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Ukwandiswa kwe-shale kwiindawo zokugcina amanzi ezidala iingxaki ezinkulu, nto leyo ekhokelela ekungazinzini kwe-wellbore. Ngenxa yezizathu zokusingqongileyo, ukusetyenziswa kolwelo lokumba olusekelwe emanzini olune-shale inhibitors eyongezelelweyo kukhethwa kune-oyile-based drilling fluid. Ii-Ionic liquids (ILs) zitsale ingqalelo enkulu njenge-shale inhibitors ngenxa yeempawu zazo eziguquguqukayo kunye neempawu ezinamandla ze-electrostatic. Nangona kunjalo, ii-ionic liquids (ILs) ezisekelwe kwi-imidazolyl, ezisetyenziswa kakhulu kwi-drilling fluids, ziye zabonakala zinobuthi, aziboli kwaye zibiza kakhulu. Ii-Deep eutectic solvents (DES) zithathwa njengenye indlela engabizi kakhulu kwaye engenabuthi kakhulu kunee-ionic liquids, kodwa zisasilela ekuzinzeni kwendalo okufunekayo. Inkqubela phambili yakutshanje kweli candelo ikhokelele ekungenisweni kwe-deep eutectic solvents yendalo (NADES), eyaziwa ngokuba nobuhlobo bokwenyani nokusingqongileyo. Olu phononongo luphande ii-NADES, eziqulethe i-citric acid (njenge-hydrogen bond acceptor) kunye ne-glycerol (njengomnikeli we-hydrogen bond) njengezongezo zolwelo lokumba. Ulwelo lokugrumba olusekelwe kwi-NADES lwenziwe ngokuhambelana ne-API 13B-1 kwaye ukusebenza kwalo kuthelekiswa nolwelo lokugrumba olusekelwe kwi-potassium chloride, ulwelo lwe-ionic olusekelwe kwi-imidazolium, kunye nolwelo lokugrumba olusekelwe kwi-choline chloride:urea-DES. Iipropati ze-physicochemical ze-NADES ezizimeleyo zichazwe ngokweenkcukacha. Iipropati ze-rheological, ukulahleka kolwelo, kunye neepropati zokuthintela i-shale yolwelo lokugrumba zivavanyiwe ngexesha lophando, kwaye kwaboniswa ukuba kwi-concentration ye-3% NADESs, umlinganiselo woxinzelelo lwe-yield/plastic viscosity (YP/PV) wonyusiwe, ubukhulu be-mud cake buncitshisiwe ngama-26%, kwaye umthamo we-filtrate wehlisiwe ngama-30.1%. Okuphawulekayo kukuba, i-NADES ifumene izinga lokuthintela ukwanda elimangalisayo lama-49.14% kwaye yandisa imveliso ye-shale ngama-86.36%. Ezi ziphumo zibangelwa kubuchule be-NADES bokutshintsha umsebenzi womphezulu, amandla e-zeta, kunye nomgama phakathi kwe-clays, ezixoxwa kweli phepha ukuqonda iindlela ezisisiseko. Olu lwelo lokugrumba oluzinzileyo kulindeleke ukuba lutshintshe ishishini lokugrumba ngokubonelela ngenye indlela engenabungozi, engabizi kakhulu, nesebenza kakhulu endaweni yezithinteli zokugrumba ze-shale zemveli, nto leyo evula indlela yeendlela zokugrumba ezinobuhlobo nokusingqongileyo.
I-Shale lilitye elinokuguquguquka elisebenza njengomthombo kunye nomthombo wee-hydrocarbons, kwaye ulwakhiwo lwayo olunemingxuma1 lubonelela ngamathuba okuvelisa kunye nokugcina ezi zixhobo zixabisekileyo. Nangona kunjalo, i-shale ityebile kwiiminerali zodongwe ezifana ne-montmorillonite, i-smectite, i-kaolinite kunye ne-illite, ezenza ukuba idumbe xa ivezwa emanzini, nto leyo ekhokelela ekungazinzini kwe-wellbore ngexesha lemisebenzi yokugrumba2,3. Ezi ngxaki zinokukhokelela kwixesha elingasebenziyo (i-NPT) kunye neengxaki ezininzi zokusebenza kubandakanya imibhobho ebambekileyo, ukulahleka kokujikeleza kodaka, ukudilika kwe-wellbore kunye nokungcola kweebhithi, okwandisa ixesha lokubuyisela kunye neendleko. Ngokwesiko, ii-oil-based drilling fluids (OBDF) bezilukhetho olukhethwayo kwi-shale formations ngenxa yokukwazi kwazo ukumelana nokwanda kwe-shale4. Nangona kunjalo, ukusetyenziswa kwee-oil-based drilling fluids kubandakanya iindleko eziphezulu kunye nemingcipheko yokusingqongileyo. Ii-synthetic-based drilling fluids (SBDF) ziye zathathwa njengenye indlela, kodwa ukufaneleka kwazo kumaqondo obushushu aphezulu akwanelisi. Ulwelo lokubhola olusekelwe emanzini (i-WBDF) lusisombululo esinomtsalane kuba lukhuselekile, lunobuhlobo nokusingqongileyo, kwaye lunexabiso eliphantsi kune-OBDF5. Ii-shale inhibitors ezahlukeneyo zisetyenzisiwe ukuphucula amandla okuthintela i-shale ye-WBDF, kubandakanya ii-inhibitors zendabuko ezifana ne-potassium chloride, ilayimu, i-silicate, kunye ne-polymer. Nangona kunjalo, ezi zithinteli zinemida malunga nokusebenza kakuhle kunye nempembelelo yokusingqongileyo, ngakumbi ngenxa yoxinzelelo oluphezulu lwe-K+ kwii-inhibitors ze-potassium chloride kunye novakalelo lwe-pH lwee-silicates. 6 Abaphandi bahlolisise amathuba okusebenzisa ii-ionic liquids njengezongezo zolwelo lokubhola ukuphucula i-rheology yolwelo lokubhola kunye nokuthintela ukudumba kwe-shale kunye nokwakheka kwe-hydrate. Nangona kunjalo, ezi zi-ionic liquids, ngakumbi ezo ziqulethe ii-imidazolyl cations, ngokubanzi ziyingozi, zibiza kakhulu, aziboli, kwaye zifuna iinkqubo zokulungiselela ezinzima. Ukusombulula ezi ngxaki, abantu baqala ukukhangela enye indlela engabizi kakhulu nenobuhlobo nokusingqongileyo, eyakhokelela ekuveleni kwe-deep eutectic solvents (DES). I-DES ngumxube we-eutectic owenziwe ngumnikeli we-hydrogen bond (HBD) kunye ne-hydrogen bond acceptor (HBA) kwi-molar ratio kunye nobushushu obuthile. Le mixube ye-eutectic ineendawo zokunyibilika eziphantsi kunezakhi zayo, ngokuyintloko ngenxa yokudilika kwetshaja okubangelwa ziibhondi ze-hydrogen. Izinto ezininzi, kubandakanya amandla e-lattice, utshintsho lwe-entropy, kunye nokusebenzisana phakathi kwee-anions kunye ne-HBD, zidlala indima ephambili ekunciphiseni i-melting point ye-DES.
Kwizifundo zangaphambili, izongezo ezahlukeneyo zongezwa kulwelo lokubhola olusekelwe emanzini ukusombulula ingxaki yokwandiswa kweshale. Umzekelo, u-Ofei nabanye bongeze i-1-butyl-3-methylimidazolium chloride (BMIM-Cl), eyanciphisa kakhulu ubukhulu bekhekhe lodaka (ukuya kuthi ga kwi-50%) kwaye yehlisa ixabiso le-YP/PV nge-11 kumaqondo obushushu ahlukeneyo. U-Huang nabanye basebenzise ulwelo lwe-ionic (ngokukodwa, i-1-hexyl-3-methylimidazolium bromide kunye ne-1,2-bis(3-hexylimidazol-1-yl)ethane bromide) ngokudibeneyo namaqhekeza e-Na-Bt kwaye yanciphisa kakhulu ukudumba kweshale nge-86.43% kunye ne-94.17%, ngokulandelelana12. Ukongeza, uYang nabanye. basebenzise i-1-vinyl-3-dodecylimidazolium bromide kunye ne-1-vinyl-3-tetradecylimidazolium bromide ukunciphisa ukudumba kwe-shale nge-16.91% kunye ne-5.81%, ngokulandelelana. 13 UYang nabanye basebenzise ne-1-vinyl-3-ethylimidazolium bromide kwaye banciphisa ukwanda kwe-shale nge-31.62% ngelixa begcina ukubuyiselwa kwe-shale kwi-40.60%. 14 Ukongeza, uLuo nabanye basebenzise i-1-octyl-3-methylimidazolium tetrafluoroborate ukunciphisa ukudumba kwe-shale nge-80%. 15, 16 UDai nabanye basebenzise ii-ionic liquid copolymers ukuthintela i-shale kwaye bafumana ukunyuka kwe-18% ekubuyiseleni okuthe ngqo xa kuthelekiswa ne-amine inhibitors. 17
Ii-ionic liquids ngokwazo zineengxaki ezithile, nto leyo eyabangela ukuba izazinzulu zifune ezinye iindlela ezinobuhlobo nokusingqongileyo endaweni yee-ionic liquids, kwaye ngaloo ndlela kwazalwa i-DES. UHanjia wayengowokuqala ukusebenzisa i-deep eutectic solvents (DES) equka i-vinyl chloride propionic acid (1:1), i-vinyl chloride 3-phenylpropionic acid (1:2), kunye ne-3-mercaptopropionic acid + itaconic acid + vinyl chloride (1:1:2), eyathintela ukudumba kwe-bentonite ngama-68%, 58%, kunye nama-58%, ngokulandelelana. Kwisilingo sasimahla, uMH Rasul wasebenzisa umlinganiselo we-2:1 we-glycerol kunye ne-potassium carbonate (DES) kwaye wanciphisa kakhulu ukudumba kweesampuli ze-shale ngama-87%19,20. UMa wasebenzisa i-urea:vinyl chloride ukunciphisa kakhulu ukwanda kwe-shale ngama-67%.21 URasul et al. Udibaniso lwe-DES kunye ne-polymer lwasetyenziswa njenge-dual-action shale inhibitor, eyafumana isiphumo esihle kakhulu sokuthintela i-shale22.
Nangona i-deep eutectic solvents (DES) ngokubanzi ithathwa njengenye indlela eluhlaza kune-ionic liquids, ikwaqulathe izinto ezinokuba yityhefu ezifana ne-ammonium salts, nto leyo eyenza ukuba i-eco-friendly yazo ithandabuzeke. Le ngxaki ikhokelele ekuphuhlisweni kwe-natural deep eutectic solvents (NADES). Zisahlulwa njenge-DES, kodwa zenziwe ngezinto zendalo kunye neetyuwa, kubandakanya i-potassium chloride (KCl), i-calcium chloride (CaCl2), i-Epsom salts (MgSO4.7H2O), kunye nezinye. Iintlanganisela ezininzi ezinokubakho ze-DES kunye ne-NADES zivula umda obanzi wophando kule ndawo kwaye kulindeleke ukuba zifumane izicelo kwiindawo ezahlukeneyo. Abaphandi abaninzi baye baphuhlisa ngempumelelo iindibaniselwano ezintsha ze-DES eziye zabonakala zisebenza kwiindlela ezahlukeneyo zokusebenza. Umzekelo, uNaser et al. 2013 wenza i-potassium carbonate-based DES kwaye wafunda iipropati zayo ze-thermophysical, ezathi kamva zafumana izicelo kwiindawo zokuthintela i-hydrate, izongezo zolwelo lokubhola, i-deignification, kunye ne-nanofibrillation. 23 UJordy Kim kunye nabanye abasebenzi baphuhlise i-NADES esekelwe kwi-ascorbic acid baza bavavanya iipropati zayo ze-antioxidant kwizicelo ezahlukeneyo. 24 UChrister nabanye baphuhlise i-NADES esekelwe kwi-citric acid baza bafumanisa amandla ayo njengomncedi weemveliso ze-collagen. 25 ULiu Yi kunye nabanye abasebenzi bashwankathele ukusetyenziswa kwe-NADES njenge-excipient kunye ne-chromatography media kuphononongo olupheleleyo, ngelixa uMisan nabanye baxoxe ngokusetyenziswa ngempumelelo kwe-NADES kwicandelo lokutya kwezolimo. Kubalulekile ukuba abaphandi bolwelo lokumba baqale ukunaka ukusebenza kwe-NADES kwizicelo zabo. kutshanje. Ngo-2023, uRasul nabanye basebenzise indibaniselwano eyahlukeneyo ye-deep eutectic solvents yendalo esekelwe kwi-ascorbic acid26, i-calcium chloride27, i-potassium chloride28 kunye ne-Epsom salt29 kwaye bafezekisa ukuthintela kwe-shale okumangalisayo kunye nokubuyiselwa kwe-shale. Olu phononongo lolunye lwezifundo zokuqala zokwazisa i-NADES (ingakumbi i-citric acid kunye ne-glycerol-based formulation) njenge-shale inhibitor enobuhlobo nokusingqongileyo kwaye isebenzayo kulwelo lokubhola olusekelwe emanzini, olune-stability entle kakhulu yokusingqongileyo, amandla okuthintela i-shale aphuculweyo kunye nokusebenza ngcono kolwelo xa kuthelekiswa nezithinteli zemveli ezifana ne-KCl, ulwelo lwe-ionic olusekelwe kwi-imidazolyl kunye ne-DES yendabuko.
Olu phononongo luza kubandakanya ukulungiswa kwangaphakathi kwe-NADES esekwe kwi-citric acid (CA) kulandele ukuchazwa okuneenkcukacha kwe-physicochemical kunye nokusetyenziswa kwayo njengesongezelelo solwelo lokubhola ukuvavanya iimpawu zolwelo lokubhola kunye nokukwazi kwalo ukuthintela ukudumba. Kolu phononongo, i-CA iya kusebenza njengesamkeli se-hydrogen bond ngelixa i-glycerol (Gly) iya kusebenza njengomnikeli we-hydrogen bond okhethiweyo ngokusekelwe kwiikhrayitheriya zokuhlola ze-MH zokwakheka/ukukhethwa kwe-NADES kwizifundo zokuthintela i-shale30. I-Fourier transform infrared spectroscopy (FTIR), i-X-ray diffraction (XRD) kunye nokulinganisa kwe-zeta potential (ZP) kuya kucacisa ukusebenzisana kwe-NADES-clay kunye nendlela esekwe ngayo ukuthintela ukudumba kodongwe. Ukongeza, olu phononongo luza kuthelekisa ulwelo lokubhola olusekwe kwi-CA NADES kunye ne-DES32 ngokusekelwe kwi-1-ethyl-3-methylimidazolium chloride [EMIM]Cl7,12,14,17,31, KCl kunye ne-choline chloride:urea (1:2) ukuphanda ukusebenza kwazo ekuthinteleni i-shale kunye nokuphucula ukusebenza kolwelo lokubhola.
I-asidi ye-citric (i-monohydrate), i-glycerol (99 USP), kunye ne-urea zithengwe kwi-EvaChem, eKuala Lumpur, eMalaysia. I-Choline chloride (>98%), [EMIM]Cl 98%, kunye ne-potassium chloride zithengwe kwi-Sigma Aldrich, eMalaysia. Ulwakhiwo lweekhemikhali lwazo zonke iikhemikhali luboniswe kuMfanekiso 1. Umzobo oluhlaza uthelekisa iikhemikhali eziphambili ezisetyenzisiweyo kolu phononongo: i-imidazolyl ionic liquid, i-choline chloride (DES), i-citric acid, i-glycerol, i-potassium chloride, kunye ne-NADES (i-citric acid kunye ne-glycerol). Itheyibhile yobungani bendalo yeekhemikhali ezisetyenzisiweyo kolu phononongo iboniswe kwiTheyibhile 1. Kwitheyibhile, ikhemikhali nganye ilinganiswe ngokusekelwe kwityhefu, ukubola kwezinto eziphilayo, iindleko, kunye nokuzinza kokusingqongileyo.
Izakhiwo zeekhemikhali zezinto ezisetyenzisiweyo kolu phononongo: (a) i-citric acid, (b) [EMIM]Cl, (c) i-choline chloride, kunye (d) ne-glycerol.
Abanikeli be-hydrogen bond (HBD) kunye nabamkeli be-hydrogen bond (HBA) abafanelekileyo kuphuhliso lwe-CA (natural deep eutectic solvent) esekelwe kwi-NADES bakhethwe ngononophelo ngokwemigaqo yokukhetha ye-MH 30, eyenzelwe uphuhliso lwe-NADES njenge-shale inhibitors ezisebenzayo. Ngokwale miqathango, izinto ezinenani elikhulu labanikeli be-hydrogen bond kunye nabamkeli kunye namaqela asebenzayo e-polar zithathwa njengezifanelekileyo kuphuhliso lwe-NADES.
Ukongeza, i-ionic liquid [EMIM]Cl kunye ne-choline chloride:urea deep eutectic solvent (DES) zikhethwe ukuze zithelekiswe kolu phononongo kuba zisetyenziswa kakhulu njengezongezo zolwelo lokubhola33,34,35,36. Ukongeza, i-potassium chloride (KCl) ithelekiswe kuba sisithinteli esiqhelekileyo.
I-asidi ye-citric kunye ne-glycerol zixutywe ngokwemilinganiselo eyahlukeneyo ye-molar ukuze kufunyanwe imixube ye-eutectic. Ukuhlolwa okubonakalayo kubonise ukuba umxube we-eutectic wawululwelo olufanayo, olucacileyo olungena-turbidity, nto leyo ebonisa ukuba umniki-mali we-hydrogen bond (HBD) kunye nommkeli we-hydrogen bond (HBA) zixutywe ngempumelelo kolu lwakhiwo lwe-eutectic. Uvavanyo lokuqala lwenziwe ukujonga indlela yokuziphatha exhomekeke kubushushu benkqubo yokuxuba i-HBD kunye ne-HBA. Ngokweencwadi ezikhoyo, umlinganiselo wemixube ye-eutectic uvavanywe kumaqondo obushushu amathathu athile ngaphezulu kwe-50 °C, 70 °C kunye ne-100 °C, nto leyo ebonisa ukuba ubushushu be-eutectic buhlala buphakathi kwe-50–80 °C. Ibhalansi yedijithali ye-Mettler isetyenzisiwe ukulinganisa ngokuchanekileyo izinto ze-HBD kunye ne-HBA, kwaye ipleyiti eshushu ye-Thermo Fisher isetyenzisiwe ukufudumeza nokuvuselela i-HBD kunye ne-HBA kwi-100 rpm phantsi kweemeko ezilawulwayo.
Iimpawu ze-thermophysical ze-deep eutectic solvent yethu (DES) eyenziweyo, kuquka uxinano, uxinzelelo lomphezulu, i-refractive index, kunye ne-viscosity, zilinganiswe ngokuchanekileyo kuluhlu lobushushu oluqala kwi-289.15 ukuya kwi-333.15 K. Kufuneka kuqatshelwe ukuba olu luhlu lobushushu lukhethwe ikakhulu ngenxa yokunqongophala kwezixhobo ezikhoyo. Uhlalutyo olupheleleyo luquke uphando olunzulu lweepropati ezahlukeneyo ze-thermophysical zale fomyula ye-NADES, olutyhila indlela eziziphatha ngayo kuluhlu lobushushu. Ukugxila kolu luhlu lobushushu oluthile kubonelela ngengqiqo kwiipropati ze-NADES ezibaluleke kakhulu kwizicelo ezininzi.
Uxinzelelo lomphezulu we-NADES olulungisiweyo lulinganiswe ukusuka kwi-289.15 ukuya kwi-333.15 K kusetyenziswa imitha yoxinzelelo lwe-interfacial (IFT700). Amathontsi e-NADES enziwa kwigumbi elizaliswe ngumthamo omkhulu wolwelo kusetyenziswa inaliti ye-capillary phantsi kweemeko ezithile zobushushu kunye noxinzelelo. Iinkqubo zemifanekiso zanamhlanje zizisa iiparameter ezifanelekileyo zejometri ukubala uxinzelelo lwe-interfacial kusetyenziswa i-Laplace equation.
I-ATAGO refractometer isetyenzisiwe ukumisela i-refractive index ye-NADES esandul’ ukulungiswa kuluhlu lobushushu oluyi-289.15 ukuya kwi-333.15 K. Esi sixhobo sisebenzisa imodyuli yobushushu ukulawula ubushushu ukuqikelela inqanaba lokurhawuzelelwa kokukhanya, kususa imfuneko yokuhlamba amanzi ngobushushu obungaguqukiyo. Umphezulu weprism we-refractometer kufuneka ucocwe kwaye isisombululo sesampulu kufuneka sisasazwe ngokulinganayo phezu kwawo. Linganisa ngesisombululo esiqhelekileyo esaziwayo, uze ufunde i-refractive index kwisikrini.
Ubungakanani be-NADES obulungisiweyo bulinganiswe kubushushu obuphakathi kwama-289.15 ukuya kuma-333.15 K kusetyenziswa i-Brookfield rotational viscometer (uhlobo lwe-cryogenic) ngesantya se-shear se-30 rpm kunye nobukhulu be-spindle obuyi-6. I-viscometer ilinganisa ubuninzi be-viscometer ngokumisela i-torque efunekayo ukuze kujikeleziswe i-spindle ngesantya esingaguqukiyo kwisampuli yolwelo. Emva kokuba isampuli ibekwe kwiscreen phantsi kwe-spindle kwaye iqiniswe, i-viscometer ibonisa ubuninzi be-viscometer kwi-centipoise (cP), inika ulwazi oluxabisekileyo malunga neempawu ze-rheological zolwelo.
Imitha yoxinano oluphathwayo i-DMA 35 Basic isetyenzisiwe ukufumanisa uxinano lwe-natural deep eutectic solvent (NDEES) esandul’ ukulungiswa kubushushu obuyi-289.15–333.15 K. Ekubeni isixhobo singenaso isifudumezi esakhelwe ngaphakathi, kufuneka sifudunyezwe kubushushu obuchaziweyo (± 2 °C) ngaphambi kokusebenzisa imitha yoxinano lwe-NADES. Tsala ubuncinane i-2 ml yesampulu ngetyhubhu, kwaye uxinano luya kuboniswa kwangoko kwiscreen. Kubalulekile ukuqaphela ukuba ngenxa yokungabikho kwesifudumezi esakhelwe ngaphakathi, iziphumo zokulinganisa zinempazamo ye-± 2 °C.
Ukuvavanya i-pH ye-NADES esandula ukulungiswa kuluhlu lobushushu oluyi-289.15–333.15 K, sisebenzise imitha ye-pH ye-Kenis benchtop. Ekubeni kungekho sixhobo sokufudumeza esakhelwe ngaphakathi, i-NADES yaqala yafudunyezwa ukuya kubushushu obufunekayo (±2 °C) kusetyenziswa i-hotplate yaze yalinganiswa ngokuthe ngqo ngemitha ye-pH. Gcwalisa ngokupheleleyo i-pH meter probe kwi-NADES kwaye urekhode ixabiso lokugqibela emva kokuba ukufundwa kuzinzile.
Uhlalutyo lwe-thermogravimetric (TGA) lusetyenzisiwe ukuvavanya uzinzo lobushushu lwe-natural deep eutectic solvents (NADES). Iisampulu zahlalutywa ngexesha lokufudumeza. Kusetyenziswa ibhalansi echanekileyo kakhulu kunye nokujonga ngononophelo inkqubo yokufudumeza, kwaveliswa isicwangciso sokulahleka kobunzima xa kuthelekiswa nobushushu. I-NADES yafudunyezwa ukusuka kwi-0 ukuya kwi-500 °C ngesantya se-1 °C ngomzuzu.
Ukuqala inkqubo, isampuli ye-NADES kufuneka ixutywe kakuhle, ihlanganiswe ngokulinganayo, kwaye kususwe umswakama womphezulu. Isampuli elungisiweyo ibekwa kwi-cuvette ye-TGA, edla ngokwenziwa ngezinto ezingangeniyo ezifana ne-aluminium. Ukuqinisekisa iziphumo ezichanekileyo, izixhobo ze-TGA ziyalinganiswa kusetyenziswa izixhobo zokubhekisa, ngokuqhelekileyo imigangatho yobunzima. Nje ukuba ilinganiswe, uvavanyo lwe-TGA luqala kwaye isampuli ifudunyezwa ngendlela elawulwayo, ngokuqhelekileyo ngesantya esingaguqukiyo. Ukubeka iliso rhoqo kubudlelwane phakathi kobunzima besampuli kunye nobushushu yinxalenye ebalulekileyo yovavanyo. Izixhobo ze-TGA ziqokelela idatha kubushushu, ubunzima, kunye nezinye iiparameter ezifana nokuhamba kwegesi okanye ubushushu besampuli. Nje ukuba uvavanyo lwe-TGA lugqityiwe, idatha eqokelelweyo iyahlalutywa ukuze kuchongwe utshintsho kubunzima besampuli njengomsebenzi wobushushu. Olu lwazi lubalulekile ekumiseleni uluhlu lobushushu oluhambelana notshintsho lomzimba kunye neekhemikhali kwisampuli, kubandakanya iinkqubo ezifana nokunyibilika, ukufuma, i-oxidation, okanye ukubola.
Ulwelo lokugrumba olusekelwe emanzini lwenziwe ngononophelo ngokwemigangatho ye-API 13B-1, kwaye ulwakhiwo lwalo oluthile ludweliswe kwiTheyibhile 2 ukuze kubhekiselwe kulo. I-Citric acid kunye ne-glycerol (99 USP) zithengwe kwiSigma Aldrich, eMalaysia ukuze kulungiswe i-natural deep eutectic solvent (NADES). Ukongeza, i-conventional shale inhibitor potassium chloride (KCl) nayo ithengwe kwiSigma Aldrich, eMalaysia. I-1-ethyl, i-3-methylimidazolium chloride ([EMIM]Cl) enobumsulwa obungaphezulu kwe-98% ikhethiwe ngenxa yempembelelo yayo ebalulekileyo ekuphuculeni i-rheology yolwelo lokugrumba kunye nokuthintela i-shale, eyaqinisekiswa kwizifundo zangaphambili. Zombini i-KCl kunye ne-([EMIM]Cl) ziya kusetyenziswa kuhlalutyo lokuthelekisa ukuvavanya ukusebenza kokuthintela i-shale kwe-NADES.
Abaphandi abaninzi bakhetha ukusebenzisa ii-bentonite flakes ukuze bafunde ukudumba kwe-shale kuba i-bentonite ineqela elifanayo "le-montmorillonite" elibangela ukudumba kwe-shale. Ukufumana iisampulu zoqobo ze-shale core kunzima kuba inkqubo yokubopha iyawuphazamisa umphezulu we-shale, nto leyo ebangela iisampulu ezingezizo ngokupheleleyo ze-shale kodwa zihlala ziqulathe umxube wesanti kunye neengqimba ze-limestone. Ukongeza, iisampulu ze-shale zihlala zingenazo amaqela e-montmorillonite abangela ukudumba kwe-shale kwaye ke ngoko azifanelekanga kwiimvavanyo zokuthintela ukudumba.
Kolu phononongo, sisebenzise amasuntswana e-bentonite aphinde akhiwa anobubanzi obumalunga ne-2.54 cm. Amasuntswana enziwe ngokucinezela i-11.5 grams ye-sodium bentonite powder kwi-hydraulic press kwi-1600 psi. Ubukhulu bamasuntswana bulinganiswe ngokuchanekileyo ngaphambi kokuba bubekwe kwi-linear dilatometer (LD). Amasuntswana emva koko antywiliselwa kwiisampulu zolwelo lokubhola, kuquka iisampulu zesiseko kunye neesampulu ezifakwe izithinteli ezisetyenziselwa ukuthintela ukudumba kwe-shale. Utshintsho kubukhulu be-granule emva koko lwajongwa ngononophelo kusetyenziswa i-LD, kunye nemilinganiselo erekhodwe kwizithuba zemizuzwana engama-60 kangangeeyure ezingama-24.
I-X-ray diffraction ibonise ukuba ukwakheka kwe-bentonite, ingakumbi i-47% ye-montmorillonite component, yinto ebalulekileyo ekuqondeni iimpawu zayo zejoloji. Phakathi kwe-montmorillonite component ye-bentonite, i-montmorillonite yeyona nxalenye iphambili, ebalelwa kwi-88.6% yezakhi zizonke. Okwangoku, i-quartz ibalelwa kwi-29%, i-illite ibe yi-7%, kunye ne-carbonate ibe yi-9%. Inxalenye encinci (malunga ne-3.2%) ngumxube we-illite kunye ne-montmorillonite. Ukongeza, iqulethe izinto ezincinci ezifana ne-Fe2O3 (4.7%), i-silver aluminosilicate (1.2%), i-muscovite (4%), kunye ne-phosphate (2.3%). Ukongeza, kukho inani elincinci le-Na2O (1.83%) kunye ne-iron silicate (2.17%), nto leyo eyenza kube lula ukuqonda ngokupheleleyo izinto eziyinxalenye ye-bentonite kunye nobungakanani bazo.
Eli candelo libanzi lophando lichaza iipropati ze-rheological kunye ne-filtration zeesampulu zolwelo lokubhola ezilungiselelwe kusetyenziswa i-natural deep eutectic solvent (NADES) kwaye zisetyenziswa njenge-drilling fluid additive kwii-concentrations ezahlukeneyo (1%, 3% kunye ne-5%). Iisampulu ze-slurry ezisekelwe kwi-NADES emva koko zathelekiswa zaza zahlalutywa ngeesampulu ze-slurry eziquka i-potassium chloride (KCl), i-CC:urea DES (i-choline chloride deep eutectic solvent:urea) kunye ne-ionic liquids. Inani leeparameter eziphambili zigutyungelwe kolu phononongo kubandakanya ukufundwa kwe-viscosity okufunyenwe kusetyenziswa i-FANN viscometer ngaphambi nasemva kokuvezwa kwiimeko zokwaluphala kwi-100°C kunye ne-150°C. Ukulinganiswa kuthathwe ngesantya sokujikeleza esahlukileyo (3 rpm, 6 rpm, 300 rpm kunye ne-600 rpm) okuvumela uhlalutyo olupheleleyo lokuziphatha kolwelo lokubhola. Idatha efunyenweyo ingasetyenziselwa ukumisela iipropati eziphambili ezifana ne-yield point (YP) kunye ne-plastic viscosity (PV), ezibonelela ngengqiqo yokusebenza kolwelo phantsi kweemeko ezahlukeneyo. Uvavanyo lokuhluza olunoxinzelelo oluphezulu (HPHT) kwi-400 psi kunye ne-150°C (amaqondo obushushu aqhelekileyo kwimithombo yobushushu obuphezulu) lumisela ukusebenza kokuhluza (ubukhulu bekhekhe kunye nomthamo wokuhluza).
Eli candelo lisebenzisa izixhobo zanamhlanje, iGrace HPHT Linear Dilatometer (M4600), ukuvavanya ngokupheleleyo iipropati zokuthintela ukudumba kweshale kwi-drilling fluids zethu ezisekelwe emanzini. I-LSM ngumatshini wanamhlanje oqulathe izinto ezimbini: i-plate compactor kunye ne-linear dilatometer (imodeli: M4600). Iiplate zeBentonite zalungiselelwa uhlalutyo kusetyenziswa iGrace Core/Plate Compactor. I-LSM emva koko inika idatha yokudumba kwangoko kwezi plate, ivumela uvavanyo olupheleleyo lweepropati zokuthintela ukudumba kweshale. Uvavanyo lokwandiswa kweshale lwenziwe phantsi kweemeko ezingqongileyo, oko kukuthi, ama-25°C kunye ne-1 psia.
Uvavanyo lokuzinza kwe-shale lubandakanya uvavanyo oluphambili oludla ngokubizwa ngokuba luvavanyo lokubuyisela i-shale, uvavanyo lwe-shale dip okanye uvavanyo lokusasazwa kwe-shale. Ukuqala olu vavanyo, iziqwenga ze-shale zahlulwe kwisikrini se-BSS #6 zize zibekwe kwisikrini se-#10. Iziqwenga emva koko zinikwa itanki yokubamba apho zixutywa khona nolwelo olusisiseko kunye nodaka lokubhola olune-NADES (Natural Deep Eutectic Solvent). Inyathelo elilandelayo kukubeka umxube kwi-oven ukuze kuqhutyekwe nenkqubo yokuqengqeleka eshushu kakhulu, ukuqinisekisa ukuba iziqwenga kunye nodaka zixutywe kakuhle. Emva kweeyure ezili-16, iziqwenga zisuswa kwi-pulp ngokuvumela i-shale ukuba ibole, nto leyo ekhokelela ekunciphiseni ubunzima beziqwenga. Uvavanyo lokubuyisela i-shale lwenziwe emva kokuba iziqwenga ze-shale zibanjwe kudaka lokubhola kwi-150°C kunye ne-1000 psi. intshi kwiiyure ezingama-24.
Ukuze silinganise ukubuyiselwa kodaka lwe-shale, saluhluza ngesikrini esicolekileyo (i-40 mesh), saza saluhlamba kakuhle ngamanzi, saza ekugqibeleni salomisa kwi-oven. Le nkqubo inzima isivumela ukuba siqikelele udaka olufunyenweyo xa kuthelekiswa nobunzima bokuqala, ekugqibeleni sibala ipesenti yodaka lwe-shale olufunyenwe ngempumelelo. Umthombo weesampuli ze-shale uvela kwiSithili saseNiah, kwiSithili saseMiri, eSarawak, eMalaysia. Ngaphambi kovavanyo lokusasazwa nokubuyiselwa, iisampuli ze-shale zenziwa uhlalutyo olupheleleyo lwe-X-ray diffraction (XRD) ukuze kulinganiswe ukwakheka kwazo kodongwe kwaye kuqinisekiswe ukuba zifanelekile na ukuvavanywa. Ukwakheka kweeminerali zodongwe kwisampuli kulandelayo: illite 18%, kaolinite 31%, chlorite 22%, vermiculite 10%, kunye ne-mica 19%.
Uxinzelelo lomphezulu yinto ephambili elawula ukungena kweendawo zamanzi kwii-shale micropores ngesenzo se-capillary, esiza kufundwa ngokweenkcukacha kweli candelo. Eli phepha lihlola indima yoxinzelelo lomphezulu kwipropati edibeneyo yolwelo lokubhola, ligxininisa impembelelo yalo ebalulekileyo kwinkqubo yokubhola, ingakumbi uthintelo lwe-shale. Sisebenzise i-interfacial tensiometer (IFT700) ukulinganisa ngokuchanekileyo uxinzelelo lomphezulu weesampuli zolwelo lokubhola, sityhila inkalo ebalulekileyo yokuziphatha kolwelo kwimeko yothintelo lwe-shale.
Eli candelo lixoxa ngokweenkcukacha ngesithuba se-d-layer, esikumgama ophakathi kwe-aluminosilicate layers kunye ne-aluminosilicate layer enye kwi-clays. Uhlalutyo lugubungele iisampulu zodaka olumanzi oluqulethe i-1%, 3% kunye ne-5% CA NADES, kunye ne-3% KCl, 3% [EMIM]Cl kunye ne-3% CC:urea based DES ukuze kuthelekiswe. I-benchtop X-ray diffractometer (D2 Phaser) yanamhlanje esebenza kwi-40 mA kunye ne-45 kV ene-Cu-Kα radiation (λ = 1.54059 Å) idlale indima ebalulekileyo ekurekhodeni iincopho ze-X-ray diffraction zeesampulu ze-Na-Bt ezimanzi nezomileyo. Ukusetyenziswa kwe-Bragg equation kwenza kube lula ukumisela ngokuchanekileyo isithuba se-d-layer, ngaloo ndlela kubonelela ngolwazi oluxabisekileyo malunga nokuziphatha kodongwe.
Eli candelo lisebenzisa isixhobo esiphambili seMalvern Zetasizer Nano ZSP ukulinganisa ngokuchanekileyo amandla e-zeta. Olu vavanyo lubonelele ngolwazi oluxabisekileyo malunga neempawu zetshaja zeesampuli zodaka oluxutyiweyo oluqulethe i-1%, 3%, kunye ne-5% CA NADES, kunye ne-3% KCl, 3% [EMIM]Cl, kunye ne-3% CC:urea-based DES yohlalutyo oluthelekisayo. Ezi ziphumo zinegalelo ekuqondeni kwethu ukuzinza kweekhompawundi ze-colloidal kunye nokusebenzisana kwazo kwiilwelo.
Iisampulu zodongwe zihlolwe ngaphambi nasemva kokuvezwa kwi-natural deep eutectic solvent (NADES) kusetyenziswa i-Zeiss Supra 55 VP field emission scanning electron microscope (FESEM) exhotyiswe nge-energy dispersive X-ray (EDX). Isisombululo somfanekiso yayiyi-500 nm kwaye amandla e-electron beam yayiyi-30 kV kunye ne-50 kV. I-FESEM ibonelela ngembonakalo ephezulu yesimo somphezulu kunye neempawu zesakhiwo seesampulu zodongwe. Injongo yolu phononongo yayikukufumana ulwazi malunga nempembelelo ye-NADES kwiisampulu zodongwe ngokuthelekisa imifanekiso efunyenwe ngaphambi nasemva kokuvezwa.
Kolu phononongo, iteknoloji ye-field emission scanning electron microscopy (FESEM) isetyenzisiwe ukuphanda impembelelo ye-NADES kwiisampuli zodongwe kwinqanaba le-microscope. Injongo yolu phononongo kukucacisa ukusetyenziswa okunokwenzeka kwe-NADES kunye nempembelelo yayo kwimo yodongwe kunye nobukhulu obuphakathi bee-particle, nto leyo eya kubonelela ngolwazi oluxabisekileyo kuphando kweli candelo.
Kolu phononongo, imivalo yeempazamo isetyenzisiwe ukuchaza ngokubonakalayo umahluko kunye nokungaqiniseki kwempazamo yepesenti ephakathi (i-AMPE) kwiimeko zovavanyo. Endaweni yokuceba ixabiso le-AMPE ngalinye (ekubeni ukuceba ixabiso le-AMPE kunokufihla imikhwa kwaye kugqithise umahluko omncinci), sibala imivalo yeempazamo sisebenzisa umthetho we-5%. Le ndlela iqinisekisa ukuba ibha nganye yeempazamo imele ixesha apho ixesha lokuzithemba le-95% kunye ne-100% yamaxabiso e-AMPE kulindeleke ukuba liwe, ngaloo ndlela kubonelela ngesishwankathelo esicacileyo nesifutshane sokusasazwa kwedatha kwimeko nganye yovavanyo. Ukusebenzisa imivalo yeempazamo ngokusekelwe kumthetho we-5% ngaloo ndlela kuphucula ukutolikwa kunye nokuthembeka kwemiboniso yemizobo kwaye kunceda ukubonelela ngokuqonda okuneenkcukacha ngakumbi kweziphumo kunye neziphumo zazo.
Ekuqulunqweni kwezinto zemvelo ezinzulu ze-eutectic solvents (NADES), iiparameter ezininzi ezibalulekileyo zifundwe ngononophelo ngexesha lenkqubo yokulungiselela ngaphakathi endlwini. Ezi zinto zibalulekileyo ziquka ubushushu, umlinganiselo we-molar, kunye nesantya sokuxuba. Uvavanyo lwethu lubonisa ukuba xa i-HBA (i-citric acid) kunye ne-HBD (glycerol) zixutywe kwi-molar ratio ye-1:4 kwi-50°C, umxube we-eutectic wenziwa. Uphawu olwahlukileyo lomxube we-eutectic kukubonakala kwawo okucacileyo, okufanayo, kunye nokungabikho kwe-sediment. Ngoko ke, eli nyathelo libalulekileyo ligxininisa ukubaluleka komlinganiselo we-molar, ubushushu, kunye nesantya sokuxuba, phakathi kwazo umlinganiselo we-molar wawuyeyona nto inefuthe ekulungiseleleni i-DES kunye ne-NADES, njengoko kubonisiwe kuMfanekiso 2.
Isalathisi sokuchasana (n) sichaza umlinganiselo wesantya sokukhanya kwi-vacuum kwisantya sokukhanya kwi-medium yesibini, exineneyo. Isalathisi sokuchasana sinomdla kakhulu kwi-natural deep eutectic solvents (NADES) xa kujongwa ukusetyenziswa kwe-optically sensitive njenge-biosensors. Isalathisi sokuchasana se-NADES esifundwe kwi-25 °C yayiyi-1.452, esezantsi ngokumangalisayo kuneye-glycerol.
Kubalulekile ukuqaphela ukuba i-refractive index ye-NADES iyancipha ngobushushu, kwaye le ndlela ingachazwa ngokuchanekileyo ngefomula (1) kunye noMfanekiso 3, apho i-absolute mean percentage error (AMPE) ifikelela kwi-0%. Le ndlela yokuziphatha exhomekeke kubushushu ichazwa kukwehla kwe-viscosity kunye noxinano kubushushu obuphezulu, okubangela ukuba ukukhanya kuhambe kwi-medium ngesantya esiphezulu, okubangela ixabiso eliphantsi le-refractive index (n). Ezi ziphumo zibonelela ngengqiqo ebalulekileyo malunga nokusetyenziswa kwe-NADES kwi-optical sensing, zigqamisa amandla azo kwizicelo ze-biosensor.
Uxinzelelo lomphezulu, olubonisa ukuthambekela komphezulu wolwelo ekunciphiseni indawo yawo, lubaluleke kakhulu ekuvavanyeni ukufaneleka kwe-natural deep eutectic solvents (NADES) kwizicelo ezisekelwe kuxinzelelo lwe-capillary. Uphononongo loxinzelelo lomphezulu kuluhlu lobushushu oluyi-25–60 °C lubonelela ngolwazi oluxabisekileyo. Kwi-25 °C, uxinzelelo lomphezulu lwe-NADES olusekelwe kwi-citric acid yayiyi-55.42 mN/m, ephantsi kakhulu kunaleyo yamanzi kunye ne-glycerol. Umfanekiso 4 ubonisa ukuba uxinzelelo lomphezulu luyehla kakhulu xa ubushushu busanda. Le nto ingachazwa ngokwanda kwamandla e-molecular kinetic kunye nokwehla okulandelayo kwamandla anomtsalane phakathi kweemolekyuli.
Ukwehla okuthe ngqo koxinzelelo lomphezulu olubonwe kwi-NADES efundwayo kunokubonakaliswa kakuhle yi-equation (2), ebonisa ubudlelwane obusisiseko bezibalo kuluhlu lobushushu obuyi-25–60 °C. Igrafu ekuMfanekiso 4 ibonisa ngokucacileyo utyekelo loxinzelelo lomphezulu kunye nobushushu obunempazamo yepesenti ephakathi (i-AMPE) eyi-1.4%, elinganisa ukuchaneka kwamaxabiso oxinzelelo lomphezulu axeliweyo. Ezi ziphumo zinempembelelo ebalulekileyo ekuqondeni ukuziphatha kwe-NADES kunye nokusetyenziswa kwayo okunokwenzeka.
Ukuqonda i-density dynamics ye-natural deep eutectic solvents (NADES) kubalulekile ukuze kube lula ukuyisebenzisa kwizifundo ezininzi zesayensi. Uxinano lwe-citric acid-based NADES kwi-25°C yi-1.361 g/cm3, ephezulu kunoxinano lwe-parent glycerol. Lo mahluko ungachazwa ngokongezwa kwe-hydrogen bond acceptor (citric acid) kwi-glycerol.
Ukuthatha i-NADES esekelwe kwi-citrate njengomzekelo, uxinano lwayo luyehla luye kwi-1.19 g/cm3 kwi-60°C. Ukwanda kwamandla e-kinetic xa kushushu kubangela ukuba iimolekyuli ze-NADES zisasazeke, nto leyo ebangela ukuba zihlale kwivolumu enkulu, nto leyo ebangela ukwehla koxinano. Ukwehla okubonwayo koxinano kubonisa ulwalamano oluthile oluhambelanayo nokunyuka kobushushu, olunokubonakaliswa ngokufanelekileyo ngefomula (3). Umfanekiso 5 ubonisa ngokucacileyo ezi mpawu zotshintsho loxinano lwe-NADES ngempazamo yepesenti echanekileyo (AMPE) ye-1.12%, ebonelela ngomlinganiselo wobungakanani bokuchaneka kwamaxabiso oxinano axeliweyo.
Ukuqina ngamandla anomtsalane phakathi kweengqimba ezahlukeneyo zolwelo oluhambayo kwaye ludlala indima ephambili ekuqondeni ukusebenza kwe-natural deep eutectic solvents (NADES) kwizicelo ezahlukeneyo. Kwi-25 °C, i-viscosity ye-NADES yayiyi-951 cP, ephezulu kuneye-glycerol.
Ukwehla okubonwayo kwe-viscosity kunye nobushushu obukhulayo kuchazwa kakhulu kubuthathaka kwamandla akhangayo phakathi kweemolekyuli. Le nto ibangela ukwehla kwe-viscosity yolwelo, umkhwa oboniswe ngokucacileyo kuMfanekiso 6 kwaye ulinganiswe yi-Equation (4). Okuphawulekayo kukuba, kwi-60°C, i-viscosity yehla iye kwi-898 cP kunye ne-avareji yepesenti ye-avareji (AMPE) ye-1.4%. Ukuqonda okuneenkcukacha kwe-viscosity ngokuchasene nokuxhomekeka kobushushu kwi-NADES kubaluleke kakhulu ekusebenziseni kwayo okusebenzayo.
I-pH yesisombululo, echongwa yi-logarithm engalunganga yoxinzelelo lwe-hydrogen ion, ibalulekile, ngakumbi kwizicelo ezinobuzaza be-pH ezifana nokwenziwa kwe-DNA, ngoko ke i-pH ye-NADES kufuneka ifundwe ngononophelo ngaphambi kokuba isetyenziswe. Ukuthatha i-NADES esekelwe kwi-citric acid njengomzekelo, i-pH ene-asidi ecacileyo ye-1.91 inokubonwa, nto leyo eyahluke kakhulu kwi-pH engathathi cala ye-glycerol.
Okunomdla kukuba, i-pH ye-natural citric acid dehydrogenase soluble solvent (NADES) ibonise ukwehla okungaqhelekanga kunye nokunyuka kwamaqondo obushushu. Le nto ibangelwa kukwanda kokungcangcazela kweemolekyuli okuphazamisa ibhalansi ye-H+ kwisisombululo, okukhokelela ekwakhiweni kwee-ions ze-[H]+ kwaye, ngokuphindaphindiweyo, utshintsho kwixabiso le-pH. Ngelixa i-pH yendalo ye-citric acid isusela kwi-3 ukuya kwi-5, ubukho be-hydrogen ene-acid kwi-glycerol buyinciphisa ngakumbi i-pH ukuya kwi-1.91.
Ukuziphatha kwe-pH ye-NADES esekelwe kwi-citrate kuluhlu lobushushu obuyi-25–60 °C kunokumelwa ngokufanelekileyo yi-equation (5), enika intetho yemathematika yethrendi ye-pH ebonweyo. Umfanekiso 7 ubonisa ngokucacileyo olu lwalamano lunomdla, ugxininisa impembelelo yobushushu kwi-pH ye-NADES, exelwe ukuba yi-1.4% ye-AMPE.
Uhlalutyo lwe-thermogravimetric (TGA) lwe-natural citric acid deep eutectic solvent (NADES) lwenziwe ngokucwangcisiweyo kumanqanaba obushushu ukusuka kubushushu begumbi ukuya kwi-500 °C. Njengoko kunokubonwa kwiMifanekiso 8a kunye no-b, ukulahleka kokuqala kobunzima ukuya kwi-100 °C kwakubangelwa kakhulu ngamanzi afunxwayo kunye namanzi adibene ne-citric acid kunye ne-glycerol ecocekileyo. Ukugcinwa okukhulu kobunzima obumalunga ne-88% kwabonwa ukuya kuthi ga kwi-180 °C, okwakubangelwa ikakhulu kukubola kwe-citric acid kwi-aconitic acid kunye nokwakheka okulandelayo kwe-methylmaleic anhydride (III) xa kufudunyezwa ngakumbi (Umfanekiso 8 b). Ngaphezulu kwe-180 °C, ukubonakala okucacileyo kwe-acrolein (acrylaldehyde) kwi-glycerol nako kunokubonwa, njengoko kuboniswe kwiMifanekiso 8b37.
Uhlalutyo lwe-thermogravimetric (TGA) ye-glycerol lubonise inkqubo yokulahleka kobunzima obunezigaba ezibini. Inqanaba lokuqala (180 ukuya kwi-220 °C) libandakanya ukwakheka kwe-acrolein, kulandele ukulahleka okukhulu kobunzima kumaqondo obushushu aphezulu ukusuka kwi-230 ukuya kwi-300 °C (Umfanekiso 8a). Njengoko ubushushu busanda, i-acetaldehyde, i-carbon dioxide, i-methane, kunye ne-hydrogen zenziwa ngokulandelelana. Okuphawulekayo kukuba, yi-28% kuphela yobunzima egcinwe kwi-300 °C, nto leyo ebonisa ukuba iipropati zangaphakathi ze-NADES 8(a)38,39 zinokuba neziphene.
Ukuze kufunyanwe ulwazi malunga nokwakheka kweebhondi ezintsha zeekhemikhali, ukumiswa okusandul’ ukulungiswa kwe-natural deep eutectic solvents (NADES) kuhlalutywe yi-Fourier transform infrared spectroscopy (FTIR). Uhlalutyo lwenziwe ngokuthelekisa i-spectrum ye-NADES suspension kunye ne-spectra ye-citric acid ecocekileyo (CA) kunye ne-glycerol (Gly). I-CA spectrum ibonise iincopho ezicacileyo kwi-1752 1/cm kunye ne-1673 1/cm, ezimele ukungcangcazela okunwebekayo kwebhondi ye-C=O kwaye zikwaphawu lwe-CA. Ukongeza, utshintsho olukhulu kwi-OH bending vibration kwi-1360 1/cm lubonwe kummandla weminwe, njengoko kubonisiwe kuMfanekiso 9.
Ngokufanayo, kwimeko ye-glycerol, utshintsho lwe-OH stretching kunye ne-bending vibrations lufunyenwe kwiinombolo zamaza ze-3291 1/cm kunye ne-1414 1/cm, ngokulandelelana. Ngoku, ngokuhlalutya i-spectrum ye-NADES elungisiweyo, kufunyenwe utshintsho olukhulu kwi-spectrum. Njengoko kubonisiwe kuMfanekiso 7, ukungcangcazela kokungcangcazela kwe-C=O bond kutshintshe ukusuka kwi-1752 1/cm ukuya kwi-1720 1/cm kunye nokungcangcazela kokungcangcazela kwe--OH bond ye-glycerol kutshintshe ukusuka kwi-1414 1/cm ukuya kwi-1359 1/cm. Olu tshintsho kwiinombolo zamaza lubonisa utshintsho kwi-electronegativity, olubonisa ukwakheka kweebhondi ezintsha zeekhemikhali kwisakhiwo se-NADES.