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Repper S.E.,University of Sheffield | Haynes A.,University of Sheffield | Ditzel E.J.,Hull Research and Technology Center | Sunley G.J.,Hull Research and Technology Center
Dalton Transactions | Year: 2017

Absorption of carbon monoxide by copper(i)-containing ionic liquids, [Cnmim][CuX2] (Cnmim = 1-alkyl-3-methylimidazolium, n = 2, 4, 6, X = Cl, Br, I) has been investigated using in situ high pressure infrared spectroscopy. For each liquid, observation of a ν(CO) band in the region 2075-2090 cm-1 indicates the formation of copper(i) monocarbonyl complexes, assigned as [Cu(CO)X2]-. The rate of growth and equilibrium intensity of the ν(CO) absorption is dependent on applied CO pressure. Binding of CO is reversible such that complete desorption occurs rapidly on heating above 100 °C and the liquids are robust over multiple gas absorption/desorption cycles. For the series of [C6mim][CuX2] salts the CO absorption ability follows the order Cl ≥ Br> I. Selective absorption of CO from CO/H2 and CO/N2 gas mixtures is demonstrated by measuring the changes in headspace CO content upon absorption and desorption of gas. For [C6mim][CuCl2], a single absorb-vent-desorb cycle yields product gas containing ∼95% CO starting from a 1:1 CO/N2 mixture, increasing to ∼98% CO starting from a 4:1 CO/N2 mixture. This is particularly promising in view of the similar boiling points of CO and N2 that hinders their separation by cryogenic distillation. © The Royal Society of Chemistry.


Carter S.,Hull Research and Technology Center | Fisher A.S.,University of Plymouth | Goodall P.S.,British Nuclear Fuels Limited | Hinds M.W.,Royal Canadian Mint | And 2 more authors.
Journal of Analytical Atomic Spectrometry | Year: 2010

It is a noticeable trend over the last couple of review periods that the number and quality of nuclear applications has been increasing. That trend has continued into this year. Semiconductors and other electronic components continue to become smaller and utilise more pure materials; hence analysing them becomes more difficult. This is especially true when depth-resolved data is required. Techniques capable of analysing with ever increasing depth resolution are therefore necessary and many studies into this have been reported. There is still a large interest in the non-destructive analysis of archaeological or historical materials (glasses, ceramics, paintings etc.). The use of solid sampling techniques that cause minimal damage is therefore still gaining in popularity. This is especially true for laser-based techniques such as LIBS and laser ablation, although the many variants of the X-ray-based techniques are also still proving very popular. The increasing trend to use multiple analytical techniques, ideally simultaneously to cause minimal damage and to obtain the maximal number of results in the shortest time, is also noted. These attempts to obtain maximum information are, again, mainly true for historical artefacts where obtaining more analytical information will lead to a better understanding of provenance, manufacturing process, etc.The real time analysis being undertaken in engines and at coal fired boilers is also an interesting development. These real time analyses allow monitoring of the systems and enable any deviations from peak performance to be identified and corrected in the shortest time possible. © 2010 The Royal Society of Chemistry.


Carter S.,Hull Research and Technology Center | Fisher A.S.,University of Plymouth | Goodall P.S.,British Nuclear Fuels Limited | Hinds M.W.,Royal Canadian Mint | And 2 more authors.
Journal of Analytical Atomic Spectrometry | Year: 2011

There is considerable interest in the non-destructive analysis of archaeological or historical materials (glasses, ceramics, paintings, materials etc.). The use of solid sampling techniques that cause minimal damage is therefore still gaining in popularity. This is especially true for laser-based techniques such as LIBS and laser ablation, although the many variants of the X-ray-based techniques are also still proving very popular. Non-destructive analysis is also the ideal scenario for forensic scientists and therefore many of these applications are using similar techniques. The increasing trend to use multiple analytical techniques, ideally simultaneously, to cause minimal damage and to obtain the maximal number of results in the shortest time, is also noted. The technique of LIBS, which offers minimal sample damage and a "stand-off" capability is still gaining in popularity, although there are still question marks regarding its quantitative capabilities for some sample types. There is also considerable interest in the growing area of thin films and depth-profiling. Substantial research is on-going to develop methods to improve depth-resolution and several different approaches have been described in the literature. These approaches often use SIMS with either a lower energy primary beam or a primary beam consisting of polyatomic molecules. © 2011 The Royal Society of Chemistry.


Gibson B.,Intertek | Carter S.,Hull Research and Technology Center | Fisher A.S.,University of Plymouth | Lancaster S.,Domino Printing science Ltd | And 2 more authors.
Journal of Analytical Atomic Spectrometry | Year: 2014

This review covers developments in the analysis of chemicals, metals and functional materials. We have strengthened the criticality of this review and have included only those papers dealing with advances in the analysis of these materials. Other papers which the reader may find useful because they cover interesting applications are included in the tables. It follows last year's review1 and should be read in conjunction with other reviews in the series.2-5 Significant developments during this review period include the continued expansion of the use of LIBS in remote analysis, especially of explosives, metals and nuclear materials. The stand-off capability of the technique makes it very desirable in these areas. The use of chemometrics for removing substrate interferences is proving to be effective in making the technique more robustly quantitative and a number of papers developing the understanding of plasma physics to improve the technique of LIBS are reviewed. Multiple spectroscopic techniques are being developed to maximize the knowledge which can be derived from the analysis, especially of high value samples, for example the combination of LIBS and Raman measurements to gain molecular and atomic spectral information. Advances in the analysis of nanomaterials and single particles are reviewed and papers dealing with single particle analysis, field flow fractionation and related techniques coupled with ICP-MS are advancing the analytical chemistry in the field. These techniques are also increasingly being used in vivo and in biological areas. Depth profiling of semiconductor materials is an important area during this review period, especially for the determination of dopant elements. There are significant changes to the writing team this year. Mike Hinds has left the team and we are pleased to welcome Bridget Gibson and Ian Whiteside. © the Partner Organisations 2014.


Carter S.,Hull Research and Technology Center | Fisher A.,University of Plymouth | Garcia R.,Technology Center | Gibson B.,Intertek | And 3 more authors.
Journal of Analytical Atomic Spectrometry | Year: 2015

There has been significant progress in the use of laser induced breakdown spectrometry (LIBS) as a method of monitoring steel production in real time. This has the benefits of both time and cost saving. There has been a drop in the number of papers reporting methods for the analysis of fuels. This may be a function of the drop in oil prices leading to reduced finance for research. However, the determination of S is one of the hot topics in this sample type. This is possibly a consequence of companies attempting to meet the increasingly strict regulations on S emissions. Analytical methodology, e.g. LA-ICP-MS, LIBS or XRF, which produces minimal damage to the samples is still increasingly popular. This is especially true for historical or archaeological sample types, e.g. paintings, pottery and old documents; but is also applicable to forensic materials. Often, with these sample types, the analytical data are then treated using chemometrics packages so that provenance may be determined or patterns detected. Similar methodology was used for the identification of different plastics types, facilitating sorting and re-cycling. The analysis of nanoparticles is an increasingly popular subject area. Simple introduction of samples containing nanoparticles through a standard nebuliser/spray chamber sample introduction system is often complicated by the particles agglomerating. This leads to under-estimations of the concentrations present. Single particle analysis has continued to be a popular research area with real samples now being extracted and analysed rather than standard solutions. Similarly, field flow fractionation coupled with ICP spectrometry (sometimes also in conjunction with single particle analysis) has also been used to characterize nano-particulates and to distinguish between particulate and ionic species. © 2015 The Royal Society of Chemistry.


Carter S.,Hull Research and Technology Center | Fisher A.S.,University of Plymouth | Hinds M.W.,Royal Canadian Mint | Lancaster S.,Domino Printing science Ltd | Marshall J.,University of Glasgow
Journal of Analytical Atomic Spectrometry | Year: 2013

This review period has seen some changes to the format of the review. These changes are intended to more accurately reflect the current state of analytical research in the analysis of metals, chemicals and materials. As a consequence, the title of the review and some of the section headings have been altered to reflect this. Significant areas of growth include the use of LIBS in remote analysis, especially of explosives and nuclear materials. The stand-off capability of the technique makes it very desirable in these areas. The use of chemometrics and procedures for removing substrate interferences are proving to be effective in making the technique more quantitative. It is also beginning to be reported for use in Process Analysis in the pharmaceuticals industry and has been employed to investigate the processes occurring within an engine and to model the processes occurring in explosions. The analysis of archaeological, cultural heritage and art objects continues to be a significant area of research, with some interesting developments in multi-analytical techniques which are employed to yield maximum information with as little disruption to the object as possible. Similarly, the high resolution capabilities of synchrotron radiation are being increasingly employed for high value objects where the cost of the analysis is outweighed by the benefits. In the field of materials analysis, the development of techniques for investigating the growth of novel material structures is a significant activity, e.g., the nucleation of alpha Alumina via titania templates, studied using a range of techniques. Papers outlining advances in the use of asymmetric field flow fractionation with a multi-detection approach for the characterisation of particle size and size distribution are reviewed as is a comparison of hydrodynamic chromatography with AFFF. Papers dealing with single particle analysis are also reviewed. The catalyst section is shorter than in previous reviews and this reflects the fact that fewer new developments in analytical chemistry are being published. The emphasis is on advances in the analysis of catalyst materials. This is the latest review covering advances in atomic spectrometric measurements of metals, chemicals and materials. It follows on from last year's review1 and should be read in conjunction with other reviews in the series.2-5 This year will be the last time that Mike Hinds will write for the review. His contribution over many years has been very significant and greatly appreciated. We welcome John Marshall to the writing team. © 2013 The Royal Society of Chemistry.


Haider M.H.,University of Cardiff | Haider M.H.,SABIC | Dummer N.F.,University of Cardiff | Knight D.W.,University of Cardiff | And 5 more authors.
Nature Chemistry | Year: 2015

The production of biodiesel from the transesterification of plant-derived triglycerides with methanol has been commercialized extensively. Impure glycerol is obtained as a by-product at roughly one-tenth the mass of the biodiesel. Utilization of this crude glycerol is important in improving the viability of the overall process. Here we show that crude glycerol can be reacted with water over very simple basic or redox oxide catalysts to produce methanol in high yields, together with other useful chemicals, in a one-step low-pressure process. Our discovery opens up the possibility of recycling the crude glycerol produced during biodiesel manufacture. Furthermore, we show that molecules containing at least two hydroxyl groups can be converted into methanol, which demonstrates some aspects of the generality of this new chemistry. © 2015 Macmillan Publishers Limited.


Owen A.W.,University of Strathclyde | Nordon A.,University of Strathclyde | Littlejohn D.,University of Strathclyde | Lynch T.P.,Hull Research and Technology Center | And 2 more authors.
Analytical Methods | Year: 2014

A thermal vaporiser has been designed for analysis of liquid streams by a process mass spectrometer normally used for gas analysis. Concentrations of benzene, toluene and o-xylene at mg kg-1levels in ethanol were determined from continuous vaporisation of the liquid. Ions with m/z values of 39, 57, 73, 77, 78, 91, 92 and 106 were selected and the optimal regression model (multiple linear regression with mean-centring) was found using an automated design of experiments approach to calibration model selection. It was discovered that the linearity of the response allowed excellent calibration to be performed using only four standards (at 0 and 110 mg kg-1for each of the three analytes) and that there were minimal inter-analyte interferences. The detection limit of benzene, toluene and o-xylene was 0.5, 0.8 and 0.5 mg kg-1, respectively. Average differences between the actual and predicted concentrations, expressed as a percentage of the actual concentrations, for 27-82 mg kg-1of benzene, toluene and o-xylene were 0.5-1.4%, 0.0-0.4% and 0.3-1.6%, respectively, while the average relative standard deviations were 1.3-2.6%, 1.0-2.5% and 1.1-2.3%, respectively. Detection of 3 mg kg-1changes in the concentration of each of the analytes (at the 36 mg kg-1level) was also demonstrated, indicating the sensitivity of the technique and the potential ability of the procedure to detect minor deviations in the specification of process streams from continuous analysis. © the Partner Organisations 2014.


Carter S.,Hull Research and Technology Center | Fisher A.S.,University of Plymouth | Hinds M.W.,Royal Canadian Mint | Lancaster S.,Domino UK Ltd
Journal of Analytical Atomic Spectrometry | Year: 2012

This review period has shown several areas of growth. The increase in popularity of LIBS continues as the problems, both real and perceived, that are associated with it (e.g., that it is capable only of qualitative analyses) are overcome. The area that appears to have seen the greatest increase in LIBS work is the nuclear industry. Presumably this is because of the stand-off ability of the technique. Another technique that is increasing in popularity is continuum source AAS. This has found substantial use in several areas of the review, notably the fuels and the organic chemicals sections. As noted in the review, the technique allows similar multi-elemental detection to ICP-OES (albeit at lower sensitivity), but at AAS running costs and is therefore likely to remain a popular technique. The necessity of causing no or minimal damage to forensic samples and for samples of archaeological or historical importance is still paramount. Therefore, micro-sampling techniques such as LIBS, LA and various X-ray-based techniques are still popular. Since the reliability of the data obtained from hand-held/portable XRF instruments has improved significantly in recent times, the use of these can be regarded as almost routine. Also noted in the review is the propensity for using multiple techniques, often simultaneously, to characterize materials more fully and more rapidly. This is the latest review covering atomic spectrometric measurements of industrial materials, metals, chemicals and advanced materials. It follows on from last year's review1 and should be read in conjunction with other reviews in the series.2-5 This year has seen the departure of Sian Shore from the writing team. Her efforts over the last few years have been very much appreciated. © 2012 The Royal Society of Chemistry.


Hemingway M.A.,UK Health and Safety Laboratory | Walsh P.T.,UK Health and Safety Laboratory | Hardwick K.R.,UK Health and Safety Laboratory | Wilcox G.,Hull Research and Technology Center
Journal of Occupational and Environmental Hygiene | Year: 2012

Many portable single-gas monitors are used for the detection of low concentrations of hydrogen sulfide (H 2S) and sulfur dioxide (SO 2) in the workplace. With the recent lowering of the H 2S and SO 2 ACGIHR ® threshold limit value ( TLVR ® ) the ability of these devices to selectively respond to these newlower levels is not well documented in petroleum industry environments, which often have potential interfering gases and vapors present aswell as varying environmental conditions. Tests were carried out to measure the ability of various monitors with their respective sensors to correctly quantify and respond to H 2S and SO 2 in a simulated petroleum industry environment. This included the identification of selected interference effects and estimation of the reliable lower limit of detection for real workplace environments. None of the H 2S monitors responded at 0.1 times the new TLV (0.1 ppm), only some of them responded at the new TLV concentration (1 ppm), and all the monitors exposed to five times the new TLV (5 ppm) responded with reasonable accuracy. There was generally little effect of interferent gases and vapors on the H 2S monitors. None of the SO 2 monitors responded at 0.1 and 1 times the new TLV (0.025 ppm and 0.25 ppm) concentrations, and all but one of them exposed to five times the new TLV (1.25 ppm) responded. There was much greater cross-sensitivity to interferents at the tested concentrations with the SO 2 monitors, which responded to six out of eight of the interferents tested. Results demonstrate that these monitors cannot reliably alarm and measure H 2S or SO 2 concentrations at the new TLVs with an acceptable degree of accuracy. However, these monitors are designed to alarm as a safety device; these results do not change this important function.

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