Isingeniso

Enqubweni yokukhiqiza imithi, ama-solvents asetshenziswa kabanzi ezicini eziningi ze-API synthesis, isizinda, ukuhlanzwa kanye nezinqubo zokwakheka. Kodwa-ke, uma lezi zinyibilikisi zemvelo zingasuswa ngokuphelele emkhiqizweni wokugcina, "izincibilikisi ezisele" zizokwakhiwa. Amanye ama-solvent anobuthi, i-carcinogenicity noma ezinye izingozi zempilo ezingase zibe khona, ngakho-ke, ukulawula okuqinile kokuqukethwe kwezincibilikisi ezisele emithini yemithi akuyona nje isixhumanisi esiyinhloko sokuqinisekisa ukuphepha kwemithi yeziguli, kodwa futhi kuyingxenye ebalulekile yokuphathwa kwekhwalithi yemithi.

Ekuhlaziyweni kwe-headspace, isampula livalwa esitsheni esithile sokushisisa, ukuze izingxenye eziguquguqukayo zikhishwe endaweni yegesi ngaphezu kwesitsha, bese le gesi yethulwa ku-chromatograph yegesi ukuze ihlaziywe. Ukuthembeka nokunemba kwalesi sinyathelo esibonakala silula kuncike kakhulu kukhiye osetshenziswayo - izitsha ze-headspace.

Uhlolojikelele lwezindlela zokuhlaziya i-Residual Solvent

Izinhlobonhlobo eziningi zezincibilikisi eziyinsalela ezingase zibe khona emithini yemithi, enezici ezihlukahlukene ezinobuthi, zidinga ukuhlukaniswa futhi zilawulwe ngokuya ngezingozi ezingaba khona lapho zihlaziywa futhi zilawulwa. Izikhumbuzi zokuhlukaniswa ngezigaba ezibuyekezwe ontanga zihlukanisa izincibilikisi eziyinsalela zibe izigaba ezintathu ezilandelayo:

1. Ikilasi 1: Izinyibilikisi ezingavunyelwe

Kubandakanya i-benzene, i-methylene chloride, i-1,2-dichloroethane, i-carbon tetrachloride, njll., ene-carcinogenicity enamandla nobungozi bemvelo, kufanele kugwenywe ekukhiqizeni. Imikhawulo ilawulwa ngokuqinile kakhulu futhi imvamisa ibalwa kumazinga we-ppm noma ngaphansi.

2. Ikilasi 2: Izincibilikisi zingaphansi kokulawulwa okulinganiselwe

Kubandakanya i-toluene, i-acetonitrile, i-DMF, i-isopropyl alcohol nokunye. Iminyaka yobudala yalezi zincibilikisi iyamukeleka ngaphansi kwemikhawulo ethile, kodwa isenazo izingozi ezithile ezinobuthi. Imikhawulo isethwe ngokusekelwe ku-ADI futhi ngokuvamile idinga ukuqapha okuqinile.

3. Ikilasi 3: Izincibilikisi ezinobuthi obuphansi

Lezi zihlanganisa i-ethanol, i-propanol, i-ethyl acetate, njll., ezinobuthi obuphansi kubantu futhi ngokuvamile zibhekwa njengephephile emithini yemithi kuze kufike ekuthathweni kwansuku zonke kwe-50 mg.

Ukuze kunqunywe ngokunembile uhlobo nokuqukethwe kwalezi zincibilikisi eziyinsalela, i-gas chromatography (GC) njengamanje iyindlela yokuhlaziya evame kakhulu, enezinzuzo ezibalulekile zokuzwela okuphezulu, ukusebenza kahle kokuhlukana okuphezulu, nokusebenza kwezinhlanganisela eziguquguqukayo, ezingahlangabezana nezidingo zokuhlaziywa kwe-solvent eyinsalela ukuze kutholwe umkhondo.

Phakathi kwezindlela ezihlukahlukene zokujova ze-meteorological chromatography, ubuchwepheshe bomjovo we-headspace busetshenziswa kakhulu ekutholeni izincibilikisi ezisele emithini yemithi. Ubuchwepheshe ngenxa yothando lwalelo sampula elivalwe ebhodleleni le-headspace, lishisiswe kumazinga okushisa afanele, yilo elincibilikisayo kusampula yokushintshashintsha kwesikhala segesi yebhodlela, bese kusuka esikhaleni ukuze kukhishwe umthamo othile wegesi eqashiswe ku-GC ukuze ihlaziywe.

Izinzuzo zokuphakelwa kwe-headspace zihlanganisa:

• Isampula yokwelashwa kwangaphambili encishisiwe: akukho misebenzi eyinkimbinkimbi yokukhipha i-solvent noma i-dilution futhi amasampula angashiswa ngokuqondile ekamelweni elivaliwe;
• Ukukhiqiza kabusha okuthuthukisiwe nokuzinza: ngokulawula ngokunembile izinga lokushisa lokushisa nesikhathi, ukuguquguquka kwesampula kuyahambisana, kunciphisa amaphutha okusebenza;
• Igwema ukungcoliswa noma ukulimala kwekholomu: ingxenye yegesi kuphela eyethulwa ohlelweni lwe-chromatography, okunciphisa kakhulu ukuphazamiseka kwezingxenye ezingaguquguquki ngekholomu nomtshina.
• Ifanele ukuhlaziya okuzenzakalelayo: isistimu yomjovo we-headspace ingaxhunywa ngaphandle komthungo ku-autosampler, ifanele izidingo zokutholwa kokuphuma okuphezulu.

Kodwa-ke, isitsha sesampula esizinzile nesinokwethenjelwa, izitsha ze-headspace, zibalulekile ekuhlaziyweni kwe-headspace okuphumelelayo nokunembile, okungalawuli kuphela ukuziphatha kokuguquguquka kanye nomthelela wokuvala wesampula, kodwa futhi kuthinta ngokuqondile imiphumela yokugcina yokuhlaziya.

Incazelo kanye nemithelela yezitsha ze-Headspace

Endleleni yesampula ye-headspace, ukushisisa nokushintshashintsha kwesampula kanye nenqubo yokutholwa kwesikhala segesi kokubili kwenzeka ezitsheni ze-headspace njengeziqukathi ezingangeni moya, nakuba kubonakala kulula, kodwa ukuklama nokusebenza kwezitsha ze-headspace kunomthelela omkhulu ekuthembekeni kwayo yonke inqubo yokuhlaziya.
Izitsha ze-Headspace ziyisampuli zamavolumu eziklanyelwe umjovo we-headspace ku-chromatography yegesi. Ukwakhiwa kwayo okujwayelekile kuqukethe izingxenye ezilandelayo:

Ibhodlela: ngokuvamile eyenziwe ngengilazi ephezulu ye-borosilicate, enokumelana okuhle kokushisa okuphezulu kanye nokungangeni kwamakhemikhali, okuvame ukutholakala ku-10ml, 20ml, noma amavolumu amakhulu;

Ukuvuleka/uchungechunge lwebhodlela: ikakhulukazi ukuvulwa okujwayelekile okungu-20mm, okufanelekile kumakepisi we-aluminium kanye nezinhlelo zokusampula ngokuzenzakalela;

Cap: ngokuvamile icindezelwe kusuka ezintweni ezithobelayo ukuze kuqinisekiswe ukuqina kwebhodlela;

I-Gasket: kukhona i-PTFE ne-silicone eyinhlanganisela yezinto zokwakha, enokumelana okuhle kwezinga lokushisa eliphezulu kanye nokungangenisi kwamakhemikhali, ingamelana nokusampula kokubhoboza okuningi ngaphandle kokuvuza.

Indima eyinhloko yebhodlela le-headspace ukuhlinzeka ngendawo evaliwe, engenzi lutho futhi elawulwayo, i-solvents eguquguqukayo kusampula ngaphansi kwezimo zokushisa yindlela oh ibhodlela ngaphezu kwesikhala segesi, ukwakheka kommeleli wokulinganisa igesi wokuhlushwa kwe-solvent kusampula yasekuqaleni.

Ikakhulukazi, indima yayo ibonakala kulezi zici ezilandelayo:

Isiqinisekiso sokuvala: ukubekwa uphawu okuhle ukuqinisekisa ukuthi isampula ekushiseni noma ekuphumuleni njalo ngeke kube ngenxa yokuvuza nokulahlekelwa kwe-solvent;

Isivikelo sezinto ezingasebenzi: ingilazi yekhwalithi ephezulu kanye nezinto ze-gasket zivimbela ukusabela ngesampula noma i-solvent, ukugwema ukwethulwa kwezinto ezingamanga noma ukuphazamiseka kwesignali;

Izimo zevolumu eziqhubekayo: amabhodlela ajwayelekile afaka isandla ekuzinzeni kwe-headspace kanye nokukhiqiza kabusha, ukwenza kube lula ukulinganisa nokuqhathaniswa kwemiphumela yokuhlaziya.

I-Headspace vials i-pessimistic antipathy isetshenziswa kusampula ye-headspace ezenzakalelayo. Ukuhamba komsebenzi ngokuvamile kuba kanje:

1. Isixazululo sesampula sengezwe ku-vial ye-headspace futhi sivalwe;
2. I-autosampler iphakela i-vial ibe imojuli yokushisisa i-thermostatic;
3. Isampula iyashiswa ku-vial kuya kumazinga okushisa amisiwe futhi izingxenye eziguquguqukayo zithuthela ku-headspace;
4. Inalithi yomjovo ibhoboza i-gasket futhi idonsa umthamo wegesi kusuka ku-headspace;
5. Igesi ifakwa ku-chromatograph yegesi ukuze kuhlukaniswe i-alamu nokutholwa.

Kule nqubo, ukuzinza kwesakhiwo, ukusebenza kwe-gasket puncture, kanye nokuvala izitsha ze-headspace kuhlobene ngokuqondile nokuvumelana kwesampula kanye nokunemba kwemodeli. Ikakhulukazi, ukusetshenziswa kwezitsha ezijwayelekile, ezinokwethenjelwa ze-headspace ekusebenzeni okuzenzakalelayo kuyisihluthulelo sokuqinisekisa ukuthi inqubo yokuhlaziya isebenza kahle futhi inciphisa izinga lokuhluleka.

Kungani I-Headspace Vials Idingeka?

Nakuba i-chromatograph yegesi nomtshina kuyizinto ezisetshenziswayo ezibalulekile ekuhlaziyeni okuncibilikayo kwensalela, indima ye-vial ye-headspace ibaluleke ngokufanayo. Njengomthwali wabahlaziyi kusukela kusampula yokwelashwa ngaphambi komjovo, ukusebenza kwayo kuhlobene ngokuqondile nokuzinza kwalo lonke uhlelo lokuhlaziya nokuthembeka kwedatha.

1. Ubuqotho besampula nokulawulwa kokushintshashintsha

Izincibilikisi eziyinsalela ngokuvamile ziyizingxube ezibilisa kancane, eziphilayo ezisengozini enkulu yokulahlekelwa ngesikhathi sokuchayeka, ukushisisa noma ukugcinwa. Uma izitsha ze-headspace zinganakekelwa ngokuvaleka okuqinile kuwo wonke umjikelezo wokuhlaziya, okuqukethwe kwe-solvent kungase kushintshe, okuholela emiphumeleni echemile.

Izitsha ze-headspace zekhwalithi ephezulu zingashiswa zibe ngaphezu kuka-100-150 ° C esimweni esivaliwe, kuqinisekiswe ukuthi izingxenye eziguquguqukayo zikhishwa kuphela futhi zihlaziywe ngaphansi kwezimo ezimisiwe;

Ukulawula okunembile kwesampula ukuze kufinyelelwe ekulinganeni koketshezi lwegesi kumazinga okushisa angashintshi kanye nevolumu kukhulisa ukunemba nokukhiqizwa kabusha kwemiphumela.

2. Umthelela wokuvala ukusebenza emiphumeleni yokuhlaziya

Isistimu yokuvala ye-Vial ye-Headspace ngokuvamile iqukethe izingxenye ezintathu: i-cap, i-gasket kanye ne-mouthpiece. Ukufakwa uphawu okungalungile kunoma iyiphi indawo kungase kubangele ukuvuza kwesampula, umsindo ongemuva ophakeme, noma ngisho nokungcoliswa kwesampula.

Ikhwalithi ephezulu ye-PTFE/silicone gaskets ayigcini nje ngokumelana namazinga okushisa aphezulu namakhemikhali, kodwa futhi ingakwazi ukumelana nama-puncture amaningi futhi igcine uphawu oluhle;

I-gasket yekhwalithi ephansi noma indlala exegayo ingabangela ukuncibilika kwe-solvent ngaphambi kokuhlaziywa noma phakathi nokushisisa, kuthinte ngokuqondile indawo ephakeme kakhulu futhi kunciphise ukunemba komthamo.

3. Ukuhambisana nezinhlelo ze-autosampling

Izijovo ezizenzakalelayo ze-headspace zivame ukusetshenziswa ezindaweni zokucwaninga zesimanje ukuze kuthuthukiswe ukusebenza kahle nokuvumelana kwemiphumela, futhi ukwakheka okujwayelekile kwe-Headspace vial kuyakuvumela ukuthi ivumelane ngqo nemikhiqizo emikhulu yezinhlelo zomjovo.

Ubukhulu obujwayelekile buqinisekisa ukuthi amabhodlela angakwazi ukubonakala ngokuzenzakalelayo, abekwe kahle futhi abhobozwe kumjovo;

Ukunciphisa amaphutha enziwa ngesandla kuthuthukisa ukusebenza kahle kokucubungula isampula kanye nokuvumelana kwedatha, okwenza i-Headspace vial ifaneleke ezimweni zokuhlolwa komphumela ophezulu.

4. Ukungangeni kwamakhemikhali kwezinto

Ikhemikhali yamabhodlela nezinto zokuvala akumele zishaywe indiva lapho kuhlaziywa ama-trace solvents. Izinto ezisezingeni eliphansi zingakhangisa noma zisabele ngama-athomu, okuholela emiphumeleni echemile.

Ingilazi ye-Borosilicate i-inert yamakhemikhali futhi izinzile ngokushisa, ivimbela i-solvent adsorption noma ukuwohloka kokushisa;

Kwezinye izinhlelo ezikhethekile ze-solvent, ama-gaskets enziwe ngezinto ezikhethekile ayadingeka ukuze kuqinisekiswe ukuzwela kokutholwa kanye nokuzinza kwesampula.

I-Headspace vial ingaphezu nje kwesitsha sesampula esilula, iyisici esibalulekile ekuqinisekiseni ukuthi imiphumela yokuhlaziywa kwe-solvent eyinsalela iyiqiniso, ayiguquki futhi iyakwazi ukukhiqizwa kabusha. Ithatha imisebenzi eminingi ebalulekile kulo lonke uchungechunge lokuhlaziya, njengokuvikela ukuvala, ukulawula ukuguquguquka, ukufaniswa kwesistimu, isiqinisekiso sokungatholakali kwamakhemikhali, njll. Ingenye yezinto ezisebenzisekayo ezingenakubuyiseleka zokubona ukuhlolwa kwezidakamizwa kwekhwalithi ephezulu.

Izinto Ezibalulekile Ekukhetheni Isitsha Se-Headspace Esifanele

Ekuhlaziyweni kwe-solvent eyinsalela, ukukhethwa kwe-vial ye-headspace efanele kuyimfuneko yokuqinisekisa ukunemba kwedatha kanye nokuvumelana kwendlela. Izidingo ezihlukile zokuhlola, izinhlobo zesampula kanye nezinkundla zezinsimbi zinezidingo ezihlukile ze-headspace vial material, isakhiwo kanye nokusebenza. Izinto ezilandelayo ezibalulekile kufanele zicatshangelwe lapho kukhethwa i-vial ye-headspace:

1. Material: uhlobo ingilazi futhi obala

• Ingilazi ye-borosilicate yekilasi I: impahla yebhodlela ekhethwayo yokuhlaziywa kwe-solvent eyinsalela. Ukumelana nokushisa kwayo okuhle kakhulu namakhemikhali kanye nokugxiliswa okuphansi kakhulu kwama-ion awanayo kuvimbela ukusabela kwamakhemikhali phakathi kwe-solvent nebhodlela, ukugwema ama-positives angamanga noma ukuphazamiseka kwesignali.
• Ukucaca okuphezulu kwebhodlela: ivumela ukubonwa okusheshayo kwesimo sesampula ngesikhathi sokugoba, ukuhlolwa noma ukuhlolwa kwekhwalithi, njengokuba khona kwezimvula, inani eliqondile loketshezi, njll., kanye nokukhonjwa kalula ngamasistimu azenzakalelayo.

2. Ukukhetha ivolumu: ukucaciswa okuvame ukusetshenziswa 10ml, 20ml

Ukukhethwa komthamo we-Vial ye-Headspace kufanele kusekelwe kwinhlanganisela yalezi zinto ezilandelayo:

• Ivolumu yesampula: Ngokuvamile ivolumu yesampula imayelana ne-50% yevolumu yebhodlela ukuze kuqinisekiswe indawo yekhanda eyanele (indawo yegesi) yokulinganisa kwe-volatilization;
• Izidingo Zendlela Yokuhlaziya: Isibonelo, indlela ye-USP <467> ye-solvent eyinsalela incoma ukusetshenziswa kwe-vial ye-headspace engu-20 ml;
• Ukuhambisana kwe-Autosampler: qinisekisa ukuthi ibhodlela elikhethiwe lisekela imodeli yensimbi esetshenzisiwe, ikakhulukazi ibhodlela elingaphezu kwe-aperture.

3. Uhlobo lwe-gasket yekhava: ukuvala uphawu nokufaneleka kwamakhemikhali

Izinto ze-Gasket: evame ukusetshenziswa kakhulu yi-PTFE eyinhlanganisela ye-gasket, isakhiwo sayo esinezingqimba ezimbili sihlanganisa inertia yamakhemikhali ye-PTFE nokunwebeka kokuvalwa kwe-silicone, ingamelana nokubhobozwa kwezinga lokushisa eliphezulu futhi igcine ukuvala kahle; ngezincibilikisi ezinamandla ezigqwalile noma ezimbi kakhulu, ungakhetha ungqimba oluqinile lwe-PTFE gasket eliqinisiwe.

Izinhlobo zamabhodlela: Izigqoko ze-Aluminium zifanele izinsimbi eziningi, ezine-gland eqinile kanye nokubekwa uphawu okuhle kakhulu; Amakepisi kazibuthe afaneleka kumasistimu esampula ngokuzenzakalelayo anokukhonjwa kazibuthe, okusiza ukuthuthukisa ukusebenza kahle kokuphakela kanye nokunemba kokuma; Amakepisi anemicu, nakuba elungele ukusebenza mathupha, angase angavali kanye nezinhlobo zezindlala futhi afaneleka kakhulu izigaba zokuthuthuka noma izimo ezingaphumeleli kakhulu.

4. Ukusebenziseka kabusha nokucatshangelwa kwezindleko

Izitsha zengilazi ezisebenzisekayo kabusha (ezidinga ukuhlanzwa kwezinga lokushisa eliphezulu nokuvalwa inzalo) zifaneleka kwezinye izindlela ezingezona ezekhemisi noma izifundo zokuthuthukisa futhi zinganciphisa izindleko zesikhathi eside;

Kodwa-ke, ekwenzeni i-GMP noma amalabhorethri asemthethweni okulawula ikhwalithi, izitsha ezisetshenziswa kanyekanye zingcono ukuze kuqinisekiswe ukuhlanzeka nokugwema ukungcoliswa;

Uma uthenga ngamaqoqo, kubalulekile futhi ukukala ikhwalithi yomkhiqizo, ukuvumelana kweqoqo-to-batch, kanye nentengo ukuze ukhethe umphakeli onikeza ibhalansi yokusebenza nezindleko.

Ukukhethwa okunengqondo kwe-vial ye-headspace akuyona nje umsebenzi oyisisekelo, kodwa futhi ukubonakaliswa kokwazi ukulawula izinga. Konke ukukhethwa kwepharamitha okubonakala kuncane kudlala indima ebalulekile ekunembeni kwemiphumela, ukuzinza kwesistimu nokusebenza kahle kwelabhorethri. Ngakho-ke, ukuqonda okujulile kwalezi zici ezibalulekile kuyikhono lochwepheshe elibalulekile kuwo wonke uchwepheshe osebenza ekuhlaziyeni kwezemithi.

Imibuzo Evame Ukubuzwa Namanothi

Nakuba izitsha ze-headspace zisetshenziswa kakhulu ekuhlaziyweni kwe-solvent eyinsalela, uchungechunge lwezinkinga lungase luvele ekusebenzeni ngenxa yokuphatha okungalungile noma ukukhethwa kwezinto ezisetshenziswayo. Okulandelayo yizinkinga ezivamile kanye nezincomo zokuvimbela:

1. Ungakugwema kanjani ukungcoliswa kwesampula

Ukungcoliswa kwesiphambano akuthinti nje kuphela ukunemba kwemiphumela yokuhlaziya, kodwa futhi kungabangela ukuphazamiseka okufihlekile kwesikhathi eside ohlelweni lokuthola, ikakhulukazi engozini enkulu lapho kuhlaziywa amazinga aphansi. Izinyathelo ezilandelayo zingagwema ngempumelelo le nkinga:

• Beka kuqala ukusetshenziswa kwezitsha ezilahlwayo nama-cap pads: lena indlela eqondile nephumelelayo, ikakhulukazi ekulawuleni izinga lezemithi kanye nokuhlolwa kokulawula;
• Shintsha noma uhlanze kahle izitsha eziphinde zasetshenziswa: uma ukusetshenziswa kabusha kudingekile, qinisekisa ukuthi ahlanzwa kahle kusetshenziswa izinyathelo ezifana namanzi akhishiwe, izinyibilikisi eziphilayo, nokomisa izinga lokushisa eliphezulu;
• Izinqubo zokusabalalisa eziqinile: sebenzisa amathuluzi akhethekile wamapayipi ukuze ugweme ukuconsa kwesampula phezu noma eduze kwebhodlela;
• Hlanza izihlalo zebhentshi zamathuluzi namagilavu: lapho uphatha ama-solvents aguquguqukayo, amagilavu ​​kufanele ashintshwe njalo ukuze avimbele ukusabalalisa ukungcola ngokuphatha.

2. Ukuvuza kwe-cap ngesikhathi sokushisa

Ekuhlaziyweni kwe-headspace, isampula idinga ukushisisa kufika ku-80-120°C noma ngisho nangaphezulu. Uma amakepisi noma ama-gaskets engavalwanga kahle, izincibilikisi zingase ziphume ngesikhathi sokushisisa, okuholela ekuguquguqukeni kwedatha noma imiphumela ephansi.

• Khetha ama-gaskets ekhwalithi ephezulu: kufanele zibe nokumelana nokushisa okuhle kanye nokunwebeka kokubhoboza ukuze kuqinisekiswe ukuthi uphawu aluxegi;
• Amandla we-capping alungile: i-capping manual noma othomathikhi idinga ukulinganisela, ikhululeke kakhulu ingase ivuze, iqine kakhulu ingase ibhubhise i-gasket noma ibangele ukuthi ibhodlela liqhume;
• Ukuhlola njalo inaliti yesistimu yokuphakelayo: inaliti egugile noma ekhubazekile ingase ivimbele i-gasket ukuthi ingazivali, okuholela ekuvuzeni;
• Ukulungiselelwa kwezinga lokushisa okunengqondo: Akufanele idlule umkhawulo ophezulu wokumelana nokushisa kwe-gasket noma i-cap, ngokuvamile elawulwa ebangeni lika-110-130 ℃ iphephile.

3. Ukuhlanza i-vial kanye nezincomo zokugcina

Ngokusetshenziswa kabusha kwe-vial okungase kuhileleke ekulawuleni izindleko noma esigabeni sokuthuthukisa indlela, ukunaka okukhethekile kudingeka kukhokhwe ekuhlanzeni nasekugcineni ukuze kugwenywe ukwethulwa kokungcola noma izincibilikisi eziyinsalela:

• Izinyathelo zokuhlanza eziphakanyisiwe: hlambulula izikhathi eziningana ngamanzi angcolile; hashaza ngama-solvents afanelekile; ukuhlanzwa kwe-ultrasonic kuye ngezinga lokungcola; izinga lokushisa eliphezulu ukomisa ku-105℃-120℃ ukuze kuqinisekiswe ukuthi akukho umswakama osele noma isincibilikisi.
• Izincomo zesitoreji: isitoreji esihlanzekile, esomile nesivaliwe, ukuze kugwenywe uthuli, izinto eziguquguqukayo ziphinde zingcoliswe; ngaphambi kokusetshenziswa uma igcinwe isikhathi eside kakhulu, kunconywa ukuthi uphinde uhlole futhi uhlanze futhi; gwema ukuchayeka isikhathi eside elangeni noma izinga lokushisa eliphezulu, ukuvimbela ukuwohloka kwengilazi noma ukuguga kwe-gasket.

Ngokwazi kahle le mininingwane yokusebenza ebalulekile, awukwazi nje ukuthuthukisa ukunemba nokuphindaphinda kokuhlolwa, kodwa futhi wandise ngempumelelo impilo yesevisi yemishini futhi unciphise izinga lokuhluleka. Ezintweni zokuhlaziya ezifana nezincibilikisi eziyinsalela, ezizwela kakhulu ekulandeleni ukuhlukahluka, ukuphathwa okunemininingwane yesixhumanisi ngasinye sokusebenza akufanele kunganakwa.

Isiphetho

Emkhakheni olawulwa kakhulu futhi onembile wokuhlaziywa kwe-solvent yezinsalela zemithi, i-headspace vial, nakuba incane, idlala indima ebalulekile nebalulekile. Kusukela ekugcineni, ukuvalwa nokushisisa isampula, kuya ekuxhumaneni nesistimu ye-autosampling, iwumugqa wokuqala wokuzivikela kulo lonke uchungechunge lokuhlaziya ukuze kuqinisekiswe ukufaneleka kwedatha.

Izitsha zekhwalithi ye-headspace azigcini nje ngokuvikela ubuqotho besampula, zivimbela ukulahlekelwa kokushintshashintsha, futhi zithuthukise ukuhambisana komjovo, kodwa futhi ziyisisekelo esidingekayo sokutholwa okuphindaphindeka kakhulu nokuzwela ekuhlaziyweni okuzenzakalelayo. Ikakhulukazi uma ubhekene nokuhlaziywa kobuningi bezinga lokulandela okudingwa izindinganiso ze-pharmacopoeia, isici esincane se-cap, impahla engafanele, noma ngisho nomsebenzi wokugcwalisa isampula okungenangqondo kuzoba nomthelela ongenakunakwa emiphumeleni yokuhlaziya.

Njengoba ukuthuthukiswa kwezidakamizwa nokulawulwa kwekhwalithi kuqhubeka nokwandisa izinga lokuzenzakalela kanye nokutholwa kokuphuma, amazinga ekhwalithi wezitsha ze-headspace nawo ayaphakanyiswa. Kusukela ekuhlanzekeni kwezinto ezibonakalayo, ukungaguquguquki kwegama kuya ekuvumelaneni kwesistimu, izitsha ze-headspace zesikhathi esizayo akufanele nje zizinze futhi zithembeke, kodwa futhi zidlale indima "yesixhumi esibonakalayo esijwayelekile" elabhorethri yokuhlela, ukusiza ukulandelelwa kwedatha, ukukhiqizwa kwendlela kanye nokuthuthukiswa okuqhubekayo kokulawulwa kwekhwalithi.