Characterisation of fluidised bed granulation processes using in situ Raman spectroscopy

Previous work by the authors Walker et al. [2007b. Fluidised bed characterisation using Raman spectroscopy: applications to pharmaceutical processing. Chemical Engineering Science 62, 3832–3838] illustrated that Raman spectroscopy could be used to provide 3-D maps of the concentration and chemical structure of particles in motion in a fluidised bed, within a relatively short (120 s) time window. Moreover, we reported that the technique, as outlined, has the potential to give detailed in-situ information on how the structure and composition of granules/powders within the fluidised bed (dryer or granulator) vary with the position and evolve with time. In this study we extended the original work by shortening the time window of the Raman spectroscopic analysis to 10 s, which has allowed the in-situ real-time characterisation of a fluidised bed granulation process. Here we show an important new use of the technique which allows in-situ measurement of the composition of the material within the fluidised bed in three spatial dimensions and as a function of time. This is achieved by recording Raman spectra using a probe positioned within the fluidised bed on a long-travel x–y–z stage. In these experiments the absolute Raman intensity is used to provide a direct measure of the amount of any given material in the probed volume, i.e. a particle density. Particle density profiles have been calculated over the granulation time and show how the volume of the fluidised bed decreases with an increase mean granule size. The Raman spectroscopy analysis indicated that nucleation/coalescence in this co-melt fluidised hot melt granulation system occurred over a relatively short time frame (t<30 s). The Raman spectroscopic technique demonstrated accurate correlation with independent granulation experiments which provided particle size distribution analysis. The similarity of the data indicates that the Raman spectra accurately represent solids ratios within the bed, and thus the techniques quantitative capabilities for future use in the pharmaceutical industry.

Development and Longer Term In Situ Evaluation of Fiber-Optic Sensors for Monitoring of Structural Concrete

In this paper, new solutions to the problem of making measurements, of carbonation and chloride ingress, in particular, in concrete structures are considered. The approach has focused on the design, development, and use of fiber-optic sensors (FOSs), recognizing the need in that conventional devices are often either inaccurate, expensive, or unsuitable for encapsulation in the material. The sensors have been designed to monitor, in situ and nondestructively, relevant physical, and chemical changes in cementitious materials. Three different types of FOS were constructed, tested, and evaluated specifically for this application, these being a temperature sensor (based on the fluorescence decay) and pH and chloride sensors, based on sol-gel (solidified gel) technology with appropriate impregnated indicators. The sensors were all designed to be inserted into the structures and evaluated under the harshest conditions, i.e., being mounted when the mortar is poured and thus tested in situ, with the temperature and pH sensors successfully embedded in mortar. The outcomes of these tests have shown that both the temperature sensor and the pH sensor were able to function correctly for the duration of the work - for over 18 months after placement. The laboratory tests on the chloride sensor showed it was able to make measurements but was not reversible, limiting its potential utility for in situ environments. Research is ongoing to refine the sensor performance and extend the testing.

In situ cross-calibration of in-fibre Bragg Grating and Electrical Resistance Strain Gauges for structural monitoring using an extensometer

Special issue on Sensor Systems for Structural Health Monitoring Abstract—This study addresses the direct calibration of optical fiber strain sensors used for structural monitoring and is carried out in situ. The behavior of fiber-Bragg-grating-based sensor systems when attached to metal bars, in a manner representative of their use as reinforcement bars in structures, was examined and their response calibrated. To ensure the validity of the measurements,this was done using an extensometer with a further calibrationagainst the response of electrical resistance strain gauges, often conventionally used, for comparison. The results show a repeatable calibration generating a suitable geometric factor of extension to strain for these sensors, to enable accurate strain data to be obtained when the fiber-optic sensor system is in use in structural monitoring applications.

In situ measurement of UHF wearable antenna radiation efficiency using a reverberation chamber

The radiation efficiency and resonance frequency of five compact antennas worn by nine individual test subjects was measured at 2.45 GHz in a reverberation chamber. The results show that, despite significant differences in body mass, wearable antenna radiation efficiency had a standard deviation less than 0.6 dB and the resonance frequency shift was less than 1% between test subjects. Variability in the radiation efficiency and resonance frequency shift between antennas was largely dependant on body tissue coupling which is related to both antenna geometry and radiation characteristics. The reverberation chamber measurements were validated using a synthetic tissue phantom and compared with results obtained in a spherical near field chamber and finite-difference time-domain (FDTD) simulation.

Self-potential signatures associated with an injection experiment at an in situ biological permeable reactive barrier

Strategies available to evaluate the performance of in situ permeable reactive barriers are currently not well developed and often rely on fluid and media sampling directly from the permeable reactive barrier (PRB). Here, we investigate the utility of the self-potential (SP) method as a technique to monitor in situ PRB performance. Our field study was conducted at in situ biological PRB in Portadown, Northern Ireland, UK, which was emplaced to assist in the remediation of groundwater contamination (e.g., hydrocarbons, ammonia) that resulted from the operations and waste disposal practices of a former gasworks. Borehole SP measurements were collected during the injection of contaminant groundwater slugs in an attempt to monitor/detect the response of the microbial activity associated with the breakdown of the added contaminants into the PRB. In addition, an uncontaminated groundwater slug was injected into a different portion of the PRB as a ‘control’ and SP measurements were collected for comparison to the SP response of the contaminant slugs. The results of the SP signals due to the contaminant injections show that the magnitude of the response was relatively small (<10 mV) yet showed a consistent decrease during both contaminant injections. The net decrease in SP recorded during the contaminant injections slowly rebounded to near background values through ~44 hours post-injection. The SP response during the uncontaminated injection showed a slight, albeit negligible (within the margin of error), 1 mV increase in the measured SP signals, in contrast to the contaminant injections. The results of the SP signals recorded from the uncontaminated groundwater injection also persisted through a period of ~47 hours after injection but show a net increase in SP relative to pre-injection values. Based on the difference in SP response between the contaminated and uncontaminated injections, we suggest that the responses are likely to be the result of differences in the chemistry of the injection types (contaminated versus uncontaminated) and in situ groundwater. We argue that the SP signals associated with the contaminated injections are dominated by diffusion (electrochemical) potential, possibly enhanced by a microbial effect. While the results of our investigation show a consistent SP response associated with the contaminant injections that is dominated by diffusional effects, further studies are required in order to better understand the effect of microbial activity on SP signals and the potential utility for the SP method to detect/monitor changes that may be indicative of biological PRB performance.