Kubaka umurongo w'ikaliburasi y'ubururu bwa metilene: ibisubizo fatizo, intera, no kuba umurongo ugororotse

Abasesenguzi babiri bakoresha icupa rimwe ry'igisubizo cy'ibanze cy'ubururu bwa metilene, buri wese akubaka umurongo w'ikaliburasi. Uwa mbere abona umurongo ugororotse unyura aho ibipimo byombi bingana na zeru, agapima ingero zifite ubwibande butazwi yizeye ibisubizo. Uwa kabiri abona umurongo ugorama ku mpera yo hejuru, agaciro k'aho ukata umurongo uhagaritse katagera hafi ya zeru, n'ibisubizo by'ingero bihinduka uko zigabanyirizwa ubwibande. Irangi ni rimwe, igikoresho ni kimwe, n'uburebure bw'umuraba ni bumwe. Itandukaniro si ubuhanga. Ni imitegurire: ibyashyizwe mu gisubizo fatizo, ubwibande bwatoranyijwe, n'uko intera yagenzuwe yagumye mu gice aho icyitegererezo kimwe cyoroheje kigikora.

Umurongo w'ikaliburasi ni amasezerano ahuza igisubizo cy'igikoresho n'ubwibande, afite agaciro gusa mu mimerere yubakiwemo. Ku bururu bwa metilene, ayo masezerano afite aho azwi ko ashobora kunanirwa. Molekile z'irangi zihuza ubwazo mu mazi, bityo ubwoko bwa molekile zimira urumuri bugahinduka uko ubwibande buhinduka. Umurongo wubatswe ukambuka iyo mpinduka ntuzagororoka, kandi nta mibare y'ibarurishamibare yabikosora. Iyi nyandiko yerekana uko wategura umurongo kugira ngo ugire icyo usobanura: hitamo igisubizo fatizo gikwiye, ugumishe intera mu mimerere yiganjemo monomeri, usubiremo ibipimo mu buryo nyabwo, kandi ufate ukugorama nk'amakuru aho kukwita urusaku rw'ibipimo.

Tangirira ku gisubizo fatizo, aho gutangirira ku bisubizo ngenderwaho

Igisubizo fatizo kigena zeru, kandi ku bururu bwa metilene kigomba kuba kirimo ibintu byose uretse irangi. Amazi yo mu rwego rumwe, igisubizo gikomeza pH kimwe na pH imwe, imyunyu imwe, umugabane umwe w'umushongi wongereweho, n'ubushyuhe bumwe. Tegurira ibisubizo by'ikaliburasi muri iyo matirise imwe. Impamvu ni iya shimi, si iy'amabwiriza gusa. Umunyu n'umushongi bihindura uburinganire hagati ya monomeri, dimeri, n'amatsinda manini ya molekile, bigahindura sipegitiri ku burebure bw'umuraba bupimirwaho. Igisubizo fatizo kigizwe n'amazi gusa ntigishobora gukosora impinduka mu bwoko bwa molekile zatewe na matirise. Isesengura rusange rya sipegitiri z'ubururu bwa metilene mu mazi, riboneka mu nyandiko yaryo iboneka ku buntu, ryahinduye ubwibande bwa sodium chloride kuva kuri 0 kugeza kuri 0.15 M kubera nyine ko imbaraga z'iyoni zihindura uburinganire, kandi kwihuza kwa molekile kwiyongeraga uko umunyu wiyongeraga.

Ingaruka imwe mu bikorwa: ntukakore ikaliburasi mu mazi yavanywemo iyoni ngo nyuma upime ingero ziri mu gisubizo cya fosifate gikomeza pH cyangwa mu mazi yanduye yayunguruwe. Iyo nta matirise itarimo ikinyabutabire gipimwa iboneka, kongera igisubizo ngenderwaho mu rugero ubwarwo biruta gukoresha umurongo wo hanze udahuje matirise. Inama zijyanye no gukora ibipimo byizewe mu bisubizo by'amazi ziri mu kiganiro kuri matirise n'ibibangamira ibipimo, naho amahame rusange yo gupima ingano y'irangi asobanurwa mu ncamake y'imitegurire y'ibipimo.

Hitamo intera yiganjemo ubwoko bumwe bwa molekile

Gupima ingano ku gice cya sipegitiri gifite uburebure bw'umuraba burebure hafi ya 664 nm bishingira ku kuba igice kinini cy'irangi kiri nka monomeri. Mu mazi asanzwe, ibyo biba ari ukuri gusa iyo ibisubizo bigifite ubwibande buke, hafi y'intera yo hasi ipimwa muri mikoromolari. Imihanamuko yabonetse mu bipimo byatangajwe yerekana aho iyo ntera igarukira: ikaliburasi zagumishijwe munsi ya hafi 7 mikoromolari mu tuvete twa 1 cm zitanga umuhanamuko uri hafi ya 82,000 M-1 cm-1, mu gihe ikaliburasi yagejejwe kuri hafi 37 mikoromolari imanuka ikagera hafi ya 67,100 kubera ko ibisubizo ngenderwaho byo hejuru biba birimo dimeri itari nke. Buri koefisiyanti yavuzwe hano yerekanywe hamwe n'imimerere yapimiwemo mu nyandiko ngenderwaho kuri sipegitiri y'ubururu bwa metilene, ari ho hakwiye kugereranyirizwa iyo mibare; iyi nyandiko iyikoresha gusa mu kugena intera.

Amabwiriza y'imitegurire ahita akurikira:

1. Gumisha igisubizo ngenderwaho cyo hejuru ku bwibande buke bihagije kugira ngo imiterere ya sipegitiri idahinduka. Mu gihe cyo gutegura uburyo bwo gupima, suzuma intera yose y'urumuri rugaragara (hafi 550 kugeza kuri 750 nm) kuri buri rwego rw'ubwibande aho gupima ku burebure bumwe bw'umuraba. Iyo sipegitiri zashyizwe ku gipimo kimwe zihindura imiterere uko ubwibande buhinduka, shimi iba ihinduka kandi intera iba ari nini cyane.
2. Kurikirana igipimo cya absorbansi hafi ya 610 nm ugereranyije na absorbansi hafi ya 665 nm ku nzego zose. Igipimo cyiyongera uko ubwibande bwiyongera gisobanura ko igice cya sipegitiri cya dimeri kiri kwiyongera kandi ko icyitegererezo cya monomeri kiri kunanirwa. Iki kimenyetso gisobanurwa birambuye mu mabwiriza ku ngaruka zo kwihuza kwa molekile n'ubwibande.
3. Koresha akavete ka 1 cm mu bipimo by'ubwibande buke bwo mu rwego rwa mikoromolari. Ku muhanamuko uri hafi ya 82,000, 5 mikoromolari zitanga absorbansi hafi ya 0.41 naho 10 mikoromolari zigatanga hafi ya 0.82, byombi bikaba bikwiriye ibikoresho byinshi.
4. Ku bisubizo by'ibanze bifite ubwibande bwinshi, gabanya uburebure bw'inzira y'urumuri aho kwemera absorbansi irenze cyane 1, ariko wibuke ko inzira ngufi ikosora ikibazo cyo gupima urumuri, atari shimi. Kwihuza kwa molekile guterwa n'ubwibande, ntiguterwa n'uburebure bw'inzira y'urumuri; bityo igisubizo cy'ibanze gifite ubwibande bwinshi kigomba gukorerwa isesengura ryacyo ryita ku bwoko bwa molekile, aho gukoresha umurongo wa monomeri ufite ubwibande buke.

Guhuza amakuru yose n'icyitegererezo byashingiweho muri byinshi muri ibi byakoresheje sipegitiri 224 kuva kuri 1.1 mikoromolari kugeza kuri 3.4 milimolari, kandi byasanze ikimenyetso cya tetrameri gishobora gutahurwa no munsi ya 34 mikoromolari. Ibyo byabonetse bitanga umurongo ngenderwaho: intera igororotse ni nto kurusha uko umuntu yabyibwira, bityo yigenzure aho kuyifata nk'iyemejwe.

Inzego z'ubwibande, ibipimo bisubiwemo, n'uko bikurikirana

Umurongo ufite utudomo dutatu nta cyo wemeza. Amabwiriza yo kwemeza uburyo muri ICH Q2(R2) asaba nibura ubwibande butanu kugira ngo hasuzumwe ukugororoka, kandi inzego esheshatu kugeza ku munani zitari zeru zitanga umurongo wo gukoresha wizewe kurushaho, cyane cyane hafi y'impera yo hejuru aho kwihuza kwa molekile gutangira. Tandukanya inzego kugira ngo zikwire intera y'ingero uteganya gupima, wongere inzego aho ukugorama gushobora kuba cyane, aho gukoresha uruhererekane rwa geometrike rwatoranyijwe gusa kubera ko rworoshye.

Pima buri rwego kabiri cyangwa gatatu, ukoresheje ibisubizo byateguwe ukwabyo aho gupima gatatu igisubizo kiri mu icupa rimwe. Ibipimo bisubiwemo ku bisubizo byateguwe ukwabyo bigaragaza amakosa yo gutegura; gusubira gupima icupa rimwe bigaragaza gusa urusaku rw'igikoresho. Ubushakashatsi rusange bwo mu 2020 bwapimye buri gisubizo gatatu, kandi ibyo biracyari uburyo bwiza bwo gutangiriraho. Hindura uko ibipimo bikurikirana mu buryo butateganijwe kugira ngo uguhindagurika kw'igikoresho, gufata ku buso bw'ikirahure, cyangwa guhinduka k'ubushyuhe bidasa n'ukugorama. Ubushakashatsi ku tuvete twa quartz bwasanze hafi 3 ku ijana by'irangi ryo mu gisubizo cya 34 mikoromolari bifata ku buso mu minota 10, bityo gumisha igihe cyo guhura n'akavete, akavete ubwako, isuku, n'uko ibikorwa bikurikirana ku buryo bumwe mu bipimo byose.

Urugero rw'imibare rwo gusobanura (si amakuru yapimwe)

Imibare iri hasi yarahimbwe kugira ngo yerekane uko ibarwa. Si ibipimo byo muri laboratwari kandi ntigomba gutangwaho nk'amakuru yapimwe y'ubururu bwa metilene. Icy'ingenzi ni uburyo bw'igenzura buyikikije.

Dufate ibisubizo ngenderwaho bitandatu biri mu gisubizo gikomeza pH gihuje matirise, bifite inzira y'urumuri ya 1 cm, bipimwa kuri 665 nm ugereranyije n'igisubizo fatizo gihuje matirise:

Guhuza impuzandengo ya absorbansi n'ubwibande ukoresheje umurongo ugororotse bitanga umuhanamuko uri hafi ya 0.0805 y'ibipimo bya absorbansi kuri mikoromolari n'agaciro k'aho umurongo ukata umurongo uhagaritse kari hafi ya zeru, gatandukanyijwe na yo n'ibice bike by'igihumbi bya absorbansi. Kugabanya umuhanamuko n'uburebure bw'inzira y'urumuri biwuhindura ubushobozi bugaragara bwo kumira urumuri: 0.0805 kuri mikoromolari bingana na hafi 80,500 M-1 cm-1, bihuye n'intera yiganjemo monomeri mu mazi. Igenzura ry'ingenzi si R squared, izagaragara ko ari nziza cyane uko byagenda kose. Ni agaciro k'aho umurongo ukata umurongo uhagaritse kari hafi ya zeru, igipimo cya A610/A665 kidahinduka kuva kuri S2 kugeza kuri S5, n'ibisigazwa by'itandukaniro hagati y'ibipimo n'icyitegererezo bitatanye nta cyerekezo bihuriyeho. Ukwiyongera guke kw'igipimo kuri S6 ni ikimenyetso nyacyo cyo gukuraho urwo rwego cyangwa kugaragaza 7 mikoromolari nk'umupaka wo hejuru w'agateganyo kuri iyo matirise n'icyo gikoresho bikoreshejwe hamwe.

Urugero rufite ubwibande butazwi rupimwe rukagira 0.245 muri iyo mimerere imwe ruhindurwa mu buryo butaziguye: 0.245 igabanyijwe na 0.0805 kuri mikoromolari itanga hafi 3.0 mikoromolari, mbere yo gukoresha umubare uwo ari wo wose ugorora igabanywa ry'ubwibande bw'urugero. Tanga igisubizo hamwe n'imimerere cyapimiwemo: uburebure bw'umuraba, inzira y'urumuri, matirise y'igisubizo fatizo, intera y'ikaliburasi, n'itariki.

Urupapuro rw'ikaliburasi rwuzuzwa

Koporora iyi nyandikorugero mu nyandiko za laboratwari kuri buri matirise nshya. Matirise imwe, urupapuro rumwe, umurongo umwe.

Umurongo werekana ubwoko bwa reagenti ufite impamvu yo kubamo. Ubururu bwa metilene bugurishwa bushobora kuba umunyu utarimo amazi cyangwa ufite amazi mu miterere yawo, nka trihydrate, kandi gukoresha uburemere bwa mole butari bwo biyobya buri bwibande buteganyijwe nta kimenyetso kigaragara. Igenzura ry'ubuziranenge n'ibisabwa ku kinyabutabire cyo gutangiriraho bisobanurwa mu mabwiriza ku buziranenge n'inzego zabwo.

Genza ukoresheje igisubizo ngenderwaho cy'igenzura cyateguwe ukwacyo

Umurongo w'ikaliburasi ntukwiye na rimwe kwisuzuma ubwawo. Nyuma yo kuwuhuza n'ibipimo, tegura igisubizo ngenderwaho kimwe cy'igenzura uhereye ku gisubizo cy'ibanze cyakozwe n'ikinyabutabire cyapimwe ukwacyo, ku bwibande buri hafi y'igice cyo hagati cy'intera yemewe, maze ugipime nk'urugero rufite ubwibande butazwi. Guhuza kw'ibisubizo bitandukanyijwe n'ijanisha rito byemeza uruhererekane rw'imitegurire; kutabihuza byerekeza ku gisubizo cy'ibanze cyangwa ku kugabanya ubwibande aho kwerekeza ku gikoresho. Subira gupima igisubizo ngenderwaho cy'igenzura kuri buri tsinda ry'ingero. Iyo ibipimo byacyo bihindagurika umurongo wo utahindutse, banza ukeke ibisubizo bikoreshwa cyangwa akavete mbere yo gukeka ingero. Aka kamenyero kamwe gatahura amakosa menshi atagaragara: uburemere bwa mole bw'ikinyabutabire gifite amazi mu miterere yacyo bwakoreshejwe ku icupa ry'ikinyabutabire kitarimo ayo mazi, mikoropipeti itagifite ikaliburasi ikwiye, cyangwa igisubizo gikomeza pH cyateguwe gifite imbaraga z'iyoni zitari zo. Andika ku rupapuro igipimo cy'ingano yagaragajwe n'igenzura ugereranyije n'iyari iteganyijwe, iruhande rw'umuhanamuko, kugira ngo uzarisoma nyuma abone ko umurongo wagenzuwe, ko utashushanyijwe gusa.

Gusobanura ukutagororoka nk'uburyo bwo kumenya ikibazo

Iyo umurongo ugoramye, imiterere y'uko kunanirwa igaragaza impamvu. Ukugorama kumanuka kuri absorbansi yo hejuru kandi imiterere ya sipegitiri idahindutse kwerekeza ku gikoresho, akenshi urumuri rutatanye rutuma absorbansi nini zigaragara nk'aho ari nto. Ukugorama guherekejwe no kwiyongera kw'igice cya sipegitiri kuri 610 nm kwerekeza kuri shimi: dimeri n'amatsinda manini ya molekile bimira urumuri mu buryo butandukanye na monomeri. Igisubizo fatizo kitagera kuri zeru, cyangwa ibisubizo ngenderwaho bigenda bitanga ibipimo bigabanuka uko igihe gihita, byerekeza ku gikoresho kibibitse: gufata ku buso bw'ikirahure cyangwa bw'utuvete, cyane cyane iyo ibihe byo guhura na byo byagiye bitandukana mu bipimo. Naho umurongo mwiza unyura mu tudomo ariko ugatanga ibisubizo bitari byo ku ngero werekeza kuri matirise: ingero zitandukanye n'ibisubizo by'ikaliburasi, bityo ongera wubake umurongo muri matirise y'ingero cyangwa ukoreshe uburyo bwo kongera igisubizo ngenderwaho. Muri buri kibazo, shushanya ibisigazwa by'itandukaniro hagati y'ibipimo n'icyitegererezo ugereranyije n'ubwibande. Gutatana kutagira icyerekezo gushyigikira icyitegererezo cy'umurongo ugororotse; imiterere imeze nk'akamwenyu cyangwa nk'agahanga kabunze irakivuguruza mu buryo bwizewe kurusha umupaka uwo ari wo wose wa R squared, ingingo yemezwa mu buryo bweruye n'amabwiriza yo kwemeza uburyo.

Ubururu bwa metilene butanga ibisubizo byiza iyo ubu buryo bwitondewe bukurikijwe. Igice cya sipegitiri ya monomeri gifite absorbansi ikomeye, shimi yabwo irazwi neza, kandi uburyo ibipimo byabwo binanirwa bugaragara muri sipegitiri mbere yo kwangiza imibare. Ubaka umurongo mu ntera nto, koresha igisubizo fatizo gihuje neza, subiramo ibipimo ukoresheje ibisubizo byateguwe ukwabyo, kandi ureke imiterere ya sipegitiri igene intera. Umurongo uvuyemo uba mugufi, ariko buri kadomo kariho kaba ari ukuri.

Imibare yo gusobanura iri muri iyi nyandiko ikoresha imibare yahimbwe kugira ngo yerekane uburyo. Koefisiyanti ngenderwaho zapimwe hamwe n'imimerere yose yapimiwemo ziboneka mu nyandiko ngenderwaho ya sipegitiri iri ku murongo watanzwe, kandi ubushakashatsi ku kwihuza kwa molekile byashingiweho buri kuri PMID 33251415.