铕浓缩同位素全蒸发-1012Ω高阻信号放大器的热电离质谱分析方法

浓缩同位素是校正质谱法、同位素稀释质谱法和双稀释剂法等同位素质谱分析技术的基础,其化学纯度及丰度量值的准确性直接影响着分析结果的准确性。但由于浓缩同位素中低丰度同位素的离子信号较难准确测量,且缺乏合适的标准物质校正,给高精准的同位素丰度分析带来挑战。本文建立了适用于微量铕浓缩同位素样品纯化的锌还原-萃取色层法,纯化后的151 Eu和153 Eu两种浓缩同位素纯度优于99.99%,有效消除了其他稀土元素杂质的干扰。通过采用1012Ω信号放大器的法拉第杯接收样品中的低丰度同位素离子信号,建立了铕浓缩同位素的全蒸发-热电离分析方法。两种浓缩同位素样品的主丰度测量结果分别为151 Eu 0.9683676(11)和153 Eu 0.9876851(21),测量重复性比1011Ω信号放大器的法拉第杯以及文献中校正质谱法的测量结果提高了3倍。     

挥发性有机化合物标准样品的碳同位素δ13C测定:以甲酸、乙酸为例

密闭石英管燃烧法制备挥发性有机化合物（VOCs）标准同位素样品时,可有效避免制备过程中因挥发所导致的同位素分馏。以市售高纯度的甲酸、乙酸为标准同位素样品,重复制备它们的同位素分析样各5次,并在Finnigan MAT-252气体同位素比值质谱仪上测定其碳同位素δ¹³C。结果显示此法具有极高的重现性,相对标准偏差分别为0.07% (n=5)、0.04% (n=5)。与之对比,另一套同位素测定系统（气相色谱-燃烧炉-同位素比值质谱,GC/C/IRMS）对同一标准物质的同位素测定结果并无显著差别,但在精度上却明显不及前者。密闭石英管燃烧-气体同位素质谱法的测定误差相对较小,可作为VOCs标准同位素样品的δ¹³C分析方法。     

一种新型超高真空电离计

本文提出了一种不同于BA式的轴向式新型超高真空电离计,它具有灵敏度高(37.5托~(-1))、零散性小(<±5%)、结构简单牢固、除气容易、光电流本底达2×10~(-11)托等效氮压强以及稳定性好等特点。其测量范围为5×10~(-4)～2×10~(-10)托;仪器的零点漂移<±1%/24小时;发射电流为0.2及2毫安,稳定度优于±1%;除气功率(电子轰击)<100瓦。     

水冷式积分球功率计

本文介绍了用粗糙面作为漫反射面的水冷式积分球功率计。经标准能量计标定,具有响应时间快(10~(-1)秒)、重复性好(优于1%)、可测激光功率范围大(数瓦—千瓦)等特点。该功率计标定误差小于±5%,测量激光输出时,与国家标准大功率计之差在1%以内。     

精确测定同位素比方法的探讨

本文推导了六个关于精密测定同位素比的双标准方法用的公式。根据这些公式可以设计用双路进样系统的各种测量同位素的方法。测量的结果在标准误差内(σ=5×10~(-5))符合较好。讨论了用双标准方法三路进样测定同位素比较用双标准方法双路进样有更多的优点。     

NG—1型全金属稀有气体纯化和质谱分析系统

本文论述了一种比玻璃纯化系统更具优点的稀有气体金属纯化系统和质谱分析系统,系统的静态真空16小时维持在10~(-7)托内。活性碳管在-195℃下将He、Ne与Ar有效地分离,以便Ne同位素的分析。用自制的金属大小球均匀分装稀释剂。质谱计的分辩能力105(峰高百分之五处),精度±2%。最小可检测限:He为1.3×10~(-5),Ar为8×10~(-5),Ne为9×10~(-5)。测得空气的~(40)Ar/~(36)Ar比值为296.05,~4He/~(40)Ar比值为1.94x10~(-4),~4He/~(20)Ne比值为0.167。该质谱分析系统可用于地质学、地震气体地球化学等的研究。     

气相色谱-燃烧-同位素比值质谱法测定发酵液中尿素δ~(13)C和δ~(15)N

在酸性环境下,尿素与丙二醛-二甲基乙缩醛反应生成2-羟基嘧啶,随后由重氮甲烷甲基化形成2-甲氧基嘧啶。本研究以酵母发酵液为例,建立了气相色谱-燃烧-同位素比值质谱(GC-C-IRMS)法测定发酵液中尿素δ~(13)C和δ~(15)N,并对前处理方法和GC条件进行了优化。结果表明:尿素在不同13 C(0~5%)和15 N(0~10%)标记丰度下,标记量与GC-C-IRMS测定结果的相关性良好,线性相关系数R2分别为0.998和0.999,说明可在极低标记浓度下对尿素中δ~(13)C和δ~(15)N进行准确测定。采用该方法测定了酵母发酵液尿素中δ~(13)C和δ~(15)N,其重复性相对标准偏差分别为0.21‰和0.30‰,再现性相对标准偏差分别为0.23‰和0.29‰。该方法精度高、准确性好,可为低稳定同位素标记尿素示踪实验以及尿素循环代谢研究提供方法基础。     

酸分馏效应对GasBench-IRMS测定碳酸盐碳、氧同位素的影响

本文利用在线制样装置(GasBench)和稳定同位素比质谱仪(IRMS)测试一系列碳酸盐标准物质和现代海洋浮游有孔虫样品,在不同测试条件下,分析不同性状碳酸盐矿物的氧同位素分馏程度,计算氧同位素酸分馏系数,探讨酸分馏效应对不同碳酸盐矿物氧同位素测定的影响机制和控制因素,以及对氧同位素测试值(δ¹⁸O_m)的校正方法。结果表明,酸分馏效应对氧同位素值的影响主要是由于生成的CO₂气体与顶空瓶中气态水(高温时主要影响)或酸中游离态自由水(低温时主要影响)之间发生氧同位素交换引起的。不同性状碳酸盐标准物质的氧同位素酸分馏系数具有显著差异,且与氧同位素组成相关。δ¹⁸O_m值发生偏移的程度与反应温度、样品量、磷酸含水量以及酸中游离态和气态水的氧同位素组成与样品氧同位素组成之间的差异等因素有关。氧同位素酸分馏效应与信号强度具有显著相关性。建议精确称量相同质量的标准物质和样品,遵循信号强度匹配的原则,并采用多种标准物质线性校正的方法有效校正氧同位素分馏现象。在较低的反应温度(25℃)下,氧同位素...     

植物性食品中稀土元素的快速测定

采用微波消解处理样品,消化液直接用ICP-MS进行分析,以建立植物性食品中稀土元素的快速测定方法。实验结果证明,该方法检出限0.01～0.2μg/kg,精密度优于10%,对3个标准参考物质的分析结果令人满意。利用该方法对植物性食品中稀土元素进行测定,完成检测只需1～2h,满足日常检验需求,较大地提高工作效率。     

同位素稀释火花源质谱法定量分析人发标准物质

本文介绍用同位素稀释火花源质谱法定量分析人发标准物质中的Fe、Ni、Sr、Mo、Ba和Pb元素。此方法的灵敏度为ppb量级,精密度优于±5%,准确度优于8%,同时讨论了样品处理的几种方法和谱线选择及最佳示踪剂的加入量,并介绍对微量样品分析十分有效的电极成形方法。     

CaF2, MgF2, SiO2, Al2O3, SiC, LiF, BaF2, and ZrO2 optical single crystals used in studies in the VUV spectral region

Spectral characteristics of single crystals—fluorite, magnesium fluoride, quartz, sapphire, silicon carbide, lithium fluoride, barium fluoride, and fianite—used as materials for optical windows in studies in the VUV spectral region are presented. Spectral and photometric studies of single crystals in the spectral range 30–700 nm were performed on a BM-70 vacuum spectrophotometer. This instrument is equipped with a vacuum chamber for measuring the light transmission and reflection at radiation angles of incidence between 10° and 70°; this allows both characteristics to be measured sequentially in time without breaking vacuum. Replaceable radiation sources (with and without a window) were used to perform studies in the spectral range 30–700 nm, including measurements in flows of atmospheric and inert gases (Ne, He, Ar, N, and H).     

Field emission from multiwall carbon nanotubes in controlled ambient gases,H2, CO,N2 and O2

Adsorption and desorption on clean pentagons at a tip of multiwall carbon nanotube (MWNT) have been investigated by field emission microscopy (FEM) in an atmosphere of various gases, i.e., hydrogen, carbon monoxide, nitrogen and oxygen. A MWNT with clean surface which is obtained by heat treatment gives FEM patterns consisting of six bright pentagonal rings. Adsorbates are recognized as bright spots in the FEM pattern. They reside preferentially on the pentagonal sites where the strong electric field is concentrated, and bring about stepwise increase in the emission current. Heat treatment of the MWNT emitter at about 1300K allows adsorbates to desorb. After the desorption of hydrogen and nitrogen, the original clean surface with pentagons is recovered, while the tip structure is destroyed after the desorption of oxygen.     

离子色谱法在饮用水安全保障预警检测体系中的应用饮用水中F-,ClO-2,ClO-3,Cl-,BrO-3,Br-,NO-2,NO-3,SO2-4,H2PO-4十种离子的同时测定

建立了用离子色谱法同时测定水中F^-，BrO3^-，Br^-，ClO2^-，Cl6-，ClO3^-，NO2^-，NO3^-，SO4^2-，H2PO4^-十种离子的方法，方法的检出限低、灵敏度高、线性范围广、抗干扰强、操作简便，可快速同时测定不同数量级浓度的离子，有效地满足饮用水安全保障预警体系中对源水、出厂水进行无机消毒副产物和其它控制阴离子的快速同时检测。     

应用液相色谱-质谱联用技术同时测定花生中的黄曲霉毒素B1、B2、G1、G2

The aflatoxin B1, B2, G1, G2 in peanut were develop by LC-MS/MS. The mass spectrometer was operated in the positive ion mode using multiple reaction monitoring. The sample was extracted with methanol, and chromatographic separation was carried out on a MGIII-C₁₈ column(2.1 mm×150 mm×1.8 μm) with eluthic sion of V(acetonitrile):V(water)＝35:65. The limit of detection is 0.5 μg•L^－1, the limit of quantitation is 0.5 μg•kg^－1. The linear plots are between 0.5 μg•L^－1 and 25.0 μg•L^－1. Overall recoveries are between 88.3% and 99.2%, and RSD values are between 1.73％ and 3.75％.     

Enhancing the Tribological Behavior of Lubricating Oil by Adding TiO2, Graphene,and TiO2/Graphene Nanoparticles

This article investigates the tribological behavior of nanoparticles (NPs) of titanium dioxide anatase TiO₂ (A), graphene, and TiO₂ (A) + graphene added to the pure base oil group ΙΙ (PBO-GΙΙ). The morphology of these two nanostructures of TiO₂ (A) and graphene was characterized by transmission electron microscopy (TEM). Oleic acid (OA) was blended as a surfactant into the formulation to help stabilize the NPs in the lubricant oil. A four-ball test rig was used to determine the tribological performance of six different samples, and an image acquisition system was used to examine and measure the wear scar diameter of the stationary balls. Field emission–scanning electron microscopy (FE-SEM) was used to examine the wear morphology. Energy-dispersive X-ray spectroscopy (EDX), element mapping, and Raman spectroscopy were employed to confirm the presence of (TiO₂ (A) + graphene) and the formation of a tribolayer/film on the mating surfaces. Moreover, a 3D optical surface texture analyzer was utilized to investigate the scar topography and tribological performance. The experiments proved that adding (0.4?wt% TiO₂ (A) + 0.2?wt% graphene) to the PBO-GΙΙ optimized its tribological behavior. These excellent results can be attributed to the dual additive effect and the formation of a tribofilm of NPs during sliding motion. Furthermore, the average reductions in the coefficient of friction (COF), wear scar diameter (WSD), and specific wear rate (SWR) were 38.83, 36.78, and 15.78%, respectively, for (0.4?wt% TiO₂ (A) + 0.2?wt% graphene) nanolubricant compared to plain PBO-GΙΙ lubricant.     

工序分散在双偏心法兰加工中的应用研究

深入分析了双偏心法兰的零件结构特点,基于工序分散原则拟定了加工工艺方案,串装三爪卡盘与四爪卡盘解决了工件双偏心轴线的找正难题,合理安排数控机床与普通机床的加工步骤,提高了生产效率,也兼顾了工人的技术水平。该双偏心法兰制造成功,为其他偏心盘套类零件制造提供了有价值的参考。     

Microstructure,Physical Properties,and Tribological Characteristics of Composite Solid Lubricant Coatings with Gas Atomized BaF2-CaF2

PS304 is a NASA-developed composite solid lubricant for friction and wear reduction at high temperatures. The microstructure, physical properties, and tribological performance of PS304 using standard comminuted BaF₂-CaF₂ and novel gas atomized BaF₂-CaF₂ were compared. Two atomized BaF₂-CaF₂ particle size distributions were used. Overall, feedstock powder with atomized BaF₂-CaF₂ flowed more freely than standard PS304 feedstock. The cohesion strength of coatings with atomized BaF₂-CaF₂ was lower than that of standard PS304, while the hardness of all of the studied coatings was essentially the same (approximately 58 HRA). Pin wear was lower against the new coatings and the coefficients of friction were essentially the same for all coatings. These results indicate that atomized BaF₂-CaF₂ can be substituted for comminuted BaF₂-CaF₂, providing a high-volume BaF₂-CaF₂ fabrication technique to reduce the cost of PS304 and improve its commercial availability.     

Label-free, all-electrical, in situ human epidermal growth receptor 2 detection

Using 3-mercaptopropyltrimethoxysilane (MPS)-coated (PbMg 1/3 Nb 2/3 O3)0.63-(PbTiO3)0.37 (PMN-PT)/tin and lead zirconate titanate/glass piezoelectric microcantilever sensors (PEMSs) with single-chain variable fragment (scFv) immobilized on the MPS surface, we have demonstrated real-time, label-free detection of human epidermal growth factor receptor 2 (Her2) in a background of 1 mg/ml bovine serum albumin. Coupled with a scFv with a KD of 3.4 x 10(-8)M, the MPS-insulated PMN-PT/tin PEMS 560 microm long and 720 microm wide exhibited a Her2 concentration sensitivity of 5 ng/ml in a background of 1 mg/ml BSA.