The interlaboratory comparison "IMEP-19 trace elements in rice"—a new approach for measurement performance evaluation

The aim of IMEP is to present objectively the quality of chemical measurements. Participants in IMEP compare their reported measurement results with independent external certified reference values with demonstrated traceability and uncertainty, as evaluated according to international guidelines. IMEP-19 focused on measurements of trace elements in rice aiming to support the Commission Regulation (EC) No. 466/2001 on maximum levels for certain contaminants in foodstuff. Measurement results for the elements Cd, Cu, Pb and Zn were reported by 267 field laboratories involved in food analysis from 43 countries. Performance criteria for the evaluation of the reported measurement results in IMEP-19 are suggested. The chosen performance indicators not only take into account the deviation of the reported measurement value from the certified reference value, but also set criteria for maximum and minimum acceptable uncertainty. The IMEP-19 participants' performance is reviewed by means of using new simple graphical tools, called "Naji plots".     

Collision complexes in dissociative single electron transfer between Ne2+ and N2

Experiments involving the coincident detection of the two monocationic products (Ne+ and N+) from the dissociative electron transfer reaction between Ne2+ and N2 at 7.8 eV collision energy allow the nascent velocity vectors of the ionic and neutral (N) products to be determined. Examination of the correlations between these vectors shows that one pathway to the products involves the dissociation of a transitory collision complex (N2Ne2+).     

Low frequency ultrasonic propagation through fibre reinforced,polymer composites

This paper concentrates upon mesoscale variations observed in the time-of-flight (TOF) area scans of shear wave propagation through 'identically processed', injection moulded, glass fibre reinforced, polypropylene plaques. The effect of these structural variations on the derived 3D stiffness constants is discussed. Hence the random measurement errors associated with the stiffness constant measurements are differentiated from the intrinsic process-induced spatial variations. Interesting correlations between TOF and received amplitudes of shear wave propagation have been found and our tentative interpretation of these data in terms of mesostructural variations in the reinforcing fibre locations and fibre orientations is presented.     

Determination of airborne wood dust in Button samples by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS)

Emerging concerns regarding the toxicity of inhaled wood dust support the need for techniques to quantitate wood content of mixed industrial dusts. The diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) analysis technique was applied to the determination of wood content of 181 inhalable dust samples (geometric mean concentration: 0.895?mg/m³; geometric standard deviation: 2.73) collected from six wood product industry factories using 25?mm glass fibre filters with the Button aerosol sampler. Prior to direct DRIFTS analysis the filter samples were treated with ethyl acetate and re-deposited uniformly. Standards ranging from 125?µg to 4000?µg were prepared for red oak, southern yellow pine, and red cedar and used for quantitation of samples depending upon the wood materials present at a given factory. The oak standards spectra were quantitated by linear regression of response in Kubelka-Munk units at 1736?cm^?1, whereas the pine standards and the cedar standards spectra were quantitated by polynomial regression of response in log 1/R units at 1734?cm^?1, with the selected wavenumbers corresponding to stretching vibration of free C=O from cellulose and hemicelluloses. For one factory which used both soft- and hard-woods, a separate polynomial standard curve was created by proportionally combining the oak and pine standards polynomial regression equations based on response (log 1/R) at 1734?cm^?1. The analytical limits of detection were approximately 52?µg of oak, 20?µg of pine, 30?µg of cedar, and 16?µg of mixed oak and pine for the factory with mixed woods. Overall, the average of dry wood dust percentage of inhalable dust was approximately 56% and the average dry wood dust weight was 0.572?mg for the Button samples. Across factories, there were statistically significant differences (p?<?0.001) for the percentage of dry wood dust in inhalable dust with factory averages ranging from 33.5 to 97.6%.     

Effect of Rayleigh-scattering distributed feedback on multiwavelength Raman fiber laser generation

We experimentally demonstrate a Raman fiber laser based on multiple point-action fiber Bragg grating reflectors and distributed feedback via Rayleigh scattering in an ~22-km-long optical fiber. Twenty-two lasing lines with spacing of ~100 GHz (close to International Telecommunication Union grid) in the C band are generated at the watt level. In contrast to the normal cavity with competition between laser lines, the random distributed feedback cavity exhibits highly stable multiwavelength generation with a power-equalized uniform distribution, which is almost independent on power.     

Loss of Internal Backbone Carbonyls: Additional Evidence for Sequence-Scrambling in Collision-Induced Dissociation of y-Type Ions

It is shown that y-type ions, after losing C-terminal H₂O or NH₃, can lose an internal backbone carbonyl (CO) from different peptide positions and yield structurally different product fragment ions upon collision-induced dissociation (CID). Such CO losses from internal peptide backbones of y-fragment ions are not unique to a single peptide and were observed in four of five model peptides studied herein. Experimental details on examples of CO losses from y-type fragment ions for an isotopically labeled AAAAHAA-NH₂ heptapeptide and des-acetylated-α-melanocyte-stimulating hormone (dα-MSH) (SYSMEHFRWGKPV-NH₂) are reported. Results from isotope labeling, tandem mass spectrometry (MSⁿ), and ion mobility-mass spectrometry (IM-MS) confirm that CO losses from different amino acids of m/z-isolated y-type ions yield structurally different ions. It is shown that losses of internal backbone carbonyls (as CID products of m/z-isolated y-type ions) are among intermediate steps towards formation of rearranged or permutated product fragment ions. Possible mechanisms for generation of the observed sequence-scrambled a-“like” ions, as intermediates in sequence-scrambling pathways of y-type ions, are proposed and discussed. ?      

Automated Deconvolution of Overlapped Ion Mobility Profiles

Presence of unresolved ion mobility (IM) profiles limits the efficient utilization of IM mass spectrometry (IM-MS) systems for isomer differentiation. Here, we introduce an automated ion mobility deconvolution (AIMD) computer software for streamlined deconvolution of overlapped IM-MS profiles. AIMD is based on a previously reported post-IM/collision-induced dissociation (CID) deconvolution approach [J. Am. Soc. Mass Spectrom. 23, 1873 (2012)] and, unlike the previously reported manual approach, it does not require resampling of post-IM/CID data. A novel data preprocessing approach is utilized to improve the accuracy and efficiency of the deconvolution process. Results from AIMD analysis of overlapped IM profiles of data from (1) Waters Synapt G1 for a binary mixture of isomeric peptides (amino acid sequences: GRGDS and SDGRG) and (2) Waters Synapt G2-S for a binary mixture of isomeric trisaccharides (raffinose and isomaltotriose) are presented. Graphical Abstract

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