漫透射视觉密度计密度片标准物质的研制

以工业射线胶片为主材,经过曝光和暗室处理等工艺,制备检定校准漫透射视觉密度计用的密度片标准物质。密度片的级数达到24级、光学密度值范围为0.03~5.00,密度片的量值、均匀性及光谱特性等参数均优于相关规程对标准密度片的规定参数,可广泛应用于漫透射视觉密度计的检定校准工作。     

原子荧光光度计检定/校准的影响因素

主要介绍了原子荧光分光光度计检定/校准的过程中常见故障,如联机故障、载气故障、点火故障和自动进样器故障等,针对无信号强度、荧光强度偏低、空白强度较高、仪器不稳定和重复性较差、线性不好等常见问题进行剖析并提出相应解决方法,根据工作经验和仪器工作原理提出了原子荧光光度计检定/校准过程中仪器参数和溶液配制方法。     

毛细管黏度计自动检定/校准系统的研制

利用自动控温系统、测温电桥、自动计时系统和计算机控制平台组成一种毛细管黏度计自动检定/校准系统,该系统具有自动吸液、自动计时以及数据自动处理功能,可用于标准黏度液定值和毛细管黏度计检定/校准。     

氧、氮、氢分析仪校准方法探讨

建立了氧、氮、氢分析仪的校准方法,介绍了氧、氮、氢分析仪的工作原理、校准要求、校准用标准物质.以北京纳克分析仪器有限公司生产的ON-3000氧氮分析仪和H-3000氢分析仪作为校准对象,对校准方法进行了验证.该方法已作为评价氧、氮、氢分析仪的依据并得到认可.     

化学测量仪器检定/校准有关问题的探讨

介绍了化学测量仪器的分类、特点、检定/校准的必要性及化学计量检定/校准的现状,分析了化学计量标准的特点,探讨了化学计量最高标准的划定和考核的有关问题。     

PC-Ⅰ型数字式pH检定测量仪原理及校准

介绍了PC -Ⅰ型数字式pH检定测量仪的工作原理及校准方法、校准步骤     

PC—Ⅰ型数字式pH检定测量仪原理及校准

介绍了ＰＣ－Ⅰ型数字式ＰＨ检定测量仪的工作原理及校准方法、校准步骤。     

有机磷化合物的研究--Ⅰ.二硫代磷酸 O,O-二乙酯的氯化反应

二硫代磷酸 O,O-二乙酯的氯化产物是硫磷醯氯 O,O-二乙酯及一氯化硫。其氯化过程的中间物,硫代磷酸 O,O-二乙酯氯化硫,双(硫代磷酸二乙酯)二硫物,双(二硫代磷酸二乙酯)三硫物俱经分离及检定,上述三化合物形成的条件,以及进一步氯化的产物均加以确定,故二硫磷酸 O,O-二乙酯的氯化过程业已阐明。志谢:本实验中的碳、氢元素分析,系中国科学院有机化学研究所代做,特此志谢。     

化学测量仪器检定／校准有关问题的探讨

介绍了化学测量仪器的分类、特点、检定／校准的必要性及化学计量检定／校准的现状，分析了化学计量标准的特点、探讨了化学计量最高标准的划定和考核的在关问题。     

定碳定硫分析仪检定规程的探讨和修订建议

JJG 395–1997《定碳定硫分析仪检定规程》中的部分技术要求和检定项目已不能满足现代碳硫分析仪器检定/校准的要求。对规程的适用性、称量稳定性、示值误差、标准物质、重复性、分析时间等进行了探讨,并给出了修订建议。探讨了评定仪器检测空白的可能性,提出了依据碳硫测定基准国标方法的仪器检定/校准方法,以评定不同用途的测试仪器,并扩展了仪器检定/校准的范围。为计量部门修订规程提供参考,同时也为实验室合理评价,验收碳硫分析仪,及时掌握仪器的运行状况,保证分析数据的准确性、一致性和溯源性提供借鉴。     

Temperature calibration of an electrical compensation DSC on cooling using thermally stable high purity liquid crystals

Temperature calibration of DSCs is usually carried out on heating. In order to accurately control the temperature during cooling experiments, the calibration has to be carried out on cooling. Therefore, three high-purity, thermally stable liquid crystals were used to perform a temperature calibration of an electrcial compensation DSC on cooling. All three liquid crystals have several liquid crystalline phases, and they all were purified to a 99.9% lovel. Temoperatures of the isotropic to nematic or cholesteric and the mesophase to mesophase transitions were used. It was verified that these liquid crystals have sufficient thermal stability for carrying out the calibration on cooling. The dependence of the real temperature on the indicated temperature has been established for all the combinations of the heating and cooling rates of practical interest. It is also shown that the vant's Hoff equation can only be applied to the crystal to a liquid crystal transition, but not to the liquid crystal to liquid crystal or liquid crystal to isotropic transitions.     

Signal processing and uncertainty in an isothermal titration calorimeter

In this paper, it is made a study of the accuracy of an isothermal titration calorimeter in the operating mode of ‘continuous injection’. The experimental equipment has been a TAM2277-201/2250 by Thermometric AB and the liquid mixtures used in the calibration have been the mixture cyclohexane+benzene and the mixture water+ethanol. The calibration contemplates different effects that affect the uncertainty in the determination of the sensitivity, the effect of the liquid injection, the treatment of the calorimetric signal, the variation of the experimental baseline and the different noises included in the calorimetric signal.     

口腔气体检测仪校准装置的研制

利用研制的三通道渗透管装置发生摩尔分数范围为0.1~1.0μmol/mol的硫化氢、甲基硫醇、二甲基硫醚混合气体,用于校准检测口腔气体检测仪。校准装置可以在固定输出总流量不变的情况下,快速改变发生硫化物的摩尔分数。对校准装置的温控系统和流量系统进行了测试,通过总硫分析仪对校准装置发生的低含量硫化物的量值进行了比较和验证。该校准装置发生的低含量硫化物量的相对扩展不确定度不大于6.8%(k=2)。     

多种方法分析与评价乙酸乙酯合成实验中产物之纯度

采用气相色谱内标法、面积归一化法及NMR内标法3种方法对乙酸乙酯合成反应中的产物进行纯度分析.GC内标法可抵消由于操作条件的波动而带来的误差,只需内标物与待测组分在同样条件下出峰且分离度较好,定量精度高,测出的乙酸乙酯纯度最低;应用NMR内标法可同步完成纯度分析和结构鉴定,且无需引入校正因子,操作简便.     

Evaluation of the calibration errors on cooling of a differential scanning calorimeter using different sets of standard metals

The temperature calibration on cooling of thermal analysis instruments is important for the accurate study of the non-isothermal crystallization kinetics of semi-crystalline polymers. In previous works, a methodology was proposed for performing the calibration on cooling of differential scanning calorimeters (DSCs) with standard metals, and the calibration errors were checked using transitions of high-purity liquid crystals. In this work, alternative, physically meaningful, procedures for carrying out the calibration on cooling are analyzed and validated. The calibration errors are evaluated also with liquid crystalline transitions, when the calibration is performed with standard metals, in a wide temperature range, and when due account is taken for the need of isothermal corrections to the temperature measurements. It is shown that any pair of standard metals may be used to calibrate on cooling, that the calibration errors increase for wider working temperature ranges and that, providing that certain conditions are fulfilled, both calibration procedures yield similar results.     

Validation of a novel method to identify in utero ethanol exposure: simultaneous meconium extraction of fatty acid ethyl esters,ethyl glucuronide,and ethyl sulfate followed by LC-MS/MS quantification

Presence of fatty acid ethyl esters (FAEE), ethyl glucuronide (EtG), and ethyl sulfate (EtS) in meconium, the first neonatal feces, identifies maternal alcohol consumption during pregnancy. Current meconium alcohol marker assays require separate analyses for FAEE and EtG/EtS. We describe development and validation of the first quantitative liquid chromatography tandem mass spectrometry assay for 9 FAEEs, EtG, and EtS in 100 mg meconium. For the first time, these alcohol markers are analyzed in the same meconium aliquot, enabling comparison of the efficiency of gestational ethanol exposure detection. 100 mg meconium was homogenized in methanol and centrifuged. The supernatant was divided, and applied to two different solid phase extraction columns for optimized analyte recovery. Limits of quantification for ethyl laurate, myristate, linolenate, palmitoleate, arachidonate, linoleate, palmitate, oleate, and stearate ranged from 25–50 ng/g, with calibration curves to 2,500–5,000 ng/g. EtG and EtS linear dynamic ranges were 5–1,000 and 2.5–500 ng/g, respectively. Mean bias and between-day imprecision were <15 %. Extraction efficiencies were 51.2–96.5 %. Matrix effects ranged from ?84.7 to 16.0 %, but were compensated for by matched deuterated internal standards when available. All analytes were stable (within ±20 % change from baseline) in 3 authentic positive specimens, analyzed in triplicate, after 3 freeze/thaw cycles (?20 °C). Authentic EtG and EtS also were stable after 12 h at room temperature and 72 h at 4 °C; some FAEE showed instability under these conditions, although there was large inter-subject variability. This novel method accurately detects multiple alcohol meconium markers and enables comparison of markers for maternal alcohol consumption.

在非水溶剂中聚甲基丙烯酸甲酯及其甲基丙烯酸共聚物与Rh6G的相互作用

本文用乙酸乙酯与不同比例乙醇配成混合溶剂, 考察在不同极性的介质中, Rh_6G对聚甲基丙烯酸甲酯及其与甲基丙烯酸共聚物分子形态的影响, 以及聚合物对Rh_6G荧光强度的影响, 发现Rh_6G与聚甲基丙烯酸甲酯没有特殊相互作用, 而与共聚物的相互作用受溶剂的极性影响很大, 随着极性增加, 从氢键作用过渡到静电作用。     

动态配气法制备氮气中乙醇扩散管气体标准物质

用动态配气装置配制体积分数为10^-6的氮气中乙醇扩散管气体标准物质，其量值不确定度为2%-3%。与静态容量法配制的乙醇气体标准物质进行比对，结果的相对误差为3.5%-4.0%。     

Dynamic structure of poly(vinyl pyrrolidone)/ethyl alcohol mixtures studied by time domain reflectometry

Dielectric studies of poly(vinyl pyrrolidone)/ethyl alcohol (PVP–E) binary mixtures with concentration variations were carried out in the frequency range of 10 MHz to 10 GHz by time domain reflectometry at 15, 25, 35, and 45 °C. One relaxation process, corresponding to ethyl alcohol molecules in the poly(vinyl pyrrolidone) (PVP) matrix, was observed in this frequency range for all the mixtures. The static dielectric constant of the PVP–E mixtures decreased linearly with an increase in the weight fraction of PVP. The observed anomalous increase in the value of the relaxation time (τ) of these mixtures was interpreted by the consideration of the variation in the local structure of self‐associated ethyl alcohol molecules and also the PVP behavior as a geometric constraint for the rotational motion of ethyl alcohol molecules. Furthermore, the τ values of these mixtures were independent of the viscosity. The energy parameters for the dielectric relaxation process (the free energy, enthalpy, and entropy of activation for the dipolar orientation) were determined to confirm the transient behavior of the heterogeneous species due to the breaking and re‐forming of hydrogen bonds with the internal rotation of ? OH groups in the ordered structure of the PVP–E mixtures. On the basis of the evaluated dielectric parameters, the formation of supermolecular structure in the PVP–E mixtures in dynamic equilibrium was sketched and examined by the consideration of the hydrogen bonding between the terminal hydroxyl groups of self‐associated ethyl alcohol flexible chains and the carbonyl groups of monomer units of PVP coiled chains. © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 1134–1143, 2005