\r\n\tThe versatility and multifarious skills of Underwater Work mean that it’s possible to operate over a wide range of activities, working in hyperbaric conditions or in confined spaces. The experience in the field and the detailed knowledge of diving procedures also enable the divers to operate in highly specific segments: inspection of civil-engineering structures; undersea foundations and welds; ship hull inspections and raising of wrecks; work in hostile and nuclear environments; dam inspections using an ROV (Remotely Operated Vehicle); installing or commissioning outfalls, undersea conduits and cables. \r\n\t \r\n\tVirtually all the civil-engineering trades and crafts can be transposed to Underwater Work, as in the case of high-pressure cleaning, cementing, welding, cutting, etc. \r\n\t \r\n\tNowadays, mainly stimulated by the development and encouragement of underwater oil exploration, the technical means in the form of diving equipment, installations, electronic equipment, compression and decompression chambers, as well as surface support vessels, are increasingly complex and require an ever better-prepared staff. \r\n\tThe main aim of this book is to expose and discuss the inner workings of Underwater Work, its challenges and opportunities. \r\n\t \r\n\tUnderwater Work - know, recognize the unknown, explore a new world.
",isbn:"978-1-78985-229-5",printIsbn:"978-1-78985-222-6",pdfIsbn:"978-1-78985-230-1",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"647b4270d937deae4a82f5702d1959ec",bookSignature:"Dr. Sérgio António Neves Lousada",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/9280.jpg",keywords:"Control Systems, Fluid Mechanics, Ocean Engineering, Structural Mechanics, Solid Mechanics, Subaquatic Morphology, Thermodynamics, Underwater Architecture, Underwater Engineering, Applied Mechanics, Maintenance, Diving",numberOfDownloads:269,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:0,numberOfTotalCitations:0,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 20th 2019",dateEndSecondStepPublish:"March 2nd 2020",dateEndThirdStepPublish:"May 1st 2020",dateEndFourthStepPublish:"July 20th 2020",dateEndFifthStepPublish:"September 18th 2020",remainingDaysToSecondStep:"a year",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"248645",title:"Dr.",name:"Sérgio António",middleName:null,surname:"Neves Lousada",slug:"sergio-antonio-neves-lousada",fullName:"Sérgio António Neves Lousada",profilePictureURL:"https://mts.intechopen.com/storage/users/248645/images/system/248645.jpeg",biography:"Sérgio António Neves Lousada is a Civil Engineer with a PhD\nin civil engineering and his area of knowledge is in hydraulics.\nHe teaches at the University of Madeira, Faculty of Exact Sciences and Engineering, in the Civil Engineering course, with a\nmajor field of hydraulics, environment and water resources and\nsecondary field of construction. Currently he is course director\nof the First Cycle in Civil Engineering, according to the statement of the Scientific Council of the Faculty of Exact Sciences and Engineering at\nthe University of Madeira. Since 2012, he has been researching hydraulic sciences,\nparticularly in the areas of hydraulics, urban hydraulics and marine and fluvial construction. He has published several articles and books and has participated in events\nmainly in the areas of hydraulics, urban planning, and land management.",institutionString:"University of Madeira",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"5",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"University of Madeira",institutionURL:null,country:{name:"Portugal"}}}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"11",title:"Engineering",slug:"engineering"}],chapters:[{id:"74156",title:"Diving as a Scientist: Training, Recognition, Occupation - The “Science Diver” Project",slug:"diving-as-a-scientist-training-recognition-occupation-the-science-diver-project",totalDownloads:68,totalCrossrefCites:0,authors:[null]},{id:"71423",title:"Progressive Underwater Exploration with a Corridor-Based Navigation System",slug:"progressive-underwater-exploration-with-a-corridor-based-navigation-system",totalDownloads:99,totalCrossrefCites:0,authors:[{id:"152460",title:"Dr.",name:"Mario",surname:"Jordán",slug:"mario-jordan",fullName:"Mario Jordán"}]},{id:"72795",title:"Cross-Correlation-Based Fisheries Stock Assessment Technique: Utilization of Standard Deviation of Cross-Correlation Function as Estimation Parameter with Four Acoustic Sensors",slug:"cross-correlation-based-fisheries-stock-assessment-technique-utilization-of-standard-deviation-of-cr",totalDownloads:69,totalCrossrefCites:0,authors:[null]},{id:"74726",title:"Underwater Technical Inspections Using ROV Applied to Maritime and Coastal Engineering: The Study Case of Canary Islands",slug:"underwater-technical-inspections-using-rov-applied-to-maritime-and-coastal-engineering-the-study-cas",totalDownloads:34,totalCrossrefCites:0,authors:[{id:"248645",title:"Dr.",name:"Sérgio António",surname:"Neves Lousada",slug:"sergio-antonio-neves-lousada",fullName:"Sérgio António Neves Lousada"}]}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"184402",firstName:"Romina",lastName:"Rovan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/184402/images/4747_n.jpg",email:"romina.r@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. 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1. Introduction
A fundamental characteristic of biological materials, which influence virtually every aspect of handling, storage, manufacturing and consumption of food products [1], including every aspect of the dehydration process and storage stability of the dried products [2], is their basic hygroscopicity. By this, it is meant that when biological materials are exposed to water vapor of a definite pressure, sorption of the water vapor by the product will occur. This chapter discusses the phenomena at play, their technological applications, factors that influence the characteristics, measurement techniques, models that are commonly used to predict them and models’ predictive performance evaluation procedures.
2. Sorption phenomena in biological materials
Biological materials at constant moisture content and temperature display characteristic vapor pressure and would tend to approach equilibrium with the temperature and vapor pressure of the surrounding gaseous atmosphere. To attain this equilibrium, the material either gains moisture from the environment or loses moisture to the environment depending on whether the vapor pressure of the surrounding is higher or lower than its vapor pressure [3]. The former process is called adsorption and the latter desorption. If the conditions of the surrounding are not changed for a sufficiently long period of time (theoretically for infinitely long time), the temperature at which the vapor pressure of the material and its surrounding is the same is established. At equilibrium, no further change in moisture content of the product occurs, and the moisture content of the material at that point is called equilibrium moisture content (EMC), while the relative humidity is known as equilibrium relative humidity. Water activity (aw) is another term used to denote the ERH in decimal unit. The definition of water activity is based on the concept of thermodynamics and refers to the availability of moisture in biomaterials for physical, chemical and biological changes [4, 5], and it is a property of the material.
2.1 Moisture sorption isotherm
When equilibrium is attained, the moisture content is termed adsorption EMC or desorption EMC depending on whether the equilibrium was reached thorough the adsorption or desorption process. The EMC obtained thorough the desorption process usually lies above the one obtained thorough the adsorption process in the isotherm plots and leads to formation of the hysteresis loop (MSI) when graphically expressed [6]. Brunauer et al. [7] classified moisture sorption isotherms into five general types (Figure 1). The type I is the Langmuir, while the type II is the sigmoid or S-shaped isotherm. The type III is known as the Flory-Huggins isotherm and is usually influence by the presence of solvent or plasticizer such as glycerol above the glass transition temperature, and type IV is due to the presence of swellable hydrophilic solid that influence the moisture sorption process until a maximum site hydration is reached, while the type V is the BET multilayer adsorption isotherm. Moisture sorption isotherms of most foods are nonlinear, generally sigmoidal in shape, and of the type II classification [1, 6].
Figure 1.
Types of moisture sorption isotherm for food. Source: Rizvi [6].
2.2 Applications of moisture sorption isotherm
In drying operation, it is the removal of water which is important, and hence the desorption equilibrium moisture relationship is required to determine the lowest attainable moisture content at the process temperature and relative humidity [8]. Labuza and Hyman [9] applied the changing of water activity of food ingredients and effective diffusivity to control moisture migration in multidomain foods, when temperature changes occur. The moisture sorption isotherms of food and agricultural products are therefore of special interest in the design of storage and preservation processes such as packaging, drying, mixing, freeze-drying and other processes that require the prediction of food stability, shelf life and glass transition and estimation of drying time [10], texture and deteriorative reactions in agricultural and food products. The precise determination of equilibrium moisture contents of dehydrated foods provides valuable information for the accurate computation of thermodynamic energies from existing theories [1].
The adsorption and desorption characteristics of agricultural and food products are affected by numerous factors [11], and these include composition, origin, postharvest history and methodology of measurement. In general, polymers sorb more water than sugars and other soluble components at lower water activities [12]. However, the soluble components sorb more water above certain water activity. The MSIs for the same material from different sources usually differ and are comparable only with qualification. The type of treatments given to the product may change the polar and other groups that bind water, along with changes in the capillary and other configurations of the food structure [13]. Greig [14] showed that the denaturation of native cottage cheese whey had no effect on the sorption isotherm at low water activities but significantly increased sorption at high water activities. Yu et al. [15] studied the moisture sorption characteristics of freeze-dried, osmo-dried, osmo-freeze-dried and osmo-air-dried cherries and blue berries and found that the EMC of osmo-air-dried cherries was generally higher than that of the osmo-freeze-dried and freeze-dried cherries at the lower temperature of 10°C, but at higher temperatures of 25 and 40°C, the difference was not significant. Similar result was reported for blue berries. San Jose et al. [16] showed that the drying method (freeze- and spray-drying) of lactose-hydrolyzed milk did not affect the adsorption isotherms but had profound effect on the desorption isotherms. Tsami et al. [17] investigated the effect of drying method on the sorption characteristics of model fruit powder and reported that freeze-dried gel adsorbed more vapor at 25°C than microwave-dried gel, which had a higher sorption capacity than vacuum- and conventionally dried product. Mittal and Usborne [18] determined the moisture sorption isotherms of meat emulsions and showed that their EMC was affected by the fat-protein ratio. Mazza [19] reported that at 40°C and in the monolayer region of the isotherm, the EMC of precooked dehydrated pea was higher than that of raw pea but that at water activities above 0.5, the sorption capacity of precooked pea was lower than that of raw pea. Aviara [20] noted that chemical modification (cross-linking and hydroxypropylation) of cassava, maize and sorghum starches had profound influence on their moisture adsorption and desorption characteristics. While cross-linking lowered the sorptive capacity of the starches, hydroxypropylation enhanced the ability of the starches to sorb or desorb moisture. Palou et al. [21] studied the moisture sorption characteristics of three cookies and two corn snacks whose main composition difference was in fat and total carbohydrate and found the EMC difference at 5% level of significance. Igbeka et al. [22], Ajibola and Adams [23] and Gevaudan et al. [24] studied the moisture sorption characteristics of cassava and presented data that were fitted by different moisture sorption isotherm models. The variance in EMC may be due to the source of the material, product’s postharvest and sorption history and varietal differences, methodology of measurement, temperature range and limitations imposed by model selection.
Several methods of determining the moisture sorption isotherm of agricultural and food products have been employed by investigators [25]. Gal [26, 27, 28] carried out a thorough review of the methods and pointed out that the basic techniques include the gravimetric, hygrometric, vapor pressure manometric and inverse gas chromatography and special method involving the use of AquaLab.
3.1 Gravimetric method
There are two common gravimetric methods of determining the EMC of agricultural and food products at different temperatures and water activities. One of these methods is the static gravimetric method which involves the placement of the product in an atmosphere with which it then comes into equilibrium (weight loss or gain stops) without mechanical agitation of the air or product. For this method, several weeks may be required for the product to come into equilibrium, and because of the long period of time, mold usually develops on high and intermediate moisture foods at water activities above 0.8. For data obtained at water activities above 0.8 to be reliable, mold growth must be prevented during equilibration. At the point of equilibration, the moisture content is then determined as the EMC. The second one is the dynamic method in which the atmosphere surrounding the product or the product itself is mechanically moved. The dynamic method is quicker but presents the problem of design and instrumentation. The static method has been used extensively and reported to be preferable for obtaining complete sorption isotherms [27]. It has also been recommended as the standard method of determining the moisture sorption isotherms of agricultural and food products [29]. It involves the placement of small sample (10–25 g) of agricultural and food material in vacuum desiccators containing different concentrations of sulfuric acid (Figure 2a) to maintain the relative humidity (water activity) of the surrounding air at different values from 0 to 100% (0.00–1.00) or saturated solution (Figure 2b) of different salts to achieve different values of relative humidity at a specified temperature. Usually a thermostatically controlled water bath or oven (Figure 3) is used to obtain the desired temperature. The water activity of sulfuric acid at different concentrations and temperatures is presented in Table 1, and that of saturated solutions of different salts at various temperatures are presented in Table 2.
Figure 2.
(a) Desiccator containing concentrated sulfuric acid: (1) locking clamp, (2) lid, (3) rubber seal ring, (4) desiccator barrel, (5) sample basket or can, (6) sample basket mounting stand and (7) concentrated sulfuric acid. Source: Spiess and Wolf [29]. (b) Desiccator containing saturated salt solution employed by Kameoka et al. [32] in determining the EMC of brown and rough rice and hull.
Figure 3.
Thermostatically controlled water bath or oven for moisture sorption isotherm determination. Source: Spiess and Wolf [29].
Percent H2SO4
Density at 25°C (g/cm3)
Temperature (°C)
5
10
20
25
30
40
50
5.00
1.0300
0.9803
0.9804
0.9806
0.9807
0.9808
0.9811
0.9814
10.00
1.0640
0.9554
0.9554
0.9558
0.9562
0.9562
0.9565
0.9570
15.00
1.0994
0.9227
0.9230
0.9237
0.9241
0.9245
0.9253
0.9261
20.00
1.1365
0.8771
0.8779
0.8796
0.8802
0.8814
0.8831
0.8848
25.00
1.1750
0.8165
0.8183
0.8218
0.8218
0.8252
0.8285
0.8317
30.00
1.2150
0.7396
0.7429
0.7491
0.7509
0.7549
0.7604
0.7655
35.00
1.2563
0.6464
0.6514
0.6607
0.6651
0.6693
0.6773
0.6846
40.00
1.2991
0.5417
0.5480
0.5599
0.5656
0.5711
0.5816
0.5914
45.00
1.3437
0.4319
0.4389
0.4524
0.4589
0.4653
0.4775
0.4891
50.00
1.3911
0.3238
0.3307
0.3442
0.3509
0.3574
0.3702
0.3827
55.00
1.4412
0.2255
0.2317
0.2440
0.2502
0.2563
0.2685
0.2807
60.00
1.4940
0.1420
0.1471
0.1573
0.1625
0.1677
0.1781
0.1887
65.00
1.5490
0.0785
0.0821
0.0895
0.0933
0.0972
0.1052
0.1135
70.00
1.6059
0.0355
0.0377
0.0422
0.0445
0.0470
0.0521
0.0575
75.00
1.6644
0.0131
0.0142
0.0165
0.0177
0.0190
0.0218
0.0249
80.00
1.7221
0.0035
0.0039
0.0048
0.0053
0.0059
0.0071
0.0085
Table 1.
Water activity of sulfuric acid solution at different concentrations and temperatures.
Acids are not used extensively because of the danger involved in its handling and the changes that can occur in its composition—it is susceptible to dilution or increase in concentration with time due to the release or absorption of water by the product—thereby effecting a change in the air-water activity. Acids also easily corrode and release fume that can be toxic in the food material. Saturated salts are safer to use, and constant humidity can be maintained by leaving excess salt in the solution. That way, the solution is made to remain saturated thoroughout the duration of the experiment in spite of the release or absorption of water by the product. The use of saturated salt solution, however, requires many salts in order to go thorough the relative humidity (water activity) range of 0–100% (0.00–1.00), whereas only one acid could be used for the same purpose.
The static gravimetric method involving the use of saturated salt solutions was applied successfully to the determination of MSIs of Jerusalem artichoke [30]; uncooked meat emulsions [18]; ground and short-time roasted coffee [31]; rice [32]; pigeon pea type-17 [33]; cassava [23]; plantain, winged bean seed and gari [34, 35, 36]; freeze-dried, osmo-freeze-dried and osmo-air-dried cherries and blue berries [15]; vetch seeds [37]; lupine [38]; high oleic sunflower seeds and kernels [39]; quinoa grains [40]; soya bean [41]; red chillies [42]; chickpea flour [43]; black gram nuggets [44]; sorghum malt [45]; IR-8 rice variety [46]; native and chemically modified starches [20]; and castor seeds [47]. Young [48], Oyelade et al. [49, 50], Al-Muhtaseb et al. [51], Bello [52] and Afkawa [53] applied the static gravimetric method involving the use of different concentrations of sulfuric acid in determining the MSIs of Virginia-type peanuts, maize flour, yam flour, potato, high amylopectin and high amylose starch powders, groundnut and neem seeds and shea nut and desert date kernels, respectively. Bosin and Easthouse [54] suggested the dynamic gravimetric method, and Igbeka et al. [22], Roman et al. [25] and Rahman and Al-Belushi [55] utilized it in establishing the MSIs of cassava and potato, apple and freeze-dried garlic powder, respectively.
3.2 Hygrometric method
Electric hygrometers are widely used for obtaining the MSIs of agricultural and food products. There are quite a lot of commercially available and specially designed hygrometers that are in use. The instrument (Figure 4) consists basically of a sensor, sample chamber and potentiometer. The sensor could use a hygroscopic chemical such as lithium chloride or an ion-exchange resin such as sulfonated polysterne; the conductivity of which changes according to the water activity above the sample. The sensor could be a humidity sensor which is based on capacitance changes in a thin film capacitor. Electric hygrometers give rapid, relatively precise results and are easy to operate. The main problems involved with the use of hygrometers are:
Evaluation of the equilibration time between the sample and sensor
Proper temperature control
Need for recalibration for some instrument
Figure 4.
Diagram of moisture sorption isotherm apparatus utilizing the hygrometer. Source: Fasina and Sokhansanj [58].
Crapiste and Rostein [57], Fasina and Sokhansanj [58], Tsami et al. [17] and Arslan and Togrul [59] employed the hygrometric method in studying the moisture sorption behavior of potatoes, alfalfa pellets, model fruit powders and crushed chillies, respectively.
3.3 Vapor pressure manometric (VPM) method
The vapor pressure manometric method involves bringing air to equilibrium with the agricultural or food product at a fixed temperature and moisture content and the relative humidity of the air measured as the equilibrium relative humidity (ERH). In this method, the vapor pressure exerted by the moisture in the product is directly measured. As a result, it is taken as one of the best methods of determining the MSI of food [60]. The equilibrium relative humidity is then obtained from the ratio of the vapor pressure in the sample to that of pure water at the same temperature. A schematic diagram of the apparatus and simplified diagram of the system set-up is shown in Figures 5 and 6, respectively. The procedure for determining the ERH of agricultural and food products using the method is as follows:
The prepared sample and VPM system are allowed to reach the desired temperature.
About 10–50 g of sample is put in the sample flask, and an equal amount of desiccant (CaSO4, CaCl2) is placed in the desiccant flask and sealed on to the apparatus using high vacuum grease.
Keeping the sample flask isolated, the system is evacuated to less than 200 μmHg (Rizvi, 1986). The cold strap should be filled with nitrogen prior to evacuation of the system to trap any moisture reaching the vacuum pump.
The space in the sample flask is then connected to the evacuated air space by opening the stopcock over the sample V4 (Figure 6), and the system is again evacuated for 1 min.
The stopcock across the manometer V5 is closed causing the oil in the micromanometer to respond to the vapor pressure exerted by the sample. When the oil level reaches a steady value, the difference is recorded as H1.
The stopcock over the sample is then closed, and the desiccant stopcock is opened to connect the system with the desiccant, causing a change in the height of the manometric oil. After the oil reaches a constant height, the micromanometer reading is recorded as H2.
The sample is removed from the system, and the moisture content is determined using a standard method.
With the data obtained, the equilibrium relative humidity is calculated using Eq. (1):
Figure 5.
Schematic diagram of vapor pressure manometric apparatus. Source: Rizvi [6].
Figure 6.
Schematic diagram of vapor pressure manometric system set-up. Source: Ajibola et al. [65].
ERH=H1−H2TsToPsE1
where ERH is the equilibrium relative humidity (%), H1 is the micromanometer reading with sample flask connected to the system (mm of manometric oil), H2 is the micromanometer reading with desiccant flask connected to the system (mm of manometric oil), Ts is the temperature of the environment surrounding the water bath taken as the temperature of sample (K), To is the temperature of the environment surrounding the micromanometer (K) and Ps is the saturated vapor pressure at sample temperature (mm of manometric oil).
The VPM method is rapid and precise but requires the use of vacuum pump, an accurate manometer and closed glass tube system. Proper temperature control is critical to this method, and volatile constituents other than water may contribute to the pressure exerted by the food.
The VPM method has been used to obtain the MSI of cereal grains and rape [61], dry milk [62], sesame seed [63], cowpea [64] and palm kernels [65].
3.4 Inverse gas chromatography
The inverse gas chromatography (IGC) is a rapid and effective system for studying the thermodynamic properties of a solid taken as the stationary phase in relation to a mobile gas phase containing selected solutes such as water. It is particularly suitable for the study of the lower region of water activity and for products with very low equilibrium moisture contents [66, 67]. With IGC the sorbed solute is injected into the carrier gas stream, and its linear transport is retarded owing to interaction with the product under study, which constitutes the stationary phase. Moisture sorption isotherms are then determined using the chromatographic data obtained and the following equations, which relate chromatograph operating parameters and peak data to the sorption isotherm:
a=maIadsmIpicE2
and
p=mahRTIpicWE3
where a is the uptake of sorbed water (g/g stationary phase), ma is the mass of water injected (g), m is the mass of stationary phase (g) and Iads/Ipic is the ratio of the areas (A + B)/B calculated from the chromatogram (Figure 7), p is the partial pressure (atm), h is the peak height (detector units), R is the gas constant (82.0567 cm3 atm mole1 K−l), T is the absolute temperature (K), W is the flow rate of carrier gas (cm3/min) and Ipic is the area B in Figure 7.
Figure 7.
Typical gas chromatogram obtained by IGC: 1 = point of injection; 2 = point of emergence of unadsorbed peak (air); 3 = point of emergence of probe peak (water), Ipic = area B; and Iads = area A + B. Source: Manuel Sa and Sereno [67].
It has been used successfully to determine the MSIs of homogeneous solid food ingredients like sucrose, glucose and starch [68] and complex heterogeneous foods like bakery products [69], wheat flour [66] and wheat and soy flour [70].
3.5 AquaLab instrument
AquaLab is the fastest, most accurate and most reliable instrument available for measuring water activity, giving readings in 5 min or less [71]. It is easy to use and provides accurate and timely results. Its readings are reliable, providing ±0.003 aw accuracy. The instrument is easy to clean and checking calibration is simple. The photograph of 4TE model of the equipment is shown in Figure 8.
Figure 8.
4TE model AquaLab moisture content—water activity measuring instrument. Source: METER Group, Inc. [71].
4. Influence of temperature on moisture sorption isotherms
Temperature affects the mobility of water molecules and the dynamic equilibrium between the vapor and the adsorbed gases [13]. If water activity is kept constant, an increase in temperature causes a decrease in the amount of sorbed water [20] (Figure 9). This indicates that the food becomes less hygroscopic. Iglesias and Chirife [72] pointed out that increase of temperature represents a condition unfavorable to water sorption.
Figure 9.
Adsorption EMC of hydroxypropylated cassava starch showing variation of MSI with temperature. Source: Aviara [20].
An exception to this rule is shown by certain sugars and other low molecular weight food constituents, which become more hygroscopic at higher temperature because they dissolve in water. Temperature shifts can have an important practical effect on the chemical and microbiological reactivity related to quality deterioration of a food in a closed container [73]. An increase of temperature at constant moisture content causes increase in water activity (Figure 10). This increases the rate of reactions and leads to deterioration [74, 75, 76]. Weisser [31] studied the effect of temperature on the sorption isotherms of roasted coffee and reported that the product showed consistent separation of the isotherms at different temperatures. However, not all foods exhibit such consistency. In the work reported by Saravacos et al. [12], crossing over occurred at high water activity (aw = 0.78) in the 20 and 30°C adsorption isotherms of sultana raisins and 5, 20 and 45°C adsorption and desorption isotherms of Chilean papaya shown in Figure 11 [77]. Such crossing over has earlier been observed by Saravacos and Stinchfield [78] on model systems of starch-glucose, Audu et al. [79] on sugars, Weisser et al. [80] on sugar and alcohols and Silverman et al. [81] on 20 and 37°C isotherms of precooked bacon. These substances contain large amounts of low molecular weight constituents in a mixture of high molecular weight biopolymers. At lower water activity values, the sorption of water is due mainly to the biopolymers, and an increase of temperature has the normal effect of lowering the isotherms [13]. As water activity is raised beyond the intermediate region, moisture begins to be sorbed primarily by the sugars and other low molecular constituents leading to the swinging up of the isotherm. Dissolution, which is favored by higher temperature, offsets the opposite effect of temperature on higher molecular weight constituents. The net result is an increase of moisture content (crossing over) of the isotherms. This has bearing on the sign and magnitude of the binding energy [13]. The binding energy of sultana raisin decreased as the temperature increased from 22 to 32°C in the low moisture region [12], but the effect of temperature showed a crossing over of the lines at higher moisture contents due to the endothermic dissolution of fruit sugars. Iglesias and Chirife [82] studied the equilibrium moisture contents of air-dried beef and found that the higher the drying temperature, the lower the sorption capacity of the dried beef. Similar results were reported for cookies and corn snacks [21] and apples [25]. Temperature changes also have effects on the water activity of saturated salt solutions, which are used in the determination of sorption isotherms. Labuza et al. [83] used experimental data and thermodynamic analysis to demonstrate that water activity of saturated salt solutions should decrease with increase in temperature.
Figure 10.
Changes in water activity at constant moisture content and in moisture content at constant water activity with changes in temperature. Source: Rizvi [6].
Figure 11.
Moisture desorption isotherms of Chilean papaya showing isotherm crossing at higher water activities with increase in temperature. Source: Vega-Galvez et al. [84].
5. Moisture sorption hysteresis
A product which attains its moisture equilibrium with the surrounding by losing moisture at a given temperature is said to have reached the desorption EMC. When the relatively dry material absorbs moisture from a high humidity environment at the same temperature, it will eventually reach the adsorption EMC. The isotherm plots may indicate a significant difference at certain water activities and temperatures between desorption and adsorption EMC values, with the desorption values being higher than the adsorption counterpart. This difference is called moisture sorption hysteresis [13, 45]. A typical hysteresis loop presented in Figure 12 could occur within the region of monolayer moisture but could begin at a higher water activity and extend down to zero water activity, depending on its class according to Kapsalis [13] classification.
Moisture sorption hysteresis has important theoretical and practical implications in foods. These include the general aspects of the irreversibility of moisture sorption process and the question of validity of thermodynamic parameters derived from a particular arm of the isotherm. Moisture sorption hysteresis has effect on chemical and microbiological deterioration of low and intermediate moisture foods.
5.1 Hysteresis classification
The hysteresis phenomenon in agricultural and food products varies in magnitude, shape and extent, depending on the type of food and temperature [13]. Hysteresis size or magnitude is depicted by the area enclosed by the loop, while the span or extent is denoted by the water activity range covered. Kapsalis [13] grouped moisture sorption hysteresis into three general types as follows:
Type I hysteresis: This type of hysteresis is normally pronounced mainly in the lower moisture content region, below the first inflection point of the isotherm. Although the total hysteresis may be large, no occurrence is normally observed above the 0.65 water activity or in the intermediate moisture range. The type I hysteresis is normally exhibited by high-sugar and high-pectin foods, exemplified by air-dried apple.
Type II: In this type, moderate hysteresis begins at high water activity, in the capillary condensation region, and extends over the rest of the isotherm to zero water activity. In both desorption and adsorption arms, the isotherm’s sigmoidal shape is retained. This type of hysteresis is normally exhibited by high-protein foods exemplified by freeze-dried pork.
Type III: In this type, large hysteresis loop occurs with a maximum at about 0.70 water activity, which is within the capillary condensation region. This type of hysteresis normally occurs in starchy foods such as freeze-dried rice.
5.2 Effect of temperature on hysteresis
Increasing temperature decreases the total hysteresis and limits the span of the loop along the isotherm [84]. Iglesias and Chirife [85] studied the effect of temperature on the magnitude of moisture sorption hysteresis of foods and reported that increasing temperature decreased or eliminated hysteresis for some foods, while for others, the total hysteresis size remained constant, or even increased. In the case where the hysteresis loop decreased, it did so more appreciably at high temperatures. The effect of temperature was found to be more pronounced on the desorption isotherms than the adsorption isotherms.
5.3 Theories of moisture sorption hysteresis
Several theories have been proposed to explain hysteresis phenomena in agricultural and food products. The most prominent of the theories are the ink bottle theory, the incomplete wetting theory, the open-pore theory, the shrinkage theory and the capillary condensation-swelling fatigue theory.
Ink bottle theory: This theory assumes that an agricultural and food product is a porous body having capillaries consisting of narrow, small-diameter necks with large bodies resembling ink bottles (Figure 13). It explains hysteresis on the basis of difference in the radii of the porous sorbent. During desorption, the small radii of necks control the emptying of the capillaries and result in a lowering of the relative humidity above the product; whereas during adsorption, the large area for the bodies needs to be filled, thus requiring higher relative humidity. The explanation can be better understood using the Kelvin equation which states that
Figure 13.
Ink bottle neck theory of moisture sorption hysteresis (left, schematic representation and, right, actual pore). Source: Kapsalis [13].
LnPPo=−2σVcosθRTrmE4
where P is the vapor pressure of liquid over the curved meniscus (Pa), Po is the saturation vapor pressure (Pa) at temperature T (K), σ is the surface tension (N/m), θ is the angle of contact (in complete wetting, θ is 0 and cosθ = 1), V is the molar volume of liquid (m3/mol) and rm is the mean radius of curvature of meniscus.
For desorption, by substituting r1 in Figure 13 for rm in Eq. (4) with cosθ = 1 (complete wetting), Eq. (4) becomes transformed into Eq. (5):
Pd=Poexp−2σVRTr1E5
In adsorption with condensation first taking place in the large diameter cavity, Eq. (4) becomes
Pa=Poexp−2σVRTr2E6
From the above, it follows that for a given amount of water sorbed, the pressure will be higher during adsorption than during desorption.
Incomplete wetting theory: This theory is also dependent on capillary condensation based on Eq. (4), but it notes that due to the presence of impurities, the contact angle of the receding film upon desorption is smaller than that of the advancing film upon adsorption. Therefore, condensation along the adsorption branch of the isotherm will be at a higher vapor pressure resulting in open hysteresis as illustrated in Figure 14. However, in foods the most common type of hysteresis is the closed-end, retraceable loop showing that this theory is limited in its application to foods.
Figure 14.
Incomplete wetting theory of hysteresis (A) contact angle and (B) open hysteresis. Source: Kapsalis [13].
Open-pore theory: this theory extends the ink bottle theory by including considerations of multilayer adsorption. It is based on the difference in vapor pressure between adsorption Pa and desorption Pd as affected by the shape of the meniscus. During adsorption, the meniscus is considered cylindrical and the Cohan equation (not presented here) applies, whereas during desorption, the shape is considered to be hemispherical in which the Kelvin equation is applied. The open-pore theory is illustrated in Figure 15.
Figure 15.
Open-pore theory of hysteresis. Source: Kapsalis [13].
Shrinkage theory: This states that while agricultural and food product is drying out, the force of attraction causes water-holding spaces to shrink (molecular shrinkage). This permanent shrinkage reduces the water-binding polar sites and water-holding capacity of the material; hence less amount of water is absorbed during the adsorption process.
Capillary condensation and swelling fatigue theory: In this theory proposed by Ngoddy-Bakker-Arkema [86], the sorption hysteresis is considered linked with condensation and evaporation in irregular voids (capillary condensation) and influence of adsorbed water molecules on such physical properties of agricultural and food products as strength, elasticity, rigidity, swelling and evolution of heat (swelling fatigue). The above combination was simulated by adopting the Cohan theory of capillary condensation with modifications and combining it with the ink bottle theory in the first approximation. The theory presented expressions for calculating the desorption isotherms of biomaterials from corresponding adsorption isotherm using bulk moduli determined as a function of moisture content.
6. Moisture sorption isotherm models
Equations for fitting the moisture sorption isotherms are of special importance in many aspects of crop and food preservation by drying. These include the prediction of the drying times, shelf life of the dried product in a packaging material and the equilibrium conditions after mixing products with varying water activities [87]. Others are the analytical determination of control for undesirable chemical and enzymatic reactions [88] and control of moisture migration in multidomain foods [9]. Moisture sorption isotherm models, therefore, not only constitute an essential part of the overall theory of drying but also provide information directly useful in the accurate and optimum design of drying equipment [1]. They are needed in the evaluation of the thermodynamic functions related to moisture sorption in biological materials [89].
Several theoretical, semi-theoretical and empirical models have been proposed and used by investigators to fit the equilibrium moisture content data of food and agricultural products. Chirife and Iglesias [87] reviewed part of the isotherm equations and presented a discussion of 23 common models, while Van den Berg and Bruin [5] presented a more comprehensive list. Ngoddy-Bakker-Arkema [1] developed a generalized moisture sorption isotherm model for biological materials based primarily on the BET and capillary condensation theories and indirectly on Polanyi’s potential theory. This model appears to possess very high versatility but needs to be modified to reduce the number of parameters and incorporate the temperature term. A thorough going and extensive testing of the model on various categories of food is also necessary to confirm its versatility and prove the generalized posture. Ferro Fontan et al. [2] and Chirife et al. [90] presented a new model, which Iglesias and Chirife [91] compared with the GAB model and reported to be an alternative. Chen [92] derived a new moisture sorption isotherm model from a reaction engineering approach. The Brunauer-Emmett-Teller (BET) [87] and Guggenheim-Anderson-de Boer (GAB) [56, 91, 93] models have been used for estimating the monolayer moisture content of agricultural and food products. Boquet et al. [94] noted that the Hailwood and Horrobin model has a remarkably good ability to fit the experimental data for most food types. A test of the model on moisture sorption data of native cassava and sorghum starches [95] showed that it has good predictive performance with R2 ranging from 0.92 to 0.99. It, however, lacked the temperature term and was modified to incorporate the term. Other commonly used models include modified Henderson, modified Chung-Pfost, modified Halsey and modified Oswin and the GAB. The modified Henderson [96] and modified Chung-Pfost [97] models have been adopted as the standard equations by the American Society of Agricultural and Biological Engineers (ASABE) for describing the EMC-aw data for cereals and oil seeds [98]. The modified Halsey [85] has been reported as the best model for predicting the EMC-aw relationships of several tropical crops [99] and alongside with the modified Oswin [100] has been shown to describe the EMC-aw data of many seed satisfactorily [101, 102]. The Guggenheim-Anderson-de Boer (GAB) model has been recognized as the most satisfactory theoretical isotherm Equation [103, 104, 105, 106] and has been recommended as the standard model for use in food laboratories in Europe [105] (1985) and the USA [107]. The GAB does not incorporate a temperature term; therefore, the determination of the effect of temperature on isotherms using the model usually involves the evaluation of up to six constants. Jayas and Mazza [108], however, developed a modified form of the GAB, which incorporates the temperature term. The MSI models considered in this study were selected from the above list and presented as follows:
where M is the moisture content, (db); Mm is monolayer moisture content, (db); aw is water activity; T is absolute temperature, (K); A, B, C and k are constants; η is primary characteristic parameter of pore structure; ε is secondary characteristic parameter of pore structure; σ is surface tension of sorbate in bulk liquid form, (N/m); Rg is universal gas constant; V is molal volume of sorbate in its bulk liquid condition, (m3/mol); Pm is vapor pressure corresponding to monolayer, (N/m2); Po is saturated vapor pressure, (N/m2); and P is vapor pressure at the condition under which the study is carried out, (N/m2).
7. Isotherm model predictive performance evaluation
Sun and Byrne [109], Sun [110] and Sun [111] evaluated the predictive performance of the moisture sorption isotherm models that have been reported for fitting the EMC and ERH data of rapeseed, rice, other grains and oilseeds and selected the models that gave the best fits.
Coefficient of terms in the moisture sorption isotherm equations is usually determined using nonlinear regression procedure, and the predictive performance of an equation on sorption data is evaluated using such goodness of fit parameters as standard error of estimate (estimate of the residual mean square), residual sum of square, coefficient of determination, mean relative percent error, fraction explained variation and residual plots. Several investigators used these parameters to evaluate the fitting ability of EMC-aw equations. For instance, Ajibola [35, 36, 37], Ajibola and Adams [34], Ajibola [112], Gevaudan et al. [24], Talib et al. [8], Pezzutti and Crapiste [113], Tsami et al. [17] and Ajibola et al. [64] used the standard error of estimate, and Young [48] and Jayas et al. [114] used the residual sum of squares to compare the fitting ability of different models. Boquet et al. [94], Chirife et al. [90], Weisser [31], Saravacos et al. [12], Pollio et al. [115], Iglesias and Chirife [91] and Khalloufi et al. [10] used the mean relative percent deviation (MRE), while Shepherd and Bhardwaj [33], Demertzis et al. [116], Diamante and Munro [117] and Sopade et al. [118] employed coefficient of determination in evaluating the fitting ability of several models. Pappas and Rao [119] used the fraction explained variation, Chen [92] used both coefficient of determination and mean relative percent error and Sun [110] and Sun [111] employed the residual sum of squares, standard error of estimate and mean relative percent error in comparing moisture sorption isotherm models for food. Other combinations of parameters that have been used include standard error of estimate and mean relative percent error [120], coefficient of determination and residual sum of squares [18] and standard error of estimate, mean relative percent deviation and residual plots [15, 41, 65, 101, 102]. A model is considered acceptable for predictive purpose, if the residuals are uniformly scattered around the horizontal value of zero showing no systematic tendency towards a clear pattern [41, 45, 64, 65]. A model is considered better than another if it has lower standard error of estimate and mean relative percent deviation and higher fraction explained variation and coefficient of determination.
Menkov [37] reported that of five moisture sorption isotherm models fitted to the experimental data on the EMC of vetch seeds, the modified Oswin model proved the best for describing the adsorption and desorption branches. Aviara et al. [41] and Oyelade [121] reported that the modified Oswin model gave the best fit to the EMC of soya bean and lafun, respectively. Santalla and Mascheroni [39] in a similar study on the EMC of sunflower seeds and kernels reported that the GAB model gave the best fit to the experimental data. Other crops whose moisture sorption isotherms have recently been studied include quinoa grains [40], crushed chillies [59], amaranth grains [122] and black gram nuggets [44].
7.1 Model parameter evaluation procedures
The procedure followed in evaluating a moisture sorption isotherm model depends on the nature of the model. For the selected models (Eqs. (7)–(16)), the procedures are as follows:
a. BET model: the BET model (Eq. (7)) can be linearized thorough algebraic manipulations to yield Eq. (17):
awM1−aw=1MmC+C−1MmCawE17
A plot of awM1−aw against aw within the water activity range of 0.01–0.5 at each temperature yields a straight line with the slope as C−1MmC and intercept on the y-axis as 1MmC, and from these, the values of Mm and C can be obtained and used as the starting values in nonlinear regression. The nonlinear regression analysis procedure minimizes the sum of deviation in the evaluation of a model using a series of iterative steps. The procedure could require that initial parameter estimates be chosen close to the true values.
b. GAB model: the GAB model (Eq. (8)) can be transformed to a quadratic form by algebraic manipulation to yield Eq. (18):
awM=Aaw2+Baw+CE18
Eq. (18) can be solved by plotting awM against aw at each temperature and fitting a polynomial of the second order to the plots. This will yield the following functions from Eq. (8):
A=kMm1C−1,B=1Mm1−2C,C=1MmCkE19
The values of Mm, C and k obtained at each temperature are then used as the initial values of the parameters in the nonlinear regression procedure of Eq. (8) to evaluate the model.
c. Modified GAB model: the modified GAB model (Eq. (9)) like the original GAB model can be transformed to a quadratic form by algebraic manipulation to yield Eq. (20):
awM=Xaw2+Yaw+ZE20
Plotting awM against aw and fitting a polynomial of the second order to the plot yield the following functions from Eq. (9):
X=BATC−1,Y=1A1−2TC,Z=1ABCE21
The average values of A, B and C are obtained and used as initial parameter estimates in the nonlinear regression analysis to evaluate the model.
d. Hailwood-Horrobin model: The Hailwood-Horrobin model (Eq. (10)) is mathematically similar to the GAB and can after algebraic manipulations be represented in the form
awM=Caw2+Baw+AE22
Plotting awM against aw and fitting a polynomial of the second order to the plot at each temperature yield the values of C,B and A for use as initial parameter estimates in the nonlinear regression procedure for the model evaluation.
e. Modified Hailwood-Horrobin model: this model (Eq. 11) also has mathematical similarity with the GAB. It can be transformed algebraically to yield Eq. (23):
awM=λaw2+μaw+φE23
Plotting awM against aw and fitting a polynomial of the second order to the plot yield the following functions from Eq. (11):
λ=CTn,μ=BTandφ=TAE24
The average values of A, B and C are obtained and used as initial parameter estimates in the nonlinear regression analysis to evaluate the model.
f. Modified Chung-Pfost model: the modified Chung-Pfost model (Eq. (12)) is transformed by algebraic manipulations to yield Eq. (25):
aw=exp−AT+Bexp−CME25
Linearizing Eq. (25) by logarithmic transformation is carried out as follows:
Lnaw=−AT+Bexp−CME26
−Lnaw=AT+Bexp−CME27
Ln−Lnaw=LnAT+B−CME28
A plot of Ln−Lnaw against M at each temperature yields a straight line with slope as -C and intercept on the y-axis asLnAT+B.
With the expression for the slope, further algebraic manipulation is carried out as follows in order to solve for the temperature-related parameters of the model:
expb=AT+B,implying thatT+B=Aexpb=Aexp−bE29
From the above,T=Aexp−b−B.
A plot of T against exp−b yields a straight line with A as slope and intercept on the y-axis as -B.
In the nonlinear regression procedure, the avC as C and A and B are used as the initial parameter estimates in the equation.
g. Modified Halsey model: the modified Halsey model (Eq. (13)) can be transformed by algebraic manipulations to yield Eq. (30):
aw=exp−expA+BTM−CE30
Linearizing Eq. (30) by logarithmic transformation yields
Lnaw=−expA+BTM−CE31
−Lnaw=expA+BTM−CE32
So
Ln−Lnaw=A+BT−CLnME33
A plot of Ln−Lnaw against LnM at each temperature yields a straight line with slope as –C and intercept on the y-axis as A + BT. Using the intercept on y-axis for different temperature plots of the above, the values of the intercepts are then plotted against temperature to yield another straight line with slope as B and intercept on y-axis as A. In the nonlinear regression analysis, the avC as C and A and B values are used as the starting values in parameter estimates for the model.
h. Modified Henderson model: the modified Henderson model (Eq. (14)) is transformed to yield Eq. (34):
aw=1−exp−AT+BMCE34
Eq. (34) is linearized by logarithmic transformation as follows:
1−aw=exp−AT+BMCE35
Ln1−aw=−AT+BMCE36
−Ln1−aw=AT+BMCE37
Ln−Ln1−aw=LnAB+T+CLnME38
A plot of Ln−Ln1−aw against LnM at each temperature yields a straight line with slope a1 = C and intercept on the y-axis b1 = LnAB+T. To solve for the temperature-related parameters, intercept on the y-axis is used.
Therefore,expb1=AT+B=AT+AB.E39
A plot of expb1 against T yields a straight line with slope a2 as A and intercept on y-axis b2 as AB. In the nonlinear regression procedure, avC and A and B are used as initial parameter estimates for the model.
i. Modified Oswin model: the modified Oswin model (Eq. (15)) can be manipulated algebraically to yield Eq. (40):
aw=1A+BTMC+1E40
1aw=A+BTMC+1and1aw−1=A+BTMCE41
Linearizing Eq. (41) by logarithmic transformation yields
CLnA+BT−CLnM=Ln1−awawE42
A plot of Ln1−awaw against LnM at each temperature yields a straight line with slope as –C and intercept on the y-axis as CLnA+BT.
The expression for intercept on the y-axis is solved further to evaluate the temperature-related parameters of the model and yield Eq. (43),
expbc=A+BTE43
A plot of expbc against T yields a straight line with slope as A and intercept on the y-axis as B. In the nonlinear regression procedure, avC as C and A and B are used as the initial parameter estimates in the model evaluation.
j. Ngoddy-Bakker-Arkema model: the Ngoddy-Bakker-Arkema model, which has been postulated to be a generalized model, has the following parameters (unknowns): σ, V, Pm, ρ, ε and η.
Evaluating the model requires a lot of care. The starting values of parameters for application in the nonlinear regression procedure can be obtained as follows:
σ, V, ρ and Po can be obtained at different temperatures from the steam table P can be calculated using the expression P = aw, ε can be taken as having a typical value of 0.1 though its value can be less, Pm is the monolayer value of P and η can be assumed to lie between −1 and +1 in the form of −1 ≤ η ≤ +1 with 0.1 as a typical starting value.
7.2. Moisture sorption isotherm model predictive indicators
After values of model constants have been determined using the nonlinear regression analysis, the suitability of a model for predictive purpose or its goodness of fit is determined using the following indices:
a. Residual plots: these are plots of residuals (difference between measured and predicted values of the EMC) against the measured values.
b. Standard error of estimate given as
SE=∑Y−Y′2df12E44
c. Mean relative percent deviation given as
MRE=100N∑Y−Y′YE45
d. Fraction explained variation given as
FEV=SSMSSTE46
e. Residual sum of squares (RSS) given as
RSS=∑Y−Y′2NE47
f. Coefficient of determination, R2.
where Y is the measured EMC value, Y′ is the EMC value predicted by the model, N is the number of data points, df is the degree of freedom, SSM is the sum of squares due to the model and SST is the total sum of squares.
8. Conclusions
Moisture sorption phenomena govern several technological processes (drying, storage, mixing and packaging to mention a few) involving agricultural and food products. Moisture sorption isotherms of these products are generally of the type II, sigmoidal in shape and temperature dependent. The isotherms can be determined using the static or dynamic gravimetric, vapor pressure manometric, hygrometric and inverse gas chromatographic methods. Desorption isotherm path could differ from that of adsorption leading to moisture sorption hysteresis.
Commonly used moisture sorption isotherm models include the BET, GAB, modified GAB, Hailwood-Horrobin, modified Hailwood-Horrobin, modified Chung-Pfost, modified Halsey, modified Henderson and modified Oswin models. Ngoddy-Bakker-Arkema model which was proposed as a generalized model was considered. While some of the models can be evaluated by fitting polynomial functions of the second order to them and applying nonlinear regression procedure, others can be solved thorough linearization by logarithmic transformation and nonlinear regression. For the Ngoddy-Bakker-Arkema model, the initial parameter estimates for use in nonlinear regression have to be obtained from the steam table. A model is considered acceptable for predictive purpose, if the residuals are uniformly scattered around the horizontal value of zero showing no systematic tendency towards a clear pattern. Model goodness of fit is determined using standard error of estimate, mean relative percent deviation, fraction explained variation, coefficient of determination and residual sum of squares.
Conflict of interest
This chapter has no conflict of interest.
\n',keywords:"adsorption, desorption, equilibrium moisture isotherm, moisture sorption isotherm models, moisture sorption isotherm hysteresis",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/68496.pdf",chapterXML:"https://mts.intechopen.com/source/xml/68496.xml",downloadPdfUrl:"/chapter/pdf-download/68496",previewPdfUrl:"/chapter/pdf-preview/68496",totalDownloads:709,totalViews:0,totalCrossrefCites:4,totalDimensionsCites:7,hasAltmetrics:0,dateSubmitted:"May 1st 2019",dateReviewed:"June 12th 2019",datePrePublished:null,datePublished:"March 11th 2020",dateFinished:null,readingETA:"0",abstract:"Moisture sorption characteristics of agricultural and food products play important roles in such technological processes as drying, handling, packaging, storage, mixing, freeze-drying and other processes that require the prediction of food stability, shelf life, glass transition and estimation of drying time and texture and prevention of deteriorative reactions. They are useful in the computation of thermodynamic energies of moisture in the products. An understanding of moisture sorption phenomena in products, moisture sorption isotherm (MSI) determination techniques and moisture sorption isotherm model evaluation procedures would be useful in the development or selection, modeling and controlling as well as optimization of appropriate processes to make for enhanced efficiency. The phenomena addressed in this chapter are equilibrium moisture content (EMC)-water activity (aw) relationships and MSI types, temperature influence on isotherms and occurrence of moisture sorption hysteresis. MSI measurement techniques highlighted are the gravimetric, vapor pressure manometric (VPM), hygrometric and inverse gas chromatographic and the use of AquaLab equipment. Commonly used moisture sorption isotherm models (BET, GAB, modified GAB, Hailwood-Horrobin, modified Hailwood-Horrobin, modified Halsey, modified Henderson, modified Chung-Pfost and modified Oswin) were selected, and their evaluation procedures using moisture sorption data were outlined. Static gravimetric technique involving the use of saturated salt solution appears to be the most widely used and recommended method of determining the EMC of agricultural and food products. Most of the MSI models can be fitted to moisture sorption data thorough linearization by logarithmic transformation, while others can be solved using such expression as second-order polynomial. Model goodness of fit can be determined using standard (SE) error of estimate, coefficient of determination (R2), mean relative percentage deviation (P) and fraction explained variation (FEV). The acceptance of a model depends on the nature of its residual plots. A model is considered acceptable if the residual plots show uniform scatter around the horizontal value of zero showing no systemic tendency towards a clear pattern. A model is better than another model if it has lower SE, lower P, higher R2 and higher FEV. Although it appears as if a generalized MSI model is yet to exist, it is recommended that the Ngoddy-Bakker-Arkema (NBA) model should be given thorough going and extensive testing on the MSI of different categories of food as it could prove true to its generalized model posture due to the fundamental nature of its derivation.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/68496",risUrl:"/chapter/ris/68496",book:{slug:"sorption-in-2020s"},signatures:"Ndubisi A. Aviara",authors:[{id:"303694",title:"Prof.",name:"Ndubisi",middleName:null,surname:"Aviara",fullName:"Ndubisi Aviara",slug:"ndubisi-aviara",email:"nddyaviara@yahoo.com",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Sorption phenomena in biological materials",level:"1"},{id:"sec_2_2",title:"2.1 Moisture sorption isotherm",level:"2"},{id:"sec_3_2",title:"2.2 Applications of moisture sorption isotherm",level:"2"},{id:"sec_4_2",title:"2.3 Factors influencing moisture sorption characteristics",level:"2"},{id:"sec_6",title:"3. Moisture sorption isotherm measurement techniques",level:"1"},{id:"sec_6_2",title:"3.1 Gravimetric method",level:"2"},{id:"sec_7_2",title:"3.2 Hygrometric method",level:"2"},{id:"sec_8_2",title:"3.3 Vapor pressure manometric (VPM) method",level:"2"},{id:"sec_9_2",title:"3.4 Inverse gas chromatography",level:"2"},{id:"sec_10_2",title:"3.5 AquaLab instrument",level:"2"},{id:"sec_12",title:"4. Influence of temperature on moisture sorption isotherms",level:"1"},{id:"sec_13",title:"5. Moisture sorption hysteresis",level:"1"},{id:"sec_13_2",title:"5.1 Hysteresis classification",level:"2"},{id:"sec_14_2",title:"5.2 Effect of temperature on hysteresis",level:"2"},{id:"sec_15_2",title:"5.3 Theories of moisture sorption hysteresis",level:"2"},{id:"sec_17",title:"6. Moisture sorption isotherm models",level:"1"},{id:"sec_18",title:"7. Isotherm model predictive performance evaluation",level:"1"},{id:"sec_18_2",title:"7.1 Model parameter evaluation procedures",level:"2"},{id:"sec_19_2",title:"7.2. Moisture sorption isotherm model predictive indicators",level:"2"},{id:"sec_21",title:"8. Conclusions",level:"1"},{id:"sec_25",title:"Conflict of interest",level:"1"}],chapterReferences:[{id:"B1",body:'Ngoddy PO, Bakker-Arkema FW. A generalized theory of sorption phenomena in biological materials (Part I: The isotherm equation). Transactions of ASAE. 1970;13(5):612-617'},{id:"B2",body:'Ferro Fontan C, Chirife J, Sancho E, Iglesias HA. 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Sorption isotherms for amaranth grains. Journal of Food Engineering. 2005;67:441-450'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Ndubisi A. Aviara",address:"nddyaviara@yahoo.com",affiliation:'
Department of Agricultural and Environmental Resources Engineering, Faculty of Engineering, University of Maiduguri, Maiduguri, Nigeria
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\n
1. Introduction
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Pectin is the major constituent of all plants and makes up approximately two-third of the dry mass of plant primary cell walls. It provides structural integrity, strength, and flexibility to the cell wall and acts as barrier to the external environment [1]. Pectin is also a natural component of all omnivorous diet and is an important source of dietary fiber. Due to the resistant in digestive system and lack of pectin digestive enzymes, human beings are not able to digest pectin directly but microorganism present in large intestine can easily assimilate the pectin and convert it into soluble fibers. These oligosaccharides promote beneficial microbiota in gut and also help in lipid and fat metabolism, glycemic regulation, etc. [2]. Being complex and highly diverse in structure, role of pectin is not only limited to the biological and physiological functions, but it has tremendous potential and contributes substantially in other applications ranging from food processing to pharmaceuticals. Pectin is a water-soluble fiber and used in various food as emulsifier, stabilizer, gelling, and thickening agent.
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Commercial pectins are extracted from citrus and apple fruit. On the basis of dry mass, apple pomace contains 10–15% pectin, whereas citrus peel possesses 20–30% pectin. However, pectin has also been extracted in higher amount from several other fruits and their by-products, such as sunflower head, mango peal, soybean hull [3], passion fruit peel [4], sugar beet pulp [5], Akebia trifoliata peel [6], peach pomace [7], banana peel [8], chickpea husk [9], and many more [10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23]. Table 1 summarizes the different types of pectin extracted from various horticultural crops. But detection and extraction of pectin in higher concentration is not sufficient to qualify that fruit as a source of commercial pectin because of the structural variation and modification in side-chain sugars, and also that pectin from different sources has different gelling properties.
Pectin is a highly complex plant cell wall polysaccharide that plays a significant role in plant growth and development. It is predominantly present in fruits and vegetables and constitutes approximately 35–40% of the primary cell wall in all the dicot plants [24]. The composition and structure of pectin is influenced by the developmental stages of plants [25, 26]. Structural analysis of pectin revealed that it is a polymer comprised of chain-like configuration of approximately 100–1000 saccharide units; therefore, it does not possess a defined structure. In general, pectin is illustrated as a heteropolysaccharide of three components namely, homogalacturonan (HG), rhamnogalacturonan-I (RGI), and rhamnogalacturonan-II (RGII) [28, 29]. The Backbone structure may branch with other neutral sugar chains such as arabinan, xylogalacturonan (XGA), arabinogalactan I (AG-I), and arabinogalactan II (AG-II).
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Homogalacturonan (HG) is a polymer of galacturonic acid (GalA), in which Gal A residues are linked together by α-1-4 glycosidic bond and the number of GalA residues in HG may vary from 72 to 100% depending on the source of pectin [30]. For instance, the HG backbone of cashew apple pectin, C. maxima pectin, sunflower pectin, citrus pectin, comprises of 69.9–85%, 71–75%, 77–85%, 80–95%, GalA residues, respectively. Amaranth pectin contains more than 80% GalA residues in HG backbone structure. Furthermore, it was also observed that HG may be methoxy-esterified at C-6 and/or O-acetylated at the O-2 and/or O-3. Some exception has also been reported in the detailed structural analysis of HG region of pectin such as C-3 substitution of the galacturonic acids of HG with xylose in pea, apple, carrot, duck weed, etc. [31], and C-2 or C-3 with apiose in duck weeds (Lemna minor) [32]. HG is susceptible to both mechanical and enzymatic deesterification and degradation.
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Rhamnogalacturonan I represents approximately 20–35% of the pectin polysaccharides. It is the highly branched and heterogeneous polysaccharide which is characterized as repeating units of α-(1 → 2)-linked rhamnose and α-(1 → 4)-linked GalA residues. It can be O-acetylated at O-2 and/or O-3 positions of GalA residues [33, 34]. Pectin from citrus peels, mung bean, kidney bean, apple fruit, and flax hypocotyls has been reported 100% methyl esterified in the RGI region [35, 36]. The composition of RGI varies in pectin extracted from different sources. In sugar beet pectin, 80 repeating units of [→2] –α-L-Rha-(1–4)- α-D-GalA-(1→) comprised the backbone of rhamnogalacturonan I (RG-I), whereas citrus pectin contains only 15–40 repeating units [37]. The polymeric side chains of galactans and arabinans are substituted at the O-4 position of RG-I backbone. Arabinogalactan I (AG-I) and arabinogalactan II (AG-II) are also reported to be present as polymeric side chains [38, 39, 40]. The side chains are often referred to as “hairs” and believed to play an important role in pectin functionality. The loss of side chains may increase the solubility of the pectin [41]. PGI is prone to enzymatic depolymerization. However, protease and acid-catalyzed cleavage of RGI has also been reported [28, 42, 43].
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The highly conserved polysaccharide of pectin is rhamnogalacturonan II which constitutes about 10% of the pectin polymer [44]. This polysaccharide is made up of (1 → 4)-linked-α-D-GalA units containing 12 monosaccharide such as apiose, acetic acid, 3-deoxy-manno-2-octulosonic acid (KDO), and 3-deoxy-lyxo-2-heptulosaric acid (DHA) as side chains [30, 39]. GalA present in backbone of rhamnogalacturonan II (RG-II) may be methyl esterified at the C-6 position. The percentage of esterified GalA and acetylated groups in HG chain is termed as the DE and DAc, respectively. It is proposed that in the early developmental stages of plants, highly esterified pectin is formed that undergoes some deesterification in the cell wall or middle lamella. In general, tissue pectin ranges from 60 to 90% DE [45]. Both the DE and the DAc of pectin may vary depending on the method of extraction and plant origin [30, 46]. The functional properties of the pectin are determined by the amount and the distribution of esterified GalA residues in the linear backbone. Presence and distribution of esterified and nonmethylated GalA in pectin define the charge on pectin molecules. Based on their degree of esterification (DE), pectins are classified as high methoxy pectins (HMP) or low methoxy pectins (LMP). DE values of HM pectin range from 60 to 75%, whereas pectin with 20–40% of DE is referred as LM pectin. It was also observed that solubility, viscosity, and gelation properties of pectin are correlated and highly dependent on structural features [47, 48]. Pectin and monovalent salts of pectins are generally soluble in water but di- and trivalent ions are insoluble. The solubility of pectin in water increases with decrease in polymer size and increase in methoxy contents. Pectin powder gets hydrated very fast in water and forms clumps. The solubility of these clumps is very slow. As the pectin molecules come in contact with water, deesterification and depolymerization of pectins start spontaneously. The rate of decomposition of pectin depends on pH and temperature of the solution. As the pH of the solution decreased, with elevated temperature, ionization of carboxylate groups also reduced, which suppresses the hydration and repulsion between the polysaccharide molecules and results in the association of molecules in the form of gels. During thermal processing, solubilization of pectin is affected by β-elimination which depolymerized the pectin molecule and reduced its chain length. Small polymers have poor affinity with cell wall framework and solubilize easily. However, preheating, as well as reduced moisture contents in thermal processing, adversely affects the solubility of pectin in water [49, 50].
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3. Pectin as food emulsifier
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Food additives that are used in food processing to blend two immiscible liquids to produce a desirable product are known as food emulsifier or emulgent. These additives act as surface-active agents on the border of immiscible layers and reduce oil crystallization and prevent water separation. Emulsifiers are used in large number of food products such as ice creams, low-fat spreads, yoghurts, margarine, salad dressings, salty spreads, bakery products, and many other creamy sauces, to keep them in stable emulsion [27]. Emulsifiers increase the whip-ability of batters, enhance mouthfeel of the products, and improve texture and shape of the dough. Moreover, emulsions also help to encapsulate the bioactives [51]. Based on the disperse phase, there are two types of emulsion: oil in water (O/W) and water in oil (W/O). Milk, mayonnaise, dressings, and various beverages are some examples of O/W emulsion, whereas butter and margarine are the typical examples of W/O emulsion. Progress in hydrocolloid chemistry has resulted in the development of multitype emulsion such as O/W/O and O/W/O type emulsion (Figure 1). These emulsions are very important for fat reduction or encapsulation of bioactives and are used in preparation and stabilization of various low-fat creams, seasoning, and flavoring of sauces [52].
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Figure 1.
Types of emulsions.
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Commonly used emulsifiers in food processing are (i) small-molecular surfactant such as lectithins, derivatives of mono- and diglycerides prepared by mixing edible oils with glycerin or ethylene oxide, fatty acid derivatives such as glycol esters, sorbitan esters, polysorbates and (ii) macromolecular emulsifiers that include proteins and plant-based polymers such as soy polysaccharide, guar gum, modified starch, pectin, etc. [53]. As far as the properties of food emulsifier are concern, a good emulsifier should be low in molecular weight, capable to reduce the surface tension rapidly at interface, and should be soluble in continuous phase [54]. Research on food additives revealed the adverse effect of synthetic food additives on human being. Chassaing et al. found that polysorbate 80(P80) or carboxy methyl cellulose (CMC) had adverse effects on gut microbiota and their continuous use triggered the weight gain and metabolic syndrome after 12 weeks of administration in mouse [55]. A recent research carried out on mice shows that regular use of P80 and CMC triggers low-grade intestinal inflammation which may ultimately lead to the development of colon cancer [56]. Therefore, safety issues with the synthetic food additives and consumer’s demand for all natural food ingredients have necessitated the use of plant-based emulsifiers and stabilizers in food.
\n
Pectin is a natural hydrocolloid which exhibits wide spectrum of functional properties. Because of the gelling ability of pectin, it is used as viscosity enhancer. During emulsification process, pectin molecules adsorb at the fine oil droplets from at O/W interface and protect the droplet from coalescing with adjacent drops (short-term stability). The quality of emulsifier is defined by its ability to provide long-term stability against flocculation and coalescence [27]. Figure 2 depicts the stages in long-term emulsion formation using pectin as emulgent. When the viscosity of the continuous phase is increased, the movements of oil droplets become restricted which improves the shelf life of emulsion [57]. In the past decade, some pectin has also been reported to exhibit surface active behavior in oil-water interface and thereby stabilizing the fine oil droplets in emulsion [42, 58]. These functions of pectin are determined by its source, structural modification during processing, distribution of functional groups in pectin backbone, and also by various extrinsic factors such as pH, temperature, ionic strength, cosolute concentration, etc. The emulsification or surface active properties of pectin, i.e., formation of fine oil droplets, are mainly contributed due to the high hydrophobicity of protein residue present in pectin [46, 59] and also by hydrophobic nature of acetyl, methyl, and feruloyl esters [42, 60], whereas emulsion-stabilizing ability is attributed to the carbohydrate moieties and their conformational features [61].
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Figure 2.
Emulsion formation and stabilization using polymer as emulgent.
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3.1 Mechanism of emulsion formation and stabilization
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The mechanism of emulsion formation is shown in Figure 3. Different models explain the emulsion formation as covalently bound protein moieties in pectin are adsorbed onto the oil-water interface [46], form anchor points at the interface, and reduce the interfacial tension while the charged carbohydrate units extend into the aqueous phase [62] and stabilize by steric and viscosity effects in the aqueous phase(Figure 3a). Now, it is a well-established fact that pectin from different source shows variability in structure and protein contents. Leroux et al. identified many anchor points in sugar beet pectin (SBP) molecules [46], and proposed a loop-and-tail model (Figure 3b). According to the authors, only a limited amount of protein is adsorbed at the oil surface and acts as main moiety in the stabilization of the emulsion. This model was further confirmed by Siew and others [62]. The study was carried out to measure the thickness of the adsorbed SBP on oil-water interface layer, proposed a multilayer adsorption model (Figure 3c). Electrostatic interactions between the positively charged protein moiety and the negatively charged carbohydrate moiety were also reported.
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Figure 3.
Different models showing pectin adsorption at oil/water interface during emulsion formation.
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Pectin O/W emulsion is generally stabilized through steric and electrostatic interaction. The carbohydrate moieties and neutral sugar side chains of RG I region of pectin confer the stability to the pectin emulsions through steric properties of the adsorbed polymers, when pectin is used as monoemulsifiers. In addition, pectin reversible association with galactan/arabinogalactan prior to emulsification also improves the emulsion stability [42, 63]. Electrostatic stabilization of emulsion is ascribed to sugar moieties and structural features of the HG units of pectin. If the pH of dispersion medium is above 3.5, nonmethylated carboxylic group of HG region gets ionized and confers charge on the pectin surface. Interaction of an ionic surfactant with oil droplets results in electrostatic stabilization [64]. Pectin viscosity also plays an important role in controlling the emulsion stability. HG region-rich pectin shows higher intrinsic viscosity ([η]); therefore, HG and RG ratio of pectin and molecular interactions that improve the intrinsic viscosity ([η]) of pectin solution also contributes in shelf life of emulsion [65, 66]. It has also observed that structural features of pectin such as pectin protein content, molecular mass, and presence of ferulic acid, and acetyl group in carbohydrate moieties of pectin also affect pectin’s emulsifying and emulsion stabilization properties [15]. Williams et al. showed that ferulic acid-rich pectin did not show significant difference in emulsifying ability of pectin when compared with pectin poor in ferulic acid [67]. Digestion of sugar beet pectin(SBP) with acidic proteases resulted in formation of larger size of oil droplet, lower creaming stability, and loss of emulsifying activity of SBP which confirms that protein contents of SBP play an important role in emulsifying ability of the polymer [42]. Nevertheless, in other research, it was also found that protein-rich fractions of SBP did not necessarily displayed better emulsifying ability; therefore, it was concluded that both protein with carbohydrate moiety together help in controlling emulsifying ability of SBP. Castellani et al. further suggest that both the carbohydrate and protein moieties function together as unit and affect the hydrophilic-hydrophobic equilibrium of the SBP molecule [68]. Therefore, when SBP is digested with proteases or other enzyme, a single moiety may function differently. Furthermore, it was also proposed that protein folding may also mask the hydrophobic effect of protein and thus affect the overall properties of the polymers [69].
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Molecular weight of pectin has also been reported to affect the emulsifying capacity of pectin. Pectin with low molecular weight was more efficient in stabilizing small emulsion droplets than high-molecular weight pectin. However, very small size of citrus pectin had negative effect on emulsion-stabilizing ability of pectin. It could be due to the poor steric stabilization of depolymerized polymer [59].
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3.2 Pectin-containing emulsion-based food
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Emulsion-based food products can be defined as a network of pectin-protein molecules entrapping the oil droplet in between. Nowadays, a large number of pectin- and polysaccharide-based emulsified low-fat dairy products, meat products, spreads or desserts, bakery products, sauces, etc., are available in market. Low-fat and low-cholesterol mayonnaise, low-fat cottage cheese, low-fat drinking yogurt, and flavored oil-containing acidified milk drinks are the few examples of pectin-based emulsified products. These products are prepared by replacing full-fat milk from skimmed milk, emulsified oil, and whey proteins [70, 71]. A low-fat cheese was prepared using skimmed milk and water-in-oil-in-water (W1/O/W2) emulsified canola oil. Different emulsifiers such as amidated low-methoxyl pectins (LMP), gum arabic (GA), carboxymethylcellulose (CMC), and combinations of GA-CMC or GA-LMP were used to stabilize the emulsion. Textural characteristics and sensory evaluation of low-fat cheese show that polymers used to stabilize the emulsion affected both microcrystalline structure and organoleptic properties. The cheese prepared using GA and LMP was almost similar in textural characteristics to the full-fat milk cheese [72]. In another study, Liu et al. compared the textural and structural features and sensory quality of full-fat and low-fat cheese analogs prepared with or without the incorporation of pectin [71]. Microstructure analysis using scanning electron microscopy revealed that full-fat cheese was denser and contained higher concentration of fat globules than low-fat cheese made with or without pectin. Comparison within the low-fat cheese analogs showed clear difference in their hardness, gumminess, chewiness, and adhesiveness. Addition of pectin had positive effect on textural and sensory attribute and scored better in mouthfeel also.
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Low-fat (Lf) mayonnaise was prepared by partial replacement of egg yolk and incorporation of pectin as emulsifier [73, 74]. Pectin weak gel, pectin microencapsulation, and whey protein isolate were used in preparation of low-fat (Lf) mayonnaise. Physicochemical and sensory properties of Lf mayonnaise were compared with full-fat (Ff) mayonnaise; Lf mayonnaise had low energy and more water contents than Ff. Textural features and rheological properties of the Lf and Ff mayonnaise were similar and both displayed thixotropic shear thinning behavior and categorized as weak gels. Moreover, Lf mayonnaise prepared using pectin had better acceptability than whey protein incorporation [75]. Emulsified oil is used as an effective delivery system of active compound in functional foods, and also serves as milk fat replacer in fat-free dairy products. To improve the nutritional value of food, low-fat dairy products are produced, whereas saturated milk fat is generally replaced with emulsified-unsaturated vegetable oils [76].
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In recent year, pectin in combination with inulin has been reported to prepare low-fat meat batter. Méndez-Zamora et al. studied the effect of substitution of animal fat with different formulations of pectin and inulin on chemical composition, textural, and sensory properties of frankfurter sausages [77]. Finding of the research showed that fracturability, gumminess, and chewiness of the low-fat sauces were slightly lower than those of the control. However, addition of 15% inulin improves the sensory properties. In a similar work, replacement of pork back fat with 15% pectin and 15% inulin was found effective in maintaining the physicochemical properties and emulsion stability of the low-fat meat batter [78].
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4. Pectin as gelling agent
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The use of pectin in food products as a gelling agent is a long tradition. Later on, it was discovered that pectin forms different types of viscoelastic solution under suitable conditions. This property of pectin is commercially exploited in preparation of jams, jellies, and marmalades. Rheological behaviors of pectin depend on pectin source, its degree of methylation, distribution of nonmethylated GalA unit on pectin backbone, and degree of acetylation, and also on various extrinsic factors such as temperature, pH, concentration, and presence of divalent ions. At a constant pH, the setting time of pectin increases with decreasing DM and degree of blockiness (DB) in the absence of bivalent ions [79]. Therefore, on the basis of gelling process, pectin is classified as rapid, medium, and slow set pectin [80].
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Gelling process of pectin and its stabilization follows different mechanisms for different types of pectin. HMP form gels in a narrow pH range (2.0–3.5) in the presence of sucrose at a concentration higher than 55% w/v in medium. During the gelatin process of HMP, junction zones are formed due to the cross-linking of two or more pectin molecules. These junctions are stabilized by weak molecular interaction such as hydrogen and hydrophobic bonds between polar and nonpolar methyl-esterified groups and require high sugar concentration and low pH [81]. These gels are thermally reversible. LMP can form gel over a wide pH range (2.0–6.0) independent of sucrose, but requires divalent ion, such as calcium [82, 83]. LMP follow the eggbox model for its gelation, where positively charged calcium ions (Ca2+) are entrapped in between the negatively charged carboxylic group of pectin. The zigzag network of Ca2+ ion and GalA molecules looks like eggbox, and therefore, model is named as eggbox model [80]. These gels are stabilized by electrostatic bonds. In the presence of Ca2+, calcium bridges are formed with pectin molecules that make the solution more viscous. At the higher pH, the ionic strength of the solution is increased and thus more Ca2+ is needed for gelation. In case of highly acetylated pectin such as sugar beet, acetyl groups cause steric hindrances and interfere with the Ca2+ ion and GalA bond formation, thus preventing gel formation. Kuuva et al. [84] reported that enzymatic modification in pectin structure, i.e., removal of acetyl groups using α-arabinofuranosidase (α-Afases) and acetyl esterase enzymes, can improve the gelling property of acetylated pectin.
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HMP are generally used in preparation of standard jams where sugar contents are above 55%, high-quality, tender confectionary jellies, fruit pastes, etc. LMP do not require sugar for its gelatin and therefore preferred choice for the production of low-calorie food products such as milk desserts, jams, jellies, and preserves, [28, 85]. LM pectins are more stable in low pH and high temperature conditions as compare to HM pectins and can be stored for more than a year.
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5. Pectin in food packaging
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Food packaging is one of the fastest growing segments of food industry. Traditionally, packaging system was limited to the containers and packaging material to transport the food items from manufacturer to the retail market and then to the consumers. Such type of packaging was unable to contribute in the extension of the shelf life and maintenance of the quality of the products. Due to the globalization of food market and increasing demand of shelf-stable processed food that retains the natural properties of food, the need of functional/active packaging material is increasing. To meet the industrial demand, a number of polymers are being synthesized and used in food packaging because of their flexibility, versatility, and cost effectiveness. Although, synthetic materials are able to fulfill all the industrial needs and keep food fresh and safe by protecting them from abiotic factors such as moisture, heat, oxygen, unpleasant odor, and biotic components such as micro- and macroorganisms. But, disposal of nonbiodegradable packaging material is a serious problem which poses a threat to the environment. Therefore, more research has been focused on the development of biodegradable packaging for food packaging applications using poly(lactic acid) (PLA), poly(hydroxyalkanoates) (PHAs), starch, etc. [86]. Among all the natural polymers, polysaccharides are gaining more attention as they are versatile in nature and easily available in relatively low cost.
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A variety of natural polysaccharides, such as pectin, chitosan derivatives, alginate, cellulose, seaweed extract, and starch are usually used in the preparation of edible films and coatings [87]. Pectin is one of the most significant renewable natural polymers which are the main component of all the biomass and ubiquitous in nature. Being flexible in nature, pectin and its derivatives are used in many biodegradable packaging materials that serve as moisture, oil, and aroma barrier, reduce respiration rate and oxidation of food [88]. Pectin along with food grade emulsifiers is also used in the preparation of edible films. These films are used in fresh and minimally processed, fruits and vegetables, foods and food products as pectin is the main component of the omnivorous diet and can be metabolized. Edible coating protects the nutritional properties of the food and also saves highly perishable food from the enzymatic browning, off-flavor development, aroma loss, retards lipid migration, and reduces pathogen attack during storage.
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At low pH, LM pectins are cross-linked with calcium cations and form hard gels. These gels have highly stable structure and act as water barriers. Because of these properties, LM pectin films are used as edible coatings [88, 89]. Extension of shelf life of avocado fruits was also reported to over a month at 10°C by using edible pectin films. It was found that when avocados were coated with edible pectin films and stored at 10°C, rate of oxygen absorption and rate of respiration decreased which results in delaying of texture and color change of fruits [90]. Oms-Oliu et al. used calcium chloride and sunflower oil cross-linked with LM pectin films onto fresh-cut melon to see the effect on extension of shelf life of cut fruits [91]. It was observed that edible pectin films maintained the initial firmness, decrease the wounding stress of fresh-cut fruits, and prevent the dehydration during storage up to 15 days at 4°C but could not reduce the microbial growth onto the fresh melon. It has been observed that to reduce the respiration rate and to prevent the off-flavor development, different pectin and emulsifier formations are required for different fruits. Edible coating film formulation consisted on pectin, sorbitol, and bee wax was successfully used by Moalemiyan et al. to keep the fresh-cut mangoes in original state for over 2 weeks [92]. Whereas in a similar study, pectin coating containing sucrose and calcium lactate was able to prevent the fruits’ respiration rate and maintain sensory properties in fresh melon fruits for up to 14 days storage at 5°C. In a similar study [93], pectin edible coating solution containing pectin (3%), glycerol (2.5%), polyvinyl alcohol (1.25%), and citric acid (1%) was prepared and applied on sapota fruits by dipping method and uncoated sapota fruits were used as control. Both the treated and control fruits were stored at 30 ± 3°C. Physicochemical parameters namely, weight, color, firmness, acidity, TSS, pH, and ascorbic acid contents of both the coated and control fruits were measured at regular interval up to 11th day of the storage at 30 ± 3°C. Reduced rate of change in weight loss and other parameters were reported in pectin-coated sapota as compared to control fruits and it was observed that pectin film formulation was able to maintain good quality attributes and extend the shelf life of pectin-coated sapota fruits up to 11 days of storage at room temperature, whereas control fruits were edible up to 6 days. Furthermore, it was also observed that sapota fruits dipped in sodium alginate containing 2% pectin solution for 2 min were more effective in maintaining the organoleptic properties up to 30 days of refrigerated storage as compared to sapota fruits dipped for 4 min and untreated sapota fruits [94]. Bayarri et al. developed antimicrobial films using lysozyme and LM pectin complex. The main purpose of the study was to control the release of lysozyme in packaged food and to target lysozyme-sensitive bacteria such as Bacillus and Clostridium. It was observed that in the presence of fungal pectinase, due to the dissociation of pectin linkage, lysozyme activity of films increased remarkably. Many food-contaminating bacteria are pectinase producing and such type of films may be used to control food contaminants. These results have opened new avenues for custom-made biodegradable film [95].
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In last few years, some researchers have focused on pectin-based coating containing edible essential to improve the antimicrobial properties and to enhance the efficiency of the pectin films. Edible coating formulation containing sodium alginate and pectin (PE) enriched with eugenol (Eug) and citral (Cit) essential oil at different concentrations was used to increase the shelf life of strawberries. Physical and organoleptic parameters of coated fruits stored at 10°C for 14 days show that formulation containing PE 2% + Eug 0.1%; PE 2% + Cit 0.15% was more suitable than sodium alginate-based formulations [96]. Pectin coating containing lemon and orange peel essential oils was reported to increase the shelf life and quality attributes of the strawberry fruits up to 12 days when stored at 5°C. It was also observed that fruits coated with pectin + 1% orange essence showed less weight loss and soluble solids as compare to their control during the storage [97]. Sanchís et al. studied the combined effect of edible pectin coating with active modified atmospheric packaging on fresh-cut “Rojo Brillante” persimmon. Persimmon fruit slices were coated by dipping in the pectin-based emulsion or in water as control. Both the treated and control slices were packed under 5 kPa O2 (MAP) or under ambient atmosphere for up to 9 days at 5°C. Various parameters, such as package gas composition, color and firmness of slice, polyphenol oxidase activity, were measured during storage. It was observed that edible coating along with MAP significantly reduced the CO2 emission and O2 consumption in the packaged fruits. Furthermore, coating was also effective in controlling microbial growth and reducing enzymatic browning and maintains good sensory parameters up to 10 days on storage [98].
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Drying is the traditional and oldest method of fruit and vegetable preservation. It decreases the enzymatic activity, reduces the moisture contents, and protects the food from microbial attack. However, drying results in loss of nutrients, vitamins, heat-labile enzymes, modifies the texture, color, and organoleptic quality of dried fruits and vegetables and therefore diminishes the market value also. Pretreatment of food products with pectin coatings containing other bioactive compound such as ascorbic acid, CaCl2, edible gum, etc., before drying or blanching has been proposed as an effective method to preserve the nutritional as well as organoleptic quality of dried food [99]. Recent researches have shown that application of pectin coating could protect the moisture and vitamin C loss in pretreated papaya slice and osmotic dehydrated pineapple. In one of the research [100], pineapple slice was pretreated with pectin coating formulation containing (50%)/calcium lactate (4%)/ascorbic acid (2%) solutions and then dried by hot-air-drying method. Physicochemical analysis of dried product showed less reduction in vitamin C contents as compared to untreated pineapple slice. In a similar work, pectin coating supplement with vitamin C (1%) was used for precoating of papaya slice. It was found that incorporation of vitamin C did not affect the drying process. However, significant increase in vitamin C content was observed in final product [101].
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Frying is a method of cooking that causes changes in chemical and physical parameters of food and enhances the taste. However, high temperature vaporizes the water of food and affects the nutritional properties due to protein denaturation and starch gelatinization. The oil uptake during frying is affected by various parameters such as type of oil used, frying temperature and duration, product moisture content, shape, porosity, prefrying treatment, etc. [102]. Surface area and pretreatment of products are the major factors that determine the oil absorbed. Edible coating has also been used successfully, to reduce the oil uptake during frying in various deep-fried products. Reduction in oil uptake and improvement of texture and quality of potato slices was reported by Daraei Garmakhany et al. in 2008. Authors found that coating of potato slices with pectin, guar, and CMC solutions can reduce the oil uptake when compared with nontreated potato chips [103]. Similar results were also obtained by Khalil, where a combination of pectin or sodium alginate with calcium chlorides significantly reduces the oil uptake of French fries. Coating formulation of 0.5% calcium chloride and 5% pectin was most effective in reducing the oil uptake [104]. Kizito et al. used different edible coatings (pectin, carboxy methyl cellulose, agar, and chitosan) at a concentration of 1–2% for pretreatment of potato chips, followed by deep frying of chips. Fried chips were analyzed biochemically and organoleptically to investigate the quality attributes of the products. It was revealed that all the coating polymers were successful in reducing the oil uptake but pectin was most effective and reduced oil uptake up to 12.93%, followed by CMC (11.71%), chitosan (8.28%), and agar (5.25%) and significantly improved moisture retention of strips (p < 0.05) [105].
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6. Conclusion
\n
The application of natural polymers in food industry is increasing day by day. Researchers are focusing more and more toward the pectin because of the ease-of-availability, structural flexibility, and versatile composition. Pectin can be sourced from a number of easily available horticulture crops (Table 1). Pectin is a hydrocolloid which is used as a food emulsifier, gelling agent, thickener, and stabilizer. It is the preferred choice of most of the food processors as fat or sugar replacer in low-calorie foods. In the recent years, increasing demand of ready-to-serve foods, fresh-cut fruits, and vegetable has opened a new market for edible films. Being biodegradable and recyclable, a lot of research is being done on pectin-based edible film formulations. These films reduce the exchange of moisture, gases, lipids, and volatiles between food and environment, and also serve as protective barrier for microorganisms.
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Even though a lot of information is available regarding pectin structure and many pectin-based products are available in market, role of many carbohydrate moieties and their effect on various function of pectin are not yet well defined. Therefore, it is necessary to understand the structural-function relationship of pectin and its interactions for developing functional food products.
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Acknowledgments
\n
The authors thank Director, CSIR-CFTRI for the encouragement.
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Conflict of interest
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The authors declare no conflict of interest.
\n
\n',keywords:"pectin, pectin oligosaccharide, food emulsifier, edible films, functional food, food stabilizer, emulsified food",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/65793.pdf",chapterXML:"https://mts.intechopen.com/source/xml/65793.xml",downloadPdfUrl:"/chapter/pdf-download/65793",previewPdfUrl:"/chapter/pdf-preview/65793",totalDownloads:1880,totalViews:0,totalCrossrefCites:5,dateSubmitted:"October 31st 2018",dateReviewed:"December 20th 2018",datePrePublished:"February 22nd 2019",datePublished:null,dateFinished:null,readingETA:"0",abstract:"Pectin is a branched heteropolysaccharide consisting of long-chain galacturonan segments and other neutral sugars such as rhamnose, arabinose, galactose, and xylose. It forms a matrix with celluloses and hemicelluloses and contributes to the cell structure. Due to the presence of several sugar moieties and different levels of methyl esterification, pectin does not have defined molecular weight like other polysaccharides. Pectin has wide applications. It is used as emulsifier, gelling agent, thickener, stabilizer, and fat or sugar replacer in low-calorie foods. Pectin and pectin-derived oligosaccharides can also be used as an important ingredient in functional foods. In recent past, a new application envisaged for pectin polymers as edible films or coating. These films act as natural barrier for exchange of moisture, gases, lipids, and volatiles between food and environment, and protect fruits and vegetable from microbial contamination. The degree of esterification of pectin and other structural modifications defines the functional properties. Herein, various functional properties of pectin in relation to food processing and packaging are discussed.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/65793",risUrl:"/chapter/ris/65793",signatures:"Thiraviam Vanitha and Mahejibin Khan",book:{id:"8504",title:"Pectins",subtitle:"Extraction, Purification, Characterization and Applications",fullTitle:"Pectins - Extraction, Purification, Characterization and Applications",slug:"pectins-extraction-purification-characterization-and-applications",publishedDate:"January 22nd 2020",bookSignature:"Martin Masuelli",coverURL:"https://cdn.intechopen.com/books/images_new/8504.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"99994",title:"Dr.",name:"Martin",middleName:"Alberto",surname:"Masuelli",slug:"martin-masuelli",fullName:"Martin Masuelli"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:null,sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Pectin structure",level:"1"},{id:"sec_3",title:"3. Pectin as food emulsifier",level:"1"},{id:"sec_3_2",title:"3.1 Mechanism of emulsion formation and stabilization",level:"2"},{id:"sec_4_2",title:"3.2 Pectin-containing emulsion-based food",level:"2"},{id:"sec_6",title:"4. Pectin as gelling agent",level:"1"},{id:"sec_7",title:"5. Pectin in food packaging",level:"1"},{id:"sec_8",title:"6. Conclusion",level:"1"},{id:"sec_9",title:"Acknowledgments",level:"1"},{id:"sec_9",title:"Conflict of interest",level:"1"}],chapterReferences:[{id:"B1",body:'Talbott LD, Ray PM. Molecular size and separability features of pea cell wall polysaccharides. Plant Physiology. 1992;92:357-368. DOI: 10.1104/pp.98.1.357'},{id:"B2",body:'Khan M, Ekambaram N, Umesh-Kumar S. Potential application of pectinase in developing functional foods. Annual Review of Food Science and Technology. 2013;4:21-34. 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DOI: 10.1111/j.1365-2621.1994.tb08132.x'},{id:"B103",body:'Daraei Garmakhany A, Mirzaei HO, Kashani Nejad M, Maghsudlo Y. Study of oil uptake and some quality attributes of potato chips affected by hydrocolloids. European Journal of Lipid Science and Technology. 2008;110:1045-1049. DOI: 10.1002/ejlt.200700255'},{id:"B104",body:'Khalil AH. Quality of french fried potatoes as influenced by coating with hydrocolloids. Food Chemistry. 1999;66:201-206. DOI: 10.1016/S0308-8146(99)00045-X'},{id:"B105",body:'Kizito KF, Abdel-Aal MH, Ragab MH, Youssef MM. Quality attributes of French fries as affected by different coatings, frozen storage and frying conditions. Journal of Agricultural Science and Botany. 2017;1(1):23-29'}],footnotes:[],contributors:[{corresp:null,contributorFullName:"Thiraviam Vanitha",address:null,affiliation:'
Department of Fruits and Vegetable Technology, CSIR-Central Food Technological Research Institute, India
CSIR-Central Food Technological Research Institute-Resource Centre, India
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IntechOpen’s Academic Editors and Authors have received funding for their work through many well-known funders, including: the European Commission, Bill and Melinda Gates Foundation, Wellcome Trust, Chinese Academy of Sciences, Natural Science Foundation of China (NSFC), CGIAR Consortium of International Agricultural Research Centers, National Institute of Health (NIH), National Science Foundation (NSF), National Aeronautics and Space Administration (NASA), National Institute of Standards and Technology (NIST), German Research Foundation (DFG), Research Councils United Kingdom (RCUK), Oswaldo Cruz Foundation, Austrian Science Fund (FWF), Foundation for Science and Technology (FCT), Australian Research Council (ARC).
Open Access publication costs can often be designated directly in the grants or in specific budgets allocated for that purpose. Many of the most important funding organisations encourage, and even request, that the projects they fund are made available at no cost to the wider public. IntechOpen strives to maintain excellent relationships with these funders and ensures compliance with mandates.
\\n\\n
In order to help Authors identify appropriate funding agencies and institutions, we have created a list, based on extensive research on various OA resources (including ROARMAP and SHERPA/JULIET) of organizations that have funds available. Before consulting our list we encourage you to petition your own institution or organization for Open Access funds or check the specifications of your grant with your funder to ascertain if publication costs are included. Where you are in receipt of a grant you should clarify:
\\n\\n
\\n\\t
Does your institution already have a budget for covering Open Access publication costs?
\\n\\t
Does your grant list Open Access publication fees as legitimate direct/indirect costs?
\\n
\\n\\n
If you are associated with any of the institutions in our list below, you can apply to receive OA publication funds by following the instructions provided in the links. Please consult the Open Access policies or grant Terms and Conditions of any institution with which you are linked to explore ways to cover your publication costs (also accessible by clicking on the link in their title).
\\n\\n
Please note that this list is not a definitive one and is updated regularly. To suggest possible modifications or the inclusion of your institution/funder, please contact us at oapf@intechopen.com
\\n\\n
Please be aware that you must be a member, or grantee, of the institutions/funders listed in order to apply for their Open Access publication funds.
Open Access publication costs can often be designated directly in the grants or in specific budgets allocated for that purpose. Many of the most important funding organisations encourage, and even request, that the projects they fund are made available at no cost to the wider public. IntechOpen strives to maintain excellent relationships with these funders and ensures compliance with mandates.
\n\n
In order to help Authors identify appropriate funding agencies and institutions, we have created a list, based on extensive research on various OA resources (including ROARMAP and SHERPA/JULIET) of organizations that have funds available. Before consulting our list we encourage you to petition your own institution or organization for Open Access funds or check the specifications of your grant with your funder to ascertain if publication costs are included. Where you are in receipt of a grant you should clarify:
\n\n
\n\t
Does your institution already have a budget for covering Open Access publication costs?
\n\t
Does your grant list Open Access publication fees as legitimate direct/indirect costs?
\n
\n\n
If you are associated with any of the institutions in our list below, you can apply to receive OA publication funds by following the instructions provided in the links. Please consult the Open Access policies or grant Terms and Conditions of any institution with which you are linked to explore ways to cover your publication costs (also accessible by clicking on the link in their title).
\n\n
Please note that this list is not a definitive one and is updated regularly. To suggest possible modifications or the inclusion of your institution/funder, please contact us at oapf@intechopen.com
\n\n
Please be aware that you must be a member, or grantee, of the institutions/funders listed in order to apply for their Open Access publication funds.
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