The calibration of activated charcoal detectors in a small Rn exposure chamber

Passive methods for radon measurements, especially those based on radon adsorption, require observation of proper calibration methods.

The calibration method for diffusion-barrier charcoal detectors in a small (211 dm³) radon chamber has been proposed. The theoretical dependence of radon concentration vs. time inside the chamber during the exposure of charcoal detectors has been obtained and verified experimentally. For this purpose, the chamber volume as well as diffusion and adsorption parameters of the detector were taken into consideration.

For two types of detectors the conformity of calibration factors obtained in two ways: calculated from theoretical points (550 or 683 Bqm⁻³/cps depending on detector type) and from experimental points (553 or 691 Bqm⁻³/cps), was achieved.

The proposed method makes it possible to calibrate different kinds of radon-adsorbing detectors (not only charcoal canisters) in small chambers without the necessity of using any reference, active device.     

Radioactive Reference Proteins for The Study of Labelled Proteins by Gel Electrphoresis : A Ready Preparation of Radiolabelled Calibration Kits

Abstract

The use of unlabelled reference proteins as molecular weight markers in the study of radioactive proteins by polyacrylamide gel electrophoresis is rather inconvenient since protein standards should be stained whereas the studied proteins are usually detected by radioautography. We describe a rapid, in vitro method for introducing a radioactive label into reference proteins: amino groups are acylated by a highly radioactive, commercially available reagent: N-succinimidyl-[2,3-³H]propionate. Both standard and studied proteins can then be visualized on a single radioautograph; this allows direct comparison of mobilities, thus improving both convenience and accuracy of M ^r determinations, and avoids some major drawbacks of staining, such as the loss of sensitivity of fluorography due to dye-induced quenching. Additionally, in vitro labelling may be used for the detection of proteins in trace amounts, as an alternative method versus silver staining procedures.     

Extent-based kinetic identification using spectroscopic measurements and multivariate calibration

Extent-based kinetic identification is a kinetic modeling technique that uses concentration measurements to compute extents and identify reaction kinetics by the integral method of parameter estimation. This article considers the case where spectroscopic data are used together with a calibration model to predict concentrations. The calibration set is assumed to be constructed from reacting data that include pairs of concentration and spectral data. Alternatively, one can use the concentration- and spectral contributions of the reactions and mass transfers, which are obtained by pretreatment in reaction- and mass-transfer-variant form. The extent-based kinetic identification using concentrations predicted from spectroscopic data is illustrated through the simulation of both a homogeneous and a gas–liquid reaction system.     

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.     

Simultaneous flow injection analysis of cadmium and lead with differential pulse voltammetric detection

A flow injection (FI) method using multiple differential pulse voltammetric detection for the simultaneous determination of two metal ions was developed and applied to the resolution of Cd(II)-Pb(II) mixtures. The metals are detected by applying two sequential pulses to a three-electrode voltammetric system that uses a flow-through cell accommodating a static mercury-drop working electrode. The influence of the electrode area, flow-rate, pulse frequency, pulse width and sampling time was investigated. Under the experimental conditions used, the two metals were found to interfere with each other. The use of a neural network allows the simultaneous determination of both, in mixtures, with good accuracy. The proposed method is applicable to other complex systems involving different working electrodes and more than two electroactive species.     

Comparison between theoretical model and experimental calibrations and its inference for track formation in bubble detectors

Calculations on the formation of a linear track of a heavy ion in bubble detector have been carried out based on a theoretical model considering the minimum energy (including bubble surface energy, internal energy, evaporation energy, expansion energy, kinetic energy and viscous energy) required during the formation of a critical bubble at the cost of the ionization energy of the heavy ion. The calculated minimum energy is 8.99 keV for dichlorodifluoromethane (R-12) at 25 °C. The results of calculations have been combined with those of calibrations of bubble detectors with heavy ions at accelerator. The threshold (1.51±0.04) MeV mg^-1 cm² is obtained in the calibration with heavy ions for the above liquid and temperature. It shows that the distance over which the heavy ion traverses and transfers energy to the superheated liquid to produce a critical bubble is 4.67 times the radius of the seed bubble. The radius of the cylinder along which the heavy ion deposits energy to form a seed bubble is about 5.2 nm. This dimension indicates that the process of track formation in bubble detectors is consistent with the model of thermal spike.     

Energy calibration of a BC501A liquid scintillator using a γ-γ coincidence technique

An accurate energy calibration of a BC501A liquid scintillator by means of Compton scattering of γ-rays is described.The energy resolution and the position of the Compton edge have been precisely determined using a γ-γ coincidence technique and fitting the coincidence spectrum with a Gaussian function superimposed on a quadratic polynomial for the background.The position of the Compton edge relative to the position of the maximum and the half height of the distribution in dependence on the relevant energy resolution is discussed in detail.The results indicate that the maximum energy of the recoil Compton electron does not occur at the half height distribution but at 0.90±0.05 of the maximum height in the energy range considered.The energy resolution varies from 15.6% to 8.02% for electrons in the energy region from 0.5 MeV to 3 MeV.     

Sum of ranking differences (SRD) to ensemble multivariate calibration model merits for tuning parameter selection and comparing calibration methods

Most multivariate calibration methods require selection of tuning parameters, such as partial least squares (PLS) or the Tikhonov regularization variant ridge regression (RR). Tuning parameter values determine the direction and magnitude of respective model vectors thereby setting the resultant predication abilities of the model vectors. Simultaneously, tuning parameter values establish the corresponding bias/variance and the underlying selectivity/sensitivity tradeoffs. Selection of the final tuning parameter is often accomplished through some form of cross-validation and the resultant root mean square error of cross-validation (RMSECV) values are evaluated. However, selection of a “good” tuning parameter with this one model evaluation merit is almost impossible. Including additional model merits assists tuning parameter selection to provide better balanced models as well as allowing for a reasonable comparison between calibration methods. Using multiple merits requires decisions to be made on how to combine and weight the merits into an information criterion. An abundance of options are possible. Presented in this paper is the sum of ranking differences (SRD) to ensemble a collection of model evaluation merits varying across tuning parameters. It is shown that the SRD consensus ranking of model tuning parameters allows automatic selection of the final model, or a collection of models if so desired. Essentially, the user’s preference for the degree of balance between bias and variance ultimately decides the merits used in SRD and hence, the tuning parameter values ranked lowest by SRD for automatic selection. The SRD process is also shown to allow simultaneous comparison of different calibration methods for a particular data set in conjunction with tuning parameter selection. Because SRD evaluates consistency across multiple merits, decisions on how to combine and weight merits are avoided. To demonstrate the utility of SRD, a near infrared spectral data set and a quantitative structure activity relationship (QSAR) data set are evaluated using PLS and RR.     

Review of validation and reporting of non-targeted fingerprinting approaches for food authentication

Food fingerprinting approaches are expected to become a very potent tool in authentication processes aiming at a comprehensive characterization of complex food matrices. By non-targeted spectrometric or spectroscopic chemical analysis with a subsequent (multivariate) statistical evaluation of acquired data, food matrices can be investigated in terms of their geographical origin, species variety or possible adulterations. Although many successful research projects have already demonstrated the feasibility of non-targeted fingerprinting approaches, their uptake and implementation into routine analysis and food surveillance is still limited. In many proof-of-principle studies, the prediction ability of only one data set was explored, measured within a limited period of time using one instrument within one laboratory. Thorough validation strategies that guarantee reliability of the respective data basis and that allow conclusion on the applicability of the respective approaches for its fit-for-purpose have not yet been proposed. Within this review, critical steps of the fingerprinting workflow were explored to develop a generic scheme for multivariate model validation. As a result, a proposed scheme for “good practice” shall guide users through validation and reporting of non-targeted fingerprinting results. Furthermore, food fingerprinting studies were selected by a systematic search approach and reviewed with regard to (a) transparency of data processing and (b) validity of study results. Subsequently, the studies were inspected for measures of statistical model validation, analytical method validation and quality assurance measures. In this context, issues and recommendations were found that might be considered as an actual starting point for developing validation standards of non-targeted metabolomics approaches for food authentication in the future. Hence, this review intends to contribute to the harmonization and standardization of food fingerprinting, both required as a prior condition for the authentication of food in routine analysis and official control.     

三维荧光二阶校正法用于血浆和尿液中柔红霉素的快速测定

文章采用三维激发发射荧光光谱与化学计量学交替三线性分解(ATLD)二阶校正法相结合,对血浆液和尿液中柔红霉素(DM)进行定量测定。实验不需对血浆和尿液预测样进行萃取等分离预处理,选取激发波长410～530nm,发射波长550～650nm,分别每隔5nm取一个数据,利用激发发射荧光扫描分别获得两个三维响应数阵(大小为21×25×12)。当组分数选择为3时,血浆和尿液校正集中盐酸柔红霉素的相对浓度与实际浓度的相关系数分别为r1=0.9990和r2=0.9952,经ATLD算法解析得到的血浆和尿液预测样中柔红霉素平均回收率分别为(92.8±7.6)%和(94.7±4.4)%。实验结果表明,此法能够解决血浆和尿液中盐酸柔红霉素药物因血浆和尿液内源物质与分析物光谱重叠所引起的难分辨的问题,可用于未知干扰共存下柔红霉素的直接快速定量测定。