Effect of HF addition on the microwave-assisted acid-digestion for the determination of metals in coal by inductively coupled plasma-atomic emission spectrometry

The microwave-assisted acid-digestion for the determination of metals in coal by ICP-AES was investigated, especially focusing on the necessity of adding HF. By testing five certified reference materials, BCR-180, BCR-040, NIST-1632b, NIST-1632c, and SARM-20, it was found that the two-stage digestion without HF (HNO₃ + H₂O₂ was used) was very effective for the pretreatment of ICP-AES measurement. Both major metals (Al, Ca, Fe, and Mg) and minor or trace metals (Co, Cr, Cu, Mn, Ni, Pb, and Zn) in coal gave good recoveries for their certified or reference values. The possibility of ‘HF-memory effect’ was cancelled by the use of a set of vessels which had been never contacted with HF. Twenty-four Japanese standard coals (SS coals) were analyzed by the present method, and the concentrations of major metals measured by the present method provided very high accordance with those from the authentic JIS (Japanese Industrial Standard) method.     

Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography II. Method performance study with a hydroxide eluent and a low noise suppressor

The two-dimensional ion exclusion chromatography/ion chromatography (ICE-IC) approach is considered to be the method of choice for the determination of trace anions in concentrated hydrofluoric acid (48-50%, w/w). In order to achieve lower detection limits, this method was for the first time used with electrolytically generated and purified hydroxide eluents in combination with a low noise electrochemical suppressor. Compared to carbonate based eluents, the achieved gain in peak height sensitivity for chloride, sulfate, nitrate and phosphate is a factor of 6, 7, 16 and 13, respectively. The instrumental detection limits, based on the background noise, are 2, 0.2, 0.4 and 1.4 microg/kg HF 50% (w/w) for the same anions. Their method detection limits, calculated according to SEMI, are all within the 6-10microg/kg HF 50% (w/w) range and thus at least 10 times lower than the current Tier C grade requirements. The chromatographic run time could be shortened with some 10 min by the use of a relatively fast high-capacity hydroxide selective anion exchange column.     

New Possible Applications of Heavy Main-Group Elements in Organic Synthesis

Aside from elements of the 2nd row, and one element of the 3rd row of the periodic system—Si, P, S, and Se, respectively, whose organoelement groups such as Me₃Si and Ph₃P^⊕ have proven useful in numerous organic syntheses—other elements of the 3rd as well as 4th and 5th row (Ge, As, Sn, Sb, Te, Pb, Bi) can also be used as components of synthetically useful organoelement groups, the elements As, Sn, and Pb, in particular, offering certain advntages over the others. Some of these organoelement groups are suitable equivalents for Li- or halogen-substituents attached to carbon; they stabilize carbanionic centers (minimum of this effect at the 3rd-row elements), and owing to their suitability as leaving groups in β-eliminations, also open up interesting synthetic possibilities. The thermally unduced syn- and silica-gel induced anti-elimination of Ph₃Sn, Ph₂Sb, Ph₃Pb, together with β-OH, are novel. With the newly synthesized compounds Ph_nEl—Ch₂—Li (El = Sn, Pb, As, Sb, Bi) and other α- and β-lithiated R_nEl- and Ph₂As(O)-reagents such organoelement groups can be introduced into organic compounds and exploited in organic and organoelement synthesis.     

Cathodic stripping voltammetry of trace Mn(II) at carbon film electrodes

A sensitive voltammetric method is presented for the determination of tract levels of Mn (II) using carbon film electrodes fabricated from carbon resistors of 2 Ω. Determination of manganese was made by square wave cathodic stripping voltammetry (CSV), with deposition of manganese as manganese dioxide. Chronoamperometric experiments were made to study MnO₂ nucleation and growth. As a result, it was found to be necessary to perform electrode conditioning at a more positive potential to initiate MnO₂ nucleation. Under optimised conditions the detection limit obtained was 4 nM and the relative standard deviation for eight measurements of 0.22 nM was 5.3%. Interferences from various metal ions on the response CSV of Mn(II) were investigated, namely Cd(II), Ni(II), Cu(II), Cr(VI), Pb(II), Zn(II) and Fe(II). Application to environmental samples was demonstrated.     

东太平洋深海锰结核的化学元素研究

用ICP-AES法测定了东太平洋深海锰结核样品中二十多种主，次及微量元素，结果表明，表面瘤状和表面光滑两种类型锰结核的化学元素含量有较明显的区别，如表面光滑的锰结核TiO2含较高，而表面瘤状的锰结核Mn/Fe之值较高等。     

Chemical separation and inductively coupled plasma–atomic emission spectrometric determination of seventeen trace metals in thorium oxide matrix using a novel extractant – Cyanex-923

Comprehensive studies have been carried out on the extraction behaviour of thorium matrix vis-a-vis 17 trace metallic elements using a novel extractant viz. Cyanex-923. The near total extraction of thorium and quantitative separation of these metals has been established using inductively coupled argon plasma–atomic emission spectrometry (ICP–AES). The recovery of few representative elements has been confirmed by radio-active tracer studies. The studies carried out here have enabled determination of μg/l amounts of all analyte elements with a precision of better than 1% RSD with prior chemical separation from as low as 1 g thorium sample in just five chemical extractions.     

交联聚异丁烯酸甲酯型负载树脂的孔结构与分离稀土性能的关系

本文报导异丁烯酸甲酯型负载树脂的交联度、致孔剂组成和含量对负载树脂孔结构的影响.结果指出,良溶剂和劣溶剂按一定比例混合作为致孔剂,可制备不同孔结构的树脂.致孔剂量增加,树脂表观比重减小,而比表面积、孔体积与平均孔径均增加.交联度从10％增加到35%,表观比重和比表面积增加,而孔体积与平均孔径减小.增加致孔剂所含良溶剂的比例,树脂的表观比重、比表面积增加,而孔体积与平均孔径减小.已制备一系列不同孔结构的2-乙己基膦酸单2-乙己基酯(P507)负载树脂,比较了它们分离La、Ce、Pr、Nd的性能.结果表明,适当孔结构的负载树脂用于萃取色层分离稀土元素具有优良的分离性能.     

二苯并-18-冠-6-甲醛聚合物柱色谱分离富集化学发光法测定痕量金

研究了用一种新的高分子冠醚聚合物(二苯并-18-冠-6-甲醛聚合物)作为色谱柱的固定相，分离富集痕量金，再用化学发光法进行测定；在盐酸介质中，高分子冠醚对金的吸附率可达100％，吸附的金可被硫脲完全解吸，吸附容量为19.40mg/g；化学发光法测定操作简便，效果令人满意；研究结果表明：把高分子冠醚聚合物作为分离富集手段与具有高灵敏度的化学发光法结合进行痕量分析是一种很有前途的方法。     

急性脑血管病患者血清元素的测定

采用高频等离子体发射光谱法测定了３４例脑梗塞、３３例脑出血和对照组２７人血清锌、铜、锰、铬、镁、钼、锶、铁、钛、钡、镉和钙共１２种元素的含量。结果显示脑梗塞和脑出血组血清锌和锌／铜比值显著高于对照组；锰和钼含量仅在脑梗塞组明显增高，锶仅在脑出血组显著增高，而其它几种元素疾病组与对照组无显著性差异。伴有高血糖、高血脂和高血压的病人，其血铬含量显著降低，表明锌、锌／铜比值、锰、钼、锶、铬元素与急性脑血     

慢性支气管炎急性发作期病人血中微量元素的变化分析

为观察慢性支气管炎急性女作期血液中微量元素的变化，对１０１例慢性支气管炎急性发作期病人和３０例正常人全血中锌、铁、铜及钙进行检测。结果显示：慢性支气管炎急性发作期病人锌、铁、铜和钙４种元素均明显于正常人。提示患者血中微量元素总量减少，可能是慢性支气官炎易反复感染、加剧病变发展的原因之一。认为合理补充缺乏的微量元素，有助于疾病的防治。