微波消解-ICP-AES法测定玉米芯中的微量元素含量

采用微波消解处理样品,以电感耦合等离子体发射光谱法(ICP-AES)测定了我国北京、山东、吉林、云南、新疆、甘肃、山西、陕西、江苏、内蒙十个省区玉米芯中Zn,Mg,Mn,Sr,Fe,Pb,Cu和Se八种元素的含量。加入1.5 mL 68%的HNO₃以及0.5 mL HF作为消解剂,在400 W微波功率下3步即可完全将样品消解。测定上述八种元素的相对偏差及回收率分别为: 0.72%～4.16%,95.5%～104.5%;1.58%～3.66%,98.2%～103.5%;0.19%～4.58%,97.0%～103.2%;1.31%～4.90%,95.7%～104.1%;1.40%～4.01%,95.9%～104.6%;1.55%～4.28%,95.1%～104.5%;2.16%～5.00%,96.4%～103.5%;2.00%～4.99%,95.1%～101.3%。方法快速、简便、灵敏度高、准确性好,可多元素同时测定,且无损失和环境污染小。     

X射线荧光光谱法测定混合稀土氧化物中稀土分量

建立了X射线荧光光谱法测试稀土氧化物中稀土分量的方法,讨论了样品制作方法,提出用聚四氟乙烯制作样品底座,分析试液1 mL滴入样品底座的吸附滤纸上,烘箱或红外灯下烘干,6 μm聚脂薄膜扣住测量,样品底座不吸附试样,吸附滤纸的位置及平整性由于内标的补偿不影响分析结果的准确性,初步探讨了薄试样的基体效应,测试的稀土含量范围为:La2O3 0.01%～50%,CeO2 0.01%～15%,Pr6O11 0.01%～12.5%,Nd2O3 0.01%～40%,Sm2O3 0.01%～40%,Eu2O3 0.01%～10%,Gd2O3 0.03%～40%,Tb4O70.01%～5%,Dy2O3 0.05%～10%,Ho2O3 0.01%～4.5%,Er2O3 0.01%～8%,Tm2O3 0.01%～2%,Yb2O3 0.01%～8%,Lu2O3 0.01%～1.5%,Y2O3 0.5%～80%,测试结果与外检吻合.方法易于操作,重现性好,适应范围广,测试了大量其他物料成分,可满足定量分析要求,已作为常规分析手段.     

离子色谱-脉冲安培检测器分析饮料中单糖和二糖

建立了等度离子色谱-脉冲安培检测分析饮料中葡萄糖、果糖、蔗糖和乳糖的方法。采用CarboPacPA10分离柱对分离条件进行了优化,确定柱温为30℃、淋洗液为52mmol.L-1的NaOH溶液,在0.10—20.0mg.L-1范围内葡萄糖、果糖、蔗糖、乳糖呈良好线性,回收率分别为93.3%—112.5%、102.2%—111.6%、96.8%—99.6%、88.0%—102.6%,检出限分别为0.8、4.0、5.0、10.0mg.kg-1,精密度分别为0.18%—1.21%、0.53%—3.76%、0.65%—2.54%、1.65%—5.11%。检测了饮料中的单糖和二糖,效果良好。     

激光拉曼光谱内标法测定葡萄糖液浓度

利用葡萄糖溶液的激光拉曼光谱中的特征峰—CCO(1 125 cm-1),以本底溶液水为内标物,组成相对强度,对葡萄糖溶液含量进行了测定研究,其线性范围为0～1.8 mol·L-1,检出限为0.022 7 mol·L-1,共存的KCl和NaCl不引起干扰,用于葡萄糖氯化钠注射液的测定获得了成功。经测定某市售标识量为葡萄糖氯化钠注射液、5%葡萄糖和10%葡萄糖注射液实测平均浓度分别为4.91%,4.93%和9.92%,其回收率分别在71.88%～126.31%,81.02%～124.89%和74.87%～121.32%之间,RSD为5.44%,4.34%和0.94%。该方法具有测定简单、操作方便,无需添加其他任何化学试剂,是一种绿色分析测定方法。     

发射光谱法同时测定钛基复合材料中的镍铁钼锰和硼的研究

研究了用碳粉、碳酸钙、氧化铜和氧化铍作缓冲剂同时测定钛基复合材料中的镍、铁、钼、锰和硼的发射光谱法,选择铍作内标线,不需分离、不需化学处理,直接压样于杯形的石墨电极中,具有简便、快速、准确。对测定条件、干扰因素进行了研究,从而建立测定镍、铁、钼、锰和硼的新方法。镍、铁、钼、锰和硼的分析线分别为300.36,248.33,315.82,260.57和249.68 nm,内标线选择为铍的298.61 nm,镍、铁、钼、锰和硼的线性范围分别为0.003%～0.30%;0.001%～0.20%;0.003%～0.30%;0.001%～0.20%;0.001%～0.20%。镍、铁、钼、锰和硼的检测限分别0.003%,0.001%,0.003%,0.001%,0.001%,其回收率在95.80%～104.8%范围内,当n=9时,相对标准偏差RSD均小于5%。用于样品的测定取得了满意的结果。     

ICP-AES测定海绵镉中的镉和锌

介绍了ICP-AES加标回收和校准曲线法测定海绵镉中Cd（30%—70%）锌（10%—30%）,线性相关系数0.99999—0.99997,加标回收率94.08%—99.59%之间,RSD在0.12%—1.13%之间。     

磁化溶液样品对ICP发射光谱的增敏效应

利用磁感应强度为0.24T的磁场处理含乙醇的水溶液,研究了样品溶液的物理性质和雾化特性以及样品溶液中元素的谱线强度随磁化时间的变化情况,并且讨论了磁化机理。实验结果表明,随着磁处理时间的延长,分析样品的有效利用率提高了;当样品中加入乙醇时,元素的谱线强度较早地出现了峰值。在磁化时间为2 h的条件下,不含乙醇的样品溶液中,元素Zn, Pb, Cd, Fe, Si, Cu, Cr和Sr的谱线强度比溶液未磁化时分别提高了22.9%, 38.8%, 25.6%, 48.3%, 52.4%, 6.0%, 22.3%和22.7%;含6%乙醇的样品溶液中,元素Zn, Pb, Cd, Fe, Si, Cu, Cr和Sr的谱线强度比溶液未磁化时分别增加了22.4%, 42.6%, 39.4%, 43.9%, 72.4%, 9.7%, 16.1%和17.1%。样品溶液磁化后进行分析, 有利于降低光谱分析检出限。     

ICP-AES测定高含量锌、镉和铜

采用ICP-AES测定高含量锌、镉和铜,选择了最佳仪器工作条件和样品处理方法。在实验优选条件下,对铜镉渣中铜的含量为8%—12%;镉的含量为35%—38%;锌的含量为21%—23%进行了测定。回收率分别为铜99.8%—100.0%,镉98.3%—99.9%,锌99.3%—99.5%。     

变风量客车空调系统性能实验研究

针对纯电动客车热泵空调系统制冷与制热性能衰减严重、耗能较高等问题,设计并搭建了一款基于R410A纯电动客车热泵空调系统实验台。该实验研究了变车外风机风量对热泵系统性能的影响。实验结果表明:低压补气制冷工况下:车内风量为100%,车外风量从40%增加到100%时,系统制冷量增加1.45%,COP_1上升12.7%,COP_2下降19.4%,压缩机功率下降11.1%,排气温度降低11%。制热工况下,系统制热量增加3.2%,COP_1上升8.5%,COP_2下降27.7%,压缩机功率下降29.5%,车内出风温度降低0.7%。     

原子吸收光谱法测定水泥中的钠、钾、镁和铁

对火焰原子吸收光谱法测定水泥中的钠、钾、镁和铁的方法进行研究。在选定的最佳仪器条件下,测定钠、钾、镁和铁的RSD分别为1.81%、1.05%、2.68%、1.12%。水泥样品中钠、钾、镁和铁的回收率分别为102.0%—104.0%、98.4%—100.4、98.0%—102.0%、98.0%—100.3%。方法操作简单,测试快速,结果准确稳定。     

紫外分光光度法测定岩盐中的硝酸盐

沸水溶解岩盐样品,过滤除去水不溶物,紫外分光光度法分别测定滤液在220nm和275nm处的吸光度值,计算出样品中NO3-含量。结果表明,3种不同类型岩盐样品中NO-3的回收率为98.0%—102.0%,相对标准偏差为1.03%—2.92%（RSD,n=5）。与百里酚分光广度法和离子色谱法相比,紫外分光光度法简单快速,准确度、灵敏度、精密度高,适用于岩盐样品中硝酸盐含量的快速检测。     

ICP-AES测定岩盐中钾、钠、钙和镁的含量

用ICP-AES测定岩盐中钾、钠、钙和镁的含量,操作简便、快速,可同时测定多元素,结果准确。精密度小于2.11%,回收率为97.2%—102.0%,满足规范要求。     

离子浓度及表面结构对岩石孔隙内水流动特性的影响

酸性环境引发的岩石孔隙表面溶解增加了孔隙内水溶液的盐离子浓度,破坏了孔隙的表面结构.本文采用分子动力学模拟的方法研究了纳米级岩石孔隙内水溶液的流动特性,分析了盐离子浓度和孔隙表面结构对水流速度分布的影响及原因.研究结果表明:纳米级岩石孔隙内的水溶液流动符合泊肃叶流动特性,流速呈"抛物线"分布;随盐离子浓度增加,水溶液内部氢键网络变得更为致密,水黏度随其呈线性增长;水溶液中离子浓度越大,孔隙表面对水流动的阻力越大,最大流速越小,速度分布的"抛物线"曲率半径越大;岩石孔隙表面结构的破坏改变了流动表面的粗糙程度,增加了孔隙表面对H2O分子的吸引力.随表面结构破坏程度的增大,水溶液在近壁区域的密度增大,流速降低;当表面破坏程度达到50%时,水溶液在近壁区域出现了明显的负边界滑移现象.     

The electrical transportation and carrier behavior of ZnSe under high pressure

With in situ electrical resistivity and Hall effect measurement, electrical transportation property and charge carrier behavior of ZnSe were investigated under high pressure using a diamond anvil cell (DAC). The electrical resistivity changed discontinuously at 7.7 and 11.9?GPa, corresponding to the phase transitions of ZnSe. In the pressure interval of 7.7–11.9?GPa, the electrical resistivity changed continuously, indicating the existence of the intermediate phase between the zinc blende and rock salt phases. The difference of carrier characteristic between the intermediate and rock salt phases can also suggest the existence of the intermediate phase. For the intermediate phase, the increase in electrical resistivity is from the decrease in mobility. While for the rock salt phase, the increase in charge carrier concentration leads to the decrease in electrical resistivity.     

GaN结构相变、电子结构和光学性质

运用第一性原理平面波赝势和广义梯度近似方法,对纤锌矿结构和氯化钠结构GaN的状态方程及其在高压下的相变进行计算研究,分析相变点附近的电子态密度、能带结构和光学性质的变化机制.通过状态方程和焓相等原理得到GaN从纤锌矿到氯化钠结构的相变压强分别为43.9 Gpa和46.0 Gpa;在相变的过程中,GaN由典型的直接带隙半导体转变为间接带隙半导体材料;氯化钠结构GaN相比于纤锌矿结构,介电函数主峰值增强,本征吸收边明显往高能方向移动,氯化钠结构GaN在低能区域的光学性质差于纤锌矿结构.     

New insights into the melting behavior of MgO from molecular dynamics simulations: the importance of premelting effects

We provide a plausible resolution of a long-standing controversy relevant to the geophysics community, namely, that the experimental slope of the melting curve Tm(P) of MgO at low pressures is about 3 times smaller than that obtained from computer simulation of the melting of the normal rock-salt-structured crystal. With increasing temperature at zero pressure, our simulations predict a solid-solid phase transition (from a rock salt to a wurtzite crystalline lattice) to occur just before melting. The coexistence of wurtzite and liquid phases at low pressures is found to be described by a Clapeyron slope which is in much better agreement with the experimental results of Zerr and Boehler [Nature (London) 371, 506 (1994)] than the calculated melting line for the rock salt structure. We also show that the existence of a certain concentration of lattice defects in the rock salt phase cannot provide an alternative explanation.     

Salt neutrino detector for ultrahigh-energy neutrinos

Rock salt and limestone are studied to determine their suitability for use as a radio-wave transmission medium in an ultrahigh energy (UHE) cosmic neutrino detector. A sensible radio wave would be emitted by the coherent Cherenkov radiation from negative excess charges inside an electromagnetic shower upon interaction of a UHE neutrino in a high-density medium (Askar’yan effect). If the attenuation length for the radio wave in the material is large, a relatively small number of radio-wave sensors could detect the interaction occurring in the massive material. We measured the complex permittivity of the rock salt and limestone by the perturbed cavity resonator method at 9.4 and 1 GHz to good precision. We obtained new results of measurements at the frequency at 1.0 GHz. The measured value of the radio-wave attenuation length of synthetic rock salt samples is 1080 m. The samples from the Hockley salt mine in the United States show attenuation length of 180 m at 1 GHz, and then we estimate it by extrapolation to be as long as 900 m at 200 MHz. The results show that there is a possibility of utilizing natural massive deposits of rock salt for a UHE neutrino detector. A salt neutrino detector with a size of 2×2×2 km would detect 10 UHE neutrino/yr generated through the GZK process.     

东营凹陷岩盐原生流体包裹体中子矿物类型的拉曼光谱分析及其地质意义探讨

准确鉴定赋存于流体包裹体中的子矿物对于揭示沉积、成岩和成矿等地质过程中相关流体的地球化学信息具有重要的意义。而应用显微激光拉曼光谱技术分析子矿物的类型具有原位无损、灵敏度高、稳定性好以及简便快捷等优势,目前已得到了广泛地应用。利用显微激光拉曼光谱技术,首次对东营凹陷始新统沙四下亚段岩盐原生流体包裹体中子矿物的类型进行了准确地鉴定,并在此基础上,详细地探讨了子矿物对东营凹陷始新世盐湖古卤水地球化学特征的指示意义。研究结果显示： 东营凹陷沙四下亚段岩盐原生流体包裹体中普遍发育有硬石膏(CaSO₄)和四水泻盐(MgSO₄·4H₂O)两类子矿物。其中,硬石膏子晶以1 018 cm-1的拉曼特征峰强度最大,同时还存在其它5个附属拉曼特征峰,依次为500,611,629,676和1 131 cm-1;而四水泻盐子晶以1 000 cm-1的拉曼特征峰强度最大,并且还存在其他三个附属拉曼特征峰,分别为462,618和1 156 cm-1。这两类子矿物的存在表明岩盐的原始析盐母液中含有少量的CaSO₄和MgSO₄成分,且此时正值盐湖古卤水的早期蒸发析盐阶段,即： 硫酸盐析出阶段的结束与氯化物盐析出早期阶段的开始,以析出石盐为主。此外,结合硬石膏和四水泻盐的沉淀温度,明确了东营凹陷始新世盐湖在早期蒸发析盐阶段时期,古卤水的温度介于37~61 ℃之间,表现为干旱的沉积环境。     

Stability,structural, elastic and electronic properties of RuN polymorphs from first-principles calculations

First-principles FLAPW–GGA calculations for six possible polymorphs of ruthenium mononitride RuN indicate that the most stable structure is that of zinc blende rather than the rock salt structure recently reported for synthesized RuN samples. The elastic, electronic properties and the features of chemical bonds of zinc-blende RuN polymorph were investigated and discussed in detail.     

Recent studies on radiation induced F-center and colloid particle formation in synthetic NaCI and natural rock salt

Radiation induced F-center and Na metal colloid formation have been studied, at temperatures between 100 and 350°C, in melt growth synthetic NaCl crystals and natural rock salt samples, using equipment for making optical measurements during 1–3 MeV electron irradiation. In both types of NaCl the damage formation kinetics are qualitatively similar. However, there are large quantitative differences which depend on irradiation temperature, dose rate, total dose, inherent strain, strain applied prior to irradiation and other factors. Natural rock salt samples from different localities exhibit markedly different radiation induced colloid formation rates. An extrapolation of the current data to the doses expected in radioactive waste depositories indicate that natural salt immediately adjacent to the planned waste canisters could develop between 0.1 and 50 percent colloidal sodium in 50 to 400 years.