Determination of cadmium and lead in fruit juices by stripping chronopotentiometry and comparison of two sample pretreatment procedures

A method for the determination of cadmium and lead in apple and pear fruit juices by stripping chronopotentiometry (SCP) is described. The results obtained after previous digestion of the sample with concentrated sulphuric acid and dry-ashing (sample pretreatment procedure “A”) and after a treatment with concentrated hydrochloric acid followed by heating in hot water bath (sample pretreatment procedure “B”) were compared. The sample pretreatment procedures were tested on real fruit juice samples and all data confirmed that the efficiency of procedure A was greater than procedure B. In particular, for samples treated with procedure A, good linearity was obtained in the range of examined concentration as is shown by the determination coefficients that were 0.998 (n = 4) for cadmium and 0.996 (n = 4) for lead. Recoveries of 86–104% for cadmium and of 87–102% for lead were obtained from a sample spiked at different levels. The accuracy was also evaluated by means of a matching reference sample of spiked skim milk powder (BCR 150—Community Bureau of Reference) to prove the reliability of the method. The detection limits were 2.0 ng g⁻¹ for cadmium and 4.8 ng g⁻¹ for lead. The relative standard deviations (mean of nine determinations), evaluated on a real sample, were 7.8% and 6.5% respectively. The average content was in the range not detectable–3.0 ng g⁻¹ for cadmium and 8.2–21.3 ng g⁻¹ for lead.     

Simple methods for rapid determination of sulfite in food products

Two simple methods for sulfite determination in food products were proposed. The modified para-rosaniline (PRA)-formaldehyde method showed a much broader linear range (0.05–5.0 mg l⁻¹ as SO₂) than the commonly used procedure for the sulfur dioxide detection in the atmosphere (0.05–1.0 mg l⁻¹ as SO₂). By using a standard reference color card, this method only needed 5 min to complete a test. The 5,5′-dithiobis(2-nitrobenzoic acid) (DTNB) method was another good alternative for rapid determination of sulfite since it only needed one main reagent and the method was robust and easy to operate with the linear range of 0.10–4.3 mg l⁻¹ as SO₂. When applying to real food samples, the DTNB method had good recoveries for all the tested samples and the results agreed well with those obtained by the official iodometric titration. The modified PRA-formaldehyde method worked well with all the tested dried food products, though matrix effect of sulfite binding was observed for the beer samples. Thus, the modified PRA-formaldehyde method has advantages of sensitivity and rapidity, but the DTNB method offers a wider range of applications. Both methods provided practical ways for in situ determination of sulfite by non-professional operators with the modified PRA-formaldehyde method suited for food samples with less sulfite binding problems.     

Aspects of the safety of fish caught off the coast of Qatar

Uncooked, edible portions (including skin) of 20 species of marine fish popular with consumers in Qatar were examined for levels of copper, zinc, lead and mercury, as well as for the presence of enteric pathogens that might indicate faecal pollution of fishing grounds or careless handling during landing of the catch. The maximum level of detected mercury was 0.24 mgkg⁻¹, while the lead content was below the level of detection in 95% of the species examined; copper and zinc were at levels that might be considered nutritionally desirable rather than toxic. No pathogens were detected, and the total colony counts ranged from 1.0×10³ to 8.0×10⁵ cfug⁻¹. Overall, the results for the parameters examined suggested that local fish can be eaten with confidence.     

Microbiological quality of fruit juices sold in Tripoli–Libya

Fruit juices are becoming an important part of the modern diet in many communities. Data regarding the microbiological quality of foods, particularly fruit juices, sold in Libya and the neighboring North African countries are few if not lacking. Using standard microbiological procedures, 146 fruit juice samples sold in Tripoli were examined. Total bacterial counts (TBC) of samples examined ranged between <1 and 3 × 10⁵ CFU/ml (mean = 5 × 10⁴). Almond juice showed the highest TBC ranging between 1.8 × 10³ and 3 × 10⁵ (mean = 1.7 × 10⁵). Staphylococcus aureus was detected in 8 (5.5%) samples, Streptococcus spp. in 4 (2.7%), coliforms in 33 (22.6%), Escherichia coli (none were of serogroup O157) in 3 (2.1%), Klebsiella pneumonia in 17 (11.6%), Aeromonas spp. in 3 (2.1%), Pseudomonas aeruginosa in 6 (4.1%), Candida albicans in 18 (12.3%), Candida spp. in 109 (74.7%) and other yeasts in 85 (58.2%). Many of these organisms can cause disease in humans, which indicates that a large number of juices tested did not fulfill the Libyan guidelines for the microbiological quality of juices. Application of the HACCP system should be introduced into the food industry sector to improve the quality of fruit juices and other foods manufactured in Libya.     

Microbiological profile of helva sold at retail markets in Izmir city and the survival of Staphylococcus aureus in this product

The objective of this research was to determine the microbiological profile of tahin helva, a low moisture confectionery. A total of 63 tahin helva samples were collected from the retail markets in Izmir, Turkey. These samples were examined by standard procedures for aerobic plate count (APC) and counts of moulds and yeasts, Enterobacteriaceae, Staphylococcus aureus and Salmonella spp. APC of samples ranged from <10 to 1.6 × 10⁵ cfu/g. The counts for moulds, yeasts and Enterobacteriaceae ranged from <10 to 1.8 × 10³, <10 to 7 × 10², <10 to 8.5 × 10² cfu/g, respectively. None of the samples contained S. aureus or Salmonella. The potential for survival of S. aureus in the product stored at refrigeration (4 °C) and room (20 °C) temperatures was evaluated by artificial contamination. S. aureus cells were still recovered after 9 months of storage at both temperatures. The results of this investigation indicate that S. aureus contamination of tahin helva, (a_w of 0.172) may constitute a potential public health hazard, depending on the extent of contamination and mishandled exercise at the sale area and the kitchen.     

Microbiological quality assessment of garri with reference to thermonuclease activity

The microbiological quality of garri obtained from open markets and traditional processing industry in Benin City with reference to staphylococcal contamination was investigated. Enumeration of the total heterotrophic bacteria, total fungal propagules and Staphylococcus aureus in food samples was carried out using appropriate media. The staphylococcal thermonuclease activity determination was used as an indicator of previous (substantial) growth of S. aureus and possible presence of staphylococcal enterotoxins. The total heterotrophic bacterial count of the open markets’ samples was 7.75±2.87×10³ cfu/g with corresponding staphylococcal count of 1.65±0.82×10³ and fungal propagule count of 2.50±1.14×10² cfu/g. Samples obtained immediately after processing from the traditional garri industry revealed total heterotrophic bacterial count of 5.00×10¹ cfu/g; staphylococcal count of 5.00×10⁰ cfu/g and no fungal count. The zone diameter of thermonuclease activity was 8.13±0.52 mm for open markets’ samples while traditional processing industry samples have 7.83±0.54 mm. From the study, it was found that there was contamination and growth of S. aureus and possibly the presence of staphylococcal enterotoxin in the product. The public health significance of the microorganisms with the production of thermonuclease and enterotoxins by S. aureus are discussed.     

Synthesis and Surface Active Properties of Novel Nonionic Aryl Oleic Diethanolamide Surfactants

A series of novel aryl oleic diethanolamide (AOD) surfactants with different hydrophobic groups were synthesized. An aromatic ring introduced to a long alkyl chain had a significant effect on reducing water surface tension. The critical micelle concentration (CMC) and the surface tension (γ_cmc) at the CMC were investigated. The CMC was 4.56 × 10^-8 mol/L to 5.83 × 10^-6 mol/L for AOD1:1 (molar ratio of aryl oleic acid: diethanolamide = 1:1) and corresponding γ_cmc was 36.4 mN/m to 39.3 mN/m. The CMC of AOD1:2 (molar ratio of aryl oleic acid: diethanolamide = 1:2) were in 1.21 × 10^-7-9.98 × 10^-6 mol/L and γ_cmc were in 31.6-34.4 mN/m.     

ESTIMATION OF TOXIC COKE DEPOSITS ON FRESH AND REGENERATED Pt/Al2O3 CATALYST FROM METHYLCYCLOPENTANE REFORMING IN H2 AND N2 ATMOSPHERES.

An estimate of the quantity of toxic coke deposited on fresh and regenerated Pt/Alj₂O₃ catalyst has been determined for methylcyclopentane (MCP) reforming in a Berty CSTR at 390°C, W/F=0·11 g min cm^-3, total pressure of 1 atm and MCP partial pressure of 9·2 × 10^-2 atm in H₂ or N₂ carrier. Eleven cycles consisting each of catalyst deactivation, regeneration and reduction were investigated with 3 in H₂ and 8 in N₂. Oxidizable (primary) coke deposits were higher in N₂. However, higher levels of toxic (secondary) coke were deposited in H₂. The ratio of oxidizable to toxic coke lies between 1-15×10³ in H₂ and 22 - 55 × 10³ in N₂ The coke-time profiles for secondary coke removal exhibited maxima suggestive of three types of secondary coke with varying reactivity in H₂. Furthermore, the results strongly suggest that the cokes were layered on acidic coke forming sites with the solid phase transformation of primary to secondary coke occurring at the catalyst-coke interface.     

The dissipation rates of cyprodinil, fludioxonil, procymidone and vinclozoline during storage of grape juice

The disappearance of the fungicides cyprodinil, fludioxonil, procymidone and vinclozoline, which are widely used to control grey mold in vineyards, from commercially sterilized white grape juice was studied. Fungicide losses from white grape juice stored at 40 °C were monitored for about 2 months in order to simulate in a fast way the shelf-life of the product at room temperature (about 1 year). The fungicides were determined by using a simple method based on a liquid–liquid extraction (LLE) and gas chromatographic separation, followed by mass spectrometric detection (GC–MSD). Fortified white grape juice subsamples were taken three times a week from the oven and the degradation of the fungicides monitored for 56 days. The half-lives at 40 °C for vinclozoline and procymidone were found to be 11 and 20 days, respectively. Those for the more recently introduced fungicides fludioxonil and cyprodinil were somewhat longer (33 and 44 days, respectively). Based on the first-order rate constants obtained, the fungicides dissipated in the following sequence: vinclozoline (0.062 d⁻¹) > procymidone (0.035 d⁻¹) > fludioxonil (0.021 d⁻¹) > cyprodinil (0.016 d⁻¹).     

Characteristics of Bacillus cereus isolates from legume-based Indian fermented foods

An antibiogram of 48 strains of Bacillus cereus isolated from 6 different kinds of legume-based Indian fermented foods (amriti, dhokla, dosa, idli, papad and wadi) was generated against 18 different antibiotics that are commonly used against foodborne diseases, mainly gastroenteritis. Each of the isolates was found to be resistant against at least nine different antibiotics. Production of extracellular enzymes, namely protease, lipase and amylase by 33%, 27% and 46%, respectively, of the isolates indicates their potentiality for food spoilage. In brain–heart infusion broth supplemented with glucose, the D_100 °C-values for the tested 12 strains ranged from 3.0 to 9.2 min. In nutrient broth, the minimum and maximum pHs permitting growth of B. cereus were 5.3 and 11.6, respectively. The minimum inhibitory concentrations of sodium chloride, benzoic acid and sorbic acid for the growth of the isolates were 65–85 mg ml⁻¹, 400–700 μg ml⁻¹ (pH 5.0–4.2) and 500–600 μg ml⁻¹ (pH 5.0–4.8), respectively. Of the tested 10 strains, eight were resistant to 300 μg nisin ml⁻¹ (pH 5.0). While studying the combined effect of selected hurdles on the growth of an isolate, the judicious combination considered was 20 mg sodium chloride, 300 μg benzoic acid and 25 μg nisin ml⁻¹ at pH 5.6. The whole-cell protein fingerprinting (WCPF) analysis using SDS–PAGE revealed a high level of diversity among the isolates. At 60% similarity level, the WCPF profiles could be grouped into four major clusters which were divided into 34 subclusters. Most of the subclusters were source-wise homogeneous.     

Effects of some Chinese medicinal plant extracts on five different fungi

Chinese medicinal plant extracts were screened against some fungal strains, such as Aspergillus niger, Botrytis cinerea, Fusarium moniliforme, Glomerella cingulata, and Phyllosticta caricae. Plants were extracted with hot water, 80% methanol or acetone. Aliquots of the extracts at variable concentrations were then incubated with different fungal strains, and the minimum inhibitory concentrations (MICs) of each plant extract determined. In this study, the methanol extracts of Cinnamomum cassia had MIC values of 13.3 mg ml⁻¹, when tested against F. moniliforme and P. caricae. The acetone extracts of C. cassia had MIC values of 8.3 mg ml⁻¹ and 10 mg ml⁻¹ respectively, when tested against B. cinerea and G. cingulata. The hot water extracts of C. cassia inhibited significantly the growth of A. niger, B. cinerea, F. moniliforme, and P. caricae with MIC values at 10, 11.7, 5, and 6.7 mg ml⁻¹ respectively. The acetone extracts of Curcuma longa inhibited effectively P. caricae with the MIC value at 6.7 mg ml⁻¹. To determine the stability, various plant extracts were stored at 4 and 25 °C over a period of one month and their effects on fungal growth examined. Results show that the acetone extracts of Cu. longa and Coptidis rhizoma maintained their activity against fungal strains when stored at 4 °C, but not at 25 °C. The methanol extracts of C. cassia lost a great portion of inhibitory activities but not all, after stored at 4 °C and 25 °C for one month. The effect of various combinations of these extracts on antimicrobial activity has also been examined. The combinations of herb extracts showed higher inhibitory effect towards tested fungi than that of individual extract. Results from these findings suggest that these herbal extracts may be used as natural antifungal agents to inhibit growth of foodborne pathogen.     

Potential application of low dose gamma irradiation to improve the microbiological safety of fresh coriander leaves

A local market survey of fresh, raw coriander leaves, which is a component of many ready-to-eat, Indian dishes showed large variation in their bacterial load (7.0×10⁶–1.36×10⁸ cfu/gm) and mold and fungi (3.0×10³–1.0×10⁴ cfu/gm) and presence of potentially pathogenic bacteria such as faecal coliforms, Listeria and Yersinia. Conventional chlorination treatment affected the structural integrity of leaves leading to enhancement of rotting. Exposure to a low dose of 1 kGy was efficient for bacterial decontamination and elimination of potential pathogens without affecting the keeping quality of coriander leaves upto two weeks storage at 8–10 °C, measured visually in terms of degree of yellowing and rotting. Irradiation at higher doses led to the increased rotting during storage. The total chlorophyll contents as well its components, chlorophyll a and b did not change significantly on irradiation and subsequent storage. Similarly, the total carotenoid levels remained unaffected by exposure to 1 kGy dose, however, a dose dependent enhancement in their extractability was observed in irradiated leaves. No qualitative differences were observed in the GLC profile of volatile oils of control and irradiated (1 kGy) samples. There were no significant quantitative changes in the constituents of the major aroma compounds obtained from these two samples. Effects of irradiation on storage of the seasoning were also assessed.     

Solute-Solute Interactions in Jet Fuel by Ultralow Conductance Measurement

Solute-solute interactions in pure organic liquids are much easier to determine than solute-solute interactions in a complex organic mixture such as a middle distillate fuel. This paper presents a method for the determination of solute-solute interaction and infinite dilution diffusion coefficient of hydrogen bond donor-acceptor species using ultralow conductance measurement. A theoretical framework was developed to obtain both complexation equilibrium constant (K) and infinite dilution diffusion coefficient, D° from a single set of measurements. These equations were applied for the study in hexadecane, a model hydrocarbon, and in jet fuel. The D° for methanol in jet fuel, 1.38 × 10^-4 cm² s^-1, is indicative of hydrophobic environments for the polar solutes in hydrocarbons media. The conditional equilibrium constant, K', was found to be maximum for methanol in jet fuel, which indicates the presence of strong hydrogen bond acceptors in jet fuel. The present method is fairly general and applicable to polar and polarizable species in hydrocarbon media.     

Evaluation of Diluted and Undiluted Trickle-Bed Hydrotreating Reactor with Different Catalyst Volume

In this work, a comparative study on the combined effects of hydrodynamics and kinetics on the hydrodesulfurization (HDS) of a straight-run gas oil (SRGO) using a trickle-bed reactor with and without diluent (SiC) and different catalyst volume (0.1, 0.07, and 0.050 × 10^-3 m³, respectively) was carried out. The tests were conducted in a pilot plant under conditions close to those used in industrial-scale units (5492 kPa, 445.4 m³(STP)/m³ H₂/oil ratio, 623-643K, 0.9 and 2.5 h^-1 LHSV values). The catalyst used was a commercial CoMoP/Al₂O₃ formulation shaped as tri-lobed extrudates (1/20 in, nominal size) or as crushed particles (d_p = 1.2 × 10^-3 m). Contrarily to that usually claimed, the undiluted systems showed better performance than those comprising small diluent (SiC) particles (d_p ~ 5 × 10^-5 m). Calculations to evaluate hydrodynamic variables (plug-flow behavior, wall effects, wetting, and back-mixing) were carried out in order to explain the observed facts. The possible influences of the size of the diluent particles used are discussed.     

正己烷在Pt/HBeta催化剂上的异构化反应动力学模型

采用等体积浸渍法制备了Pt/HBeta催化剂,并在10 mL固定床反应装置上评价了反应温度和质量空速对Pt/HBeta催化正己烷临氢异构化反应的影响,在此基础上建立正己烷异构化反应动力学模型。结果表明：在 240~260  ℃内正己烷临氢异构化反应可以用拟一级动力学模型来描述,反应的活化能Ea=139.06 kJ/mol,指前因子A=7.3814×1013 h-1;建立了连串反应动力学模型,第一步反应活化能Ea=167.80 KJ·mol-1,A=7.2130×1016 h-1,第二步反应活化能Ea=118.34 KJ·mol-1,A=1.3053×1011 h-1;当反应温度大于260 ℃,拟一级动力学模型不再适合,修正后270 ℃时的反应级数为1.3,280  ℃时的反应级数为1.7。     

THERMAL EFFECT ON THE PERMANENT VISCOSITY OF A SASKATCHEWAN HEAVY OIL

Future energy demands will likely cause increased activity towards the recovery of heavy oil using non-conventional means. Most non-conventional attempts to recover Saskatchewan's heavy oil resources have utilized thermal techniques.

This report discusses the permanent viscosity changes which occur when heavy oil.is subjected to thermal processes from 220 to 425°C. It was observed that under closed operating conditions, the oil viscosity drops in a manner which can be modeled by a first order, kinetic reaction model. The rate constant for this reaction varied from 0.3 × 10^-3 to 6.0 × 10^-3 h^-1 depending on temperature and the assumed molecular weights of the model components. These findings closely parallel earlier results.

Experimental observations on thermal effects during opened operating conditions indicate a dramatic and rapid rise In the remaining crude oil viscosity. The oil was observed to increase its permanent absolute viscosity by a factor as high as 21 times its original absolute viscosity. The single product, first order kinetic model was not capable of predicting this rise in oil viscosity. A simple, two product, first order kinetic model was developed and found to fit the data satisfactorily with a rate constant of 0.6 h^-1 for heavy product formation and a rate constant of 0.03 h^-1 for light product formation at 275°C.     

An evaluation of the effect of storage and processing temperatures on the microbiological status of sous vide extended shelf-life products

The microbiological and organoleptic quality of selected sous vide products was monitored over a storage period of up to five weeks at 3°C and 8°C, respectively. Sous vide products stored at the recommended temperature of 3°C showed negligible microbial growth and were found to be organoleptically acceptable throughout the storage period. Total plate counts at the end of the fourth week of storage were in the range <10–7×10³ CFU/g for all 19 products under study. Listeria monocytogenes, Salmonella, Clostridium perfringens, Bacillus cereus and Enterobacteriaceae were not detected in any of the processed samples. At 8°C, under temperature abuse conditions, while some products had acceptable microbial levels of 10²–10⁴ CFU/g after three weeks, others such as chicken chasseur had counts above 10⁶ CFU/g by the second week of storage. Lactic acid bacteria and Pseudomonas species were dominant in the microbial flora of spoilt samples and B. cereus (>3×10⁴ CFU/g) was isolated from spoilt chicken chasseur samples in the fourth week of storage at 8°C. Critical factors affecting sous vide product safety are discussed.     

STUDY ON COKING KINETICS OF CHINESE GUDAO VACUUM RESIDUE

Using a molten metal bath as heat source of reaction, the coking kinetics of Gudao vacuum residue in temperature ranges of 400 - 440°C and 460-500°C were studied and kinetic models were developed. The order of reaction, pre-frequency factor and apparent activation energy of thermal-cracking were determined as 1.0, 7.853 × 10¹⁰ min^-1 and 175.3KJ/mol respectively. The results laid a solid foundation for technological computation, reconstruction and design of the tubular furnace using the residuum as its feedstock.     

Rapid gas-chromatographic method for the determination of diacetyl in milk, fermented milk and butter

In this work, a simple and fast method for the determination of diacetyl by gas-chromatographic technique coupled with flame ionisation detector (GLC-FID) was developed. Diacetyl is the typical butter flavour, but it is also commonly present in others fermented dairy products. Recently, diacetyl determination has also attracted interest because it is one of the parameters on which lactic acid bacteria (L.A.B.) are characterized and valued. Only acetone and 2,3-pentanedione were used as chemicals. After centrifugation of acetone–milk mixture, supernatant was filtered and directly injected into gas-chromatographic apparatus, without a further purification procedure step.

This method was accurate and precise; diacetyl recovery on milk was 97% and the detection limit was 1 mg L⁻¹. Finally, by using this method, diacetyl was easily determined in fresh and high-temperature treated milk, commercial butter, yoghurt and also in a series of L.A.B. performance tests.     

Computer modelling for the control of particulate sterilization under dynamic flow conditions

A finite difference model was used for predicting the centre temperature of particulates during ultra-high temperature processing under continuous flow conditions. This model compared favourably with the analytical solutions. A sensitivity analysis was carried out on the input parameters to the numerical model, which indicated that particulate size and thermal diffusivity were the most critical parameters influencing process lethality and cook value. For example, a spherical particulate (thermal properties defined) of 20 mm diameter required a holding time greater than 5 min at 135°C to achieve a minimum safe cook (F₀ of 3.0 min for Clostridium botulinum), compared to a 10 mm spherical particulate which would have received an F₀ value of 68 min after 5 min processing at 135°C. The centre temperatures predicted using the model were sensitive to changes in the convective surface heat transfer coefficient in the range 100–300 W m⁻² K⁻¹, but became less sensitive as the values increased up to 500 W m⁻² K⁻¹. An initial product temperature change from 20 to 60°C resulted in an 8 min increase in process lethality for a 15 mm spherical particulate processed for 5 min at 135°C. The determination of experimental results in particulates of less than 20 mm (the critical dimension) was found to be significantly affected by conduction errors through the thermocouple wires, and therefore the model presented will be a useful prediction tool in situations of experimental uncertainty.