An experimental investigation into the pre-treatment of synthetic membranes using sodium hydroxide solutions

In this paper the effect of two pre-treatment methods are compared experimentally for the filtration of (i) a spent sulphite liquor (17.8 wt.% dry solids) using a 20 kg mol⁻¹ molar mass cut off (MMCO) fluoropolymer membrane and (ii) a molasses solution (45° Brix) using a polysulphone (Psf) membrane (1.5 μm pore size). Both feeds are industrially relevant, and subject to severe fouling issues when membranes are used in their subsequent processing. The pre-treatment methods evaluated were: (i) conditioning with water at 60 °C only [Protocol 1], and (ii) conditioning with water at 60 °C followed by cleaning with 0.5 wt.% NaOH [Protocol 2]. Results are presented that confirm the benefits of sodium hydroxide preconditioning upon performance, supporting the suggestion by some membrane manufacturers that this step be included as part of the pre-treatment protocol.     

Effect of previous enzymatic recirculation treatment through a tubular ceramic membrane on ultrafiltration of model solution and apple juice

The process of ultrafiltration of a model solution and 12% soluble solids apple juice containing pectins through tubular membranes of 100 and 300 kDa (1 and 3 channels) was studied. Furthermore, in order to obtain a higher permeate flow, the fluids were previously treated with pectinolytic enzymes recirculating through a tubular membrane at different concentrations and treatment times. The permeate flow was analyzed with respect to time and the influence of enzymatic treatment on different parameters: viscosity, density, absorbance at 420 nm, reducing sugars, °Brix, color and pH. Depectinization increased the permeate flow for the model solution and apple juice with 67.52% and 53.11% when the pectinolytic enzyme preparation re-circulated across the tubular membrane. Using the lowest concentration of enzyme treatment and the longest recirculation treatment, an increase in permeate flow was obtained leading to a more favourable clarification process and economic benefits.     

The effect of pre-treatment on the anthocyanin and flavonol content of black currant juice (Ribes nigrum L.) in concentration by reverse osmosis

Reverse osmosis process for the concentration of black currant juice was carried using AFC-99 tubular membrane at 30 °C and 45 bar. The contents of selected flavonols and anthocyanins were analyzed after centrifugation; enzyme treatment by Panzym Super E and by Rohapect berry followed by centrifugation; and ultrafiltration black currant juices and juice concentrates. The total soluble solid (TSS) content of the juices increased from the initial 17.6–17.9 °Brix to 24–24.8 °Brix in the case of the centrifuged juice in the concentration process. Similarly, it increased from 14.5–15.5 °Brix to 23.1–23.4 °Brix for the Panzym Super E treated juice, and from 16.1–16.9 °Brix to 22.5–23.1 °Brix for the Rohapect berry treated black currant juices. The ultrafiltered juice had the lowest initial TSS content between 14.1 and 14.9 °Brix and it increased to 22.1–23.1 °Brix. The average permeate fluxes during the concentration process were 7.3 L m⁻² h⁻¹ for the centrifuged juice, 11.9 L m⁻² h⁻¹ for the Panzym Super E treated juice, 9.2 and 13.1 L m⁻² h⁻¹ for the Rohapect berry treated and ultrafiltered juice, respectively. Analysis indicated that the enzymatic treatment resulted in the increase of anthocyanin and flavonol content of the juices. The centrifugation process decreased the amount of anthocyanins and flavonols to some extent. The juice clarified by ultrafiltration had significantly lower concentrations of anthocyanins and flavonols, while the juices treated by Panzym Super E had the highest levels of these flavonoids. This study recommends enzymatic pre-treatment by Panzym Super E, since it improves the permeate flux in reverse osmosis during the concentration process, and results in a juice concentrates highest in anthocyanins and flavonols.     

Fluid dynamic gauging of microfiltration membranes fouled with sugar beet molasses

Fluid dynamic gauging (FDG) was used to track the thickness of the cake layer formed during the microfiltration of a 45° Brix molasses solution using a 1.5 μm polysulphone membrane. A simultaneous measure of flux and deposit thickness throughout the full membrane operating cycle is reported. Asymptotic fouling thicknesses of ca. 100 μm are developed after 30 min of filtration. Accordingly, flux declines are severe at ca. 93%. Permeate line closed (PLC) operation leads to the complete removal of the deposit layer, and the recovery of 60% of the flux. However, permeate line open (PLO) operation leads to only a 50% flux recovery and an asymptotic deposit thickness of 10 μm. An initial increase and subsequent reduction in flux during chemical cleaning has also been recorded for both acid and alkali cleaning regimes. Effective cleaning regimes for membranes fouled by molasses require an alkali stage followed by an acid stage.     

Effect of membrane property and operating conditions on phytochemical properties and permeate flux during clarification of pineapple juice

The effects of membrane property on the permeate flux, membrane fouling and quality of clarified pineapple juice were studied. Both microfiltration (membrane pore size of 0.1 and 0.2 μm) and ultrafiltration (membrane molecular weight cut-off (MWCO) of 30 and 100 kDa) membranes were employed. Membrane filtration did not have significant effects on the pH, reducing sugar and acidity of clarified juice whereas the suspended solids and microorganism were completely removed. The 0.2 μm membrane gave the highest permeate flux, total vitamin C content, total phenolic content and antioxidant capacity as well as the highest value of irreversible fouling. Based on these results, the membrane with pore size of 0.2 μm was considered to be the most suitable membrane for the clarification of pineapple juice. The optimum operating conditions for the clarification pineapple juice by membrane filtration was a cross-flow velocity of 3.4 ms⁻¹ and transmembrane pressure (TMP) of 0.7 bar. An average flux of about 37 lm⁻² h⁻¹ was obtained during the microfiltration of pineapple juice under the optimum conditions using batch concentration mode.     

Chicory juice clarification by membrane filtration using rotating disk module

Clarification is the first step of inulin production from chicory juice, and membrane filtration as an alternative can greatly simplify this process, increase juice yield, improve product quality, and reduce the cost and waste volume. In this study, a rotating disk module (RDM) was used to investigate the clarification of chicory juice by four micro- and ultrafiltration membranes. Compared with dead end filtration, the RDM had a much higher permeate flux and product quality. High rotating speeds produced high permeate fluxes and reduced flux decline, because of the strong back transport of foulant from fouling layer to feed solution. At high rotating speeds of 1500–2000 rpm, the permeate flux increased with membrane pore size and transmembrane pressure (TMP), while at low rotating speeds (<1000 rpm), permeate flux was independent of membrane type and TMP due to a thick deposited fouling layer as a dominant filtration resistance, while carbohydrate transmission decreased at higher TMP because of denser cake layer as an additional selective membrane. The highest carbohydrate transmission (∼98%) and desirable permeate turbidity (2.4 NTU) was obtained at a TMP of 75 kPa and a rotating speed of 2000 rpm for FSM0.45PP membrane. With the RDM, the Volume Reduction Ratio (VRR) could reach 10 with a high permeate flux (106 L m⁻² h⁻¹) in the concentration test, and permeate was still rich in carbohydrate and well clarified. Chemical cleaning with 0.5% P3-ultrasil 10 detergent solution was able to recover 90% water flux of fouled membrane.     

Effect of high or low molecular weight of components of feed on transmembrane flux during forward osmosis

The possible mechanism of water transport from feed to osmotic agent side during forward osmosis in situation when feed contains high or low molecular weight compounds and their combination has been presented. The orientation of membrane was found to influence the transmembrane flux. When the feed contains mixture of low and high molecular weight compounds mode I (feed towards the support layer) was found to result in lower flux values as compared to Mode II (feed towards active layer) due to significant external concentration polarization. Forward osmosis resulted in the concentration of betalains content in beetroot juice and anthocyanin content in grape juice from 50.92 mg/L to 2.91 g/L (57.1 fold) and from 104.85 mg/L to 715.6 mg/L (6.8 fold), respectively. Total soluble solids in case of beetroot, grape and pineapple juice were found to increase from 2.3 to 52 °Brix, from 8.0 to 54.6 °Brix from 4.4 to 54 °Brix, respectively.     

Behavior of functional compounds during freeze concentration of tofu whey

The liquid waste generated from tofu production, denominated as Tofu Whey (TW), contains important amounts of isoflavones that can be evaluated by various separation techniques. In this work TW was concentrated by falling-film freeze concentration from 1.9 to 15.5 °Brix, up to levels of 208 mg of isoflavones per 100 g solids. The levels of isoflavones, proteins, sugars, calcium and magnesium were determined both in the ice and in the concentrate obtained. It was found by rheological characterization that TW shows a Newtonian behavior at concentrations between 1.9 and 15.5 °Brix with freezing points of −0.6 to −2.7 °C.     

Freeze concentration of whey in a falling-film based pilot plant: Process and characterization

Falling-film freeze concentration is a technique for concentration of liquids by freezing the available water in the form of a layer of ice on a refrigerated surface. Processing at low temperatures keeps the organoleptic properties of the initial product. In this study the freeze concentration of whey was investigated as an technological alternative for the use of this byproduct of the dairy industry. Freeze concentration tests were carried out in pilot-scale equipment and the increase in soluble solids content of the whey and the amount and purity of the ice formed were analysed. Electrical conductivity, viscosity and freezing point of the concentrated whey were determined. The concentrate obtained had a solid concentration of up to 21.8 °Brix. The ice formed in the last stage of the freeze-concentration process had a lactose content of 11.3 g/L and protein content of 3.45%. The electrical conductivity of the ice formed increased exponentially to a value of 29.40 mS/cm. Freeze-concentrated whey of 10, 15, and 20 °Brix behaves as a Newtonian fluid in the temperature range of −4 °C-4 °C.     

Recovery and concentration of phenolic compounds in blood orange juice by membrane operations

Cross-flow ultrafiltration (UF) and osmotic distillation (OD) were implemented on laboratory scale to obtain formulations of interest for food and/or pharmaceutical industry starting from the blood orange juice produced in the Calabria region. The freshly squeezed juice, after a depectinization step, was submitted to an UF process in order to recover natural antioxidants, such as hydroxycinnamic acids, hydroxybenzoic acids, flavanones, flavan-3-ols, and anthocyanins. The UF permeate, with an initial total soluble solids (TSS) content of 10.5°Brix, was concentrated by OD up to a final concentration of 61.4°Brix.     

Effects of temperature,solid content and pH on the stability of black carrot anthocyanins

Anthocyanin stability of black carrots was studied at various solid contents (11, 30, 45 and 64° Brix) and pHs (4.3 and 6.0) during both heating, at 70–90 °C, and storage at 4–37 °C. Monomeric anthocyanin degradation fitted a first-order reaction model. Degradation of monomeric anthocyanins increased with increasing solid content during heating, while it decreased during storage. For example, at pH 4.3, half-life periods for anthocyanins at 30, 45 and 64° Brix were, respectively, 8.4, 6.9 and 5.2 h during heating at 80 °C and 18.7, 30.8 and 35.9 weeks during storage at 20 °C. At 30–64° Brix, increasing pH from 4.3 to 6.0 enhanced the degradation of anthocyanins during heating. The effect of pH on thermal stability of anthocyanins was also studied at six different pHs (2.5–7.0) in citrate-phosphate buffer solutions and significant decrease in anthocyanin stability was observed at pHs above 5.0. Higher activation energies (E_a) were obtained during heating than during storage with increasing solid contents. At 30–64° Brix, E_a values ranged from 68.8 to 95.1 kJ mol⁻¹ during heating and from 62.1 to 86.2 kJ mol⁻¹ during storage. Q₁₀ values at 20–37 °C were as high as 3.1 at 45° Brix and 3.6 at 64° Brix.     

Response Surface Modeling of the Multiphase Juice Composition from the Compaction of Sardine Discards

In this work, sardine fish was processed in a hydraulic press in order to obtain a solid cake and a press juice presenting solid, aqueous, and oil phases. The influence of pressing conditions, such as total pressure (50–350 bar), compression speed (0.935–3.135 cm/min), number of pressing stages (1–5), and time of relaxation between two consecutive pressing stages (100–300 s), was studied following a rotatable central composite design. Response surface methodology was used to relate the yields of each phase with the operation parameters. According to the regression equations, the content of solids in the press liquor was markedly affected by the target pressure, attaining a maximal yield at 350 bar (0.028 g solids/g sardine). The yield of both liquid phases was maximum after an intensive compacting treatment comprising five pressing steps at the highest compression speed. Under these conditions, the maximum yield of oil was achieved after 100 s of time of relaxation (0.021 g oil/g sardine), while longer times of relaxation increased the amount of blood water and solids in the press liquor to the detriment of the oily phase.     

Application of osmotic membrane distillation process in red grape juice concentration

The osmotic membrane distillation process was applied in dehydration of red grape juice (Most de Raïm Concentrat Negre) of different concentrations (5–20 °Brix). Experiments were performed using polytetrafluoroethylene (PTFE) hydrophobic membranes of different nominal pore diameter. Red grape juice solution and concentrated calcium chloride solution (50 wt.%) were used as feed and stripping solutions, respectively. The permeate flux, the initial and the final juice concentration, the total phenolic content (TPC) and the antioxidant activity (TEAC) were measured for each single experiment.     

Physico-chemical characteristics of juice extracted by blender and mechanical press from pomegranate cultivars grown in Georgia

Pomegranate juice is consumed widely for its possible health benefits. The aril juice from 15 pomegranate cultivars grown in Georgia were analysed for juice yield based on fresh weight (FW) and physico-chemical properties, using blender and mechanical press extraction. Blender had a higher juice yield (42.04% FW) compared to mechanical press (38.05% FW). Total phenolics and antioxidant capacity was determined by Folin–Ciocalteau method and ferric reducing antioxidant power (FRAP), Trolox equivalent antioxidant capacity (TEAC), and oxygen radical absorbance capacity (ORAC) assays, respectively. Total monomeric anthocyanins were determined by pH differential method and RP-HPLC. The major anthocyanin was delphinidin 3-glucoside. High negative and significant (p ? 0.05) correlations were found between pH and titratable acidity (TA). The total soluble solids content (TSS) averaged 15.59 in blender and 14.94 °Brix in mechanical press. Chemical analysis of juice showed significant differences among cultivars and extraction methods. Overall, blender was more efficient than mechanical press juice extraction.     

A physicochemical investigation of membrane fouling in cold microfiltration of skim milk

The main challenge in microfiltration (MF) is membrane fouling, which leads to a significant decline in permeate flux and a change in membrane selectivity over time. This work aims to elucidate the mechanisms of membrane fouling in cold MF of skim milk by identifying and quantifying the proteins and minerals involved in external and internal membrane fouling. Microfiltration was conducted using a 1.4-μm ceramic membrane, at a temperature of 6 ± 1°C, cross-flow velocity of 6 m/s, and transmembrane pressure of 159 kPa, for 90 min. Internal and external foulants were extracted from a ceramic membrane both after a brief contact between the membrane and skim milk, to evaluate instantaneous adsorption of foulants, and after MF. Four foulant streams were collected: weakly attached external foulants, weakly attached internal foulants, strongly attached external foulants, and strongly attached internal foulants. Liquid chromatography coupled with tandem mass spectrometry analysis showed that all major milk proteins were present in all foulant streams. Proteins did appear to be the major cause of membrane fouling. Proteomics analysis of the foulants indicated elevated levels of serum proteins as compared with milk in the foulant fractions collected from the adsorption study. Caseins were preferentially introduced into the fouling layer during MF, when transmembrane pressure was applied, as confirmed both by proteomics and mineral analyses. The knowledge generated in this study advances the understanding of fouling mechanisms in cold MF of skim milk and can be used to identify solutions for minimizing membrane fouling and increasing the efficiency of milk MF.     

Effects of palm oil-based fatty acids on fouling of ultrafiltration membranes during the clarification of glycerin-rich solution

Ultrafiltration (UF) is an alternative option that can be used to clarify glycerin-rich solutions in the oleochemical industry. However, the UF membranes used in the process were observed to have been seriously fouled in our preliminary study. Thus, the ultrafiltration of a glycerol-water-fatty acid mixture was carried out to investigate the membrane binding properties of the components and their contributions to membrane fouling. Palmitic, stearic, and oleic acid were used as fouling substances in the glycerol-water mixture. The flux decline experiments were carried out using polyvinylidenefluoride (PVDF) as well as polyethersulphone (PES) membranes with a MWCO of 30 and 25 kDa, respectively at specific conditions (T = 40 °C; ΔP = 2 bar). It was found that the PES membrane exhibited severe fouling for all types of fatty acids in solution with glycerol-water. As the pH decreased to acidic conditions, the PES membrane tended to exhibit more severe fouling than the PVDF membrane.     

Effect of postharvest dehydration on the composition of pinot noir grapes (Vitis vinifera L.) and wine

This study was conducted in order to improve our understanding of how phenolics and aroma compounds change in wine grapes during postharvest dehydration. Pinot noir grapes grown in the Willamette Valley of Oregon were harvested at 22.0 and 24.0 °Brix. Grapes harvested at 22.0 °Brix were divided into three equal lots with one lot immediately used for wine production, and the remaining two lots placed inside an air tunnel with an air speed of 1.0–1.8 m s⁻¹, 38% relative humidity and a temperature of 22 °C. The soluble solids content and weight loss were measured daily and wines were made from grapes when they reached 24.8 and 26.7 °Brix. The soluble solids of grapes increased about 1 °Brix per day; therefore, on the third and fourth day the berries reached the desired concentration; weight loss was 14 and 16%, respectively. Results from berry phenolic analysis indicated that per berry anthocyanin amount remained unchanged during dehydration. The composition of proanthocyanidins isolated from berries changed during dehydration. Volatile compounds in wines made from dehydrated grapes contained more terpenes and norisoprenoids (β-ionone, β-damascenone) when compared to wine made from the original fruit. Wines made from increasingly dehydrated grapes tended to resemble the composition and flavour profile of wines made from grapes left on the vine (i.e. with extended ripening). The results of this study suggest that postharvest flavour changes consistent with changes during fruit ripening can occur in grapes when harvested early and allowed to dehydrate under controlled conditions prior to fermentation.     

Utilization of Cheese Whey Permeate in Canned Beans and Plums

Navy and kidney beans (Phaseolus vulgaris) were hydrated in water, then canned in brines designated as control, whey permeate (WP), and hydrolyzed lactose whey permeate (HP). Hunter Lab Color Difference and Kramer Shear texture analyses indicated general darkening and increased firmness in permeate treated beans. Total solids and ash increased significantly in the treated samples. There was a significantly lower preference for beans treated with permeate fractions than for control beans. Plums were canned in a control sucrose syrup (20° Brix) and in syrups with 5, 10, 15, 20, and 25% replacement of sucrose with HP, or crystalline glucose-galactose (GG) mixture. HP plums were generally darker in color and similar in texture to the control samples. Sensory tests showed that general acceptability of HP plums was similar to control samples.     

Ultrafiltration and reverse osmosis for clarification and concentration of fruit juices at pilot plant scale

The process of ultrafiltration of raw juices (peach, pear, apple and mandarin) through tubular polysulphone membranes (8 kDa) and finally concentrated by reverse osmosis membranes of tubular composite polyamide film (99 g/100 g NaCl rejection) with filtration area of 0.9 m² was studied. Furthermore, in order to obtain a higher permeate flow, the fluids were previously treated with commercial pectinolytic enzyme.The following parameters were analyzed: permeate flow, soluble solids, viscosity, density, pH, acidity, formol index, starch, pulp content, color and presence of pectin. The use of a pectinolytic enzyme provides increased permeate flux of approximately 40%, retaining the juice properties. The highest total soluble solids content was clarified peach juice from 12.2 °Brix concentrated up to 30.5 and 21.52 °Brix by using RO with transmembranes pressures of 4 and 2 MPa respectively.The results show a cross-flow velocity (1.8 m/s) which corresponds with Reynolds number that is on the lower border of a laminar flow and above of transition rate (2090 < Re < 2900). Also the (VCF) for mandarin (1.49), pear (1.53), apple (1.56) and peach (1.58) was obtained for RO process. The membranes used were characterized morphologically using scanning electron microscopy.     

One option for the management of wastewater from tofu production: Freeze concentration in a falling-film system

Tofu whey is a liquid by-product from tofu production. Although it contains oligosaccharides, proteins and isoflavones, which could be isolated and used as ingredients for functional products, it is currently not utilized but disposed as a waste stream. However, when disposed directly to the environment tofu whey can cause bad odours and pollution of the surface and ground water, so that treatment is necessary. The wastewater treatment of industrial tofu production by current technologies is problematic, because of the high expenses and the lack of knowledge about their efficient operation. Hence the need to use alternative technologies such as freeze concentrations. Falling-film freeze concentration tests of tofu whey were carried out on pilot-scale equipment in three stages. The increase in soluble solids content of the tofu whey and the amount and purity of the ice formed were analysed. It was observed that the concentration could be increased by a factor of 8 (from an initial concentration of 1.9°Brix to a final concentration of 15.5°Brix). The electrical conductivity of the tofu whey at the last stage was 6.48 mS/cm and the pH was 5.22. The process efficiency was 82.9% at the first stage but dropped to lower values at later stages. Falling film freeze concentration is a promising alternative to recover the solutes retained in the effluent from the tofu industry, reducing its volume and improving environmental management.