对硼进行光谱分析的酸性酯沉积

R. Adu, R. Roto, A. Kuncaka
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引用次数: 0

摘要

研究了酸催化硼酸酯的生成及其在分光光度法分析硼中的应用。通过优化酸催化剂的种类和浓度,提高硼酸酯化量,提高硼分析方法的灵敏度。将硼酸溶于醇中分离硼,脱水成姜黄素,分光光度法测定?555海里。采用乙酸、甲酸、磷酸、硫酸和浓度为2.5的盐酸,考察了酸催化剂的种类和浓度对酯化率的影响;4.5;6.5;8.5%和10.5%。在最优条件下对方法进行了验证,并用于裂解样品中硼及其衍生物的测定。在H2SO4浓度为2.5%时,硼-姜黄素络合物的吸光度最大。硼酸酯精馏分光光度法分析硼的回收率为99.98 ~ 104.62%,重复性为?2%。检出限为0.316,定量限为1.056 mg L-1。该方法灵敏度高,摩尔吸光度值为4.7x105 Lmol-1cm-1。裂解样品中硼含量为2.936 ~ 4.912 mg -1。关键词:酸性催化剂,硼,硼酸酯,蒸馏,分光光度法。
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PEMBENTUKAN ESTER BORAT TERKATALISIS ASAM UNTUK ANALISIS BORON SECARA SPEKTROFOTOMETRI
The formation of borate ester catalyzed by acid for spectrophotometric analysis of boron was investigated.  It was conducted to improve the sensitivity of the boron analysis method by optimizing the type and concentration of acid catalyst that can increase the quantity of esterified boric acid. Boron was separated from the sample matrices by dissolving the boric acid in alcohols, then dehydrated into curcumin followed by spectrophotometric determination at ? 555 nm. The influence of the type and concentration of acid catalyst against the esterification rate was observed by using acetic acid, formic acid, phosphoric acid, sulfuric acid, and hydrochloric acid with a concentration of 2.5; 4.5; 6.5; 8.5, and 10.5%. Method validation was carried out under the optimal conditions and used to measure boron and its derivatives in the crackers sample. Maximum absorbance of the boron-curcumin complex was obtained by using an H2SO4 catalyst at the concentration of 2.5%. Spectrophotometric analysis of boron through borate ester distillation gave a good recovery in the range of 99.98-104.62% and acceptable repeatability of ? 2%. The limit of detection and limit of quantification was found to be 0.316 and 1.056 mg L-1, respectively. This method has a high sensitivity level with a molar absorptivity value of 4.7x105 Lmol-1cm-1. Boron content in the cracker sample ranged from 2.936 to 4.912 mgkg-1. Keywords: acid catalyst, boron, borate ester, distillation, spectrophotometry.
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