Thermal and structural behavior of milk fat. 3. Influence of cooling rate and droplet size on cream crystallization

Crystallization of triacylglycerols (TG) within milk fat globules of creams is studied with an instrument coupling time-resolved synchrotron X-ray diffraction (XRDT) at both small and wide angles and high-sensitivity differential scanning calorimetry (DSC) at cooling rates of -3 and -1 degrees C/min from 60 to -10 degrees C and compared to that of the anhydrous milk fat (AMF). Simultaneous thermal analysis permits correlation of the formation of the different crystalline species monitored by XRDT to the DSC events. Under the above cooling conditions, milk fat TG sequentially crystallize, within the globules, from about 19 degrees C, in three different lamellar structures with double-chain length (2L) stackings of 47 and 42 A and a triple-chain length (3L) stacking of 71 A, all of alpha type, which are correlated to two or three overlapped exothermic peaks recorded by DSC. Compared to what is observed for AMF, TG crystallization in emulsion (i) favors sub-alpha formation at low temperature and (ii) induces layer stacking defects in 3L crystals. Subsequent heating at 2 degrees C/min shows numerous structural rearrangements before final melting, confirming that (i) cooling at -1 degrees C/min leads to the formation of unstable crystalline varieties in the dispersed state and (ii) a monotropic transition alpha-->beta' takes place. Similar behavior is observed for cooling at -3 degrees C/min and subsequent heating. An overall comparison of the thermal and structural properties of the crystalline species formed as a function of the cooling rate, between >1000 and 0.15 degrees C/min, and stabilization time at 4 degrees C is given. Depending on the cooling rate, at least five crystalline subcell species are observed at wide angles, alpha and sub-alpha, two beta' and one beta. At small angles, at least six lamellar stackings are identified, three 3L and three 2L. However, a single subcell packing (e.g., alpha) might correspond to several longitudinal chain stackings, demonstrating the usefulness of the small-angle XRD technique. Reconstituted emulsions homogenized under different pressures are used to determine the influence of droplet size on crystallization. The decrease of droplet size induces (i) a higher supercooling/supersaturation and (ii) a higher disorder and/or a smaller size of TG crystals within the emulsion droplets. At the supramolecular scale, polarized light microscopy shows that various cooling rates applied in situ using a temperature-controlled stage directly influence crystal sizes and their type of organization within milk fat globules. The faster the cooling rate, the smaller the size of the crystals within the globules.     

Synchrotron radiation macrobeam and microbeam X-ray diffraction studies of interfacial crystallization of fats in water-in-oil emulsions

Using macrobeam and microbeam techniques, we performed synchrotron radiation X-ray diffraction (SR-XRD) analyses of fat crystallization in water-in-oil (W/O) emulsion, in combination with DSC and polarized optical microscopic observation. Particular focus was on the crystallization of the fats around water droplets in the W/O emulsion systems using food emulsifiers of polyglycerol polyricinoleate (PGPR) alone (PGPR emulsion), and PGPR and monobehenoylglycerol (MB) (PGPR+MB emulsion). We obtained the following results: (1) macrobeam SR-XRD confirmed that adding MB promoted fat crystallization during cooling, (2) microbeam SR-XRD indicated that the lamellar planes of fat crystals near the water and oil interfaces are arranged almost parallel to the interface planes in both PGPR emulsion and PGPR+MB emulsion, and (3) adding MB resulted in the formation of tiny fat crystals because it promoted crystallization, which occurred both in the bulk oil phase and at the W/O interfaces. The present study is the first to apply microbeam SR-XRD to observe the microscopic features of fat crystallization in W/O emulsion, following fat crystallization in the oil droplets in the oil-in-water (O/W) emulsion (Arima, S.; Ueno, S.; Ogawa, A.; Sato, K. Langmuir 2009, 25, 9777-9784).     

Retardation of crystallization-induced destabilization of PMF-in-water emulsion with emulsifier additives

An oil-in-water (O/W) emulsion, in which the oil phase is semi-solid fat, is easily destabilized when stored below the crystallization temperature of the oil phase. Such destabilization, characterized by loss of fluidity at chilled temperature and oil-water separation after re-heating, is caused by inter-droplet bridging of fat crystals protruding out of the emulsion droplets. In the present study, we found that the simultaneous use of additives of highly hydrophobic sucrose oligoester (SOE; P-170) and highly hydrophilic SOE (P-1670) containing palmitic acid moiety remarkably retarded the crystallization-induced destabilization of the O/W emulsion that contains palm-mid-fraction (PMF) as the oil phase. Without the additives, destabilization occurred when the emulsion was cooled from 60 to 0 degrees C and kept at 0 degrees C for 1 day. Microscopic observation revealed that destabilization was caused by coalescence of the oil droplets, which was triggered by the growth of needle-shaped PMF crystals protruding out of the emulsion membranes. However, the addition of P-170 to PMF increased the crystallization temperature of PMF and at the same time retarded the destabilization. Furthermore, the simultaneous addition of P-170 and P-1670 retarded the crystallization-induced destabilization even more. Optical observation, DSC, and synchrotron radiation X-ray diffraction measurements indicated that the P-170 additive enhanced interfacial heterogeneous crystallization to form tiny PMF crystals in the droplets, and that the P-1670 additive retarded morphological change of the PMF crystals into long needle shapes in association with polymorphic transformation from alpha to beta'.     

Spreading of partially crystallized oil droplets on an air/water interface

The influence of crystalline fat on the amount and rate of oil spreading out of emulsion droplets onto either a clean or a protein-covered air/water interface was measured for β-lactoglobulin stabilized emulsions prepared with either anhydrous milk fat or a blend of hydrogenated palm fat and sunflower oil. At a clean interface, liquid oil present in the emulsion droplets was observed to completely spread out of the droplets unimpeded by the presence of a fat crystal network. Further, the presence of a fat crystal network in the emulsion droplets had no effect on the rate of oil spreading out of the droplets. At a protein-covered interface, the spreading behavior of emulsion droplets containing crystalline fat was evaluated in terms of the value of the surface pressure (Π_AW) at the point of spreading; Π_AW at spreading was unaffected by the presence of crystalline fat. We conclude it is unlikely that the role of crystalline fat in stabilizing aerated emulsions such as whipped cream is to reduce oil spreading at the air/water interface. However, the temperature of the system did have an effect: spontaneous spreading of emulsion droplets at clean air/water interfaces occurred for systems measured at 5 °C, but not for those measured at 22 or 37 °C. Thus, temperature may play a more important role in the whipping process than commonly thought: the entering and spreading of emulsion droplets was favored at lower temperatures because the surface pressure exerted by protein adsorbed at the air/water interface was reduced. This effect may facilitate the whipping process.     

Synthesis of poly(methyl methacrylate) nanocomposites via emulsion polymerization using a zwitterionic surfactant

The synthesis of nanocomposites via emulsion polymerization was investigated using methyl methacrylate (MMA) monomer, 10 wt % montmorillonite (MMT) clay, and a zwitterionic surfactant octadecyl dimethyl betaine (C18DMB). The particle size of the diluted polymer emulsion was about 550 nm, as determined by light scattering, while the sample without clay had a diameter of about 350 nm. The increase in the droplet size suggests that clay was present in the emulsion droplets. X-ray diffraction indicated no peak in the nanocomposites. Transmission electron microscopy showed that emulsion polymerization of MMA in the presence of C18DMB and MMT formed partially exfoliated nanocomposites. Differential scanning calorimetry showed an increase of 18 degrees C in the glass transition temperature (Tg) of the nanocomposites. A dynamic mechanical thermal analyzer also verified a similar Tg increase, 16 degrees C, for the partially exfoliated nanocomposites over poly(methyl methacrylate) (PMMA). Thermogravimetric analysis indicated a 37 degrees C increase in the decomposition temperature for a 20 wt % loss. A PMMA nanocomposite with 10 wt % C18DMB-MMT was also synthesized via in situ polymerization. This nanocomposite was intercalated and had a Tg 10 degrees lower than the emulsion nanocomposite. The storage modulus of the partially exfoliated emulsion nanocomposite was superior to the intercalated structure at higher temperatures and to the pure polymer. The rubbery plateau modulus was over 30 times higher for the emulsion product versus pure PMMA. The emulsion technique produced nanocomposites of the highest molecular weight with a bimodal distribution. This reinstates that exfoliated structures have enhanced thermal and mechanical properties over intercalated hybrids.     

Thermal imidization and structural evolution of thin films of poly(4,4'-oxydiphenylene p-pyromellitamic diethyl ester)

The evolution of chemical composition and structure during the thermal imidization of an ester-type polyimide precursor, poly(4,4'-oxydiphenylene p-pyromellitamic diethyl ester), in micrometer scale films were studied for a heating rate of 2.0 degrees C/min with time-resolved synchrotron X-ray diffraction, in-situ infrared spectroscopy, and modulated differential scanning calorimetry. Our analyses show that the precursor polymer undergoes imidization in a two-step process. In the first step, the precursor polymer is decomplexed from the residual solvent molecules, and in the second step, it undergoes imide ring formation with the release of ethanol as a byproduct. The imidization reaction starts around 210 degrees C and continues up to 320 degrees C. The thermal imidization reaction induces the structural evolution of the film. As the imidization reaction proceeds, the coherent length along the polymer chain axis increases. This imidization-induced structural evolution was found to occur via three steps: (i) initiation, (ii) the first crystallization, and (iii) the second crystallization. The initiation step is necessary prior to the evolution of the crystalline structure to increase the chain mobility of the precursor polymer chains, and it requires thermal heating up to at least 238 degrees C at which point 22.5% of the imidization is complete. Thereafter, the first crystallization occurs up to 310 degrees C, at which point 98.3% of the imidization is complete. In the range 310-380 degrees C, the second crystallization occurs and produces almost complete imidization of the polymer chains.     

Synthesis and structural evolution of rusb3, a new metastable skutterudite compound

A thin-layer synthesis technique was used to synthesize bulk amounts of the metastable phase, RuSb(3), a novel compound with the skutterudite structure. The compound crystallized at 350 degrees C and was stable to 525 degrees C. When annealed above 550 degrees C, it decomposed into RuSb(2) and Sb. Rietveld refinement of X-ray diffraction data showed the presence of excess Sb residing in the interstitial site in the skutterudite structure. X-ray diffraction and thermal analysis experiments allowed us to examine the evolution of the sample as a function of annealing and determine the reaction pathway. The activation energy for the crystallization of the compound was determined to be 3 eV/nucleation event, while the activation energy for decomposition was approximately 8 eV.     

Melting characteristics of fat present on the surface of industrial spray-dried dairy powders

The melting characteristics of the fat present on the surface (surface free-fat) of two industrial spray-dried dairy powders (cream powder and whole milk powder) were investigated in comparison with those of other milk fat fractions present in the powder, such as free-fat from the interior of the powder particle (inner free-fat) and encapsulated fat. The melting characteristics of the milk fat fractions were studied by fatty acid composition, melting profile and solid fat content profile. The results indicated that all milk fat fractions including surface free-fat contained various triglycerides with melting points ranging from -40 to +40 degrees C. However, some fractionation was observed among the different milk fat fractions. The free-fat fractions (surface free-fat and inner free-fat) had a greater proportion of high-melting triglyceride species than the encapsulated fat. Furthermore, the high-melting triglyceride species present in the free-fat fractions were slightly accumulated at the surface of powder. This phenomenon was observed in both cream powder and whole milk powder and its effect on wetting time was established. This indicates that manipulation of the surface fat content during drying operation may hold the key to functionality improvement.     

Thermal transitions and fat droplet stability in ice-cream mixmodel systems

We studied thermal transitions and physical stability of oil-in-water emulsions containing different milk fat compositions, arising from anhydrous milk fat alone (AMF) or in mixture (2:1 mass ratio) with a high melting temperature (AMF–HMT) or a low melting temperature (AMF–LMT) fraction. Changes in thermal transitions in bulk fat and emulsion samples were monitored by differential scanning calorimetry (DSC) under controlled cooling and reheating cycles performed between 50 and –45°C (5°C min^–1). Comparison between bulk fat samples and emulsions indicated similar values of melting completion temperature, whereas initial temperature of fat crystallization (T_onset) seemed to be differently affected by storage temperature depending on triacylglycerols (TAG) composition. After storage at 4°C, T_onset values were very similar for emulsified and non-emulsified AMF–HMT blend, whereas they were lower (by approx. 6°C) for emulsions containing AMF or mixture of AMF–LMT fraction. After storage at –30°C, T_onset values of re-crystallization were higher in emulsion samples than in bulk fat blends, whatever the TAG fat composition. Light scattering measurements and fluorescence microscopic observations indicated differences in fat droplet aggregation-coalescence under freeze-thaw procedure, depending on emulsion fat composition. It appeared that under quiescent freezing, emulsion containing AMF–LMT fraction was much less resistant to fat droplet aggregation-coalescence than emulsions containing AMF or AMF–HMT fraction. Our results indicated the role of fat droplet liquid-solid content on emulsion stability.     

Influence of environmental stresses on stability of oil-in-water emulsions containing droplets stabilized by beta-lactoglobulin-iota-carrageenan membranes

An oil-in-water emulsion (5 wt% corn oil, 0.5 wt% beta-lactoglobulin (beta-Lg), 0.1 wt% iota-carrageenan, 5 mM phosphate buffer, pH 6.0) containing anionic droplets stabilized by interfacial membranes comprising of beta-lactoglobulin and iota-carrageenan was produced using a two-stage process. A primary emulsion containing anionic beta-Lg coated droplets was prepared by homogenizing oil and emulsifier solution together using a high-pressure valve homogenizer. A secondary emulsion containing beta-Lg-iota-carrageenan coated droplets was formed by mixing the primary emulsion with an aqueous iota-carrageenan solution. The stability of primary and secondary emulsions to sodium chloride (0-500 mM), calcium chloride (0-12 mM), and thermal processing (30-90 degrees C) were analyzed using zeta-potential, particle size and creaming stability measurements. The secondary emulsion had better stability to droplet aggregation than the primary emulsion at NaCl 相似文献   

Crystallization, transformation and microstructures of polymorphic fats in colloidal dispersion states

This article reviews new information about polymorphic structures, kinetic and microscopic properties of fat crystals in colloidal dispersion states such as aggregates (spherulite), oil-in-water (O/W) emulsion and water-in-oil (W/O) emulsion. The kinetic processes of fat crystallization under external factors such as different cooling rates, shear and ultrasound irradiation are reviewed. Microstructures of fats revealed by synchrotron radiation microbeam X-ray diffraction techniques in bulk and emulsion states are also reviewed for the first time.     

Emulsion stability based on phase behavior in sodium naphthenates containing systems: gels with a high organic solvent content

Addition of heptane to a sodium naphthenates/toluene/water system at 25 degrees C reduces the lamellar liquid-crystal phase range and increases the microemulsion phase range. Both of these effects result in the extension of the composition range where emulsions have low stability. This effect is even stronger at 40 degrees C. Heptane addition also results in the formation of very stable emulsions within the overlapping phase-existence ranges of aqueous (L1) and organic (L2) phases. Stable non-birefringent gel observed in equilibrium with L1 and L2 phases contains only a small percentage of water and sodium naphthenates. The swelling behavior of an unstable gel, an emulsion previously compressed by centrifugation, appears to be due to a stepwise thickening of the thin liquid films between the droplets.     

Effect of surfactant sucrose ester on physical properties of dairy whipped emulsions in relation to those of O/W interfacial layers

Dairy foams were manufactured on a pilot plant with various sucrose ester contents. Oil-in-water emulsions were produced by high-pressure homogenisation of anhydrous milk fat (20 wt%) with an aqueous phase containing skim milk powder (6.5 wt%), sucrose (15 wt%), hydrocolloids (2 wt%), and sucrose esters. Sucrose ester content was varied from 0 to 0.35 wt%. Firmness and stability of dairy foams were determined. The fraction of protein associated with emulsion fat droplets and the compression isotherms of those droplets were determined as a function of sucrose ester content. With less than 0.1 wt% sucrose ester, no foam could be produced. The most firm and stable foams were obtained with ca. 0.1 wt% sucrose ester. The fraction of protein associated with emulsion droplets suddenly falls from 60% at a sucrose ester content lower than 0.1125% down to ca. 10-20% for higher surfactant content. Compression isotherms of emulsion droplets at the air-water interface show that, in the presence of surfactant, emulsion droplets disrupt and spread at the interface whilst without surfactant they become dispersed. This means that the presence of sucrose ester causes some destabilisation of fat droplet interfacial layers. There is hence an optimal sucrose ester content that allows some destabilisation of the oil-water interface without concomitant protein displacement from that interface. Consequently, with the recipe and manufacturing process used to produce dairy foams, there exists a compromise in sucrose ester content with regards to manufacture and shelf-life of dairy foams.     

Crystallization behaviors of nanosized MgO particles from magnesium alkoxides

The effects of the size of the alkoxy group on the thermal decomposition behavior of magnesium alkoxides (magnesium methoxide and ethoxide) and the crystallization behavior of MgO was investigated using thermogravimetry, Fourier-transformed infrared spectroscopy, X-ray powder diffraction, and transmission electron microscopy. As the size of the alkyl group increased, the decomposition temperature decreased and resultant MgO crystallization of the alkoxide precursor was enhanced. In an inert N(2) atmosphere, the decomposition temperature of magnesium ethoxide was about 260 degrees C, which was lower than that of magnesium methoxide by approximately 70 degrees C. The degree of the crystallization of MgO particles from the ethoxide was also significantly higher than that of the methoxide. This result is explained in terms of the O-R bonding strength of the alkoxide. With use of the Kissinger method, the activation energy for the thermal decomposition of magnesium alkoxide was found to be dependent on the size of the alkyl group. The activation energies were 161+/-23 and 130+/-24 kJ/mol for the magnesium methoxide and the magnesium ethoxide, respectively.     

Influence of iota-carrageenan on droplet flocculation of beta-lactoglobulin-stabilized oil-in-water emulsions during thermal processing

The influence of thermal processing on droplet flocculation in oil-in-water emulsions stabilized by either beta-lactoglobulin (primary emulsions) or beta-lactoglobulin-iota-carrageenan (secondary emulsions) at pH 6 has been investigated. In the absence of salt, the zeta-potential of the primary emulsion was less negative (-40 mV) than that of the secondary emulsion (-55 mV) due to adsorption of anionic iota-carrageenan to the anionic beta-Lg-coated droplet surfaces. The zeta-potential and mean diameter (d(43) approximately 0.3 microm) of droplets in primary and secondary emulsions did not change after storage at temperatures ranging from 30 to 90 degrees C. In the presence of 150 mM NaCl, the zeta-potential of the primary emulsion was much less negative (-27 mV) than that of the secondary emulsion (-50 mV), suggesting that the latter was less influenced by electrostatic screening effects. The zeta-potential of the primary emulsions did not change after storage at elevated temperatures (30-90 degrees C). The zeta-potential of the secondary emulsions became less negative, and the aqueous phase iota-carrageenan concentration increased at storage temperatures exceeding 50 degrees C, indicating iota-carrageenan desorbed from the beta-Lg-coated droplets. In the primary emulsions, appreciable droplet flocculation (d(43) approximately 8 microm) occurred at temperatures below the thermal denaturation temperature (T(m)) of the adsorbed proteins due to surface denaturation, while more extensive flocculation (d(43) > 20 microm) occurred above T(m) due to thermal denaturation. In the secondary emulsions, the extent of droplet flocculation below T(m) was reduced substantially (d(43) approximately 0.8 microm), which was attributed to the ability of adsorbed carrageenan to increase droplet-droplet repulsion. However, extensive droplet flocculation was observed above T(m) because carrageenan desorbed from the droplet surfaces. Differential scanning calorimetry showed that iota-carrageenan and beta-Lg interacted strongly in aqueous solutions containing 0 mM NaCl, but not in those containing 150 mM NaCl, presumably because salt weakened the electrostatic attraction between the molecules.     

Fat crystallization in complex food emulsions: Effects of adsorbed milk proteins and of a whipping process

Crystallization of fat droplets in complex emulsions, which differed only by the initial structure of proteins, was studied by differential scanning calorimetry, before and after application of a whipping process. Upon cooling at 5 or 1°C min^–1, the temperature needed to initiate fat crystallization was lower, and one more distinguishable crystallization peak was detected in emulsions containing caseins, in comparison with the emulsion containing pure whey proteins. Furthermore, the whipping process was accompanied by more protein depletion from the fat droplet surface, less resistance to coalescence, and a lower supercooling effect in the emulsion based on pure whey proteins.This revised version was published online in November 2005 with corrections to the Cover Date.     

Controlled nucleation and growth of CdS nanoparticles in a polymer matrix

In-situ synchrotron X-ray diffraction (XRD) was used to monitor the thermal decomposition (thermolysis) of Cd thiolates precursors embedded in a polymer matrix and the nucleation of CdS nanoparticles. A thiolate precursor/polymer solid foil was heated to 300 degrees C in the X-ray diffraction setup of beamline W1.1 at Hasylab, and the diffraction curves were each recorded at 10 degrees C. At temperatures above 240 degrees C, the precursor decomposition is complete and CdS nanoparticles grow within the polymer matrix forming a nanocomposite with interesting optical properties. The nanoparticle structural properties (size and crystal structure) depend on the annealing temperature. Transmission electron microscopy (TEM) and photoluminescence (PL) analyses were used to characterize the nanoparticles. A possible mechanism driving the structural transformation of the precursor is inferred from the diffraction features arising at the different temperatures.     

Fat retention at the tongue and the role of saliva: adhesion and spreading of 'protein-poor' versus 'protein-rich' emulsions

Fat perception of food emulsions has been found to relate to in-mouth friction. Previously, we have shown that friction under mouth-like conditions strongly depends on the sensitivity of protein-stabilized emulsion droplets to coalescence. Here, we investigated whether this also implies that oral fat retention depends in a similar manner on the stability of the emulsion droplets against coalescence. We investigate the separate contributions of droplet adhesion and droplet spreading to fat retention at the tongue, as well as the role of saliva. We perform ex vivo (Confocal Raman Spectroscopy; Confocal Scanning Laser Microscopy) experiments using pig's tongue surfaces in combination with human in vivo experiments. These reveal that protein-poor (unstable) emulsions are retained more at the tongue than protein-rich (stable) emulsions. Furthermore, the layer formed by adhering protein-poor droplets is more stable against rinsing. Saliva is found to be very efficient in removing fat and emulsion droplets from the oral surface but its role in fat retention needs further research. We relate our results to the colloidal forces governing droplet adhesion and spreading.     

Production and characterization of oil-in-water emulsions containing droplets stabilized by multilayer membranes consisting of beta-lactoglobulin, iota-carrageenan and gelatin

The influence of environmental conditions (pH, NaCl, CaCl2, and temperature) on the properties and stability of oil-in-water (O/W) emulsions containing oil droplets surrounded by one-, two-, or three-layer interfacial membranes has been investigated. Three oil-in-water emulsions were prepared with the same droplet concentration and buffer (5 wt % corn oil, 5 mM phosphate buffer, pH 6) but with different biopolymers: (i) primary emulsion: 0.5 wt % beta-Lg; (ii) secondary emulsion: 0.5 wt % beta-Lg, 0.1 wt % iota-carrageenan; (iii) tertiary emulsion: 0.5 wt % beta-Lg, 0.1 wt % iota-carrageenan, 0-2 wt % gelatin. The secondary and tertiary emulsions were prepared by electrostatic deposition of the charged biopolymers onto the surfaces of the oil droplets so as to form two- and three-layer interfacial membranes, respectively. The stability of the emulsions to pH (3-8), sodium chloride (0-500 mM), calcium chloride (0-12 mM), and thermal processing (30-90 degrees C) was determined. We found that multilayer emulsions had better stability to droplet aggregation than single-layer emulsions under certain environmental conditions and that one or more of the biopolymer layers could be made to desorb from the droplet surfaces in response to specific environmental changes (e.g., high salt or high temperature). These results suggest that the interfacial engineering technology used in this study could lead to the creation of food emulsions with improved stability to environmental stresses or to emulsions with triggered release characteristics.     

Determination of fat in dairy products using pressurized solvent extraction

Gravimetric fat data were obtained for a wide range of dairy products with fat contents ranging from 0.5 to 83% using pressurized solvent extraction at elevated temperatures and pressure (80-120 degrees C; 10.3 MPa). Extraction performance was sensitive to solvent composition, temperature, and sample matrix. By optimizing solvent mixtures, sample-solvent contact times of 8-10 min were sufficient for high recoveries from all products tested. The most successful solvents with regard to speed of extraction, selectivity, and recovery (average recovery, %) were various mixtures of hexane (or petroleum ether)-dichloromethane-methanol for dried cream (99.8%), dried whole milk (99.6%), dried buttermilk (98.2%), dried skim milk (97.0%), dried whey protein concentrate (97.5%), casein (95.0%), and caseinate (102.1%); petroleum ether-acetone-ethanol or petroleum ether-acetone-isopropanol for cheddar-type cheese (99.4%); petroleum ether-acetone for butter (99.9%); petroleum ether-acetone-isopropanol for cream (100.3%); and petroleum ether-isopropanol for liquid milks (99.0%). Relative standard deviations for repeatability were obtained for dried whole milk (0.2%), dried whey protein concentrate (0.7%), cheese (0.3%), butter (0.1%), and ultraheat treated (UHT) milk (0.7%). Solvent removal and drying of extracts with a heated block evaporator saved time compared with conventional drying ovens. Estimated savings in labor (50-75%) and solvents (80%) were substantial compared with the manual Mojonnier methods.