igama elingundoqo

Ipetroli; Izongezo; I-Aniline; I-Gas Chromatography;

1. Intshayelelo Ngenxa yokuthintelwa kwamandla epetroliyam asekhaya kunye netekhnoloji yokucoca, iimveliso zeoli eziveliswa ziindawo zokucocisa eziqhelekileyo kwimarike azifumaneki, nto leyo eyenza inani elikhulu leemveliso zeoli ezixutyiweyo lizalise imarike. Ipetroli exutyiweyo eqhelekileyo ixutywe kakhulu ne-aromatic naphtha (ioyile ekhaphukhaphu) njengezinto eziluhlaza. Nangona kunjalo, ngenxa yamaxabiso aphezulu ezinto eziluhlaza kunye nokwandiswa kwenzuzo, iikhompawundi ze-aniline zihlala zisetyenziswa njengezongezo zepetroli ezingaqhelekanga. Ukuze umgangatho wepetroli onezongezo ezinjalo uhlangabezane nomgangatho wepetroli yemoto kazwelonke, umzekelo, ukongeza i-1% (inxalenye yobunzima) i-N-methylaniline inokunyusa inani le-octane ngeeyunithi ezi-2-4 [1]. Nangona kunjalo, izongezo ze-aniline zineengozi ezinokubakho ekuhambeni nasekukhuselekeni kwezithuthi, kwaye ii-N-methylanilines ziikhompawundi ezine-nitrogen, eziya kukhokelela ekwandeni komxholo we-nitrogen oxides kwi-exhaust yemoto, nto leyo ebangela iziphumo eziyingozi kwindalo esingqongileyo nakwimpilo yabantu. Izinto eziphambili zezongezo ze-aniline ziquka i-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-methylaniline kunye ne-N, n-dimethylaniline. Okwangoku, iindlela ezixhaphakileyo zokufumanisa iikhompawundi ze-methylaniline ziquka i-naphthalene diethylamine spectrophotometry, i-gas chromatography-nitrogen chemiluminescence detection, i-high performance liquid chromatography, njl.njl. [2-4]. I-naphthalene diethylamine spectrophotometry yendabuko iphazamisana nesiphumo sokumisela ngenxa yokwenzeka kwe-side reaction, kwaye indlela ye-HPLC ngokungenakuphepheka ichaphazeleka kukuphazamiseka kwe-gasoline matrix.

Indlela yokufumanisa i-gas chromatograph-nitrogen chemiluminescence ifuna ukulungiswa kwesixhobo sokubona i-nitrogen chemiluminescence esibizayo esinokubona i-nitrogen ngokukhetha. Umgangatho wesizwe osandul’ ukubhalwa (ongekapapashwa) “I-Gas Chromatography yokuQondwa kwee-Oxycompounds kunye nee-aniline Compounds kwiGasoline” uchaza nendlela yohlalutyo kusetyenziswa i-Deans switch kwiikholamu ezimbini ezichaseneyo ze-polarity kusetyenziswa isixhobo sokubona i-hydrogen ion esiqhelekileyo nesingabizi kakhulu. Kule ndlela, i-ThermoFisher Scientific ipapashe iphepha lesicelo (Amanqaku esicelo C GC-50). Njengendlela yokwenza lula, eli phepha lazisa indlela yekholamu enye ekhawulezayo esekelwe kwi-DB37/T-2650 esemgangathweni yendawo ekhutshwe yiShandong Province ngo-2015 [5]. Iziphumo zibonisa ukuba le ndlela ilula ukuyisebenzisa, inokuphinda-phinda okuhle kunye nokuchaneka okuphezulu. Kwangaxeshanye, le ndlela yenziwe ngcono ukusombulula ingxaki yokuphazamiseka kokulinganiswa kwe-aniline ngokwakhiwa kwe-gasoline matrix.

2. Isishwankathelo somgaqo wendlela Kwikholamu ye-polar polyethylene glycol (PEG), iikhompawundi ze-aniline kwipetroli yemoto zahlulwe kwi-matrix yepetroli, kwaye i-acetophenone yasetyenziswa njengomgangatho wangaphakathi. Okuqulethwe yi-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-toluidine kunye ne-N, n-dimethylaniline kwipetroli yemoto kumiselwe yi-chromatograph yegesi exhotyiswe nge-flame ionization detector (FID), kwaye uxinzelelo lwecandelo ngalinye lubalwe ngokubhekiselele kumgangatho wangaphakathi.

3. Izixhobo

3.1 I-Chromatograph yegesi yeTrace 1300E ene-shunt/non-shunt inlet,

Isampuli ezenzekelayo ye-AS1310, isixhobo sokubona i-ionization yelangatye (i-FID);

3.2 Isoftware yeChameleon

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

4. Izinto ezisetyenziswayo kunye nezinto ezisetyenziswayo

4.1 Ikholamu: Ikholamu yePolar, i-TG-Wax, ubude bekholamu yi-60m,

Ububanzi bangaphakathi yi-0.25mm, ubukhulu befilimu engamanzi yi-0.25μm

4.2 Ngaphandle kokuba kuchazwe ngenye indlela, ii-reagents ezisetyenzisiweyo kule ndlela zicocekile kwaye zivumelekile ngokwezibalo

Sebenzisa ezinye ii-reagents ezicocekileyo kakhulu.

Ii-reagents ezisetyenziselwa iinjongo zobunjani kunye nobungakanani, kuquka 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) kunye ne-N, n-dimethylaniline (CAS#121-69-7), umgangatho wangaphakathi yayiyi-phenylene

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

5. Iindlela zovavanyo

5.1 Ukusekwa kwe-standard curve

5.1.1 Ukulungiswa kwesisombululo esiqhelekileyo: Zonke izinto ezisemgangathweni ziyi-isooctane (zimsulwa ngokwe-chromatographically)

Umxube, owenziwe ngokulandelelanayo ngezinto ezintandathu ze-aniline kwi-0.1%, 0.2%, 0.5%, 1%,

Kwiisampulu ezisemgangathweni kumanqanaba e-1.5% kunye ne-2%, jonga iTheyibhile 1 ukuze ufumane ulwazi oluneenkcukacha ngoxinaniso.

Itheyibhile 1. Itheyibhile yoxinaniso lweesampuli eziqhelekileyo

5.1.2Iisampulu ezisemgangathweni zihlalutywe ngokwendlela ye-GC kwiTheyibhile 2

Itheyibhile 2. Indlela ye-GC

5.1.3 Umgangatho: Iinxalenye zisemgangathweni ngokwexesha lokugcinwa kwenxalenye nganye, kwaye i-chromatogram yesampulu esemgangathweni yohlobo oluqhelekileyo (inqanaba loxinzelelo lwe-0.1%) iboniswe kuMfanekiso 1.

Umfanekiso 1. I-Chromatogram yesampulu eqhelekileyo esemgangathweni

5.1.4 Misela i-curve esemgangathweni. Hlela indlela yokulinganisa kwindlela yokucubungula idatha kwisoftware yeChameleon, uhlobo lokulinganisa luyi-linear (alunyanzelwanga ngaphezu kwemvelaphi), uhlobo lovavanyo luyindawo yencochoyi, kwaye umgangatho wangaphakathi uyaguquguquka. I-standard curve equation kunye ne-linear correlation coefficient yecandelo ngalinye iboniswe kwiTheyibhile 3, kwaye i-standard curve yecandelo ngalinye iboniswe kuMfanekiso 2-7。

itheyibhile 3. Idatha yejika lokulinganisa

5.1.5 Ubalo lweziphumo: Umlinganiselo wendawo encochoyiweyo yecandelo ngalinye kwindawo encochoyiweyo ye-acetophenone ubalwe. Inxalenye yomthamo wobunzima becandelo ngalinye elihambelana nomlinganiselo ifundwa kwi-curve yokulungisa efanelekileyo, kwaye isiphumo sichanekile ukuya kwi-0.01%.

6. Iziphumo neengxoxo

6.1 Ijika eliqhelekileyo: Ijika eliqhelekileyo lisekwe ziimveliso ezi-6 ezisemgangathweni, uluhlu loxinzelelo lwevolumu luqala kwi-0.01% ukuya kwi-2.0%, kwaye i-coefficient yolungelelwaniso oluchanekileyo R2 ingaphezulu kwe-0.999, ngokulandelelana (jonga iTheyibhile 3 ukuze ufumane iinkcukacha).。

6.2 Ukuqinisekiswa kwendlela kunye nokwenza ngcono: Xa kuthelekiswa nendlela yokutshintsha yeDeans, indlela yekholamu enye engeniswe kweli phepha ineengenelo zexabiso eliphantsi, ukusebenza okulula kunye nokuphindaphinda okuphezulu. Nangona kunjalo, ezinye izinto kwi-matrix yepetroli zinokuchaphazela iikhompawundi ze-aniline.

Umzekelo, ngokwendlela echazwe kweli phepha, xa kuvavanywa isampuli ye-petroli matrix engenanto, kufunyaniswe ukuba emva kokuthelekisa ne-chromatogram yesampuli esemgangathweni, kukho incochoyi emalunga ne-0.04min (ububanzi bencochoyi yi-0.07min) ukusuka kwinxalenye ye-aniline yemveliso esemgangathweni, ephazamisana nohlalutyo lwe-aniline. (jonga uMfanekiso 2)

3

UMZOBO 2. Uthelekiso phakathi kwe-aniline standard solution spectra kunye ne-blank gas matrix spectra

Ukuze kuqinisekiswe ukuba le nto ayisiyo i-aniline, kwaye kupheliswe ukuphazamiseka kokulinganiswa kwe-aniline. Indlela ekule phepha yenziwe ngcono, kwaye inkqubo yokunyuka kwamaqondo obushushu iyasebenza.

Inkcazo ye-DB37/T-2650 ye-5℃ /min itshintshiwe yaba yi-4℃ /min. Iisampulu ze-petroli matrix ezineesampuli ezisemgangathweni ezongeziweyo zihlalutywe ngale ndlela. Njengoko kunokubonwa kwiFIG. 3,

Indlela ephuculweyo ingahlula le nxalenye kwi-aniline kwi-gasoline matrix, kwaye iqinisekisa ukuba isampuli yeoyile ingafunyanwa ngendlela ye-DB37/T-2650.

Incopho kwimizuzu engama-21.905 yayingeyiyo i-aniline. Iqela lokuphazamiseka lifunyenwe njenge-naphthalene nge-qualitative mass spectrometry kunye nokuthelekiswa okuqhelekileyo.

UMZOBO 3. Uthelekiso lwee-spectra zeesampuli zeoyile, iisampuli ze-aniline kunye ne-petroli matrix (indlela ephuculweyo)

6.2 Uvavanyo lwezinga lokubuyisela kunye nokuchaneka: Uvavanyo lwezinga lokubuyisela oluqhelekileyo lwenziwe nge-blank gas matrix, kwaye kwenziwa izinga lokubuyisela eliqhelekileyo elinenqanaba lokongeza le-100ppm (n=5). Iziphumo ziboniswe kwiTheyibhile 4.

itheyibhile 4. Iziphumo zovavanyo lwezinga lokuchacha kunye nokuphindaphinda

7.isiphelo

Olu vavanyo lubhekisa kwi-DB37/T-2650 esemgangathweni yengingqi yePhondo laseShandong, kwaye yamkela isixhobo sokubona i-FID ukufumanisa iikhompawundi ze-aniline kwipetroli. Le ndlela ilula kwaye isiphumo sithembekile. Nangona ukuphazamiseka kungasetyenziswa kuhlalutyo lokwenyani, ukuphazamiseka kwe-naphthalene kwezinye ii-substrates zepetroli kuhlalutyo lwe-aniline kunokuthintelwa ngokuphucula iimeko.

Iireferensi:

［1］UZhong Shaofang, WEN Huan et al. Ukumiselwa kwezongezo zeMethylaniline kwiMotor Gasoline yiGas Chromatography [J]. I-Spectrum Laboratory, 2012, uMqulu 29, Issue 6, 3564-3567.

［2］Zhang Maolin, LI Baoding, ZHANG Yufa.Uphononongo malunga nokumiselwa kwe-N-methylaniline yiSpectrophotometry [J]. Ijenali yeYunivesithi yaseZhengzhou Grain, 2000, 21(2): 86-88.

［3］ULiu Baomin, uLIU Minghong, uXU Hong nabanye. Uphononongo malunga nokuchonga ngaxeshanye i-aniline, i-N-methylaniline kunye ne-N, i-N-dimethylaniline emoyeni nge-chromatography yolwelo olusebenza kakuhle [J]. Ijenali yaseTshayina yoVavanyo lwezeMpilo, 2009, 19(8): 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng. Ukusasazwa kweekhompawundi ezine-nitrogen kwi-catalytic gas gas chromatography-Nitrogen chemiluminescence detection [J]. Chromatography, 2010, 28(4): 336 — 340

I-DB37/T-2650, Ukuchonga iikhompawundi ze-aniline kwipetroli yemoto nge-chromatography yegesi