Richard J. Ewen

Highly sensitive mixed oxide sensors for the detection of ethanol

Sensors consisting of mixtures of tin dioxide and zinc oxide powders in a range of proportions were constructed. Each mixture was applied to an electrode-bearing alumina substrate either as a paste, or by screen printing. The responses of these sensors, and of three commercially-available Figaro sensors, to ethanol vapour in the 1–1000 parts-per-billion (ppb) range were measured. At 100 ppb of ethanol vapour, the most sensitive paste sensor (25% SnO2/75% ZnO) exhibited a response that was more than twice that of the screen-printed sensors, and almost 60 times greater than that of the most sensitive Figaro sensor (TGS822).

The development of a sensor system for the early detection of soft rot in stored potato tubers

A number of sensor types were fabricated and tested for their electrical resistance changes to compounds known to be evolved by potato tubers with soft rot caused by the bacterium Erwinia carotovora. On the basis of these tests, three sensors were selected for incorporation into a prototype device. The device was portable and could be used without computer control after threshold values and sensor settling criteria had been downloaded. The prototype was assessed for its discriminating power under simulated storage conditions. The device was capable of detecting one tuber with soft rot in 100 kg of sound tubers in a simulated storage crate. The device was also able to detect a tuber inoculated with E. carotovora, but without visible signs of soft rot, within 10 kg of sound tubers. The same system was able to follow the progression of the disease in a tuber stored amongst 10 kg of sound tubers when operated at 4 °C and 85% relative humidity (conditions typical of a refrigerated storage facility).

Novel composite organic–inorganic semiconductor sensors for the quantitative detection of target organic vapours

Composites of tin dioxide (an n-type semiconductor) and derivatives of the conducting polymer polypyrrole (a p-type semiconductor) gave reversible changes in electrical resistance at room temperature when exposed to a range of organic vapours. The optimum amount of polymer giving highest sensitivity was found by experiment to be 2.5% by mass for the polypyrrole chloride-tin dioxide composite. Composites containing 2.5% polymer by mass but differing in polymer derivative, were fabricated and exposed to low concentrations of ethanol, methanol, acetone, methyl acetate and ethyl acetate. All were found to give significant and reversible decreases in electrical resistance. Direct comparison with sensors constructed solely of tin dioxide or polypyrrole at room temperature showed the composites to be more sensitive. The gas sensitivity of the composite materials depended on the type of polymer derivative incorporated and the dopant anion associated with the polymer. The composites were simple to fabricate and gave differing response profiles to a range of organic vapours.

Identification by gas chromatography-mass spectrometry of the volatile organic compounds emitted from the wood-rotting fungi Serpula lacrymans and Coniophora puteana, and from Pinus sylvestris timber

Volatile organic compounds (VOCs) emitted by two wood-rotting basidiomycete fungi, Serpula lacrymans (dry rot fungus) and Coniophora puteana (cellar fungus), and the timber of Pinus sylvestris (Scots pine), were identified. Several volatile collection techniques were employed including dichloromethane solvent extraction, solid-phase microextraction (SPME) and thermal desorption of VOCs entrained on Tenax GR. In addition, a new method of solid sample injection (SSI) is described which utilises a low injector temperature and an all-glass deactivated injector liner designed to minimise both the formation of pyrolysis products and analyte degradation. All the volatile compounds collected were analysed using electron impact capillary gas chromatography-mass spectrometry (GC-MS) on HP-5, HP-Innowax and beta-cyclodextrin columns. SSI and Tenax thermal desorption were found to be the most effective extraction methods. A total of 19 VOCs were observed from S. lacrymans grown on glass slides and pine, 15 from C. puteana grown on glass slides and 12 from P. sylvestris timber. S. lacrymans was found to emit, in low abundance, six unique VOCs, of which 2-methylbutanal was the greatest. The major volatile compound emitted by S. lacrymans was 1-octen-3-ol, which was also found in lower abundance from C. puteana. Six VOCs, including diethylene glycol and 4-methyl methylbenzoate, were found to be unique to C. puteana, all in medium abundance: From P. sylvestris, the major volatiles identified were S-alpha-pinene and 3-carene.

Dark DC conductivity and spectroscopy of clean and gas doped thin films of organic semiconductors

Abstract The dark DC conductivity of thin films of phthalocyanine (I), meso -tetra( p -methylphenyl)porphin (II), meso -tetraphenylporphin (III), hemiporphyrazine (IV), dihydrodibenzo [ b , i ][1,4,8,11] tetra-azacyclotetradecine (V) and three derivatives of V have been studied in vacuo and in the presence of a wide range of gases. The only gases to produce marked increases in the conductivity were electron acceptors; however, IV was unaffected even by these. The interactions of I, II, III and V and its derivatives with NO 2 N 2 O 4 (NOX) were of particular interest and were studied by conductivity measurements, UV/VIS and IR transmission spectroscopy and IR reflectance spectroscopy. The material most sensitive to NOX and other electron acceptors was I; however, V has a favourable combination of sensitivity coupled with reversibility at room temperature. The Interactions of NOX with I, II and HI are complex, and there is spectroscopic evidence for the generation of NO 2 and the organic radical cations.

Cospray-dried unfractionated heparin with L-leucine as a dry powder inhaler mucolytic for cystic fibrosis therapy

Accumulation of inspissated secretions that are difficult to clear and congest the airways is a feature of lung disease in patients with cystic fibrosis (CF). These secretions restrict airflow, harbour infection and limit the delivery of inhaled drugs including gene therapy vectors to the underlying target cells. Unfractionated heparin (UFH) has mucolytic properties suggesting that it may be a useful therapeutic agent for lung disease in these patients. For the pulmonary delivery of UFH to patients with CF, the dry powder inhaler has potential advantages over systems using nebulised suspensions. However, spray-dried particles in the appropriate size range (1-5 microm) may absorb atmospheric moisture, causing aggregation. UFH has been cospray-dried with L-leucine (1%, w/w) to produce particles that are less cohesive than UFH alone and show good aerosolisation performance. Rheological analysis has shown that spray-dried UFH and UFH cospray-dried with L-leucine significantly (p < 0.05) reduce the elasticity and yield stress of CF sputum. The superior physical properties of UFH/L-leucine indicate this is the preferred formulation for development as an inhaled mucolytic.

A study of the catalytic and vapour-sensing properties of zinc oxide and tin dioxide in relation to 1-butanol and dimethyldisulphide

Abstract Thick film sensors were produced from pastes of tin dioxide, zinc oxide and a mixture of the two materials. The sensors were operated at a temperature of 350°C and their electrical responses to 1-butanol and DMDS in the concentration range 1–100 vpm were monitored. Thin film tin dioxide sensors were also fabricated by evaporating tin metal through an oxygen plasma and the resulting sensors tested for their responses to the vapours. A number of commercially available Figaro sensors were also tested against the same vapours for comparison. The sensors comprising tin dioxide and zinc oxide combined gave the largest changes in electrical resistance when exposed to the test vapours. The catalytic effect of tin dioxide, zinc oxide and a composite material of the two upon selected test vapours was elucidated using GC-MS and 1 H -NMR spectroscopy. The results offer some insight into the mechanisms by which metal oxide semiconductors catalytically break down organic vapours at elevated temperatures. The results also show that these mechanisms differ in the case of tin dioxide and zinc oxide.

An analysis of volatiles in the headspace of the faeces of neonates

A gas chromatography/mass spectrometry (GCMS) analysis of the headspace from the faeces of neonates was undertaken to record the volatiles associated with preterm babies on a neonatal unit. The compounds ethanol, acetone, 2-ethyl-1-hexanol, 3-methylbutanal, hexanal and 2,3-butanedione occurred with the highest frequency. The volatiles analysed were then compared to a previously published study of the volatiles from asymptomatic adult faeces. Fewer compounds were found in the neonatal faeces and virtually no sulfides were detected, in contrast to the adult samples where carbon disulfide, dimethyl disulfide and dimethyl sulfide were ubiquitous. In addition, 7 of the most abundant 15 volatile compounds were found to be aldehydes, while in contrast only 2, acetaldehyde and benzaldehyde, were present in the most abundant 15 compounds found in the headspace of adult faeces. 2-Ethyl-1-hexanol was considerably more abundant in the neonate stool compared to adult stool, and probably reflects high exposure to plastic materials containing plasticizers. The potential of disease diagnoses from the analysis of volatiles emitted from neonate faeces is discussed.

Inhibiting bacterial adhesion onto surfaces : the non-stick coating approach

The use of low-surface-energy poly(methylpropenoxyfluoroalkylsiloxane) or poly(perfluoroacrylate) coatings as a potential means of inhibiting the bacterial colonisation of surfaces, is described and discussed.

A sensor system for monitoring the simple gases hydrogen, carbon monoxide, hydrogen sulfide, ammonia and ethanol in exhaled breath.

A sensor array system was constructed incorporating electrochemical sensors for hydrogen, carbon monoxide, hydrogen sulfide and ethanol, a ceramic sensor for total volatiles and a dye-based optical ammonia sensor. The system was calibrated using standard gases balanced with dry air. Limit of detection and % relative standard deviation values (n = 10) for the sensors in the array are hydrogen (0.1 ppm, 2.6%), carbon monoxide (0.4 ppm, 2.1%), ethanol (0.5 ppm, 1.5%), hydrogen sulfide (0.1 ppm, 1.5%) and ammonia (0.6 ppm, 10.7%). Humidity effects were assessed by calibrating with humidified standard gases (hydrogen, carbon monoxide) or spiked breath samples in Tedlar bags (hydrogen sulfide, ethanol and ammonia). The calibration data were used to establish a cross-sensitivity matrix. The concentration of breath volatiles was found to be dependent on exhalation rate and exhalation volume. A test protocol based on these data required volunteers to exhale 1 litre of breath at a rate between 7.5 and 17.5 l min(-1). Sensor responses were measured for 40 s then purged at 7 l min(-1) (150 s). A longitudinal study was undertaken of ten asymptomatic volunteers over a five-day period. Volunteers ate an ad hoc diet, but fasted prior to giving the first breath sample and then gave samples every hour for 8 h. Breath hydrogen levels for volunteers showed large variations within a day and also from day to day. Fasting levels ranged between 0.3 and 34.1 ppm (mean 9.1 ppm). The carbon monoxide levels for non-smokers were between 0.6 and 4.9 ppm (mean 2.1 ppm), whilst for smokers they were between 8.3 and 18.7 ppm (mean 12.8 ppm). The measured levels of other gases on breath were as follows: hydrogen sulfide (0-1.3 ppm, mean 0.33 ppm), ethanol (0-3.9 ppm, mean 0.62 ppm) and ammonia (0-1.3 ppm mean 0.42 ppm). The system was capable of direct quantitative measurements of low concentrations of a range of volatiles on exhaled breath. The measured values for compounds on the breath of asymptomatic volunteers were in broad agreement with quoted literature ranges. The system will now be assessed in a clinical setting.