Environmentally superior cleaning of diatom frustules using sono-Fenton process: Facile fabrication of nanoporous silica with homogeneous morphology and controlled size

Existing techniques for the preparation of silica structures from diatom cells include cleaning of frustules through baking at high temperature and oxidant cleaning using concentrated sulfuric acid, hydrogen peroxide, nitric acid, or sodium dodecyl sulfate (SDS)/ethylenediaminetetraacetic acid (EDTA). In this study, sono-Fenton (SF) process was examined to prepare nanoporous silica through cleaning diatom frustules, while preserving their structural features. Single colonies of Cyclotella sp. were cultivated in batch mode f/2-enriched seawater. Combination of Fenton process with ultrasonication was found to be more efficient than the sum of individual processes in the removal of organic compounds from Cyclotella sp. structure. The optimized amounts of operational parameters were determined as suspension pH of 3, diatom cell density of 4.8 × 10⁵ cell mL⁻¹, H₂O₂ concentration of 60 mM, Fe²⁺ concentration of 15 mM, ultrasound irradiation power of 400 W and the temperature of 45 °C. The results of energy-dispersive X-ray spectroscopy (EDX) and thermal gravimetry (TG) analyses proved that organic materials covering the cell wall were significantly removed from the frustules through SF process. Scanning electron microscopy (SEM) images showed that after SF treatment, silica nanostructures were produced having uniform pores less than 15 nm in diameter. N₂ adsorption–desorption isotherms demonstrated that almost non-porous structure of diatom frustules became mesoporous during removing the organic matrix. Lipids, amino acids, carbohydrates and organic acids or their oxidized products were identified using GC–MS analysis as the main organic compounds released from diatom cells to the solution after SF treatment. Treated frustules exhibited adsorption capability of 91.2 mg/g for Methylene Blue, which was almost 2.5 times higher than that of untreated frustules (34.8 mg/g).     

Studies of a novel sensor for assessing the spatial distribution of cavitation activity within ultrasonic cleaning vessels

This paper describes investigations of the spatial distribution of cavitation activity generated within an ultrasonic cleaning vessel, undertaken using a novel cavitation sensor concept. The new sensor monitors high frequency acoustic emissions (>1 MHz) generated by micron-sized bubbles driven into acoustic cavitation by the applied acoustic field. Novel design features of the sensor, including its hollow, cylindrical shape, provide the sensor with spatial resolution, enabling it to associate the megahertz acoustic emissions produced by the cavitating bubbles with specific regions of space within the vessel. The performance of the new sensor has been tested using a 40 kHz ultrasonic cleaner employing four transducers and operating at a nominal electrical power of 140 W under controlled conditions. The results demonstrate the ability of the sensors to identify 'hot-spots' and 'cold-spots' in cavitation activity within the vessel, and show good qualitative agreement with an assessment of the spatial distribution of cavitation determined through erosion monitoring of thin sheets of aluminium foil. The implications of the studies for the development of reliable methods of quantifying the performance of cleaning vessels are discussed in detail.     

Ultrasound-enhanced membrane-cleaning processes applied water treatments: influence of sonic frequency on filtration treatments

Ultrasound (US) cleaning technique was applied to remove fouling of ultrafiltration (UF) and microfiltration (MF) membranes which were used to treat peptone and milk aqueous solutions, respectively. Membrane operations were performed by cross-flow filtration with 60 kPa operating pressure in an US field. The US employed had 28, 45 and 100 kHz frequency with 23 W/cm(2) output power. For each polymeric membrane made of polysulfone UF and cellulose MF, cleaning experiments were carried out with and without US after fouling. The fouled UF and MF membranes showed volume flux decline, but the membrane property was recovered by US irradiation. It was found in 28 kHz frequency that water cleaning was effective for recovery of declined condition due to fouling. Also, US-enhanced permeability of membranes was discussed in both membrane systems. We observed that US decreased the fouling condition in both membrane systems when US was irradiated before fouling. It was found that 28 kHz frequency US could enhance formation of the fouled layer in both filtration systems of peptone and milk solution.     

Corrosion of stainless steel in food and pharmaceutical industry

Stainless steels are widely used in the food and pharmaceutical industry because of their high corrosion resistance and superior mechanical properties. These features are crucial because produced foodstuffs and drugs must comply with high purity and quality standards. Just a proper selection of stainless steel grade can prevent corrosion phenomena that can be detrimental to the whole manufacturing process. Food/drugs production process phases will be here analyzed and discussed with a particular emphasis on the possible corrosion mechanism of stainless steels in those particular operating conditions. Recent advances on the methods to assess corrosion of stainless steels in food and pharmaceutical industries will be disclosed.     

Effect of high pH column regeneration on the separation performances in reversed phase chromatography of peptides

Caustic regeneration procedures are often used in chromatographic purification processes of peptides and proteins to remove irreversibly bound impurities from the stationary phase. Silica-based materials are the most commonly used materials in reversed phase chromatography of peptides. Their limited chemical stability at high pH can be, however, problematic when high pH column regeneration (i.e. cleaning in place) is required. The effect of cleaning in place on the surface chemistry of the stationary phase has been investigated using the Tanaka test. It has been shown that the high pH treatment does not significantly affect the hydrophobicity of the material, but it strongly increases its silanol activity. A representative peptide purification process has been used to investigate the impact of cleaning in place on the separation performance. It has been shown that the caustic regeneration increases the peptide retention at high pH (pH 6.5), due to the interactions between the peptide and the negatively charged silanol groups. These unwanted interactions reduce the separation performances by decreasing the selectivity between the late eluting impurities and the main peptide. However, it has been shown that the effect of the silanol groups on the peptide adsorption and on the separation performance can be minimized by carrying out the purification process at low pH (pH ∼ 2). In this case, the silanol groups are protonated and their electrostatic interactions with the positively charged analyte (i.e. peptides) are suppressed. In these conditions, the peptide adsorption and the impurity selectivity is not changing upon high pH column regeneration and the separation performance is not affected.     

Membrane fouling from ammonia recovery analyzed by ATR-FTIR imaging

The composition of the fouling layer formed during ammonia stripping via membrane distillation from model pig manure and the change in fouling composition as a result of three cleaning procedures was examined using ATR-FTIR imaging and k-means clustering. The use of ATR-FTIR imaging is advantageous as it is a label free technique that provides information on the chemical composition of the fouling as well as a high spatial resolution. The model manure was designed to resemble average Danish pig manure containing representative concentrations of inorganic and organic compounds and particle size distribution similar to the liquid fraction from mechanically separated manure. The fouling layer deposited on polypropylene, PP, and polytetrafluoroethylene, PTFE, membranes were investigated in combination with three cleaning procedures applying deionized water, 1 M NaOH solution followed by a 1 M citric acid solution or Novadan cleaning agents. The spectral data revealed that the fouling layer deposited on both PP and PTFE membranes before cleaning mainly consisted of carbohydrates, protein and lipids. Carboxylates and free fatty acids originating from reactions between NaOH and straw and proteins and lipids, respectively, and lignin were identified in some of the samples. The combination of PTFE membrane and Novadan cleaning agent resulted in the cleanest membranes, as only residual lipids were identified on these samples.     

Comparison of mechanisms and effects of Nd:YAG and CO2 laser cleaning of titanium alloys

The paper compares laser cleaning trials performed using a Q-switched Nd:YAG laser, λ = 1.064 μm and a continuous wave (CW) CO₂ laser, λ = 10.6 μm, applied to aerospace-grade, contaminated titanium alloys. The mechanisms for cleaning using each laser system are modelled to determine the mode and extent of contaminant removal. The model results are then compared with the surface chemistry and micro-structural results from the cleaning trials performed. The results show the dominant cleaning process for Nd:YAG cleaning to be by evaporation of the contaminant via conduction through surface heating, while for CO₂ laser cleaning the small fraction of the beam coupling directly with the contaminant is sufficient for direct heating and selective evaporation. The results for experimental cleaning, electron beam (EB) welding and diffusion bonding align well with the model, particularly when secondary reactions are taken into account.     

Chemical Cleaning of Microfiltration Membranes Fouled by Whey

Millipore hydrophobic polyvinylidene fluoride (PVDF) microfiltration membranes were used for whey processing. Fouled membranes were cleaned with acid (HCl), alkaline (NaOH) and surfactant (Triton‐X100). The latter resulted in maximum flux recovery and resistance removal. Hydrochloric acid had a moderate effect and sodium hydroxide was the weakest cleaning agent. This is due to the cleaning strength of emulsifiers compared to acid or alkali. However acids are more efficient than alkaline solutions for removal of mineral compounds which remain on the membrane surface. Cleaning efficiency depends on the concentration of cleaning agent being higher for higher surfactant concentration. For acids and alkali, the efficiency increases with increasing the concentration of the reagent reaches a maximum (optimum concentration) and then decreases. This can be explained by changes in permeability of the deposit layer with the concentration of the cleaning agent. Another explanation is the breakage of proteins by acid or alkali which produces more fouling materials and causes less cleaning efficiency. Operating conditions affect the cleaning process. At higher stirring speeds (turbulent flow) or longer cleaning time better removal of deposits and higher cleaning efficiency were observed. The sequential cleaning process may or may not improve the cleaning efficiency. When acidic cleaning was followed by washing with a surfactant an improvement was achieved. This can be attributed to the incomplete removal of deposits by acid. However further cleaning with acid can not improve the cleaning efficiency. During whey processing fouling occurs by deposition of foulants of mostly proteins and macromolecules on the membrane surface or in the membrane matrix. Large substances (compared to the membrane pores) settle on the membrane surface and the small species penetrate and are adsorbed in the membrane pores. Cleaning dissolves and removes the adsorbed foulants from the membrane.     

Comparison of monolithic and microparticulate columns for reversed-phase liquid chromatography of tryptic digests of industrial enzymes in cleaning products

Enzymes of several classes used in the formulations of cleaning products were characterized by trypsin digestion followed by HPLC with UV detection. A polymeric monolithic column (ProSwift) was used to optimize the separation of both the intact enzymes and their tryptic digests. This column was adequate for the quality control of raw industrial enzyme concentrates. Then, monolithic and microparticulate columns were compared for peptide analysis. Under optimized conditions, the analysis of tryptic digests of enzymes of different classes commonly used in the formulation of cleaning products was carried out. Number of peaks, peak capacity and global resolution were obtained in order to evaluate the chromatographic performance of each column. Particulate shell-core C18 columns (Kinetex, 2.6 μm) showed the best performance, followed by a silica monolithic column (Chromolith RP-18e) and the conventional C18 packings (Gemini, 5 μm or 3 μm). A polymeric monolithic column (ProSwift) gave the worst performances. The proposed method was satisfactorily applied to the characterization of the enzymes present in spiked detergent bases and commercial cleaners.