igama elingukhiye

Uphethiloli; Izithasiselo; I-Aniline; I-chromatography yegesi;

1. isingeniso Ngenxa yokuvinjelwa kwamandla kaphethiloli wasekhaya kanye nobuchwepheshe bokucwengisiswa, imikhiqizo kawoyela ekhiqizwa izindawo ezijwayelekile zokuhluza emakethe iyashoda, okwenza inani elikhulu lemikhiqizo kawoyela ehlanganisiwe igcwale imakethe. Uphethiloli oxutshwe njalo uhlanganiswa ne-naphtha enamakha axutshwe (amafutha alula) njengezinto ezingavuthiwe. Kodwa-ke, ngemuva kwamanani aphezulu wezinto ezibonakalayo kanye nokukhuliswa kwenzuzo, izinhlanganisela ze-aniline zivame ukusetshenziswa njengezithasiselo zikaphethiloli ezingajwayelekile. Ukuze wenze inkomba yekhwalithi kaphethiloli enezithasiselo ezinjalo ihlangabezane nezindinganiso zikaphethiloli wezimoto kazwelonke, ngokwesibonelo, ukungeza i-1% (ingxenye enkulu) i-N-methylaniline ingandisa inombolo ye-octane ngamayunithi angu-2-4 [1]. Kodwa-ke, izithasiselo ze-aniline zinezingozi ezingase zibe khona ekuhambeni nokuphepha kwezimoto, kanti i-N-methylanilines iyinhlanganisela equkethe i-nitrogen, okuzoholela ekwandeni kokuqukethwe kwe-nitrogen oxides ekukhishweni kwezimoto, okubangela imiphumela eyingozi endaweni yomoya nempilo yabantu. . Izingxenye eziyinhloko zezithasiselo ze-aniline zifaka i-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-methylaniline ne-N, i-n-dimethylaniline. Njengamanje, izindlela ezivame ukubikwa zokutholwa kwezinhlanganisela ze-methylaniline zihlanganisa i-naphthalene diethylamine spectrophotometry, i-gas chromatography-nitrogen chemiluminescence ukuthola, ukusebenza okuphezulu kwe-chromatography ye-liquid, njll. [2-4]. I-naphthalene diethylamine spectrophotometry yendabuko iphazamisa umphumela wokunquma ngenxa yokuvela kokusabela okuseceleni, futhi indlela ye-HPLC ithinteka ngokungagwemeki ngokuphazanyiswa kwe-matrix kaphethiloli.

Indlela yokuthola igesi ye-chromatograph-nitrogen chemiluminescence idinga ukulungiswa komtshina obizayo we-nitrogen chemiluminescence ongathola ngokukhetha i-nitrogen. Izinga likazwelonke elisanda kubhalwa (elisazoshicilelwa) elithi "I-Chromatography Yegesi Yokunqunywa Kwe-Oxycompounds kanye Nezingxube ze-aniline Kuphethiloli" liphinde lichaze indlela yokuhlaziya kusetshenziswa ama-Deans switch kumakholomu amabili aphambene kusetshenziswa umtshina womlilo we-hydrogen ion ion ovamile futhi ongabizi kakhulu. Ngale ndlela, i-ThermoFisher Scientific ishicilele iphepha lesicelo (Amanothi ohlelo C GC-50). Njengokwenza lula, leli phepha lethula indlela yekholomu eyodwa esheshayo esuselwe kuzinga lendawo le-DB37/T-2650 elikhishwe iSifundazwe saseShandong ngo-2015 [5]. Imiphumela ibonisa ukuthi le ndlela ilula ukuyisebenzisa, ngokuphindaphinda okuhle nokunemba okuphezulu. Ngasikhathi sinye, indlela yathuthukiswa ukuxazulula inkinga yokuphazanyiswa kwe-aniline quantification ngokwakhiwa kwe-matrix kaphethiloli.

2. Uhlolojikelele lwesimiso sendlela Kukholomu ye-polar polyethylene glycol (PEG), izinhlanganisela ze-aniline kuphethiloli wezimoto zahlukaniswa ne-matrix kaphethiloli, futhi i-acetophenone yasetshenziswa njengezinga langaphakathi. Okuqukethwe kwe-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-toluidine ne-N, i-n-dimethylaniline kuphethiloli wezimoto kwanqunywa i-chromatograph yegesi efakwe umtshina we-ionization wamalangabi (FID), futhi ukugxila kwengxenye ngayinye kwaba kubalwe ngereferensi yezinga langaphakathi.

3. Izinsimbi

3.1 Trace 1300E Gas Chromatograph nge-shunt/non-shunt inlet,

AS1310 isampula okuzenzakalelayo, Flame ionization umtshina (FID);

3.2 Isofthiwe ye-Chameleon

3.3 I-Microsyringe: umthamo ngu-10uL.

4. Ama-reagents nezinto zokwakha

4.1 Ikholomu: Ikholomu ye-Polar, i-TG-Wax, ubude bekholomu 60m,

Ububanzi bangaphakathi bungu-0.25mm, ukujiya kwefilimu ewuketshezi ngu-0.25μm

4.2 Ngaphandle kwalapho kucaciswe ngenye indlela, ama-reagents asetshenziswe kule ndlela ahlanzekile ngokohlaziyo futhi avumelekile

Sebenzisa amanye ama-reagents wokuhlanzeka okuphezulu.

Ama-reagents asetshenziselwa izinjongo zekhwalithi nenani, okuhlanganisa i-aniline (Ca #62-53-3), N-

I-Methylaniline (CAS#100-61-8), i-o-methylaniline (CAS#95-53-4),

I-P-methylaniline (CAS#106-49-0), i-m-methylaniline (CAS#188-44-)

1) kanye ne-N, n-dimethylaniline (CAS#121-69-7), izinga langaphakathi kwakuyi-phenylene

I-Ketone (CASA #96-86-2).

5. Izindlela zokuhlola

5.1 Ukusungulwa kwejika elijwayelekile

5.1.1 Ukulungiswa kwesixazululo esijwayelekile: Zonke izinto ezijwayelekile ziyi-isooctane (i-chromatographically pure)

I-Dilution, ngokulandelana elungiselelwe ngezinto eziyisithupha ze-aniline ku-0.1%, 0.2%, 0.5%, 1%,

Ukuze uthole amasampula ajwayelekile kumazinga angu-1.5% no-2%, bheka Ithebula 1 ukuze uthole ulwazi oluningiliziwe lokuhlushwa.

Ithebula 1. Ithebula lesampula elijwayelekile lokuhlushwa

5.1.2Amasampula ajwayelekile ahlaziywa ngokwendlela ye-GC kuThebula lesi-2

Ithebula 2. Indlela ye-GC

5.1.3 Ikhwalithi: Izingxenye ziyikhwalithi ngokuya kwesikhathi sokugcinwa kwengxenye ngayinye, futhi i-chromatogram yesampula evamile yohlobo olujwayelekile (izinga lokugxilisa elingu-0.1%) liboniswa kuMfanekiso 1.

Umfanekiso 1. I-Chromatogram yesampula evamile evamile

5.1.4 Misa ijika elijwayelekile. Hlela indlela yokulinganisa endleleni yokucubungula idatha kusofthiwe ye-Chameleon, uhlobo lokulinganisa luqondile (aluphoqelelwe phezu komsuka), uhlobo lokuhlola luyindawo ephakeme kakhulu, futhi izinga langaphakathi liyahlukahluka. Isibalo sejika esijwayelekile kanye ne-coefficient yokuhlobana komugqa yengxenye ngayinye kuboniswa kuThebula 3, futhi ijika elijwayelekile lengxenye ngayinye liboniswa kuMfanekiso 2-7.

ithebula 3. Idatha yejika yokulinganisa

5.1.5 Ukubalwa kwemiphumela: Isilinganiso sendawo ephakeme kakhulu yengxenye ngayinye endaweni ephakeme kakhulu ye-acetophenone sibaliwe. Ingxenye yevolumu yobuningi bengxenye ngayinye ehambisana nesilinganiso ifundwa kujika elifanele lokulungisa, futhi umphumela unembile ukuze ufike ku-0.01%.

6. Imiphumela nengxoxo

6.1 Ijika elijwayelekile: Ijika elijwayelekile lisungulwa ngemikhiqizo engu-6 ejwayelekile, ububanzi bokugxiliswa kwevolumu busuka ku-0.01% ukuya ku-2.0%, futhi i-coefficient yomugqa ongu-R2 inkulu kuno-0.999, ngokulandelanayo (bona Ithebula 3 ukuze uthole imininingwane).

6.2 Indlela yokuqinisekisa nokwenza kahle: Uma kuqhathaniswa nendlela yokushintsha amaDini, indlela yekholomu eyodwa eyethulwe kuleli phepha inezinzuzo zezindleko eziphansi, ukusebenza okulula kanye nokuphindaphindeka okuphezulu. Kodwa-ke, ezinye izingxenye ze-matrix kaphethiloli zingathinta ama-aniline compounds.

Isibonelo, ngokwendlela echazwe kuleli phepha, lapho kuhlolwa isampula ye-matrix kaphethiloli engenalutho, kutholakala ukuthi ngemva kokuqhathanisa ne-chromatogram yesampula evamile, kukhona ukuphakama okungaba ngu-0.04min (ububanzi besiqongo buwububanzi obungu-0.04min). 0.07min) kusuka engxenyeni ye-aniline yomkhiqizo ojwayelekile, ophazamisa ukuhlaziya i-aniline. (bheka Umfanekiso 2)

3

I-FIG. 2. Ukuqhathaniswa phakathi kwe-aniline standard solution spectra kanye ne-blank gasoline matrix spectra

Ukuze uqinisekise ukuthi le nto ayiyona i-aniline, futhi isuse ukuphazamiseka kwe-aniline quantification. Indlela kuleli phepha ilungiselelwe, futhi inqubo yokwenyuka kwezinga lokushisa injalo

Incazelo ye-DB37/T-2650 ye-5℃/min ishintshile yaba ngu-4℃/min. Amasampula e-matrix kaphethiloli anamasampuli ajwayelekile angeziwe ahlaziywa ngale ndlela. Njengoba kungabonwa ku-FIG. 3,

Indlela elungiselelwe ingahlukanisa le ngxenye ku-aniline ku-matrix kaphethiloli, futhi iphinde ifakazele ukuthi isampula likawoyela lingatholwa ngendlela ye-DB37/T-2650

Inani eliphakeme ku-21.905min lalingeyona i-aniline. Iqembu lokuphazanyiswa linqunywe ukuthi libe yi-naphthalene nge-qualitative mass spectrometry kanye nokuqhathanisa okujwayelekile.

I-FIG. 3. Ukuqhathaniswa kwe-spectra yamasampuli kawoyela, amasampula e-aniline kanye ne-matrix kaphethiloli (indlela elungiselelwe)

6.2 Izinga lokutholwa kanye nokuhlolwa okunembayo: Ukuhlolwa kwesilinganiso sokuthola kabusha okujwayelekile kwenziwa nge-matrix kaphethiloli engenalutho, nezinga elijwayelekile lokutakula ngezinga elingeziwe elingu-100ppm lenziwe (n=5). Imiphumela ikhonjisiwe kuThebula lesi-4.

ithebula 4. Izinga lokululama kanye nemiphumela yokuhlolwa kokuphindaphinda

7.isiphetho

Lokhu kuhlola kubhekisela ku-DB37/T-2650 evamile yendawo yesiFundazwe saseShandong, futhi kusebenzisa umtshina we-FID ukuze kutholwe izinhlanganisela ze-aniline kuphethiloli. Indlela ilula futhi umphumela unokwethenjelwa. Nakuba ukuphazamiseka kungase kusetshenziswe ekuhlaziyweni kwangempela, ukuphazanyiswa kwe-naphthalene kwamanye ama-substrates kaphethiloli ekuhlaziyweni kwe-aniline kungagwenywa ngokuthuthukisa izimo.

Izithenjwa:

［1］UZhong Shaofang, WEN Huan et al. Ukunqunywa Kwezithako ze-Methylaniline ku-Motor Gasoline nge-Gas Chromatography [J]. I-Spectrum Laboratory, 2012, Volume 29, Issue 6, 3564-3567.

［2］Zhang Maolin, LI Baoding, ZHANG Yufa.Ucwaningo ngokunqunywa kwe-N-methylaniline nge-Spectrophotometry [J]. Ijenali yase-Zhengzhou Grain University, 2000, 21(2) : 86-88.

［3］U-Liu Baomin, u-LIU Minghong, u-XU Hong et al. Ucwaningo ngokunqunywa ngesikhathi esisodwa kwe-aniline, i-N-methylaniline ne-N, i-N-dimethylaniline Emoyeni ngokusebenza okuphezulu kwe-chromatography ye-liquid [J]. Ijenali yaseShayina Yokuhlolwa Kwezempilo, 2009, 19(8) : 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng.Ukusatshalaliswa kwezinhlanganisela eziqukethe i-nitrogen kuphethiloli we-catalytic nge-gas chromatography-Nitrogen chemiluminescence ukuthola [J]. I-Chromatography, 2010, 28(4): 336 - 340

I-DB37/T-2650, Ukunqunywa kwezinhlanganisela ze-aniline kuphethiloli wemoto nge-gas chromatography