溶剂萃取原子吸收光谱法测定高纯石英砂中痕量铁

高纯石英砂用HF等溶剂溶解并蒸干后,在微酸性介质中用抗坏血酸还原Fe^3＋为Fe^2＋,与1,10-二氮杂菲形成Fe2＋3络合物,加入适量ClO4^-阴离子与之形成离子缔合物,用硝基苯萃取,原子吸收测定有机相,本法检出限1.1μg/g,样品分析结果的RSD%为：4.52～10.3.     

催化电解杀菌与次氯酸钠杀菌的对比

油田回注水催化电解杀菌与次氯酸钠杀菌在杀菌机理、效果及应用成本3方面的对比结果表明,催化电解产生有效氯是主要的杀菌机理.催化电解产生的有效氯质量浓度与电解时间呈线性关系,杀菌率随着有效氯质量浓度的增大而增大.定量杀菌的对比结果表明,油田回注水催化电解杀菌比次氯酸钠杀菌效果好,且不须投加任何药剂,只消耗电能,运行成本低.     

Surfactant Enhance DLLME/FO‐LADS: Assay of Malachite Green Level in Aquatic Environment of Trout Fish

Malachite green (MG), a traditional agent used in aquaculture although is not approved; its low cost and high efficacy make illicit use likely. We developed a small‐scale, simple, and sensitive dispersive liquid–liquid microextraction procedure for the assay of trace amounts of MG in aquatic environment of Trout fish. Fiber optic‐linear array detection spectrophotometry with charge‐coupled device detector benefiting from a microcell was used for this purpose. The method is based on enhancement effect of an anionic surfactant on the extraction of MG in to very fine multidroplets of microextraction solvent which made assisted by disperser solvent. Under the optimum conditions, the enrichment factor 77.5 was obtained from a 5‐mL water sample. The calibration graph was linear up to 5 × 10^?7 mol L^?1 with detection limit of 1 × 10^?8 mol L^?1. The relative standard deviation for seven replicate measurements of 4 × 10^?7 and 5 × 10^?8 mol L^?1 of MG were 3.3 and 4.5%, respectively.     

吡啶偶氮类试剂在光度分析中的应用进展

吡啶偶氮类试剂是一类性能优良的络合滴定指示剂和光度显色剂,迄今已合成了200余种,在分光光度分析测定各种金属离子方面得到了广泛的应用。为了进一步改善这类试剂的灵敏度和选择性等分析性能,近年深入研究了吡啶偶氮类试剂的结构与性能的关系,进而相继开发出一系列性能优异的吡啶偶氮类试剂。文章综述了1990—2010年以来常见的吡啶偶氮类试剂及其在分光光度分析测定金属离子方面的进展。从反应体系、最大吸收波长、灵敏度、线性范围等方面归纳了吡啶偶氮类试剂在实际样品中的应用情况,为此类试剂的开发和应用提供一些理论依据。     

安徽省金寨县沙坪沟钼矿中贵重分散元素铼的分析

采用Na2O2-CaO混合熔炉,达到完全分解辉钼矿和其它难溶矿的目的,干扰元素经两次沉淀分离消除,利用高铼酸根对碲酸还原产生催化极谱波,进行碲加入量和和干扰元素的试验,采用H2SO4-Na2SO4-Te底液催化极谱法,在JP-2D极谱仪上中辉钼矿痕量的铼,收到满意效果。解决了地勘一线实验室无ICP-MS等大型设备测定辉钼矿中分散元素铼     

An Optimised 1,10‐Phenanthroline Method for the Determination of Ferrous and Ferric Oxides in Silicate Rocks,Soils and Minerals

A precise, accurate and rapid method for the sequential determination of FeO and Fe₂O₃ in rocks, soils and some non‐refractory minerals by 1,10‐phenanthroline spectrophotometry is described. Fe(II) and Fe(III) were leached from the sample (?200 mesh) using a mixture of NH₄HF₂ and H₂SO₄ at 40–80 °C for 10 min on a hot plate. Both Fe(II) and Fe(III) could be conveniently estimated sequentially from the same reaction mixture at the μg g^?1 to percentage level. The method is better than the existing wet chemical methods, including the commonly used Pratt's titrimetric redox method, for Fe(II) and Fe(III) determinations in rock and soil samples in terms of precision, accuracy and rapidity. The throughput of the method was very high; at least forty to fifty samples could be estimated easily in a day. The results obtained compare favourably with those obtained by Pratt's method, as well as for certified/recommended values of a set of eleven certified reference materials having FeO and Fe₂O₃ contents in the range 0.21–14.63% and 0.58–8.48%, respectively. The optimised 1,10 phenanthroline method was found to be accurate to within 0.21% m/m FeO and 0.30% m/m Fe₂O₃ compared with the literature values of the certified reference materials studied.     

辉钼矿中微量锡的分离与测定

报道了在强碱性介质中用钡盐以钼酸钡形式沉淀大量Ｍｏ（Ⅵ）,使微量锡与大量钼分离,过量钡用碳酸盐清除。深液中残余的少量钼用Ｈ２Ｏ２掩蔽,从而实现了大量钼存在下微量锡的光度法测定。方法已用于辉钼矿中微量锡的测定,结果与国标法杆符,加标回收率在９４％～１０５％,８次测定的ＲＳＤ≤３．３％。     

MCM-41/β介孔—微孔复合分子筛的合成、表征及催化性能

以β分子筛为前驱体,水玻璃和硫酸铝为外加硅铝源,采用二元混合表面活性剂为结构导向剂,水热晶化合成MCM-41/β介孔—微孔复合分子筛,并利用XRD、SEM、TEM、N2吸附—脱附和Py-IR等对复合分子筛进行表征,以十氢萘为模型化合物考察复合样品的催化裂解反应性能.结果表明:MCM-41/β介孔—微孔复合分子筛中存在MCM-41分子筛六方介孔结构和β分子筛微孔结构,对十氢萘具有较强的催化反应活性,催化裂解转化率为93.16%.     

巯基棉富集-光度法连续测定铬铁矿中的铂钯

在建立巯基棉富集-分光光度法联用系统的基础上,对螯合反应的pH、吸附酸度、显示剂用量、显色温度及体系稳定性等进行了优化选择,并将联用系统成功地应用于实际样品的富集分离分析。在盐酸介质中,α-呋喃二肟与钯得黄色络合物,于λmax=380nm处测定其吸光度,HSCT与铂反应生成2：1稳定络合物,于λmax=540nm处测定其吸光度,对Pt,Pd的检测限（3）分别为0．01μg／ml,0．005μg／ml,对国家一级标准物质进行验证,结果与标准值相符,加标回收率98．0％～102．5％,相对标准偏差为3．88％～8．97％。应用于实际样品的测定．结果满意。     

微波消解-火焰原子吸收光谱法测定石英砂中的氧化钙和氧化镁

采用微波消解-硼酸络合-火焰原子吸收光谱法测定石英砂中的氧化钙和氧化镁。样品在MK-Ⅲ型实验室微波炉上消解,消解压力为2.0 MPa、消解时间为5 m in,以硼酸络合消除氢氟酸的影响。方法已用于实际样品的测定,7次测定的相对标准偏差(RSD)小于5%,加标回收率为95.0%~104.2%。