雾化进样石墨炉原子吸收光谱法的研究 Ⅰ.直接雾化进样装置及其性能

介绍一种自行设计和加工的直接雾化石墨炉进样装置的结构、工作原理和操作方法。该装置由微机控制与石墨炉加热程序同步工作,可以实现自动控制和自动测量。对雾化进样石墨炉分析的仪器参数和实验条件进行了研究和选择。结果表明,该装置与石墨炉结合具有自动化程度高、重现性好、样品利用率高和分析速度快等特点。     

A numerical investigation of the destruction of peroxy radical by Cu ion catalysed reactions on atmospheric particles

To determine if Cu mediated reactions on atmospheric particles are important to HO₂ chemistry in the ambient atmosphere, Cu molalities were calculated from measured Cu aerosol particle concentrations, mass and number size distribution data from a site in central Sweden. A comparison of characteristic times indicates that at low relative humidities the reaction is limited by the mass transport of gas phase HO₂ to the particle surface and not by the chemical kinetics of the aqueous reaction. Comparison of half-lives for particle reactions and the gas phase destruction of HO₂ to form H₂O₂ indicate that heterogeneous reactions on aerosol particles may have important consequences on the chemistry of HO₂ and H₂O₂ in the troposphere.     

塞曼石墨炉原子吸收法直接测定海水中的铜

本文选择酒石酸消除海水基体对铜信号的干扰,用塞曼石墨炉原子吸收法直接测定海水中的铜。从Cu的原子化曲线可知,加入酒石酸后,背景值减小,Cu原子吸收信号增强,且出现时间提前,表明酒石酸是有效的海水基体改进剂。用P.E.Z3030光谱仪测得双蒸水及海水中的元素Cu的特征质量(m。)分别为12.5pg及12.7pg;检测限分别为0.18μg/L和0.19μg/L,表明基体效应已消除,符合海洋监测要求。可用纯Cu标准溶液作校正曲线,以国家海洋局的两个标准海水样品中的Cu评定本法的准确度,相对偏差为0及-4.6%,与经典的经富集后的FAAS法的结果相比,相对偏差在3.0—6.5％范围内。用不同类型的光谱仪测定了30个海水样品,回收率在89—104％范围内。本法操作简便、快速。     

塞曼石墨炉原子吸收法直接测定海水中的铬

海水基体对Cr有增感作用。本文研究了抗坏血酸、柠檬酸三铵、酒石酸、乙酸铵等有机基体改进剂对消除基体干扰效果。前二者均有效地消除基体干扰,但1％抗坏血酸 1％柠檬酸三铵混合试剂的效果更好,它不仅可以消除基体干扰,还可降低背景及噪声,Cr的吸收峰也较平滑。本法准确,相对偏差在0.7—4.4％范围内。回收率在92—109％范围内。若海水Cr含量低于定量下限时,可采用多次进样法。     

Overbreak and underbreak in underground openings Part 2: causes and implications

Summary The newly developed light sectioning method has been used to investigate some of the causes and costs of overbreak and underbreak. Investigations at the Aquamilpa Hydroelectric Project in Mexico have shown decreased overbreak and increased underbreak as a result of increased rock quality and decreased explosive energy. A new measure of explosive energy, the perimeter powder factor (PPF), has been defined and shown to be useful in the context of tunnel-wall rock damage. Tentative results indicate that explosive energy (PPF) may be a more important factor in producing underbreak, whereas rock quality may be a greater factor in producing overbreak. A site-specific equation is given for predicting overbreak or underbreak as a function of rock quality and explosive energy, with an evaluation of the cost of underbreak and overbreak.     

In situ time resolved synchrotron powder diffraction study of thaumasite

Structural changes during dehydration and subsequent decomposition in thaumasite Ca₃Si(SO₄)(CO₃)(OH)₆·12 H₂O were studied by in situ synchrotron powder diffraction between 303 and 1,098 K. Evolution of the crystal structure was observed through 28 structure refinements, by full profile Rietveld analysis performed in the P6₃ space group, between 300 and 417 K, whereupon the thaumasite structure was observed to breakdown. Within this temperature range, the cell parameters of thaumasite increased as a function of temperature in a nearly linear fashion up to about 393 K, at which temperature, a slight slope change was observed. Above 400 K, the thermogravimetric analysis revealed that the dehydration process proceeded very rapidly while the refined occupancy of water molecules dropped below a critical level, leading to instability in the thaumasite structure. At a same time, a remarkable change in the unit cell parameters occurring at about 417 K indicated that the crystal structure of thaumasite collapsed on losing the crystallization water and it turned amorphous. This result indicated that the dehydration/decomposition of thaumasite was induced by the departure of the crystallization water. At about 950 K, anhydrite and cristobalite crystallized from the thaumasite glass.     

三类高强度悬式瓷绝缘子的成分和物相分析

为探讨高原牌70kN和进口120，210kN瓷绝缘子的成分和结构性能，中采用原子吸收光谱（AAS）和X射线衍射（XRD）方法，对三类产品进行了检测。结果表明，有效成分除K2O外，70kN和210kN的SiO2,Al2O3,Fe2O3含量接近，主晶相基本相同，有刚玉，莫来石、石英和长石等；结晶相总量：70kN35%，120kN40%,210kN48%，这表明机械强度愈大，结晶相含量愈高，只需调整70kN原样的部分成分，粒度和工艺，即生产出高等级（如210kN)瓷绝缘子。     

用双孔热解石墨管原子吸收法测定微量金

石墨炉原子吸收法在对化探样品微量金的测试过程中存在因载气进入而使待测样品溅出的问题。利用自制的双孔热解石墨管代替普通石墨管可解决上述问题。通过大量的实验证明,仪器在最佳工作条件下,硫脲介质浓度10g·l-1、解脱时间40min时,获得检出限0 10×10-9、加标回收率为98 4%～103 7%的分析结果。     

重油凝胶色谱制备样品中痕量镍的分析研究

研究表明微波密闭消解法对重油凝肢色谱制各样品的前处理，不造成易挥发有机金属化合物的损失，对样品无污染。采用消解前定容，配合石墨炉二次进样富集样品，可以测定样品中低至10^—9级的镍。方法应用于镍在渣油中随相对分子质量分布分析中，标准样品对照数据吻合好，相对标准偏差(RSD，n＝11)为8％。     

利用高铁钾长石粉合成13X沸石分子筛的实验研究

对江苏丰县的富钾页岩进行预处理，得到钾长石含量达76．4％的钾长石粉，其Fe2O3含量高达7．52％。以此钾长石粉为原料经过焙烧处理、水热合成实验，在铁含量较高情况下成功合成了13X沸石分子筛，并采用正交实验法确定了优化工艺参数。对实验产物的主要性能测试表明，合成的富铁沸石产品与13X沸石分子筛工业产品相似，吸附量达到国家化学工业产品标准，可用于对含重金属离子废水的吸附处理。