顶空气相色谱法测定漓江底泥中的三氯乙烯和四氯乙烯

采用Na Cl溶液提取,顶空气相色谱法测定底泥中的三氯乙烯和四氯乙烯,方法在0.098 ng/L~1.03 ng/L范围内线性良好,三氯乙烯和四氯乙烯的方法检出限分别为0.013 ng/g和0.016 ng/g。对空白样品做3个质量比水平的加标回收试验,7次测定结果的RSD为2.0%~3.8%,平均加标回收率为94.0%~109%。将该方法用于桂林市漓江底泥样品的测定,结果三氯乙烯和四氯乙烯均为未检出,实际样品加标回收率为92.0%~107%。     

Novel mesoporous microspheres of Al and Ni doped LMO spinels and their performance as cathodes in secondary lithium ion batteries

A facile, scalable, and solution-based technique is used to fabricate Al and Ni-doped (LiAl_0.1Mn_1.9O₄ and LiAl_0.1Ni_0.1Mn_1.8O₄) microspheres of lithium manganese oxide (LMO) spinels for use as reversible cathode materials for lithium ion batteries (LIBs). The spheres of the two samples exhibit different porosities. Cells with these LMO-based cathodes are then cycled between 4.5 V and 2 V to study their stabilities while simultaneously being subjected to the undesirable Jahn-Teller distortion that occurs around the ~3 V regime. The LiAl_0.1Mn_1.9O₄ (LAMO) and the LiAl_0.1Ni_0.1Mn_1.8O₄ (LANMO) cells exhibit comparable open circuit voltages (OCV) of 2.94 V and 2.97 V, respectively. During cell cycling, the LAMO cell exhibits a maximum specific capacity of 122.51 mAh g^?1 with a capacity fade of 65.35% after 75 cycles. The LiAl_0.1Ni_0.1Mn_1.8O₄ (LAMO) sample fares better and exhibits a maximum of 140.49 mAh g^?1 and a capacity drop of 52.59%. Detailed structural studies indicate that Ni doping and the greater degree of porosity of the LANMO sample to be a stabilizing factor. This is further confirmed by cyclic voltammetry (CV) and AC impedance spectra analysis.     

国产多核处理器芯片TDBI技术研究

随着集成电路的功能越来越复杂,超大规模集成电路的动态老炼越来越成为一项困难的工作。传统针对超大规模集成电路的老炼多采用静态老炼方法,这种方法不能使电路内部的功能节点动作起来,无法保证老炼效果,因此能够实现电路内部所有功能模块全动态激励的TDBI技术越来越受到人们的关注。本文以国产多核处理器芯片为测试对象,为研究多核处理器芯片的TDBI方法进行了芯片老炼测试软硬件系统开发,解决了多核处理器老炼中大功率电源供电、图形存储空间不足等关键技术。     

多氯联苯Aroclor系列的弗罗里硅土小柱淋洗条件

使用商品化弗罗里硅土小柱对废水中的Aroclor进行净化。比较了不同极性洗脱溶剂和洗脱体积下弗罗里硅土小柱的净化效果。采用1 g/6 mL的弗罗里硅土小柱净化时，洗脱液体积大于8.0 mL，洗脱完全，未有目标物质被检出。淋洗溶剂的极性改变，对初始洗脱体积（0~3.0 mL）的洗脱效率会产生一定影响。随着极性的增加，目标物的回收率随之增加，但是共流出的干扰物也随之增加。     

顶空固相微萃取-气相色谱法测定水中氯苯类化合物

采用顶空固相微萃取（HS －SPME）技术萃取水中6种氯苯类化合物，全面分析对目标物萃取效率的影响因素，并确定萃取试验的最佳条件。用顶空固相微萃取联合气相色谱法（HS －SPME －GC）测定水中6种氯苯类化合物，方法在0.500 ng／L～2.00×10^5 ng／L范围内线性良好，检出限为0.05 ng／L ～2000 ng／L，空白样品加标回收率为69.8％～121％， RSD为4.8％～18.3％。用该方法测定实际水样，平行双样的相对偏差低于20％。     

气相色谱-高分辨双聚焦磁质谱测定水中超痕量多氯萘

采用固相萃取法处理水样，气相色谱-高分辨双聚焦磁质谱法测定水中超痕量多氯萘，同位素内标法定量，并对样品前处理条件和仪器条件进行优化。试验表明：方法在0．500 ng/L～500 ng/L范围内线性良好；当取样体积为1 L时，方法检出限为0．005 ng/L～0．01 ng/L；对实际水样进行2个质量浓度水平的加标回收试验，平行测定6次的 RSD为2．7％～8．7％，回收率为70．2％～110％。方法适用性试验表明，水样中复杂的基质对测定无影响。     

Application of the QuEChERS method for the determination of organochlorine pesticide residues in Brazilian fruit pulps by GC-ECD

The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was applied to the extraction of 14 organochlorine pesticides (OCPs) residues from commercial fruit pulps available in supermarkets in Fortaleza, Northeastern Brazil. The analyses were carried out by gas chromatography (GC), coupled to an electron-capture detector (ECD), and were confirmed by GC-tandem mass spectrometry (MS). The parameters of the analytical method, such as accuracy, precision, linear range, limits of detection and quantification, were determined for each pesticide. The results showed good linearity (R² ≥ 0.9916) and the overall average recoveries were considered satisfactory obtaining values between 69 and 110%, RSD of 2–15 %, except for hexachlorobenzene (HCB) in açai, acerola and guava pulp samples. The OCPs were detected in guava (α–HCH; lindane) and soursop (α, β–HCH isomers) samples. The QuEChERS method and GC–ECD were successfully used to analyze OCPs in commercially available Brazilian fruit pulps and can be applied in routine analytical laboratories.     

降水中甲酸、乙酸和草酸的离子色谱法测定及样品保存研究

甲酸、乙酸和草酸是降水中有机酸的主要成分。研究选用离子色谱法同时测定降水中的甲酸、乙酸和草酸,并对降水样品中3种有机酸的保存条件进行了研究。优化后的色谱条件为4. 0 mmol/L Na_2CO_3和1. 2 mmol/L NaHCO_3混合淋洗液,淋洗液流速为1. 0 m L/min,进样体积为200μL,电导池温度为30℃,柱温为室温。甲酸、乙酸和草酸的检出限分别为0. 002、0. 005、0. 005 mg/L,实际降水样品测定时平行样的相对标准偏差为1. 4%～12%,加标回收率为95%～118%。样品采集后需尽快用0. 45μm聚醚砜微孔滤膜过滤,4℃以下冷藏密封保存,2 d内测定。若用氢氧化钠溶液调节p H至8～10,样品可保存7 d。     

顶空-气相色谱法(氮磷检测器)测定固定污染源废气中三甲胺

建立了顶空-气相色谱法测定固定污染源废气中三甲胺的分析方法。弱酸性吸收液采集固定污染源废气中的三甲胺,碱液中和后顶空进样气相色谱仪氮磷检测器分析。并对平衡温度、平衡时间、盐析效应、氨水和氢氧化钠条件实验进行优化,在最佳实验条件下,三甲胺的方法检出限为0. 46μg/m~3(以采集20 L空气样品计),加标回收率为97%～107%,相对标准偏差在9. 26%以下。利用该方法对垃圾焚烧发电厂厂界空气及鱼粉厂有组织废气中三甲胺进行检测分析,该方法能够满足国家标准及上海地方标准中三甲胺排放限值的要求。     

新型硅镁胶(MgO·2SiO_2)对模拟放射性废水中Co~(2+)的吸附性能

以泡花碱和氯化镁为原料合成出了一种新型硅镁胶(MgO·2SiO2)吸附材料,用傅里叶红外光谱仪对其进行了表征,并对模拟放射性废水中的Co2+进行吸附实验。结果表明,控制合成pH在10.50~11.00,可以得到目标硅镁胶(MgO·2SiO2),在460 cm-1处出现了较强的吸收峰,这是由Mg—O伸缩振动和Si—Mg—O弯曲振动引起。在500℃焙烧4h后,可以得到吸附性能良好的硅镁胶,随着溶液pH的升高,去除率增大,在pH为4~8时达到最大。25℃时,最大吸附量可达135.5 mg/g,吸附过程符合Langmuir等温吸附方程和准二级动力学方程。重复使用4次,对Co2+的吸附量仍然达到130 mg/g,说明硅镁胶是一种可重复利用的吸附剂。