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。     

The mitigation of the vibration effects caused by tunnel blasts in urban areas: a case study in Istanbul

Ground vibrations generated by commercial explosives in tunnel construction may cause structural damage in urban areas. Therefore, suppressing the vibration effects and mitigating the possible hazard after blasting is important. We present a new method of controlled blasting that is environmentally friendly, and easy to utilize for tunnel construction. Small charges in this method are detonated sequentially to produce minimum side effects. The efficiency of the charges may be increased based on the previously monitored shots. This method is utilized in a tunnel construction in Istanbul with five experimental shots. In these experiments, the duration and also the quantity of explosives were carefully controlled. We were able to obtain better results with short durations (480 ms) instead of long durations (9,000 ms) although the vibration levels defined as peak particle velocity (PPV) became bigger while the quantity of the explosive charge increased from 3.088 to 9.264 kg.     

土壤聚合物对几种重金属离子固化效果的研究

土壤聚合物是一种新型的无机聚合物,其分子链由Si、O、Al等以共价键或离子键连接而成,形成网络结构,对重金属有较强的固定作用.本文试图利用土壤聚合物固化铜、锌、铅三种重金属离子,实现资源化利用.实验以固化体抗压强度和浸出毒性作为性能表征量,结果表明:土壤聚合物对不同重金属的固化有各自的极限浓度,Cu2 、Zn2 、Pb2 的理想固化量分别为0.9%、1%、2%;若固化过程中添加一定量的高炉矿渣,则可以提高固化体的抗压强度.本文通过土壤聚合物固化体SEM分析,从固化体微观结构的形态来阐述土壤聚合物宏观上的优越表现.     

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。     

转炉钢渣对两种对虾幼虾的急性毒性效应

初步研究了一定粒径的转炉钢渣对日本对虾（Penaeus japonicus）幼虾和中国明对虾（fenneropenaeus chinensis）幼虾的急性毒性效应。实验结果显示，当钢渣质量浓度为1.8g／L时，日本对虾幼虾96h的最高死亡率为33．33％；随着钢渣质量浓度的增加，死亡率增高；当钢渣质量浓度为18g／L时，其96h的最大死亡率达到了75％。相对于日本对虾幼虾，钢渣质量浓度为18g／L时中国明对虾幼虾96h的最高死亡率只有36．67％。运用直线内插法求出钢渣对日本对虾幼虾96h半致死浓度为1．62g／L，钢渣对日本对虾的安全浓度为0．162g／L，而在实验条件下中国明对虾幼虾的半致死浓度要明显高于日本对虾幼虾。     

Timing effects on the fragmentation of small scale blocks of granodiorite

A series of small scale tests, simulating multi-hole blasts have been performed to establish the effect of delays on blast fragmentation. The blasts were performed in high quality granodiorite blocks, which were cut from stone prepared by dimensional stone quarry operations. The pattern used was equilateral triangular, with a distance of 10.2 cm between boreholes, which had a diameter of 11 mm, were loaded with detonating cord and the coupling medium was water. The delays used were achieved using different lengths of detonating cord for the cases of delays between 0 and 100 μs between holes and a sequential blasting machine firing seismic detonators for larger delays up to 4 ms. All fragments were collected and screened. The experiments showed that the worst fragmentation was achieved with simultaneous initiation of all charges. Fragmentation improved with the delay time between holes up to 1 ms between holes. If the experiments are scaled up, the results show that in granodiorite, fragmentation optimization requires delays of few milliseconds per metre of burden. The findings, agree with previously published work, involving larger scale experiments and other rock types.     

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％。     

悬浮液进样—石墨炉原子吸收测定钒钛磁铁矿中痕量镓

研究了悬浮液进样＿石墨炉原子吸收测定钒钛磁铁矿中痕量镓的分析方法。以Ｎｉ（Ⅱ）作为基体改进剂时，可直接用镓标准溶液进行校准。样品粒度＜３８μｍ、悬浮液中试样质量浓度在０１～８０ｇ／Ｌ、含镓质量浓度不超过１００μｇ／Ｌ时呈良好线性关系，检出限为２４μｇ／Ｌ镓。用所拟方法测定了含镓量在１６～４２μｇ／ｇ的标准矿样，结果与标准值相符，６次平行测定的相对标准偏差不超过９％，满足痕量分析的要求。     

涂钨热解石墨管－石墨炉原子吸收法测定天然水中痕量钡

选择涂钨热解石墨管测钡，克服了钡的碳化物形成而提高了方法的灵敏度，采用钙做基体补偿不仅克服钙对测钡的影响，同时也对测钡起增敏作用，结合其它测定条件的优化实现了石墨炉原子吸收法测定天然水中的痕量钡。其线性范围在０～７０μｇ／Ｌ检出限３．３ｐｇ，特征质量为２．９ｐｇ／１％吸收，对５μｇ／ＬＢａ试液测定１１次，其ＲＳＤ为６．９％，加标回收率８９％～１２０％。方法经标样分析验证，结果与标准值相符。