Industrial Crops and Products 58 (2014) 188193Contents lists available at ScienceDirectIndustrialCropsandProductsj our nal homepage: www. el sevi er . com/ l ocat e/ i ndcr opModulationofpomegranatepeelcolourantcharacteristicsfortextiledyeingusinghighenergyradiationsMuhammadAjmala,ShahidAdeelb,MuhammadAzeema,MuhammadZuberc,NasimAkhtard,NaeemIqbala,aDepartment of Botany, Govt. College University, 38000 Faisalabad, PakistanbDepartment of Chemistry, Govt. College University, 38000 Faisalabad, PakistancDepartment of Applied Chemistry and Biochemistry, Govt. College University, 38000 Faisalabad, PakistandNuclear Institute for Agriculture and Biology, Jhang Road, Faisalabad, Pakistanarticl einfoArticle history:Received 31 January 2014Received in revised form26 March 2014Accepted 12 April 2014Keywords:IrradiationMordantingPomegranate peelsSilk dyeingSpectraashabstractThepresentstudywasconcernedwithextractionofnaturalcolourantsfrompomegranate(Punicagrana-tumL.)rindpowderandcharacterizationofextracteddyeundertheinuenceofgammaradiations.Bothdyeingpowderandsilkfabricwereexposedtodifferentabsorbeddoses(20,25,30, 35and40kGy)ofhighenergyradiationsusingCs-137gammairradiator.Aqueous,alkaliandalcoholsolubilizedextractswereobtainedfromun-irradiatedandirradiatedpomegranaterindpowders.Aluminium,copper,chromiumandtannicacid(210%each)wereemployedtoimprovecolourstrengthofextracteddye.Exposureofpomegranatepeelcolourantandsilkfabrictogammaradiationgreatlyimprovedtheextractionanddye-ingprocessby reducingmaterialtoliquorratio,dyeingtime,dyeingtemperatureandsaltconcentration.Gammaraytreatmentsalsohadstronginuenceon colourstrengthandfastnesscharacteristicsofsilkfabricsdyedwithirradiatedpomegranatepeel.Gammaraytreatmentof40kGywasthemosteffectivedoseforcolourantextractionfrom pomegranatepeel andsurfacemodicationofsilkfabric.Thegoodcolourstrengthwasobtainedby dyeingsilkwith pomegranatepeel fabricsat50C for40min,keepingdyebathpH at6.0withsaltconcentrationof10g/L.Theresultfrommordantingexperimentsindicatedthat10%ofaluminiumaspre-mordantand10%oftannicacidas post-mordantwerethebesttoenhancecolourstrengthofextracteddye.It wasalsoobservedthatgammaray treatedpomegranaterindhadagoodpotentialtoalternateyellowandgoldensyntheticdyesintextileindustry. 2014ElsevierB.V.Allrightsreserved.1. IntroductionThe revival of interest towards the use of natural colourants intextile is attributed to the increased awareness about environmen-tal contamination created by intermediates and chemicals beingused in synthetic dyeing process (Panidian et al., 2011; Shahidet al., 2013). The natural colourants are considered as non carcino-genic, easily biodegradable and non toxic for human health (Daset al., 2011; Ghoulia et al., 2012). Considering energy saving andenvironmental safety, natural dyes have attracted the attention ofresearchers and industrialists to be used in textiles and other alliedindustries (Khan et al., 2014; Tutak and Benli, 2012). Moreover,plants based natural dyes also exhibit antimicrobial, antioxidantCorresponding author. Tel.: +92 41 9201488; fax: +92 41 9201032.E-mail addresses: shahidadeelchemist@gmail.com(S. Adeel),naeemgc@yahoo.com, naeemiqbaluaf@yahoo.com(N. Iqbal).andanticarcinogenic activities (Kulkarni andAradhya, 2005; Anwaret al., 2009; Riaz et al., 2002), which make these ideal to be used inthe textile and other related industries.A lot of techniques are being used to improve dyeing behaviourof natural dyes and modication of fabric either by improvingextraction process or by enhancing dye uptake activity of fab-ric to get good shades and fastness properties. These techniquesmayinclude, colour isolation on fabrics (Ali et al., 2010), biopol-ishing (Mehmood and Liakopoulou, 2010; Vankar et al., 2007),bioscouring of fabrics (Malik et al., 2005; Niaz et al., 2010), cation-ization (Guesmi et al., 2011), mercerization of fabric (Bhatti et al.,2012a), Chitosan treatment (Dev et al., 2009), enzyme treatment(Kan et al., 2010), ultrasonic treatments (Kamel et al., 2005; Kumaret al., 2007), UV exposures (Adeel et al., 2012; Bhatti et al.,2012b) and microwave treatments (Sinha et al., 2011; Kale andBhat, 2011). In addition, plasma treatment is also used as a pre-treatment to improve the absorption of natural dyes to textiles(Haji and Shoushtari, 2011; Haji, 2013; Haji et al., 2014). Recenthttp://dx.doi.org/10.1016/j.indcrop.2014.04.0260926-6690/ 2014 Elsevier B.V. All rights reserved.M.Ajmal et al. / Industrial Crops and Products 58 (2014) 188193 189studies have clearly indicated that gammaray treatment is alsovery effective in improving dye extraction and colour strength andfastness properties of natural colourants (Adeel et al., 2009; Batoolet al., 2013; Khan et al., 2014). Gammaray treatment has beenused in wastewater treatments (Tackacs et al., 2001), dye degrada-tion (Wojnarovits et al., 2010) and surface modication of cottonthrough alkali treatment or combined processes (Foldvary et al.,2003; Tackacs et al., 2001). This widespread use in textile is due tohigh treatment speed, cheap and energy saving characteristics ofgammaradiations (Ferrero and Monica, 2011).Pomegranate (Punica granatum L.), a native of Persia belongingto the family Punicacea is generally cultivated in warm countriesof the world. The rind of pomegranate is composed of tannin andabout 19% of pelletierine (Tiwari et al., 2010). The abundant colour-ing pigment in the Punica granatum L. is granatonine, the alkaloidform (Goodarzian and Ekrami, 2010). Pomegranate peel is gener-allyconsideredoneof theoldest sources of natural colourants. It hasanti-carcinogenic characteristics andcontains antioxidants (Lanskyand Newman, 2006; Kolkarni et al., 2005). The peels are also richsource of vitamin C and act as effective moisturizer with a lot ofother medicinal importance (Goodzarine and Ekrami, 2010). Keep-inginviewthebenecial effects of applicationof gammaradiations,we have conducted the study with the objective to improve extrac-tionof colourant frompomegranatepeels andtoenhancethecolourstrength of dyed silk fabric through its surface modication usinghigh energy radiations.2. Materials and methods2.1. Sample preparationPomegranate (Punica granatum L.) peels were collected fromlocal fresh fruit juice sellers. The pomegranate rinds were washedand dried at roomtemperature and ground nely up to 20 meshesne powder. Plain woven gummed commercial silk fabric wasobtained from local textile market of Faisalabad. To remove fats,oils and other impurities, the fabric was degummed by boilingusing soap solution as documented by Clark (2011). All the chemi-cals used in extraction, dyeing and mordanting were of commercialgrades.2.2. Extraction and irradiation processSilk fabrics and pomegranate rind powder were exposed toabsorbed doses of 20, 25, 30, 35 and 40kGy using Cs-137 gammairradiator at Nuclear Institute of Agriculture and Biology (NIAB),Faisalabad, Pakistan (Batool et al., 2013). Aqueous (heat solubi-lized), alkaline (alkali solubilized) andalcoholic solubilizedextractswere obtained by boiling irradiated and un-irradiated powder(RP/NRP) for different time intervals with varying material liquor(M:L) ratios (Prusty et al., 2009). After dyeing, samples were eval-uated for colour strength (%) characteristics at Quality ControlLaboratory of Noor Fatima Ltd, Faisalabad, Pakistan.2.3. Optimization of dyeing parametersThe irradiated (RS) and un-irradiated (NRS) silk fabrics weretreated with extracts of pomegranate peel to optimize dyeing con-ditions. To observe the effects of temperature on dyeing, the silkfabrics were dyedat 30, 40, 50, 60 and70Cfor one hour. Inanotherexperiment, optimal extracts were employed for 30, 40, 50, 60and 70minto optimize dyeing time using dye baths of differentpH values (512) (Amoudi and Osmon, 2009). To achieve maxi-mum exhaustion of dye onto optimal fabric, 4, 6, 8, 10 and 12g/Lof Glauber,s salt was employed. Extract concentrations were alsooptimized by employing different materials to liquid ratios(1:301:70) (Lee et al., 2008).2.4. Optimization of mordanting conditionFor improving colour strength and fastness properties, 4, 6, 8and 10% of each of aluminium, chrome, copper sulphate and tannicacid were used as pre- and post-mordants at 50C for 40min(Aliet al., 2010). After pre- mordanting, fabrics were dyed at optimalconditions using pomegranate peel extract. In post- mordanting,dyed fabrics were used for achieving good tinctorial strength andfastness properties.2.5. Evaluation of quality characteristics of dyes and fabricsAll the dyed fabrics were subjected to standard ISO methodsto observe the effect of gammaray treatment in improving colourfastness properties. For the purpose, different methods such as, ISO105 CO3 for washing using rota wash, ISO105x12 for rubbing usingcrock metre and ISO BO2 for light using fado metre was employed.All the samples were subjectedtoCIELabsystemusingspectra ashspectrophotometer SF 650 with an illuminant of D65 10 observerfor evaluation of colour strength (%) (Kumaresan et al., 2012).3. Results and discussionThe results of the study clearly indicated that alkali solubilizedextracts obtainedfromirradiatedpowder of pomegranate peel (RP)produced more darker and deeper shades on to irradiated fabric(RS). Fig. 1(b) indicates that gammaray treatment of powder stim-ulated the solubilization of pomegranate in alkaline media. Hence,after irradiation, more colourant was extracted frompeel and upondyeing shared more sorption onto treated fabric. While, in aqueousmedia, other impurities got maximum chance to sorb onto fabricowing to insolubility of colourant in water. This caused either fab-ric dyeing unevenness or gives less colour depth (Fig. 1(a)). The lesstinctorial strength of the dye extracted in alcoholic media showedthat some other materials such as, waxes and anthocyanin mightalso be extracted along with the colourant, which upon dyeingshowed less tinctorial strength as shown in Fig. 1(c). Hence, max-imum dye was extracted from gammaray treated pomegranatepeel, particularly irradiated with 40kGy of high energy radiations.Considering the surface modication of silk fabric to gammaray treatments, low absorbed dose did not activate the surfaceto sorb colourant. Similarly, higher than 40kGy absorbed doses ofgammarays were not helpful in surface modications of silk fab-rics to sorb more colourant frompomegranate peel. This behaviourcould be explained by the fact that silk fabrics treated with higherdoses of gammarays had caused weight loss (Machnowski et al.,2013; Xiong et al., 2011), which upon dyeing showed less tinctorialstrength. Such dyed fabrics during investigations in spectra ashshowed less colour strength as reported by Xue and Jin-Xin (2011).Hence gammaray treatment through surface modication givesgood colour strength using extracts of irradiated powder.Dyeing conditions optimization experiments indicated that50C was the optimal temperature for dyeing of irradiated silk (RS,40kGy) using alkali solubilized extract of irradiated pomegranaterind powder. Below that temperature, heat could not activate thedye molecule to rush towards the fabric while above that temper-ature; the colourant might had faced the hydrolytic degradation(Ansari and Thakar, 2000). In both cases the strength of actualcolourant (granotanine) weakenedandinvestigations usingspectraash showed the dull shades. At the 50C, the colourant signif-icantly sorbed onto the fabric as a single molecule evenly andshowed the darker shades. Upon investigationin spectra ash, highcolour strength was observed (Fig. 2).190 M. Ajmal et al. / Industrial Crops and Products 58 (2014) 188193Fig. 1. Effect of absorbed doses of high energy radiations on the colour strength of silk using heat solubilized (aqueous) (a), alkali solubilized (b) and alcoholic solubilized (c)extractsof irradiated and un-irradiated dye powder.The data displayed in Fig. 3 showed that dyeing of irradiated silkusingalkali solubilizedextract of irradiatedpomegranatepeel pow-der for 40mingave goodcolour strengthindicating that gammaraytreatment was time effective. Dyeing for long time (60min) causedbreak down of molecules and desorption of colourant, while dye-ing for short time (30min) might caused surface sorption (Shenai,1992). Henceat optimal time(40min) theirradiatedsilksorbs max-imum dye and gives darker shades. It is also proved that gammarays treatment is time effective as it reduces the time of dye-ing.Fig. 2. Effect of dyeing temperature onthe colour strengthof irradiatedsilk (40kGy)using alkali solubilized extract of irradiated dye powder.The dyeing media pH optimization studies showed that underalkaline conditions, fabric might have gainedthe negative potentialandrepelledthe dye towards the solution. While inmediumhavingpH below 6.0, dye rapidly gathered on to fabric. In dyeing mediawith mild pH (6.0), the dye molecules uniformly sorbed on to thefabric and provided the good colour strength. Moreover, the strongacidic conditions might favour the absorption of other associatedcomponents like galic acid onto the fabric. Hence, dyeing of silkfabric with pomegranate rind powder at pH 6.0 gave good colourstrength (Fig. 4).Fig. 3. Effect of dyeing time on the colour strength of irradiated silk (40kGy) usingalkali solubilized extract of irradiated dye powder.M.Ajmal et al. / Industrial Crops and Products 58 (2014) 188193 191Fig. 4. Effect of dyeing pH on the colour strength of irradiated silk (40kGy) usingalkali solubilized extract of irradiated dye powder.Gammaray treatment of fabric alsoreducedthe amount of pow-der used to make extract. The results indicated that 1:40 wastheoptimal material liquor ratio to get best colourant extraction, max-imumcolour strength and levelled dyeing (Fig. 5). More the liquorconcentration, the more unevenness was observed due to accumu-lation of aggregates on surface modied fabrics.Datashowedthat 10g/L of solublesalt was theoptimumamountof electrolyte to get maximum exhaustion and good colour uni-formity (Fig. 6). Addition of higher amount (greater than 10g/L)salt caused maximum exhaustion and gathering of dye moleculesin cluster onto surface modied fabrics. This rapid accumulationof aggregates onto surface caused unevenness of dyed silk fab-rics. The non-signicant contribution of dye towards silk fabricsin a medium containing less than 10g/L of salt as observed in thepresent study had also been reported by Broadbent (2001). Thusoptimumsalt concentrationfor dyeingof silkfabrics withirradiatedpomegranate peel was 10g/L of NaCl.The data displayed in Fig. 7a showed that 10% of the aluminiumwas the best mordant, produced deeper and darker shades wheninteracted with the dye. Previously, it had been reported thatdyebre interaction was due to presence of phenoxide ion of tan-nins and electron decient NH3+group of silk as well as interactionbetween hydrophobic part of dye and silk fabric (Bird, 1982). Uponinvestigation in spectraash high colour strength wasobservedcompared with bre treated with other mordants. This might bedue tothe chelatingabilityof aluminiumas well as its higher chargeFig. 5. Effect of extract concentration (M:L) on the colour strength of irradiated silk(40kGy)using alkali solubilized extract of irradiated dye powder.Fig. 6. Effect of salt concentration on the colour strength of irradiated silk (40kGy)using alkali solubilized extract of irradiated dye powder.than copper, chromiumand tannic acid (Amoudi and Osman, 2009;Haque et al., 2013). The results indicated that the behaviour inpost-mordanting was reversed, where 10% of tannic acid producedbetter effects on colour strength and fastness of the dyed fabric(Fig. 7b). Hence for achieving good colour strength and fastnessproperties, 10% of aluminium as pre-mordant and 10% of tannicacid as post-mordant were optimal conditions.The rating results of dyed silk fabrics given in Tables 1 and 2showed that gammaray treatment improved the colour fastnessof the fabric dyed with pomegranate rind powder. This might bedue to the presence of conjugated systemand benzene ring in thedye molecules. After mordanting due to metal dye complex, therm bonding showed great resistance to detach when exposed toagents such as light, heat and detergents (Naz et al., 2011). Goodcolour fastness properties can also be due to photochromic effector phototropic behaviour, dye particle size as well as successfulnucleophilic reaction of dye with modied fabrics before and aftermordanting. When such well interacted dyed fabric is exposed toTable 1Effect of gammaradiation on colour fastness properties of pre-mordanted silk fabricdyed at optimal conditions.MordantingconditionsMordantconcentration(%)WashfastnessDryrubbingfastnessWetrubbingfastnessLightfastnessAluminiumControl 23 3 3 2323 3 4 4434 3 4 464 3 4 484 3 4 410 4 3 34 45ChromeControl 23 3 3 2323 3 4 443 3 4 464 3 4 484 3 34 410 4 3 4 45CopperControl 23 3 3 2324 3 4 444 3 4 463 3 4 584 3 34 410 4 3 4 4TannicacidControl 23 3 3 2324 3 4 444 3 4 464 3 4 584 3 4 410 4 3 34 45192 M. Ajmal et al. / Industrial Crops and Products 58 (2014) 188193Fig. 7. Effect of pre-mordanting (a) and post-mordanting (b) on colour strength of Irradiated silk (40kGy) using alkali solubilized extract of irradiated dye powder.Table 2Effect of gamma radiationoncolour fastness properties of post mordantedsilk fabricdyed at optimal conditions.MordantingagentsMordantconcentration(%)WashingfastnessDryrubbingfastnessWetrubbingfastnessLightfastnessAluminiumControl 23 3 3 234 4 3 4 46 4 3 4 48 4 34 4 410 4 34 4 4ChromeControl 4 3 4 454 4 3 4 46 4 3 4 58 4 34 4 410 4 34 4 4CopperControl 4 3 4 44 4 3 4 46 4 3 4 58 4 3 4 410 4 3 4 4TannicacidControl 4 3 4 44 4 3 4 46 4 3 4 58 4 3 4 410 4 3 4 45agencies (heat, light, detergents and rubbing), show more resis-tance to detach. Thus gammaray treatment of silk fabric followedby mordanting and dyeing at optimal conditions enhanced colourfastness properties frompoor to good.4. ConclusionIt can be concluded frompresent research work that,1) Pomegranate (Punica granatum L.) peels are suitable source ofcolourant for textile industry.2) Gammaray treatment of 40kGy is an effective dose for improv-ing extraction of natural colourants frompomegranate peel andenhancing silk fabric dye uptake ability by dyeing at 50C for40minusing dye bath of pH 6.0.3) Aluminium (10%) is the best as compare with copper, chromeand tannic acid for pre mordanting agent to improve colourstrength of pomegranate peel extracts.4) Tannic acid (10%) is the best as compare with copper, chromeand aluminiumfor post mordanting to improve colour strengthof pomegranate peel extracts.5) The colour fastness to light, washing and rubbing has beenimproved by dyeing irradiated silk fabrics (40kGy treated) atoptimal conditions of mordanting.ReferencesAdeel, S., Ali, S., Bhatti, I.A., Zsila, F., 2009. Dyeing of cotton fabric using pomegranate(Punica granatum) aqqueous extract. Asian J. 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