Influence Of Physicochemical Characteristics Of Neem Seeds .
biomoleculesArticleInfluence of Physicochemical Characteristics ofNeem Seeds (Azadirachta indica A. Juss) onBiodiesel ProductionBakari Hamadou 1,2 , Djomdi 2, *, Ruben Zieba Falama 1,3 , Delattre Cedric 4 ,Pierre Guillaume 4 , Dubessay Pascal 4 and Michaud Philippe 41234*Energy Research Laboratory, Renewable Energy Section (LRE/SENC), Institute for Geological and MiningResearch (IRGM), Nlongkak Yaounde P.O. Box 4110, Cameroon; hamadou.bakari@yahoo.fr (B.H.);rubenziebafalama@yahoo.fr (R.Z.F.)Department of the Renewable Energies, The National Advanced School of Engineering of Maroua,University of Maroua, Maroua P.O. Box 46, CameroonDepartment of Physics, Faculty of Sciences, University of Maroua, Maroua P.O. Box 814, CameroonCNRS, SIGMA Clermont, Institut Pascal, Université Clermont Auvergne, F-63000 Clermont-Ferrand, France;cedric.delattre@uca.fr (D.C.); guillaume.pierre@uca.fr (P.G.); pascal.dubessay@uca.fr (D.P.);philippe.Michaud@uca.fr (M.P.)Correspondence: ngdjomdi@yahoo.fr; Tel./Fax: 237-222-29-31-12 Received: 27 May 2019; Accepted: 5 July 2019; Published: 17 April 2020Abstract: The aim of this work is to study the influence of the physicochemical characteristics ofneem seeds, according to their mass and oil content, on the production of biodiesel. After thephysical characterization of the seeds and extraction of the oil (triglycerides), biodiesel was producedfrom crude neem seed oil by transesterification with ethanol in the presence of sodium hydroxide.This study shows that the physicochemical characteristics of these seeds vary according to the originof the samples. The seeds from Zidim, with a mass average of 200 seeds evaluated at 141.36 g and analmond content of 40.70%, have better characteristics compared to those collected in the city of Maroua,with average values evaluated at 128.00 g and 36.05%, respectively. Almonds have an average lipidcontent of 53.98 and 56.75% for the Maroua and Zidim samples, respectively. This study also revealsthat neem oil, by its physicochemical characteristics, has a satisfactory quality for a valorization inthe production of biodiesel. However, its relatively high free fatty acid content is a major drawback,which leads to a low yield of biodiesel, evaluated on average at 89.02%, and requires a desacidificationoperation to improve this yield. The analysis of biodiesel indicates physicochemical characteristicsclose and comparable to those of petrodiesel, particularly in terms of calorific value, density, kinematicviscosity, acid value, evaluated at 41.00 MJ/kg, 0.803, 4.42 cSt, and 0.130 mg/g, respectively.Keywords: biodiesel; neem seed; transesterification; sanitation; biofuel1. IntroductionNeem (Azadirachta indica A. Juss) is a tree of Indian origin that adapts well to poor soils and issupported in warm and dry climates [1]. It is present in all the dry and subtropical tropical areas ofOceania, Asia, Africa and America [2]. It was introduced in the northern part of Cameroon thanks tothe reforestation strategy called “Operation Green Sahel” set up by the Cameroonian government inthe 1970s to fight against desertification. In the town of Maroua, capital of the Far North region ofthe country, this species represents about 80% of the trees population. These plants generate hugequantities of biomass, mainly leaves and seeds, which are not recovered, but are often swept away aswaste and dumped or simply burned, causing sanitation and pollution problems. Indeed neem startsBiomolecules 2020, 10, 616; lecules
Biomolecules2020,Biomolecules2019,10,9, 616x FOR PEER REVIEW2 of 210of 10quantities of biomass, mainly leaves and seeds, which are not recovered, but are often swept awayas waste anddumpedor simplyburned,sanitationand reachespollutionIndeedneem atfructificationmostcommonlybetweenthe causingages of 3–5years andtheproblems.maximumproductionbetweenthe anagesof 3–5years andestimatedreaches atthe30–50maximum10startsyears fructificationthat continuesmostuntilcommonly150–200 years[3]. Withannualproductionkg for anproductionat 10yearsthat continuesyearsWith anestimatedadulttree, neemseedscontainalmondsuntilvery150–200rich in oilwith[3].contentsupannualto 60%productionof its dry matter[1,3,4].at 30–50kg foran adulttree,neemneemseedseedsoilcontainalmonds veryin oilcontents up to 60% ofThefatty acidprofileof theis characterizedbyricha ratioofwithsaturated/unsaturatedfattyits drymatter[1,3,4].fattyprofileof thecharacterizingneem seed oiltheis characterizedby aofratioofacidsrangingfrom0.53Theto 0.54[5].acidSeveralstudiesfatty acid profilethe neemsaturated/unsaturatedfatty acidsfrombeen0.53 identified,to 0.54 [5]. Severalthe fattyseedoil report that fourteenfatty rangingacids havefour ofstudieswhich characterizingare in the nd(predominant fatty acid) is a monounsaturated fatty acid representing 25 to 58% [5–8], palmiticare in the majority. Oleic (predominant fatty acid) is a monounsaturated fatty acid representing 25 tostearicwhich are saturated, and linoleic which is polyunsaturated. In addition, the global energy58% [5–8], palmitic and stearic which are saturated, and linoleic which is polyunsaturated. Indemand with a predominance of fossil fuel sources, the use of which leads not only to its depletion,addition, the global energy demand with a predominance of fossil fuel sources, the use of which leadsbut also, and above all to global warming, is ever-increasing and requires us to develop renewable andnot only to its depletion, but also, and above all to global warming, is ever-increasing and requiressustainable alternative energy sources. Therefore, an effective and viable way to promote this sanitationus to develop renewable and sustainable alternative energy sources. Therefore, an effective andis the energy recovery of this derivative of neem as the recovery of neem seeds could be useful for theviable way to promote this sanitation is the energy recovery of this derivative of neem as the recoveryproductionof biodieseltransesterification.Biodiesel,whicha “clean”, biodegradable,of neem seedscould bebyusefulfor the productionof biodieselby istransesterification.Biodiesel, non-toxicwhichandbiofuel, will notnon-toxiconly reducegas emissions,willalso reducethe problemis arenewable“clean”, biodegradable,and greenhouserenewable biofuel,will notbutonlyreducegreenhousegasofemissions,energy security.thisreduceend, ittheis thereforeimportantto characterizethis itbiomassin orderto betterbut willToalsoproblem ofenergy security.To this end,is thereforeimportantcontrolits energythispotentialandimpactof thevariabilityof thesecharacteristicsaccordingto theto characterizebiomassin theorderto bettercontrolits energypotentialand the impactof thedifferentgeographicaland climaticaccordingzones fromwhichthe seedscome. Thisaimsto studyvariabilityof these characteristicsto evariabilityphysicochemicalcharacteristicsof theseedsaccordingto their mass andcharacteristicsoil content andwhich theofseedscome. This workaims to studyvariabilityof physicochemicalof toestablishtheir influencebiodieseltransesterification.seeds accordingto theironmassand oil productioncontent and byto establishtheir influence on biodiesel productionby transesterification.2. Material and Methods2. Material and Methods2.1. Collection and Pretreatment of Plant Material (Neem Seeds)2.1.ThereCollectionandonePretreatmentof neemPlant Material(NeemSeeds)A. Juss) in Cameroon. The two lots of neemis onlyvariety of(Azadirachtaindicaseeds samplesusedonefor varietythis studycome(Azadirachtafrom two localitiestheinFarNorth regionof CameroonwithThere is onlyof neemindica A. inJuss)Cameroon.The twolots of ics.Samplesinofwere regioncollectedin three differentseeds samplesused forstudy comefrom two localitiestheseedsFar Northof esandof seedswere collectedin threefromdifferentdistrictsofgeographicthe city o”)and Zidim,aa locality of the department of Mayo Tsanaga, located about 48 km from the city of Maroua. Threelocalitywereof thecollecteddepartmentof MayolocationsTsanaga, inlocatedabout48twokm localities.from the cityof Maroua.Threesamplesat differenteach oftheseTheseneem seedsweresamplesduringwere collectedat differentlocationsinineachof theseThese dried,neem seedswere atobtainedthe en cleaned,and storedobtainedduring theabundantfromfruitingin Marchand2018thenandthethencleaned,dried,and storedatroomtemperature,protectedlightperiodand moisturestudieswereconductedin andthenthestudieswereconductedinApril2018. Their moisture contents were 9.533 0.089 and 9.470 0.049% for the Maroua and Zidim2018. Their moisture contents were 9.533 0.089 and 9.470 0.049% for the Maroua and Zidimsamples,respectively. The trials were carried out on whole seeds, depulpated seeds, almonds, hullssamples, respectively. The trials were carried out on whole seeds, depulpated seeds, almonds, hullsand pulps. In order to perform a physicochemical characterization of whole seeds, the samples receivedand pulps. In order to perform a physicochemical characterization of whole seeds, the samplesa series of pretreatment operations. They were cleaned and then dewatered by dipping them in water.received a series of pretreatment operations. They were cleaned and then dewatered by dipping themThe depulped seeds were dried at room temperature and then peeled to separate the shell from thein water. The depulped seeds were dried at room temperature and then peeled to separate the shellkernel as shown in Figure 1.from the kernel as shown in Figure 1.Whole seedsDehulled seedsFigure 1. Cont.
Biomolecules 2020, 10, 6163 of 10Biomolecules 2019, 9, x FOR PEER REVIEWAlmonds3 of 10Simple hullsHulls with pulp and eemSeedsSeeds2.2.PhysicochemicalPhysicochemical CharacterizationCharacterization mond andand shell odeterminedbyweighingthreesamples of 200 depulped seeds. The pulp and skin content were also determined by weighing threesamplesofof 200200 gg ofof seeds,seeds, beforebefore andThedrydrymatterwaswasdeterminedsamplesand Thematterdetermined C untilaccordingtotothethemethodmethod of AFNORweredriedat 105 C untila masssamplessamplesweredriedat 105a essedasapercentage,wascalculatedmass was obtained and the dry matter content, expressed as a percentage, was calculated afteraftercoolingin a desiccator,accordingto the followingformula:incoolinga desiccator,accordingto the followingformula:𝑀𝑓 𝑇𝐷𝑀𝐶 (1)M f T100 100(1)DMC𝑀 𝑖 𝑇Mi TIn the above equation, DMC is the dry matter content (%), Mf is the mass of the crucible andsampleafterdrying(g), Mi isDMtheCmassofdrythe crucibleand sampledrying(g),ofTtheis theemptyandIn theaboveequation,is thematter content(%), beforeMf is themasscruciblecrucibleaftertare drying(g).sample(g), Mi is the mass of the crucible and sample before drying (g), T is the emptyThemoisturecontentof the samples (MC) was deducted from the value of the dry mattercrucible tare (g).accordingtothefollowingrelation:The moisture content of the samples (MC ) was deducted from the value of the dry matter accordingto the following relation:(2)𝑀𝐶 100 𝐷𝑀𝐶MC 100 DMC(2)The inorganic material was determined from the dry matter samples by electric ovenincinerationat 550 material C for fourhoursand its valuecalculatedthe followingformula:The inorganicwasdeterminedfromwasthe drymatterbysamplesby electricoven incineration at 550 C for four hours and its value was calculatedbythefollowingformula:𝑀𝑓 𝑇𝐼𝑀 100(3)𝑀𝑖 𝑇Mf TIM to DM (%), 100where IM is the rate of mineral matter comparedMf is the mass of the crucible and sample (3)Mi Tafter calcination (g), Mi is the mass of the crucible and dry sample before calcination (g), T is theemptyIMcrucibletare of(g).mineral matter compared to DM (%), Mf is the mass of the crucible and samplewhereis the rateThe lipid contentdeterminedbycrucibleoil extractionof sampleswith theSoxhlet accordingto theafter calcination(g), Miwasis themass of theand drysample beforecalcination(g), T is theorganicsolventandthedurationofthecrucible tare (g).extractionoperationh. After this operation,the solventwas removedbySoxhletevaporationand theThe lipidcontentwaswas8 determinedby oil extractionof sampleswith theaccordingto theoil was driedin an byoven.methoddescribedUICPA [10]. Hexane was used as the organic solvent and the duration of theThe lipid content(h)wasin percentageis expressedaccordingto the formula:extractionoperation8 h. After drythis matteroperation,the solventwas removedby evaporation and the oilwas dried in an oven.H ((m1 m0)/m1) * 100 * 100/DMC(4)The lipid content (h) in percentage dry matter is expressed according to the formula:where m1 is the mass of the flask containing the fat after steaming, m0 is the mass of the empty balloon.H ((m1 m0 )/m1 ) * 100 * 100/DMC(4)2.3. Neem Oil Extractionwhere m1 is the mass of the flask containing the fat after steaming, m0 is the mass of the empty balloon.The mechanical extraction method is carried out with hot water after grinding almonds to a finegrain size. The almonds were previously crushed using a CORONA Moulinex and the groundmaterial obtained was sieved using a sieve of 2 mm mesh size. A few drops of hot water at 60 to 70 C were added to the grind while stirring vigorously until a black color was obtained which was
Biomolecules 2020, 10, 6164 of 102.3. Neem Oil ExtractionThe mechanical extraction method is carried out with hot water after grinding almonds to a finegrain size. The almonds were previously crushed using a CORONA Moulinex and the ground materialobtained was sieved using a sieve of 2 mm mesh size. A few drops of hot water at 60 to 70 C wereadded to the grind while stirring vigorously until a black color was obtained which was followed by asqueezing operation to separate the oil from the cake. The oil extraction rate was determined by theratio of the amount of oil collected by the oil content of the almond milling sample introduced into theextraction unit.2.4. Physicochemical Characterization of Extracted Neem OilThe iodine value (II ) which indicates the degree of unsaturation of the fatty acids in the oil wasdetermined by the Wijs reagent method described by UICPA [10].The iodine number was calculated through the relation:II 12.69 T (VO V1 )/m(5)In Equation (5), VO is the volume of 0.1 N thiosulfate solution used for the blank test, V1 is thevolume of the thiosulfate solution used for the sample, T is the exact title of the thiosulfate solution,m is the mass in g of the test sample.The saponification value (IS ) is the number of milligrams of KOH (Potassium hydroxide) neededto saponify 1 g of fat [10]. It is determined using the colored indicator (phenolphthalein) according tothe method described by [10]. The saponification value (IS ) was calculated according to the formula:IS 56.1 N (Vo V1)/m(6)where 56.1 is the molecular weight of KOH, N is the normality of the HCl solution, m is the mass in gof the test sample, Vo is the volume of HCl used for the blank test, V1 is the volume of HCl used forthe test portion.The acid value (IA ) is the number of milligrams of potassium hydroxide required to neutralizethe free fatty acids present in 1 g of material [10]. It was determined using the colored indicator(phenolphthalein) according to the method described by UICPA [10] as:IA 56.1 NKOH (V0 V1)/m(7)where V0 is the volume of the standard KOH solution used for the blank test, V1 is the volume of thestandard solution of KOH used for the sample, NKOH is the normality of the KOH solution, m is themass in grams of the test sample, 56.1 is the molar mass of KOH.The peroxide value (IP ) was determined by the colored indicator method using starch paste as acolored indicator [10].The peroxide value expressed in milliequivalents of active oxygen per kg of fat is given by:IP 1000 N (V0 V1) / m(8)In Equation (8), M is the mass in g of the test sample, Vo is the volume of the thiosulfate solutionused for the blank test, V1 is the volume of the thiosulfate solution used for the sample, N is the exactnormality of the sodium thiosulfate solution used.The lower calorific value (PCI) was determined by calculation using the saponification value andiodine value according to the empirical relationship of Haidara [11] reported by Faye [2] as:PCI 11,380 II 9.15 * IS(9)
Biomolecules 2020, 10, 6165 of 10The viscosity is evaluated at 40 C using a type C Haake viscometer. The density of the oil sampleswas determined according to the AFNOR standard [9] at 25 C by the weighing method and calculatedaccording to the following formula:d m/meau(10)where d is the oil density, m is the oil mass (g), and meau is the mass of the same volume of water (g).2.5. TransesterificationIt is an ethanolysis reaction of esters, also called triglycerides, contained in neem oil in the presenceof a basic catalyst, the NaOH in this case, at a moderate temperature, that leads to the formation ofBiomolecules 2019, 9, x FOR PEER REVIEWglyceroland ethyl monoesters. It is materialized according to the reaction illustrated in Figure 2.5 of 10Biomolecules 2019, 9, x FOR PEER REVIEW5 of 10FigureFigure 2.2. tionprincipleprinciple[12].[12].The reaction conditions and parameters are optimally set based on literature results in order toThe reaction conditions and parameters are optimally set based on literature results in order toFigureoil2. Transesterificationreaction principleinvestigate the potential of neemfor biodiesel production.This[12].synthesis was carried out usinginvestigate the potential of neem oil for biodiesel production. This synthesis was carried out usingNaOH as a catalyst at 1% of the neem oil mass, an ethanol/oil molar ratio of 6:1. The temperature ofNaOH asThea catalyst1% of theneemoil mass,ethanol/oilmolarof 6:1.The eanoptimallyset basedonratioliteratureresultsorder tothe reaction was set at 70 C, at atmospheric pressure and with mechanical stirring for four hours ofinvestigatethesetpotentialof atneemoil for biodieselproduction.Thissynthesis wascarriedusingthe reactionwasat 70 C,atmosphericpressureand withmechanicalstirringforoutfourhours ofthe reaction time. The mass yield of the reaction was calculated according to Equation (11).NaOH astime.a catalystat 1% yieldof the ofneemmass, anethanol/oilmolarratio of 6:1.The temperaturethe reactionThe masstheoilreactionwascalculatedaccordingto Equation(11). ofthe reaction was set at 70 C, at atmospheric pressure and with mechanical stirring for four hours ofRR (m/m(11)(mbwasb/m) 100 according to Equation (11).(11)hh)calculatedthe reaction time. The mass yield of the biodiesel(g),(g),mmh isis(11)theneemneemR yield yield(mb/mh) 100In(%),mmbbisisthethehoilmass(g).oil mass (g).In the above equation, R is the reaction yield (%), mb is the mass of biodiesel (g), mh is the neemAtmasstheendendof thethe reaction,reaction, thethe ethylethyl esterester (biodiesel)(biodiesel) isis separatedseparated fromfromthethe glycerolglycerolandand thethe otherotherAttheoil(g).ofby-productsofendthe ofreaction,by elsfor and24 hhtheasothershown ininAt thethe reaction,the ethylester (biodiesel)separatedfromfunnelsthe gseparatingfor24asshown ieselatatemperatureof90 singtheseparatingfunnelsfor24hasshowninFigure 3. The excess ethanol was distilled off from the biodiesel at a temperature of 90 C. The biodieselFigure3. Theexcessethanolwas distilledfromtheat soap,a temperatureof 90 C. esofbiodieselcatalyst,etc.)withby hotwashingwith lyst,soap,etc.) bywashingwaterat 60 esofcatalyst,soap,etc.)bywashingwithhotwater at 60followedby statich (FigureThe fromresidualfromthe washingfollowedby Cstaticdecantationfordecantation24 h (Figurefor3). 24Theresidual3).waterthe waterwashingoperationwaswater at60 Cfollowedbydryingstatic decantationfor 24hsteaming(Figure 3).atTheresidualwaterfrom the washingoperationwasremovedbythebiodieselby140 Cfor20min. removed by drying the biodiesel by steaming at 140 C for 20 min.operation was removed by drying the biodiesel by steaming at 140 C for 20 min.Reaction products separationReaction products separationBiodiesel washingWashing water purgePure biodieselBiodiesel washingWashing water purgeFigure3. Illustrationofofbiodieselbiodiesel separationseparation andoperations.Figure3. Pure biodieselFigure 3. Illustration of biodiesel separation and purification operations.2.6. Physicochemical Characterization of Biodiesel2.6. Physicochemical Characterization of BiodieselThe characterization of the biodiesel produced consisted of determining its intrinsic propertiesThecharacterizationof thebiodieselproduced consistedof determiningits intrinsicpropertiesasfuelsand then comparingthemto the physicochemicalcharacteristicsof neem crudeoil as wellasthoseof thenpetrodieselfixedthemby internationalstandards. Thesephysicochemicalcharacteristics,as fuelsandcomparingto the physicochemicalcharacteristicsof neemcrude oil as inwell as
Biomolecules 2020, 10, 6166 of 102.6. Physicochemical Characterization of BiodieselThe characterization of the biodiesel produced consisted of determining its intrinsic properties asfuels and then comparing them to the physicochemical characteristics of neem crude oil as well as thoseof petrodiesel fixed by international standards. These physicochemical characteristics, in particular thedensity, the viscosity, the calorific value, and the acid value, have been determined according to thesame method and under the same conditions as those of the physicochemical characterization of thecrude neem oil.The statistical analysis of all the data in this study were recorded in an Excel spreadsheet usingMicrosoft Office software version 2013 and the results are expressed as average standard deviation.The variation in the data collected and the statistical significance of the treatment effect were analyzedby analysis of variance. Statistical differences with a probability value less than 0.05 (p 0.05) areconsidered significant. When the probability is greater than 0.05 (p 0.05) the statistical differences arenot significant.3. Results and Discussions3.1. Variability of Physicochemical Characteristics of Neem SeedsCovered with a thin skin, the neem fruit consists of a pulp containing seeds with one to threealmonds depending on the seed size considered. The physicochemical characteristics of the studiedseed samples presented in Table 1 vary according to their origin.Table 1. Physicochemical characteristics of neem seeds studied compared to those of Senegaleseneem seeds.Neem Seeds from This StudyCharacteristics of SeedsMoisture content (%)Average mass for 200 seeds (g)Almond content (%)Hull content (%)Pulp and skin content (%)MarouaZidim9.533 0.089 a128.000 0.133 a34.050 0.067 a17.317 0.156 b48.617 0.089 b9.470 0.049 a141.367 0.178 b40.700 0.076 b14.817 0.165 a44.467 0.056 aNeem Seeds 48.03-Superscript letters indicate that statistical analysis doing by ANOVA, numbers with the same superscript letters onthe same line indicate that these values are not significantly different at p 5%.An analysis of the results indicate that samples of neem seeds from the Zidim locality have betterphysical properties compared to those collected in Maroua town. With a mass average of 200 seedsevaluated at 141.36 g and an almond content of 40.70%, these characteristics are significantly highercompared to the samples collected at Maroua, evaluated at 128.00 g and 34.05% for the mass averageof 200 seeds and the almond content, respectively. These seeds have almond contents slightly lowerthan that of the Senegalese neem seeds studied by Faye in 2010, which ranged from 51.97% to 52.32%depending on the origin of the samples [2]. This variability of characteristics could be explained notonly by the variation in climatic conditions including temperature and rainfall [12], but mainly by thediversity of the type of soil and the genotype of the trees. In addition, the seeds studied have a pulpand skin content slightly higher than that of the kernel with rates estimated on average at 48.61% and44.46% for the samples of neem seeds from Maroua and Zidim, respectively.Table 2 presents the centesimal distribution of the main constituents of the neem seeds studied.It can be seen from Table 2 that the kernel concentrates most of the lipid reserves of the seed and itslipid content varies according to the seed’s origin. These rates are estimated on average at 53.97% and56.74% for samples from Maroua and Zidim, respectively. This means that the sample from Zidimis 2.77% more than the one from Maroua. Difference can be mainly explicated by harvest periodand climatic, edaphic influence. These results are slightly higher than those obtained by Sagoua [13]and Nitièma [1] who evaluated lipid contents of almonds at 50% and 45.1%, respectively. However,
Biomolecules 2020, 10, 6167 of 10this content is much closer to that of Senegalese neem seed kernels, which is about 55.95 to 58.38%depending on the origin of the samples [2]. A similar study in India also indicates that neem seedshave an oil content of between 40% and 60% [4]. In addition, the kernel also has a slightly higherdry matter content compared to that of the hull and that of pulp and hides. However, the essentialmineral matter of the seeds (4.4%) is evenly distributed between the hull (2.0%) and the almond (2.0%),which confirms the results of Faye [2].Table 2. Percentage distribution of the main constituent elements of neem seeds.Whole seedCharacteristicsAlmondShellPulp and y Matter (%)90.467 0.08990.530 0.04996.467 0.17796.333 0.04493.235 0.32693.333 0.41791.155 0.03191.217 0.046Mineral Matter (%)4.422 0.0044.457 0.0492.073 0.0042.076 0.0022.050 0.0182.027 0.0220.609 0.0140.631 0.011Lipid (%)31.926 0.14732.764 0.36753.978 0.51756.749 0.357----3.2. Physicochemical Characteristics of Neem OilWith a strong odor and a very bitter taste, the physicochemical characteristics of the neem oilvary slightly with the provenance of the samples. The main physicochemical properties of the samplesstudied compared to other oils are summarized in Table 3.Table 3. Physicochemical characteristics of the neem oils studied compared to those of other oils.PhysicochemicalCharacteristics of OilsNeem Oil, this StudyMarouaZidimNeemOil [2]NeemOil [14]NeemOil [15]JatrophaOil [16]Iodine value (mg I2 /100 g)74.448 0.56473.814 0.36675.9365–80-89–95Saponification value (mg/g)200.090 1.247199.810 1.584199.17175–20-196–208Acide value (mg/g)8.976 0.6109.163 0.8207.93-28.641.8–2.5Peroxyde value (meq/Kg)6.433 0.1516.900 0.3006.00---Lower Calorific value (MJ/Kg)39.64239.66539.6332–4039.501-Density at 25 C0.833 0.0120.850 0.0140.860.912–0.9650.930.895–0.902Kinematic Viscosity at 40 C (cSt)26.34 1.3626.67 1.57-20.5–48.540.7512-Table 3 shows that the physicochemical properties of the studied neem oil samples vary very littleaccording to the provenance of the samples. The acid value, one of the intrinsic characteristics of the oil,which strongly influences the transesterification yield, is evaluated on average at 8.97 and 9.16 mg/g.These values are relatively high compared to those of other oils such as jatropha and sunflower, whoseaverage range from 1.8 to 2.5 mg/g [16] and from 1.56 to 1.88 mg/g [17], respectively. Moreover, the acidnumber values of the samples studied are in contradiction with those of Banik et al. [16] who alsoconducted a similar study on neem seed oil and reported an acid value of 28.6 mg/g. The density,evaluated on average at 0.833 and 0.850 for the Maroua and Zidim samples, respectively, were in linewith the results reported by Banik et al. [14] in 2018, who also conducted a similar study on neemseed oil. The density results were lower than those of the neem oil obtained by some other authorswhich varied between 0.912 and 0.965 [3,15]. However, the results are closer to that of Senegaleseneem seeds studied by Faye [2] with an average value of 0.864. The kinematic viscosity of our oilsamples, evaluated on average at 26.34 and 26.67 cSt for Maroua and Zidim, respectively, confirmsthe results of Sekhar et al. [14], who obtained values between 20.5 and 48.5. Moreover, the calorificvalues of the samples are close to those of the neem oils found in the literature varying between 32 and40 MJ/kg [17]. The saponification values are comparable to those of the jatropha
Biomolecules 2020, 10, 616 3 of 10 Biomolecules 2019, 9, x FOR PEER REVIEW 3 of 10 Almonds Simple hulls Hulls with pulp and hides Figure 1. Images of the seed pretreatment operation. 2.2. Physicochemical Characterization of Neem Seeds The almond and shell contents were
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