双脉冲激光诱导击穿光谱结合多元定标法定量分析大豆油中的铅

应用双脉冲激光诱导击穿光谱(DP-LIBS)对大豆油中的铅(Pb)含量进行检测。配制9个大豆油样品,采用一定规格圆柱形桐木对样品中Pb进行富集,然后通过Ava-Spec二通道高精度光谱仪采集其LIBS光谱信号。根据样品的LIBS谱线图和美国国家标准技术研究所(NIST)原子光谱数据库,确定选用CaⅡ393.284 nm,CaⅡ396.752 nm,NⅡ399.399 nm和PbⅠ405.685 nm的特征谱线强度作为自变量,得到Pb含量的多元线性回归定量分析模型,并通过方差分析和t检验验证分析模型的可行性。结果表明,采用Pb元素直接定标法得到的平均相对误差约为16%,拟合度R2为0.981 8;采用多元线性回归模型得到的平均相对误差为7.25%,拟合度R2为0.997 1,3个检验样品的相对误差均在合理范围内。采用多元校正分析模型可以充分利用光谱中的有效信息,降低基体效应的影响,从而提高LIBS分析的准确性。     

Quantitative analysis of topical gels and ointments by FT-Raman spectroscopy

A method for quantitative determination of ibuprofen (IBU), naproxen (NAP), methyl salicylate (MES) and menthol (MNT) in commercial topical gels and ointments using partial least squares (PLS) models based on FT-Raman spectra is described. The calculated relative standard errors of prediction (RSEP) were found to be in the range of 2.1–3.2% for the calibration and validation data sets. Two commercial topical gels containing 5.0% of IBU and 10% of NAP (w/w), as well as one ointment containing 15% of MES and 10% of MNT (w/w) as active pharmaceutical ingredients (APIs), were successfully quantified using the developed models with recoveries in the 99.2–101.5% range. The proposed procedure can be used as a fast, reliable and economic method for the quantification of APIs in topical gels and ointments.     

Transfer of multivariate regression models between high‐resolution NMR instruments: application to authenticity control of sunflower lecithin

In recent years the number of spectroscopic studies utilizing multivariate techniques and involving different laboratories has been dramatically increased. In this paper the protocol for calibration transfer of partial least square regression model between high‐resolution nuclear magnetic resonance (NMR) spectrometers of different frequencies and equipped with different probes was established. As the test system previously published quantitative model to predict the concentration of blended soy species in sunflower lecithin was used. For multivariate modelling piecewise direct standardization (PDS), direct standardization, and hybrid calibration were employed. PDS showed the best performance for estimating lecithin falsification regarding its vegetable origin resulting in a significant decrease in root mean square error of prediction from 5.0 to 7.3% without standardization to 2.9–3.2% for PDS. Acceptable calibration transfer model was obtained by direct standardization, but this standardization approach introduces unfavourable noise to the spectral data. Hybrid calibration is least recommended for high‐resolution NMR data. The sensitivity of instrument transfer methods with respect to the type of spectrometer, the number of samples and the subset selection was also discussed. The study showed the necessity of applying a proper standardization procedure in cases when multivariate model has to be applied to the spectra recorded on a secondary NMR spectrometer even with the same magnetic field strength. Copyright © 2016 John Wiley & Sons, Ltd.     

Extended THz measurements of nitrous oxide, N2O

High precision measurements of the atmospheric trace gas nitrous oxide have been extended up through 1.5 THz. The data set includes ground state, ν₂, 2ν₂, ¹⁵NNO, N¹⁵NO, and N₂¹⁸O spectra up to J = 68. Improved Hamiltonian parameters are given.     

Linear optics calibration and nonlinear optimization during the commissioning of the SSRF storage ring

Phase I commissioning of the SSRF storage ring on 3.0 GeV beam energy was started at the end of December 2007. A lot of encouraging results have been obtained so far. In this paper, calibrations of the linear optics during the commissioning are discussed, and some measured results about the nonlinearity given. Calibration procedure emphasizes correcting quadrupole magnetic coefficients with the Linear Optics from Closed Orbit (LOCO) technique. After fitting the closed orbit response matrix, the linear optics of the four test modes is substantially corrected, and the measured physical parameters agree well with the designed ones.     

Detection efficiency of fission tracks in apatite related to mica external detectors by the spike irradiation technique

Detection efficiency of fission tracks in non-annealed and annealed Durango apatite crystals related to mica external detectors for fission track dating was estimated experimentally using the spike irradiation technique [Suzuki, 2002a. Abstracts of 21st International Conference on Nuclear Tracks in Solids, p. 22]. The relation of the fission track density between apatite samples and mica external detectors is an important parameter for the determination of fission track ages using an absolute approach especially for crystalline minerals. Spike irradiation of uranium-235-induced fission fragments was carried out using a high uranium content glass, GE1497, fixed firmly on the sample surface. Experimental works were carried out for sections parallel and perpendicular to the crystallographic c-axis of apatite. The detection efficiency of fission tracks in non-annealed apatite related to the mica external detectors was estimated to be 0.90 for the prism face and 0.99 for the basal face. The fission track age of Durango apatite averaged for the prism and basal faces was estimated to be 30.6 (±2.5) Ma, which is concordant with reference values reported previously, using the detection efficiency data with a B₀ value of the CN5 monitor glass and a U-238 spontaneous decay constant value of . The results also indicate that the B₀ age calibration method can be used effectively for the absolute evaluation of fission track ages of apatite.     

Treating the polyelectrolytes as polymers with a draining effect. II. The behavior in the gel permeation chromatography

The behavior of the polyelectrolytes in the gel permeation chromatography (GPC) can be better understood if the modified universal calibration (log([η]M/Φ) vs. elution volume) is used instead of the “classical” universal calibration (log[η]M vs. elution volume). The value of Flory's parameter Φ is obtained from an equation established for nonionic polymers presenting a draining effect, considering that polyelectrolytes also behave as polymers with a draining effect. The modified universal calibration does not apply as successfully to polyelectrolytes as to nonionic polymers, because of their electrostatic exclusion in the pore surface of the GPC columns. Nevertheless, when polyelectrolytes are found in a high salt concentration solution, the modified universal calibration can be used to obtain their molecular mass, using nonionic hydrosoluble polymers as standard polymers. Moreover, considering polyelectrolytes as polymers presenting a draining effect and applying the modified universal calibration provides a better explanation for the electrostatic exclusion of these polymers from the pores of the GPC columns, using the Dubin–Tecklenburg model. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 1106–1113, 2006     

XRFS-绝对量薄样法分析闪锌矿、黄铜矿单矿物的研究

本文用XRFS-绝对量薄样法研究了闪锌矿、黄铜矿等单矿物中主元素和次元素的测定。重点研究硫工作曲线的直化,实验表明,结果令人满意。     

Preliminary round-robin studies on the ICTAC certified reference materials for DTA

The ICTAC Committee on Standardisation has formed a Task Group to investigate the suitability of the ICTAC Certified Reference Materials for DTA, covering the temperature range 450°–1100°C, for accurate temperature calibration purposes and to evaluate their potential as enthalpy calibrants for DTA and DSC equipment. This paper reports the results of preliminary round-robin studies on barium carbonate and strontium carbonate, using a dual-point calibration method based on the melting points of aluminium and gold. In addition the fusion of ICTAC potassium sulphate has been investigated as a possible calibration transition.     

软X射线绝对光强测量系统及其标定

详细介绍了软X射线绝对光强测量系统的设计和结构及其标定的情况和结果,测量系统包括电离室、监测(或待标定)探测器及其传动系统两部分,可作为50—2000eV软X射线绝对强度测量的一级标准探测器. 并给出了系统的偏差.