深孔预裂爆破技术在低透气性回采工作面中的试验研究

为解决低透气性回采工作面采煤过程中,瓦斯抽采困难、施工周期长等问题,提出了利用深孔预裂爆破技术,增加煤层裂隙,提高煤层透气性的方法,并研究了深孔预裂爆破技术的作用机理,阐述了深孔预裂爆破技术的工艺流程,对增透效果进行了现场考察.研究表明:深孔预裂爆破后与爆破前相比,平均瓦斯抽采量提高了2.32倍,平均煤层透气性系数提高了5.6倍,最大提高了11.5倍,有效提高了瓦斯抽采率;工作面回采周期大幅度缩短,为安全、快速回采提供了保障.     

胃肠模拟体外法的生理参数对室内灰尘中邻苯二甲酸酯与磷系阻燃剂的生物有效性的影响

室内灰尘吞食暴露是邻苯二甲酸酯与磷系阻燃剂的主要暴露途径,测定室内灰尘中该类有机污染物的生物有效性对其暴露风险评价至关重要.本研究选择胃肠模拟体外方法-生理原理提取法(PBET)法测定室内灰尘中邻苯二甲酸二正丁酯(Dibutyl phthalate,DBP)、邻苯二甲酸丁基苄基酯(Butyl benzyl phthalate,BBP)、邻苯二甲酸二(2-乙基己基)酯(Di(2-ethylhexyl)phthalate,DEHP)和三(2-氯乙基)磷酸酯(Tris(2-chloroethyl)phosphate,TCEP)的生物有效性.研究了PBET法中胆盐含量、模拟肠液p H值、液固比及同时摄入奶粉等生理参数对生物有效性的影响.结果表明,4种有机污染物的生物有效性从1.5%(DEHP)到52%(TCEP),随污染物辛醇水分配系数的增加而降低.随着模拟液胆盐含量增加,DBP、BBP与DEHP的生物有效性逐渐增加,并在10 g·L~(-1)附近达到最大值后趋于平稳.TCEP由于其较好的水溶性,生物有效性并未随着胆盐含量的增加而明显变化.奶粉含量的增加则显著增加了DBP、BBP、DEHP和TCEP的生物有效性,在10 g·L~(-1)附近达到最大值后普遍呈现下降趋势.随着液固比的增加,DBP和DEHP的生物有效性显著提升,然而BBP与TCEP的生物有效性却未发生明显改变.在p H 6~8范围内,均未对4种有机物的生物有效性产生显著影响.     

炼油厂碱渣废水络合萃取法脱酚实验研究

实验选用磷酸三丁酯(TBP)-煤油溶液为萃取剂络合萃取碱渣废水中的酚,研究了不同萃取剂浓度、pH值、温度及萃取比条件下体系的萃取性能;采取NaOH溶液对萃取剂进行反萃再生,研究了碱液浓度、温度及反萃取比对萃取剂再生效果的影响;确定了萃取与反萃取的最佳操作条件。实验结果表明,TBP-煤油溶液可以有效脱除碱渣废水中的高浓度酚,是一种良好的工业萃取脱酚剂。     

Apparent diffusion coefficients and chemical species of neptunium (V) in compacted Na-montmorillonite

Diffusion of neptunium (V) in compacted Na-montmorillonite was studied through the non-steady state diffusion method. In this study, two experimental attempts were carried out to understand the diffusion mechanism of neptunium. One was to establish the diffusion activation energy, which was then used to determine the diffusion process in the montmorillonite. The other was the measurement of the distribution of neptunium in the montmorillonite by a sequential batch extraction. The apparent diffusion coefficients of neptunium in the montmorillonite at a dry density of 1.0 Mg m-3 were from 3.7 x 10(-12) m2 s-1 at 288 K to 9.2 x 10(-12) m2 s-1 at 323 K. At a dry density of 1.6 Mg m-3, the apparent diffusion coefficients ranged between 1.5 x 10(-13) m2 s-1 at 288 K and 8.7 x 10(-13) m2 s-1 at 323 K. The activation energy for the diffusion of neptunium at a dry density of 1.0 Mg m-3 was 17.5 +/- 1.9 kJ mol-1. This value is similar to those reported for diffusion of other ions in free water, e.g., 18.4 and 17.4 kJ mol-1 for Na+ and Cl-, respectively. At a dry density of 1.6 Mg.m-3, the activation energy was 39.8 +/- 1.9 kJ mol-1. The change in the activation energy suggests that the diffusion process changes depending on the dry density of the compacted montmorillonite. A characteristic distribution profile was obtained by the sequential extraction procedure for neptunium diffused in compacted montmorillonite. The estimated fraction of neptunium in the pore water was between 3% and 11% at a dry density of 1.6 Mg m-3 and at a temperature of 313 K. The major fraction of the neptunium in the montmorillonite was identified as neptunyl ions sorbed on the outer surface of the montmorillonite. These findings suggested that the activation energy for diffusion and the distribution profile of the involved nuclides could become powerful parameters in understanding the diffusion mechanism.     

烧结法提取沸腾炉渣中的铝和铁

近年来,热电厂和钢厂产生了大量的沸腾炉渣.这些炉渣不仅占用了大量的土地,还污染了土壤、地下水和大气.由于该沸腾炉渣中氧化铝的含量很高,因此,评估其氧化铝提取的可利用性是必要的.本文对内蒙古包头钢铁厂的沸腾炉渣进行了粒径分布试验和化学成分分析试验.X-荧光分析显示,该炉渣中SiO2含量为42.60%,Al2O3含量为32.60%,Fe2O3含量为2.43%,CaO含量为2.16%,K2O含量为0.74%,MgO含量为0.44%,Na2O含量为0.16%,TiO2含量为0.88%,还有一些其他痕量元素.将沸腾炉渣和石灰及精煤混合制成小球,然后在约1 000 ℃下烧结.取不同烧结时间的样品,用硫酸浸取,得到含铝离子和铁离子的溶液.试验结果表明,使用浓度为4 mol·L-1的硫酸,在80 ℃下浸取烧结球样品(质量比为50%沸腾炉渣:40%精煤:10%石灰),24 h可以得到铝和铁的最大提取率,分别为86.50%和94.60%.滤渣可以作为固化材料用于高速公路的路基建设或水泥生产中的添加剂.     

蜂蜜中氯霉素残留的检测及净化方法研究

建立了反相高效液相色谱-离子阱质谱法检测蜂蜜中氯霉素残留的方法.前处理采用改良的QuEChERS方法进行快速提取和净化.采用初级次级胺进行固相分散净化,可有效吸附蜂蜜中的糖类及有机色素等杂质.提取物在流动相甲醇:水(0.2%乙酸胺)=45:55(体积比)中,用整体色谱柱进行快速分离和质谱检测.并对MS检测中2种离子化方式(电喷雾ESI及大气压化学APCI)、各种离子化方式下正负离子模式及离子检测方法(总离子检测TIC和选择性离子监测MRM)进行了综合比较,最终确定采用电喷雾电离法(ESI)负离子模式、多反应离子监测(MRM)对氯霉素进行定性定量分析.在0.2～200μg/kgg添加浓度下,添加回收率水平在78%～93%间,变异系数在3.9%以下.该方法的检出限为0.1μg/kg,在0.1～100 μg/L浓度范围内,线性方程为y=58.753x 34867,相关系数R2=0.999 5.     

水中三嗪类除草剂的检测与分析质量控制

三嗪类除草剂作为预防农田杂草生长的除草剂在世界范围内广泛使用.由于水中农药残留浓度属痕量级,建立高效富集与分析方法非常重要.选取了6种三嗪类物质,建立了对水中痕量三嗪类物质的SPE-HPLC分析方法,并对其分析方法进行了质量保证与质量控制QA/QC研究.研究结果表明: 6种三嗪类物质的回收率在94%～116%之间,方法检测限在0.08～0.18 μg·L-1之间,方法重复性和检测限均能满足痕量分析及其质量控制的要求.3种水样的实际测试结果表明,在某河水中测得莠去津和扑草净的质量浓度分别为(5.28±0.43) μg·L-1和(7.12±0.54) μg·L-1.这说明该水体三嗪类农药的污染需受到重视.     

Determination of trichloroacetic acid in environmental studies using carbon 14 and chlorine 36

Radioisotopes carbon 14 and chlorine 36 were used to elucidate the environmental role of trichloroacetic acid (TCA) formerly taken to be a herbicide and a secondary air pollutant with phytotoxic effects. However, use of ¹⁴C-labeling posed again known analytical problems, especially in TCA extraction from the sample matrix. Therefore—after evaluation of available methods—a new procedure using decarboxylation of [1,2-¹⁴C]TCA combined with extraction of the resultant ¹⁴C-chloroform with a non-polar solvent and its subsequent radiometric measurement was developed. The method solves previous difficulties and permits an easy determination of amounts between 0.4 and 20 kBq (10–500 ng g⁻¹) of carrier-less [1,2-¹⁴C]TCA in samples from environmental investigations. The procedure is, however, not suitable for direct [³⁶Cl]TCA determination in chlorination studies with ³⁶Cl. Because TCA might be microbially degraded in soil during extraction and sample storage and its extraction from soil or needles is never complete, the decarboxylation method—i.e. 2 h TCA decomposition to chloroform and CO₂ in aqueous solution or suspension in closed vial at 90 °C and pH 4.6 with subsequent CHCl₃ extraction—is recommended here, estimated V < 7%. Moreover, the influence of pH and temperature on the decarboxylation of TCA in aqueous solution was studied in a broad range and its environmental relevance is shown in the case of TCA decarboxylation in spruce needles which takes place also at ambient temperatures and might amount more than 10–20% after a growing season. A study of TCA distribution in spruce needles after below-ground uptake shows the highest uptake rate into current needles which have, however, a lower TCA content than older needle-year classes, TCA biodegradation in forest soil leads predominatingly to CO₂.     

超临界流体萃取固体物料动力学模型的研究进展(英文)

文章总结与讨论了超临界流体萃取固体物料的动力学模型。这些动力学模型包括经验模型,基于热传递类推的模型以及基于微分质量平衡的模型。所有这些都有助于实现过程的数学模拟放大,有助于投资前的经济预算,有效减小投资风险,也可作为超临界流体萃取过程的研究手段,减少实验探索的工作量。