Recommendations for rationalizing cleaning-in-place in the dairy industry: case study of an ultra-high temperature heat exchanger.

The objective of this work was to propose a new strategy, based on objective and rational arguments and calculations, that can be implemented by plant designers and operators in the dairy industry to reduce operating time and the volume and load of effluents. The strategy is based on the on-line and off-line use of sensors and tracers, the accuracy, relevance, and robustness of which were evaluated for each phase of the sequence used for cleaning an industrial sterilizer. The efficient duration of each phase of the cleaning sequence (management of the end of operation) and the sorting of the fluids (management of mixtures and destination of fluids) were determined in real time. As a result, significant reduction in total overall duration of the cleaning sequence, wastewater volume (waste volume was reduced by half), and detergent volume (caustic soda and acid was reduced by up to a few tens of kilograms per cleaning) was achievable.

Effect of prehydrolysis of milk fat on its conversion to biogas.

Milk fat is considered to be the main limiting component of the kinetics of dairy wastewater anaerobic digestion. The objective of this work was to give a better understanding of the nonelucidated anaerobic degradation steps of milk fat. For that purpose, the kinetics of fat degradation was quantified in comparison with other milk components (lactose, proteins), regarding the milk fat polluting load and structure [globular (native state), triglycerides]. This work confirms that milk fat is degraded after a lag phase of several days, with a maximal degradation rate 2 to 5 times less than the degradation rate of the other milk components. It was shown that (1) the structure of the fat does not influence the limits of its anaerobic degradation; (2) the lag phase before biogas production is mainly due to unsaturated free fatty acids (FFA); and (3) conversion to biogas occurs at a lower rate for saturated than for unsaturated FFA. Therefore, the prehydrolysis of fat, which increases the instantaneous concentration of unsaturated FFA, sharply increases the length of the lag phase with no significant change in the maximal biogas production rate. To reduce the delay imposed in the biogas production, it is necessary to reduce the concentration of unsaturated FFA.

The membrane role in an anaerobic membrane bioreactor for purification of dairy wastewaters: a numerical simulation.

A simplified modelling and a simulation of a membrane-coupled anaerobic bioreactor, AMBR were performed to assess the potential of controlled retention of solutes by the membrane, R, on biomass growth and of purified water quality. R was shown to be a major parameter, which enables to uncouple the hydraulic resistance time, HRT from the solute retention time, independent of biomass retention, and has a significant effect on purified water quality. Therefore, from a theoretical point of view, it facilitates reaching high biodegradation in a small volume membrane reactor. The simulation makes it possible: (i) to anticipate the effect and relative weight of model parameters in the mechanisms that rule the AMBR behaviour and (ii) to identify the AMBR parameters and operating modes in order to avoid reactor washout or overload, amplified by R. From the analysis, it appears that it is possible to use any type of membrane, which at least retain the biomass: (i) low R values using microfiltration or ultrafiltration membranes require long HRT or small influent concentration and larger reactor volume to achieve good water quality; (ii) high R values using nanofiltration or reverse osmosis membranes, which will retain the solutes as well as the small-degraded molecules within the anaerobic reactor volume, require short HRT for highly purified water, but necessitate a large investment.

Denitrification potential and rates of complex carbon source from dairy effluents in activated sludge system.

A predictive model for the denitrification performance of complex carbon sources was proposed based on compositional data. Potential and rates of denitrification of single dairy components (lactose, lactate, proteins, fat), as well as binary and complex (modelled "process water") mixtures were assessed using test for nitrogen uptake rate (NUR). In all experiments, denitrification potential of mixtures was found to be significantly higher than the sum of individual potentials and denitrification rate with the readily biodegradable moiety of the mixtures was similar to the highest rate obtained with individual components (lactose or lactate). This work shows that activated sludge acclimated to dairy components can be modelled as a single biomass where the maximal anoxic growth rate of the biomass limits the denitrification rate with dairy components. As a consequence, lactose or lactate determine the maximal denitrification rate possible using dairy effluents.

Process steps for the preparation of purified fractions of alpha-lactalbumin and beta-lactoglobulin from whey protein concentrates.

Fractions enriched with alpha-lactalbumin (alpha-la) and beta-lactoglobulin (beta-lg) were produced by a process comprising the following successive steps: clarification-defatting of whey protein concentrate, precipitation of alpha-lactalbumin, separation of soluble beta-lactoglobulin, washing the precipitate, solubilization of the precipitate, concentration and purification of alpha-la. The present study evaluated the performance of the process, firstly on a laboratory scale with acid whey and then on a pilot scale with Gouda cheese whey. In both cases soluble beta-lg was separated from the precipitate using diafiltration or microfiltration and the purities of alpha-la and beta-lg were in the range 52-83 and 85-94% respectively. The purity of the beta-lg fraction was higher using acid whey, which does not contain caseinomacropeptide, than using sweet whey. With the pilot scale plant, the recoveries (6% for alpha-la; 51% for beta-lg) were disappointing, but ways of improving each step in the process are discussed.

Ionic interactions in nanofiltration of beta casein peptides

Nanofiltration (NF) membrane technology shows interesting potentials for separating organic components on the basis of solute charge and size in the range of 300-1000 g mol-1. Separation properties of two inorganic NF membranes were studied with a set of 10 small peptides (molecular mass range: 300-900 g mol-1; 3 < pI < 10) contained in a well-characterized tryptic beta casein hydrolysate. Peptides transmission strongly depended on ionic interactions in the system. Physicochemical conditions such as ionic strength and especially pH were crucial to the separation, because the membrane and peptides showed amphoteric properties. Thus, the three categories of peptides (acid, basic, neutral) were separated according to their pI because of presumed concentration gradients of charged peptides at the membrane: positive for basic peptides and negative for acid peptides. At optimum pH 8 this led to high transmissions of basic peptides (even over 100%), intermediate transmissions for neutral peptides, and low transmissions for acid peptides. The addition of multicharged cationic and anionic species in the hydrolysate induced a markedly enhanced selectivity when the polyelectrolyte was a membrane coion and a complete reversion of selectivity when it was a membrane counterion. Copyright 1998 John Wiley & Sons, Inc.

Selective separation of amino acids with a charged inorganic nanofiltration membrane: effect of physicochemical parameters on selectivity.

A charged organic-inorganic nanofiltration (NF) membrane prototype was used to separate a mixture of nine amino acids (AA) on the basis of differential electrostatic interactions with the membrane because, for a given pH, some of them were positively charged, some were negative, and some were zwitterions. Effect of pH, amino acid concentration (C(r)), and added ionic strength ([NaCI]) on the process selectivity was studied. A global statistical study revealed that pH was the dominant parameter regarding fractionation. C(r) and [NaCI] had a weaker effect, but the ratio C(r)/[NaCI] demonstrated a pronounced effect on system selectivity. Two split-ups of the mixture were obtained at pH 2 and at pH 12, for a 1-g/L total AA concentration and a C(r)/[NaCI] ratio of 0.16. Under these conditions, the differences in transmissions between basic and acid AA were higher than 70%. Interpretation of the results according to the Donnan theory allows us to foresee the potentialities of charged nanofiltration membranes for the fractionation of a complex mixture, such as peptidic hydrolysate to streams containing peptides and amino acids having different isoelectric points. (c) 1997 John Wiley & Sons, Inc. Biotechnol Bioeng 54: 291-302, 1997.

Whey protein fractionation: isoelectric precipitation of alpha-lactalbumin under gentle heat treatment.

The selective precipitation of alpha-lactalbumin (alpha-LA) at a pH around its isoelectric point (4.2) under heat treatment is the basis for a fractionation process of whey proteins. In these conditions, beta-lactoglobulin remains soluble, whereas bovine serum albumin and immunoglobulins co-precipitate. Knowledge of the mechanism governing the alpha-LA precipitation influences the choice of operating conditions and enables optimization of the fractionation process. alpha-LA is a calcium metallo-protein and its isoelectric precipitation is governed by the protein-calcium complexation equilibrium. Citrate, a sequestrant of calcium, decreases the free calcium concentration and displaces the precipitation phenomenon to a lower temperature range. A study of the effect of citrate on the precipitation phenomena of whey proteins is presented. Whatever the citrate content, precipitation curves for bovine serum albumin (BSA) and alpha-LA intersect at a temperature around 45 degrees C. For a temperature of heat treatment lower than 40 degrees C, a selective enrichment in alpha-LA of the precipitated phase is observed. As addition of citrate leads to high alpha-LA precipitated fractions at a temperature around 35 degrees C, the precipitation step may be performed at this temperature. It results in a reduced heat denaturation of whey proteins and in a higher alpha-LA purity in the precipitated fraction. (c) 1997 John Wiley & Sons, Inc. Biotechnol Bioeng 56: 391-397, 1997.

Transient and stationary operating conditions on performance of lactic acid bacteria crossflow microfiltration.

A filtration rig equipped with a tubular alumina membrane was used to study the performance of crossflow microfiltration of Lactobacillus helveticus. Experiments were performed at constant permeation flux. High cell concentrations and fast transient conditions to the stationary J adversely affected permeability. Membrane fouling was due to a fast irreversible layer formation and to a reversible cell cake. This microbial deposit characteristics were dependent on the ratio permeation flux/wall shear stress, J/tau(w). Fouling was faster and more severe when J/tau(w) was greater than a critical value of 1.15 L(-1) x h(-1) x m(-2) x Pa(-1). The disordered structure of this cell cake seemed to lead to a macromolecule deposit between the cells which adversely affected the membrane permeability.

Thermal isoelectric precipitation of alpha-lactalbumin from a whey protein concentrate: Influence of protein-calcium complexation.

The selective precipitation of alpha-lactalbumin (alpha-LA) at a pH around its isoelectric point (4.2) under heat treatment is the basis for a fractionation process of whey proteins. As precipitation is a phenomenon dependent on the protein hydrophobicity, and as the release of the tightly bound calcium occurring at pH around 4 modifies the alpha-LA hydrophobicity, the specific role of calcium on isoelectric precipitation is investigated. A study of the extent of alpha-LA precipitation in a whey protein concentrate under various operating conditions of pH, temperature, protein concentration, and calcium content is presented. We propose a mechanism for this phenomenon as a combination of a complexation equilibrium and of an irreversible precipitation, to account for the influence of temperature, alpha-LA concentration total ionic content, and calcium concentration, and also to estimate the complexation equilibrium constant. (c) 1995 John Wiley & Sons, Inc.

Selective separation of tryptic beta-casein peptides through ultrafiltration membranes: Influence of ionic interactions.

Peptide separation by selective membrane filtration has numerous potential applications such as production of peptides with biological activities or spectific enrichment in compounds acting as flavoring agents or as growth factors required by the fermentation industry. The retention of peptides arising from tryptic hdroysis of beta-casein using an M5 Carbosep membrane (molecular wieght cutoll = 10,000 D) has been studied. The peptides with known sequences were characterized by their molecular weight, isoelectric point, and hydrophobicity. Our experiments highlighted that their transmission involves mechanisms other than size exclusion as developed elsewhere. The effect of ionic interactions between peptides and membrance has been investgated by vrying pH, ionic strength of bulk, and electric potential of filtering material. The charge of both peptides and membrane plays an important role in the transmission, particularly with small size and high or lkow isoelectric point. Then, peptides with the same sign as the membrane have lower transmission than expected from the size xclusion model, whereas peptides with opposite sign have higher trnsmission than expected, and even higher than 1 with some of them. (c) 1995 John Wiley & Sons, Inc.

Efficiency of cleaning agents for an inorganic membrane after milk ultrafiltration.

Cleaning of inorganic membranes after ultrafiltration (UF) of skim milk has been assessed using hydraulic, physicochemical and spectroscopic (i.r. and X-ray photoelectron spectroscopy) measurements. A cleaning sequence using hypochlorite alone or hypochlorite followed by HNO3 restored the membrane hydraulic resistance, in contrast to cleaning with HNO3 alone. When using NaOH, addition of Ca complexants (EDTA, gluconate, tripolyphosphate) and surfactants was required to obtain similar results. Three types of criteria (hydraulic, kinetic, chemical) are available to assess the effect of the sequestrant and surfactant types. In all the cases studied, traces of protein and Ca were detected on and within the membrane after cleaning. Nevertheless, it was concluded that it is possible to develop a single-step alkaline product to clean inorganic milk UF membranes if suitable surfactants and Ca sequestrants are included in its formula.

Separation of beta-casein peptides through UF inorganic membranes.

Ultrafiltration of peptide mixtures is studied under various operating conditions (transmembrane pressure, tangential flow-rate) using two ultrafiltration inorganic membranes M5 and M1 with molecular weight cut-offs, MWCO 10 and 70 kD, respectively. It is shown that the separation of peptides is controlled by a dual mechanism: size exclusion and electrostatic repulsion. When the ionic strength is high enough to screen out the electrostatic interactions, experimental data are in good agreement with a sieving model developed to estimate the intrinsic transmission from the molecular weight of a component and from the MWCO of the membranes. Although the transmission so found is altered by concentration polarisation and pore blocking mechanisms, the results explain the apparent low transmission of peptides by ultrafiltration membranes. If the ionic strength of the fluid is low, electrostatic interactions can influence the transport phenomena, provided that the molecules are highly charged (at pHs away from the pI). For attractive interactions, an apparent partition coefficient larger than 1 is observed. Otherwise, the transmission is lower than predicted by the sieving theoretical equation, as if the partition coefficient were smaller than 1.

Cleaning of inorganic membranes after whey and milk ultrafiltration.

Cleaning of an inorganic ultrafiltration membrane has been quantified through hydraulic, physicochemical, and spectroscopic (infrared and x-photoelectron spectroscopy) analyses. An efficient cleaning sequence of nitric acid followed by sodium hypochlorite has been proposed for cleaning of defatted whey protein concentrate and milk ultrafiltration membranes. The influence of reversed sequence and time reduction are discussed together with the action of both cleaning chemicals. In spite of residual fouling left after every cleaning sequence studied, hydraulic cleanliness of the membrane was achieved, particularly after the standard procedure.

Role of some whey components on mass transfer in ultrafiltration.

Ultrafiltration through Carbosep M(4) mineral membrane of protein solutions of decreasing complexity (whey before and after centrifugation or clarification, beta-lactoglobulin) was studied. Mathematical models were used to explain variations in flux with time. Taking into account variations in protein retention and hydraulic resistance of the membrane during ultrafiltration, proteins and lipoproteins were found to be involved not only in the polarization layer (reversible fouling leading to a difference in the osmotic pressure), but also in irreversible fouling by adsorption. Morever, the presence of particles (e.g., inorganic precipitates) in whey explains the build-up of a deposit over and within the membrane which contributes to the decline in flux after 1 h ultrafiltration. The relative importance of these phenomena was quantified.