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Paper des Monats
- ja (2)
Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are critical components of every industrial chemical process as they provide information on the concentrations of individual compounds and by-products. These processes are carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been developed to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra to train an ANN with better prediction performance and speed than state-of-theart analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a possible strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control.
For the classification of chemicals, special standardized test procedures have been developed and are used world-wide. Safe handling and use of these chemicals depend on the correct classification which therefore must be based on the precise and correct execution of the tests and their evaluation. In this context interlaboratory tests (round robin tests, interlaboratory comparisons / intercomparisons) are a crucial element of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025.
The present document reports on the results of the interlaboratory test 2009/2010 on the test methods UN O.2 “Test for oxidizing liquids” [1] / EC A.21 “Oxidizing Properties (Liquids)” [2] which was organized by the Center for Quality Assurance for Testing of Dangerous Goods and Hazardous Substances.
The test methods UN O.2 and EC A.21 are applied to characterize the oxidizing properties of liquid chemical substances or mixtures. To differentiate between chemicals with hazardous / dangerous oxidizing properties and chemicals which are not classified as hazardous / dangerous, the substance’s oxidizing properties are compared to those of a standard reference substance.
Since the methods (UN O.2 / EC A.21) were developed and came into force in the early nineties a systematic review concerning the practical application of the test method has not been carried out.
The classification of solid oxidizers according to the GHS (Globally Harmonized System of Classifica-tion and Labelling of Chemicals) and according to regulations on the transport of dangerous goods (based on the UN Recommendations/Model Regulations and implemented in all carrier domains as transport by road, railway, sea, air) is performed on the basis of the results of the UN test O.1 (―Test for oxidizing solids‖ described in chapter 34.4.1 in the Recommendations on the Transport of Danger-ous Goods, Manual of Tests and Criteria, Fifth revised edition, United Nations, New York and Geneva, 2009). This test was introduced into the UN Test Manual in 1995 as a replacement for a similar test from 1986. Even though the O.1 test is much better than the previous one there are still many prob-lems with this test. For this reason the IGUS-EOS working group (international group of experts on the explosion risks of unstable substances – working group: energetic and oxidizing substances) installed an ad-hoc working group in 2002 assigned with the task of proposing solutions for the existing prob-lems. The adequacy of such proposals has to be proven preferably by interlaboratory comparison (interlaboratory test) before they are presented to the UN Sub Committee for adoption into the UN Test Manual. The present report is the evaluation of an interlaboratory test which was designed by the Ad-hoc working group in order to find out whether the current method of comparing combustion times of test mixtures with those of reference mixtures is suitable in principle and whether some approaches for improvement of the method can be identified.
Die Mikro- und Nanotechnologie gehört zu den Schlüsseltechnologien des 21. Jahrhunderts mit hohen Wachstumsprognosen, wie auch die im Auftrag des BMBF durchgeführte Studie “Nanotechnologie als wirtschaftlicher Wachstumsmarkt” von 2004 ausführlich darstellt. Aus diesem Trend resultiert ein steigender Bedarf an Messsystemen, die Nanostrukturen prozessnah bzw. im Fertigungsprozess charakterisieren können. Virtuelle Messgeräte liefern Erkenntnisse zur Entwicklung neuartiger Messsysteme, Analyse und Optimierung bestehender Verfahren sowie die Bestimmung der Messunsicherheit und modellbasierten Korrektur systematischer Fehler. Der virtuelle Messprozess umfasst neben dem Messmittel auch die Probe und die Wechselwirkungen zwischen beiden. In diesem Beitrag werden virtuelle Messgeräte vorgestellt sowie deren Anwendung diskutiert.
The classification of solid oxidizers according to the regulations on the transport of dangerous goods (based on the UN Recommendations/Model Regulations and accepted by all international organisations for the transport of dangerous goods as ADR, IMO, IATA) and in future also according to the GHS (Globally Harmonized System of Classification and Labelling of Chemicals) is performed on the basis of the results of the UN test O.1 (UN test O.1 ―Test for oxidizing solids‖ described in chapter 34.4.1 in the Recommendations on the Transport of Dangerous Goods – Manual of Tests and Criteria, see [1]). This test was introduced into the UN Manual of Tests and Criteria in 1995 as a replacement for a similar test from 1986. Even if the UN O.1 test as described in the current 5th revised edition of UN Manual of Tests and Criteria gives some improvements compared to the old test, which had had many deficiencies, there are still some problems left with this test in terms of e.g. repeatability or reproducibility of test results, how to handle compacted or multilayer formulations like tablets, toxicity and partly significantly varying particle size distribution within defined fractions of 150 μm to 300 μm of the reference oxidizer potassium bromate (KBrO3). For this reason the IGUS EOS working group installed an ad-hoc working group in 2002 assigned with the task to propose solutions for the existing problems. The appropriateness of such proposed solutions has to be proved by the method of interlaboratory (round robin) tests before they are presented for the adoption to the UN Committee of Experts on the TDG and on the GHS with a proposal of a completely revised test procedure.
Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are critical components of every industrial chemical process as they provide information on the concentrations of individual compounds and by-products. These processes are carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been developed to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra to train an ANN with better prediction performance and speed than state-of-theart analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a possible strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control.
For the classification and safe handling and use of the chemicals, special standardized testing proce-dures have been developed and are used world-wide. Safety experts must be able to fully rely on the precise execution of the respective laboratory tests and assessments. In this context interlaboratory tests (round robin tests, interlaboratory comparisons / intercomparisons) are a crucial element of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025.
The present document reports on the results of the interlaboratory test 2010/2011 on the test method DIN EN 15188:2007 “Determination of the spontaneous ignition behaviour of dust accumulations” [1] which was organized by the Center for Quality Assurance for Testing of Dangerous Goods and Haz-ardous Substances.
The test method DIN EN 15188:2007 is applied to characterize the self-ignition behaviour of combus-tible dusts. The experimental basis for describing the self-ignition behaviour of a given dust is the de-termination of the self-ignition temperatures (TSI) of differently-sized volumes of the dust sample by isoperibolic hot storage experiments (storage at constant oven temperatures) in commercially availa-ble ovens. The results thus measured reflect the dependence of self-ignition temperatures upon dust volume [1].
Several internal investigations and interlaboratory comparisons in the past have shown significant differences between the lab-specific results of hot storage tests.
Figure 2-1 shows the Pseudo-Arrhenius plot of hot storage tests of eight different laboratories (Round Robin Test 2002, BAM). The dust under this investigation was Lycopodium powder (spores). The par-ticipants of this interlaboratory test used different laboratory ovens (size, ventilation) as well as differ-ent sample baskets (shape, mesh size, single- and double-walled).
Figure 2-1 shows clearly that this test failed to produce reasonable reproducibility of the TSI between the different laboratories. As possible reasons for the deviations have been identified lab-specific dif-ferences, e.g.:
- oven ventilation (enforced, natural convection),
- oven size,
- sample baskets,
- radiation effects,
- measuring precision (temperature difference between tests with ignition and no ignition),
- minimum sample size.
To reduce the differences between the labs it was necessary to ameliorate the testing method and to improve the execution of the method by the lab. From there, the installation of an inner chamber into the laboratory oven was suggested as experimental set-up in EN 15188:2007 to provide more repro-ducible test conditions. The aappropriateness of this set-up has not been verified yet.
The current interlaboratory test 2010-2011 focuses on the use of a special mesh wire screen and spe-cial volumes of the sample baskets (cubes) to normalise/harmonise the test conditions in the different labs. In preparation for the interlaboratory test a joint program between Syngenta and BAM has been initiated in 2009. As a result of these investigations a modified set-up ( chapter 3) has been identi-fied to be probably more appropriate than the suggested set-up in DIN EN-15188:2007.
Due to the time-consuming test procedure and to optimize the workflow for the laboratories this in-terlaboratory test should be performed stepwise as a multi-level test ( chapter 5.4) on one typical test sample.
Digital image analysis
(2011)
Comparatiye digital analysis was performed on the five moon drawings from the New York copy of the Sidereus Nuncius and the copperplate etchings printed in the Graz and Florence copies. The sequences of figures for the drawings on pages 8r, 9v and lOv demonstrate the process of digitally enhancing the black material on the drawings, isolating that material and then overlaying it on the etchings. Using an image editing program (Image Pro® Plus by Media Cybernetics) the black material on the drawings and the letterpress-printed text were isolated and segmented from the brown drawing media. As shown in Figs. 4, 6 and 8, the isolation was possible and the black material clearly overlaps the demarcation line in the drawings. To compare the drawn and printed images of each moon, the images were laid on top of each other with Adobe Photoshop® (Adobe Systems). In these images, the printed text was used for alignment and scale. By decreasing the opacity of the image on top, the lines of each image were compared. This technique revealed an almost one-to-one correlation between the demarcation line in the drawing (as indicated by the black material) and that on the etching. In each case, the similarities and concurrences by far outnumbered the minor deviations in line. One precondition of this work was that all the photographs be at the same angle, plane-parallel, so that the drawings could be compared with the etchings. A slight aberration in the plane could distort the geometry of the illustrations. Rectification of the image plane was carried out by means of the program metigo® MAP 2.2 (Fokus GmbH Leipzig). To validate the method, photographs from the same detail of the New York copy taken with different photographic cameras and different Parameters were rectified with metigo® MAP and compared in Adobe Photoshop®. The overlay of these photographs shows a good correlation in the layout of the lettering and moon figures with only small aberrations. The distribution of the black material on the drawings can be followed as clearly in the rectified photographs as in the unrectified photographs, the information is the same.
Leaching experiments on the release of heavy metals and PAH from C&D waste and MSWI bottom ash
(2010)
Leaching tests are fundamental tools for the assessment of long-term impact of
contaminated waste materials on the soil-groundwater pathway. Waste materials should be
tested under conditions equal to their actual application in re-use scenarios to achieve reliable
results. Since the standards for leaching procedures available on international level so far are
either not validated or considered inadequate in respect to coarse grained materials, new
standards had to be developed. Therefore column percolation and batch test procedures have
been standardized and validated to enable their introduction to new German regulations
concerning waste management. Practical aspects of the test procedures as well as the
boundary conditions compared to the already existing standards will be described. Examples
including round robin test results will be given to justify the selection of the new
specifications.