igama elingukhiye

Uphethiloli; Izithasiselo; I-Aniline; I-Gas chromatography;

1. Isingeniso Ngenxa yokuvinjelwa kwamandla kaphethiloli wasekhaya kanye nobuchwepheshe bokucwenga, imikhiqizo kaphethiloli ekhiqizwa izindawo zokucwenga ezivamile emakethe ayitholakali kalula, okwenza inani elikhulu lemikhiqizo kaphethiloli ehlanganisiwe ligcwale emakethe. Uphethiloli ohlanganisiwe ojwayelekile uxutshwa kakhulu ne-naphtha exubile ephunga (uwoyela olula) njengezinto zokusetshenziswa. Kodwa-ke, ngemuva kwamanani aphezulu ezinto zokusetshenziswa kanye nokwandiswa kwenzuzo, ama-aniline compounds avame ukusetshenziswa njengezithasiselo zikaphethiloli ezingavamile. Ukuze inkomba yekhwalithi kaphethiloli enezithasiselo ezinjalo ihlangabezane nezinga likazwelonke likaphethiloli wezimoto, isibonelo, ukwengeza u-1% (ingxenye yobuningi) i-N-methylaniline ingandisa inombolo ye-octane ngamayunithi angu-2-4 [1]. Kodwa-ke, izithasiselo ze-aniline zinezingozi ezingaba khona ekuhambeni nasekuphepheni kwezimoto, kanti ama-N-methylanilines angama-compound aqukethe i-nitrogen, okuzoholela ekwandeni kokuqukethwe kwama-nitrogen oxides emhubheni wezimoto, okubangela imiphumela eyingozi endaweni ezungezile kanye nempilo yabantu. Izingxenye eziyinhloko zezithasiselo ze-aniline zifaka i-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-methylaniline kanye ne-N, n-dimethylaniline. Njengamanje, izindlela ezivame ukubikwa zokuthola ama-methylaniline compounds zifaka phakathi i-naphthalene diethylamine spectrophotometry, i-gas chromatography-nitrogen chemiluminescence detection, i-high performance liquid chromatography, njll. [2-4]. I-naphthalene diethylamine spectrophotometry yendabuko iphazamisa umphumela wokunquma ngenxa yokuvela kokusabela okungekuhle, futhi indlela ye-HPLC ithinteka ngokungenakugwenywa ukuphazamiseka kwe-gasoline matrix.

Indlela yokuthola i-gas chromatograph-nitrogen chemiluminescence idinga ukulungiswa kwe-detector ye-nitrogen chemiluminescence ebizayo engakwazi ukubona i-nitrogen ngokukhetha. Indinganiso kazwelonke esanda kubhalwa (engakashicilelwa) ethi “Gas Chromatography for the Determination of Oxycompounds and aniline Compounds in Gasoline” ichaza nendlela yokuhlaziya kusetshenziswa i-Deans switch kumakholomu amabili aphikisanayo e-polarity kusetshenziswa i-detector ye-hydrogen ion flame evamile futhi engabizi kakhulu. Kule ndlela, i-ThermoFisher Scientific ishicilele iphepha lesicelo (Amanothi esicelo C GC-50). Njengendlela yokwenza lula, leli phepha lethula indlela yekholomu eyodwa esheshayo esekelwe ku-DB37/T-2650 ejwayelekile yendawo ekhishwe yiShandong Province ngo-2015 [5]. Imiphumela ikhombisa ukuthi le ndlela ilula ukuyisebenzisa, ngokuphindaphindwa okuhle kanye nokunemba okuphezulu. Ngesikhathi esifanayo, le ndlela yenziwe ngcono ukuxazulula inkinga yokuphazamiseka kokulinganiswa kwe-aniline ngokwakhiwa kwe-gasoline matrix.

2. Ukubuka konke kwesimiso sendlela Kukholomu ye-polar polyethylene glycol (PEG), ama-aniline compounds kuphethiloli yezimoto ahlukaniswe ne-gasoline matrix, kwathi i-acetophenone yasetshenziswa njengendinganiso yangaphakathi. Okuqukethwe yi-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-toluidine kanye ne-N, n-dimethylaniline kuphethiloli yezimoto kunqunywe yi-gas chromatograph efakwe i-flame ionization detector (FID), futhi ukuhlushwa kwengxenye ngayinye kubalwe ngokubhekisela kundinganiso yangaphakathi.

3. Izinsimbi Zomculo

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

isampula ezenzakalelayo ye-AS1310, i-flame ionization detector (FID);

3.2 Isofthiwe ye-Chameleon

3.3 I-Microsyringe: umthamo wayo ungama-10uL.

4. Ama-reagent nezinto zokwakha

4.1 Ikholomu: Ikholomu ephansi, i-TG-Wax, ubude bekholomu obungu-60m,

Ububanzi bangaphakathi 0.25mm, ukujiya kwefilimu ewuketshezi 0.25μm

4.2 Ngaphandle kokuthi kuchazwe ngenye indlela, ama-reagent asetshenziswe kule ndlela ahlanzekile futhi avumelekile ngokokuhlaziya

Sebenzisa ezinye izinto ezihlanzekile kakhulu.

Ama-reagent asetshenziselwa izinjongo zokuhlola kanye nokulinganisa, okuhlanganisa i-aniline (Ca #62-53-3), i-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, i-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 kwesisombululo esijwayelekile: Zonke izinto ezijwayelekile ziyi-isooctane (zimsulwa ngokwe-chromatographic)

Ukuxuba, okuhlelwe ngokulandelana 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 elijwayelekile lokuhlushwa kwesampula

5.1.2Amasampula ajwayelekile ahlaziywe ngokwendlela ye-GC kuThebula 2

Ithebula 2. Indlela ye-GC

5.1.3 Ikhwalithi: Izingxenye zikhwalithi ngokwesikhathi sokugcinwa kwengxenye ngayinye, futhi i-chromatogram yesampula ejwayelekile yohlobo olujwayelekile (izinga lokuhlushwa elingu-0.1%) iboniswe kuMfanekiso 1.

Isithombe 1. I-Chromatogram yesampula ejwayelekile ejwayelekile

5.1.4 Misa ijika elijwayelekile. Hlela indlela yokulinganisa endleleni yokucubungula idatha kusofthiwe ye-Chameleon, uhlobo lokulinganisa luqondile (aluphoqelelwe ngaphezu komsuka), uhlobo lokuhlola luyindawo ephakeme, kanti izinga langaphakathi liyaguquguquka. I-standard curve equation kanye ne-linear correlation coefficient yengxenye ngayinye kuboniswe kuThebula 3, kanti ijika elijwayelekile lengxenye ngayinye liboniswe kuMfanekiso 2-7.

ithebula 3. Idatha yejika lokulinganisa

5.1.5 Ukubalwa kwemiphumela: Isilinganiso sendawo ephakeme yengxenye ngayinye nendawo ephezulu ye-acetophenone sibaliwe. Ingxenye yevolumu yobuningi yengxenye ngayinye ehambisana nesilinganiso ifundwa kusukela ku-curve yokulungisa efanele, futhi umphumela unembile ku-0.01%.

6. Imiphumela nengxoxo

6.1 Ijika elijwayelekile: Ijika elijwayelekile lisungulwa yimikhiqizo esezingeni eli-6, ububanzi bokuhlushwa kwevolumu busukela ku-0.01% kuya ku-2.0%, kanti i-coefficient yokuxhumana okuqondile R2 inkulu kuno-0.999, ngokulandelana (bheka Ithebula 3 ukuthola imininingwane).。

6.2 Ukuqinisekiswa kanye nokwenza ngcono indlela: Uma kuqhathaniswa nendlela yokushintsha ye-Deans, indlela yekholomu eyodwa eyethulwe kuleli phepha inezinzuzo zezindleko eziphansi, ukusebenza okulula kanye nokuphindaphinda okuphezulu. Kodwa-ke, ezinye izingxenye ku-matrix kaphethiloli zingathinta ama-aniline compounds.

Isibonelo, ngokwendlela echazwe kuleli phepha, lapho kuhlolwa isampula ye-gasoline matrix engenalutho, kutholakala ukuthi ngemva kokuqhathaniswa ne-chromatogram yesampula ejwayelekile, kukhona ukuphakama cishe ku-0.04min (ububanzi obukhulu be-peak bungu-0.07min) kusuka engxenyeni ye-aniline yomkhiqizo ojwayelekile, okuphazamisa ukuhlaziywa kwe-aniline. (bheka Umfanekiso 2)

3

UMFANEKISO 2. Ukuqhathanisa phakathi kwe-aniline standard solution spectra kanye ne-blank gasoline matrix spectra

Ukuze kuqinisekiswe ukuthi le nto ayiyona i-aniline, futhi kuqedwe ukuphazamiseka kokulinganisa i-aniline. Indlela ekuleli phepha yenziwe ngcono, futhi inqubo yokwenyuka kwezinga lokushisa lohlelo i-

Incazelo ye-DB37/T-2650 engu-5℃/min ishintshelwe ku-4℃/min. Amasampula e-gasoline matrix anamasampula ajwayelekile engeziwe ahlaziywe ngale ndlela. Njengoba kungabonakala ku-FIG. 3,

Indlela elungiselelwe kahle ingahlukanisa le ngxenye ku-aniline ku-gasoline matrix, futhi ifakazela ukuthi isampula kawoyela ingatholakala ngendlela ye-DB37/T-2650.

Isilinganiso esiphezulu kumaminithi angu-21.905 kwakungeyona i-aniline. Iqembu lokuphazamiseka latholakala ukuthi liyi-naphthalene nge-qualitative mass spectrometry kanye nokuqhathaniswa okujwayelekile.

UMFANEKISO 3. Ukuqhathaniswa kwama-spectra amasampula kawoyela, amasampula e-aniline kanye ne-gasoline matrix (indlela elungiselelwe)

6.2 Izinga lokutakula kanye nokuhlolwa kokunemba: Ukuhlolwa kwezinga lokutakula okujwayelekile kwenziwe nge-blank gasoline matrix, kanti izinga lokutakula elijwayelekile elinezinga lokwengeza elingu-100ppm lenziwe (n=5). Imiphumela iboniswe kuThebula 4.

ithebula 4. Imiphumela yokuhlolwa kwezinga lokululama kanye nokuphindaphinda

7.isiphetho

Lokhu kuhlola kubhekisela ku-DB37/T-2650 ejwayelekile yendawo yeSifundazwe saseShandong, futhi kusebenzisa i-FID detector ukuthola ama-aniline compounds kuphethiloli. Indlela ilula futhi umphumela uthembekile. Nakuba ukuphazamiseka kungasetshenziswa ekuhlaziyeni kwangempela, ukuphazamiseka kwe-naphthalene kwezinye izingxenye zephethiloli ekuhlaziyweni kwe-aniline kungagwenywa ngokwenza ngcono izimo.

Izinkomba:

［1］UZhong Shaofang, WEN Huan nabanye. Ukunqunywa kwezithasiselo ze-Methylaniline ku-Motor Petroline yi-Gas Chromatography [J]. I-Spectrum Laboratory, 2012, uMqulu 29, Udaba 6, 3564-3567.

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

［3］ULiu Baomin, uLIU Minghong, uXU Hong nabanye. Ucwaningo ngokunqunywa ngasikhathi sinye kwe-aniline, i-N-methylaniline kanye ne-N, i-N-dimethylaniline emoyeni nge-chromatography yoketshezi esebenza kahle kakhulu [J]. I-Chinese Journal of Health Inspection, 2009, 19(8): 1804-1807.

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

I-DB37/T-2650, Ukunqunywa kwamakhemikhali e-aniline kuphethiloli yemoto nge-gas chromatography