SPECTROPHOTOMETRIC DETERMINATION OF BORON IN IRON AND STEEL WITH CURCUMIN AFTER SEPARATION BY 2-ETHYL-1,3-HEXANEDIOL-CHLOROFORM EXTRACTION

SPECTROPHOTOMETRIC DETERMINATION OF BORON IN IRON AND STEEL WITH CURCUMIN AFTER SEPARATION BY 2-ETHYL-1,3-HEXANEDIOL-CHLOROFORM EXTRACTION
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DOI:
10.1016/0039-9140(81)80024-0
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发表时间:
1981-01-01
期刊:
影响因子:
6.1
通讯作者:
DONALDSON, EM
DONALDSON, EM
中科院分区:
化学1区
文献类型:
--
作者:
DONALDSON, EM

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本文介绍了一种简便可靠的测定铁和低、高合金钢中总硼含量0.0001%以上的∼的方法。在过氧化氢和氟化氢的存在下,样品在<70℃分解后,不溶物质被过滤掉,最终与碳酸钠熔化。将冷却的熔体溶解在稀盐酸中,并将溶液与主溶液结合。氟化物随后与锆络合,通过从1M硫酸介质中萃取含2-乙基-1,3-己二醇的氯仿作为硼酸盐,从铁和其他元素中分离出硼。在冰醋酸-浓硫酸介质中,姜黄素玫瑰花苷形成络合物后,在乙醇介质中,用分光光度法在550 nm波长处测定1毫升提取物中的硼。还可测定酸溶硼和酸不溶硼。常见离子,包括大量的锰、铬、钒、钛、钼、钨、铌和钽不干扰。
A simple and reliable method for determining ∼ 0.0001% or more of total boron in iron and low- and high-alloy steels is described. After the sample is decomposed at <70° in the presence of hydrogen peroxide and potassium hydrogen fluoride, the insoluble material is filtered off and ultimately fused with sodium carbonate. The cooled melt is dissolved in dilute hydrochloric acid and the solution is combined with the main solution. Fluoride is subsequently complexed with zirconium and boron is separated from iron and other elements by extraction as borate from 1Msulphuric acid medium into chloroform containing 2-ethyl-1,3-hexanediol. Boron, in a 1-ml portion of the extract, is ultimately determined spectrophotometrically at 550 nm in an ethanol medium, after formation of the curcumin rosocyanin complex in a glacial acetic acid—concentrated sulphuric acid medium. Acid-soluble and acid-insoluble boron can also be determined. Common ions, including large amounts of manganese, chromium, vanadium, titanium, molybdenum, tungsten, niobium and tantalum do not interfere.