]甲基二磺隆和甲基碘磺隆钠盐的标准偏差分别为0.015和0.005,变异系数分别为1.49%和2.68%,平均回收率分别为99.8%和99.9%,线性关系分别为0.999 6和0.999 1。[结论]方法具有简便、快速、分离效果好、精密度和准确度高、线性关系好的优点,是较理想的分析方法。     

碘甲磺隆钠盐分析方法述评

总结了文献报道的碘甲磺隆钠盐的分析方法。碘甲磺隆钠盐的分析主要采用高效液相色谱法,可用于碘甲磺隆钠盐原药、制剂的分析。     

碘甲磺隆钠盐的水解特性

通过实验室的模拟试验研究了碘甲磺隆钠盐在不同温度、pH值及不同水体条件下的水解动态。结果表明：碘甲磺隆钠盐在正常的环境条件(水的pH值为7,25℃,灭菌)下,碘甲磺隆钠盐难以水解,其降解半衰期长达157．5d,而在酸性条件下稳定性较差,容易水解,其半衰期缩短了10倍,仅为15．5d;温度对碘甲磺隆钠盐的水解速率有一定的影响,当pH为4时,其水解速率随温度的升高而加快,当温度为15℃、25℃、35℃时,半衰期分别为23．9、15.5、12.3d;碘甲磺隆钠盐在蒸馏水中的水解速率与在河水中的水解速率相似。     

碘的液膜分离富集与测定

提出用非流动载体液膜分离富集碘,研究了用L113B/SPAN80(混合表面活性剂)、聚丁烯(膜的增强剂)、煤油(溶剂)和内相(Na_2SO_3溶液)液膜体系,分离富集水和食盐中的微量碘。碘被扩散迁移穿膜渗透到乳状液膜内相中,立即与内相中Na_2SO_3溶液发生选择性、不可逆反应,生成NaI(非渗透物)。碘不断从水试液浓缩到内相中去,然后用银量法测定富集的NaI溶液,此法已用于富集测定水、工业废水和食盐中微量碘,结果较准确。     

52%砜嘧·碘甲钠盐·噻酮·环丙磺酰胺WG的高效液相色谱分析

建立同时测定复配产品52%砜嘧磺隆·碘甲磺隆钠盐·噻酮磺隆·环丙磺酰胺WG中有效成分和安全剂的高效液相色谱分析方法。选用Agilent C₁₈柱，检测波长250 nm，以甲醇-乙腈-0.1%磷酸水为流动相对各有效成分和安全剂进行有效分离和定量检测。砜嘧磺隆、碘甲磺隆钠盐、噻酮磺隆和安全剂环丙磺酰胺线性相关系数分别为0.999 5、0.999 6、0.999 5和0.999 7，平均添加回收率分别为99.91%、99.52%、99.75%和99.71%，标准偏差分别为0.04、0.01、0.04和0.03，变异系数分别为0.32%、0.69%、0.28%和0.12%。该方法简便、精确度高且重现性好，满足该复配剂型的快速准确的质量控制检测。     

分光光度法研究十二烷基硫酸钠的临界胶束浓度

在碘的水溶液和I<'-><,3>溶液2种体系中测定了十二烷基硫酸钠(SDS)的临界胶束浓度(CMC),并讨论了在I<'-><,3>体系中,不同硫酸钠和氯化钾2种盐对测定结果的影响,在碘的水溶液中研究了不同碘浓度对SDS的CMC的影响.采用分光光度法求得SDS在两种体系中的CMC值,硫酸钠与氯化钾对CMC的值有影响,且无...     

Studies on chemically modified cotton. V. Effect of zinc chloride solutions on swelling and other properties of cotton

This paper describes the effect of zinc chloride solutions of different molarity at different temperatures, viz., 10°, 25°, 36°, 55°, and 75°C, on various properties of cotton fiber such as degree of swelling, accessibility to water vapor and iodine absorption, infrared ratio, barium activity number (BAN), and leveling-off degree of polymerization (LODP). Zinc chloride solution caused inter- and intrafibrillar swelling in cotton fiber depending on conditions of treatment, viz., concentration of solution and temperature employed. Fibers treated in 10.07 moles/1. (M) solution of zinc chloride in slack state showed rapid increase in degree of swelling up to 2 hr, followed by a slow increase, reaching the maximum after 3 hr of treatment. Fibers swollen with fixed ends without allowing shrinkage showed gradual increase with maximum swelling after 6 hr of treatment. Cotton fibers treated in different molar solutions of zinc chloride at 55°C showed varying degrees of swelling (inter- and intrafibrillar) and a somewhat different trend compared to that observed at 10°C. Electron micrographs revealed mostly intercrystalline swelling in case of samples treated with 9.26M at 10°C, while the same concentration produced intracrystalline swelling at 55°C. Accessibility to water vapor, iodine absorption, and BAN of treated samples showed specific effect of temperature with regard to effectiveness of concentrations of zinc chloride solutions. Similar effects of temperature with regard to concentrations of reagent were observed on infrared ratio and LODP. Accessibility by iodine absorption and LODP correlate with BAN; also, the accessibility by iodine absorption correlates with the LODP.     

活性生物猪骨炭纯化盐湖工业氯化钾

生产食品级和药用氯化钾主要采用工业级产品通过进一步纯化的方法制备得到。盐湖工业氯化钾制备方法是采用浮选剂进行浮选制备,因此存在浮选剂残留和部分重金属超标的情况。经测定所用盐湖工业氯化钾样品中,铵和铅的质量分数分别为1.698×10^-4和1.63×10^-5。为了制备食品级氯化钾,采用猪骨为原料,以磷酸为活化剂制备得到了比表面积为147.26 m²/g、碘吸附值为297.5 mg/g的活性生物猪骨炭,实验结果表明,用10 g的活性猪骨炭和商品炭分别对1 L的氯化钾溶液做吸附处理,活性猪骨炭吸附后溶液中各离子含量均符合GB 25585—2010《食品添加剂 氯化钾》的要求,成功制备了食品级氯化钾。     

A colorimetric microdetermination of peroxide values utilizing aluminum chloride as the catalyst

A colorimetric microassay is described for the determination of lipid hydroperoxides. Hydroperoxides are reacted with potassium iodide in the presence of an acid catalyst and liberated iodine is measured. Aluminum chloride, an alcohol-soluble Lewis acid, is used as catalyst. Liberated iodine is measured colorimetrically at 560 nm after addition of starch in 0.01 N hydrochloric acid. The range of the measurement was 0.05–0.5 μmol of hydroperoxides.     

合成环己酮乙二醇缩酮的催化剂研究进展

评述了近年来国内采用甲烷磺酸盐、对甲苯磺酸、氨基磺酸、强酸性阳离子交换树脂、磺化聚氯乙烯、六水三氯化铁、二水氯化亚锡、五水四氯化锡、四水氯化锰、硫酸铜、水合硫酸铁、十二水合硫酸铁铵、硫酸钛、四水硫酸锆、氯化锆、四水硫酸高铈、水合硝酸镧、活性炭固载硫酸镧、铌酸、树脂固载Lewis酸、壳聚糖硫酸盐、一水硫酸氢钠、碘、磷酸二氢钠、固体超强酸、杂多酸、分子筛和维生素C等固体酸催化合成环己酮乙二醇缩酮的实验结果。研究结果表明,固体酸能够代替硫酸作为合成环己酮乙二醇缩酮反应的催化剂。     

A new rapid titration method for determining the halogen ratio of Wijs solution and of iodine monochloride

The free iodine in Wijs solution is titrated directly, in strong hydrochloric acid solution, with standard potassium iodate solution. From this titration and the usual sodium thiosulfate titration for total halogen, the iodine/chlorine ratio is calculated. Results agree closely with those obtained by the longer chlorine-water method of Lopes. The halogen ratio of reagent grade iodine monochloride, a convenient material from which to prepare Wijs reagent directly, is also determined by the new titration method.     

The Synthesis of Covalent Triazine-Based Frameworks via Friedel–Crafts Reactions of Cyanuric Chloride with Thienyl and Carbazolyl Derivatives for Fluorescence Sensing to Picric Acid,Iodine and Capturing Iodine

A multifunctional thiophene-based covalent triazine framework (TTPATTh) with triphenylamine as core is synthesized by Friedel–Crafts reaction of cyanuric chloride with thienyl derivative for the first time. The yield of TTPATTh (99.59%) is far higher than that of the carbazole-based CTF (TTPATCz, 47.03%). TTPATTh and TTPATCz possess high BET surface areas with 1235 and 2501 m² g^–1 as well as high pore volumes with 1.60 and 2.23 cm³ g^–1, respectively. TTPATTh and TTPATCz have high thermal stability with high thermal decomposition temperatures of 514 and 598 °C in nitrogen atmosphere. With the introduction of triazine rings, the fluorescence sensing sensitivities of TTPATTh and TTPATCz to picric acid and iodine are improved significantly. Especially for TTPATTh, the K_sv values reach 5.95 × 10⁵ and 1.61 × 10⁴ L mol^–1, and LODs reach 1.02 × 10^–12 and 1.86 × 10^–12 mol L^–1. To the best of the knowledge, this is the most sensitive value among thiophene-based porous organic polymers to PA and I₂. Furthermore, TTPATTh and TTPATCz can also adsorb iodine in vapor phase, cyclohexane solution and aqueous solution, and release iodine by heating or in ethanol solution. The efficiency of controlling the release of iodine is higher than that in ethanol.     

Scandium Extraction from Chloride Solutions by a Mixture of Tributyl Phosphate and Molecular Iodine

It has been established that the addition of elemental iodine significantly enhances the extraction of scandium by means of tributylphosphate. The metal distribution coefficients exhibit an increase with increasing TBP and iodine concentration in the organic phase as well as with increasing chloride ion concentration in the aqueous phase. As an outsalting agent, chlorides of alkali, alkaline earth and other weakly extracted metal cations can be used. The process is promising for the extraction of scandium from solutions of hydrochloric- acid leaching of mineral and man-made materials.

     

化妆品中碱金属氯酸盐的检测方法研究

建立了薄层色谱法和电位滴定法联用测定化妆品中碱金属氯酸盐含量的方法。用薄层色谱将氯酸盐从其他卤酸盐中分离,与碘化物形成碘来鉴别碱金属的氯酸盐。通过鉴别试验后,在酸性条件下氯酸盐被锌粉还原,所形成的氯化物用硝酸银溶液进行电位滴定。试验结果表明：在0．03％～3．41％（以氯酸根离子计）的质量分数范围内,加标回收率为81．4％～105．2％,相对标准偏差（RSD）≤10％;定性检出限为0．03％（质量分数）,定量检出限为0．10％（质量分数）。     

Cationic starch iodophores

Cross‐linked cationic starches N‐(2‐hydroxyl)propyl‐3‐trimethyl ammonium starch chloride (CQS chloride), N‐(2‐hydroxyl)propyl‐3‐trimethyl ammonium starch iodide (CQS iodide), and N‐(2‐hydroxyl)propyl‐3‐trimethyl ammonium starch iodide–iodine (CQS triiodide) with the degree of substitution (DS) according to cationic groups from 0.04 to 0.62, as well as cross‐linked starch–iodine complexes were synthesized and tested as potential antibacterial agents. Cationic starch iodine derivatives were obtained during ion exchange reaction between CQS chloride and iodide or iodide–iodine anions in aqueous solutions. CQS_DS≤0.3 chloride can form several types of iodine complexes, such as the blue amylose–iodine inclusion complex and ionic CQS⁺I^?·(I₂)_m complex (m ≥ 1). The antibacterial activity of modified starches–iodine samples against different pathogenic bacterial cultures and contaminated water microorganisms was evaluated. CQS chloride and CQS iodide were found to be bacteriostatic. A strong antibacterial activity was characteristic of CQS triiodides in which molecular iodine is present in both ionic and inclusion complexes. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013