igama elingundoqo

Ipetroli; izongezo; uAniline; Ichromatography yegesi;

1. intshayelelo Ngenxa yothintelo lwamandla epetroleum yasekhaya kunye nobuchwepheshe bokusulungekiswa, iimveliso ze-oyile eziveliswa ziindawo zokucokisa rhoqo kwimarike zinqongophele, nto leyo eyenza ukuba inani elikhulu leemveliso ze-oyile ezidityanisiweyo zikhukulise imakethi. Ipetroli edityanisiweyo rhoqo idityaniswa ne-naphtha enevumba elimnandi (i-oyile elula) njengezinto ezikrwada. Nangona kunjalo, kwimvelaphi yexabiso eliphezulu lezinto eziluhlaza kunye nokunyuswa kweenzuzo, iikhompawundi ze-aniline zihlala zisetyenziswa njengezongezo zepetroli ezingaqhelekanga. Ukuze wenze isalathisi somgangatho wepetroli kunye nezongezelelo ezinjalo zihlangabezane nemigangatho yepetroli yemoto yesizwe, umzekelo, ukongeza i-1% (iqhezu lobuninzi) i-N-methylaniline inokunyusa inani le-octane ngamayunithi angama-2-4 [1]. Nangona kunjalo, izongezo ze-aniline zineengozi ezinokubakho ekuhambeni kunye nokhuseleko lwezithuthi, kwaye i-N-methylanilines i-nitrogen-containing compounds, eya kukhokelela ekwandeni komxholo we-nitrogen oxides kwi-exhaust yemoto, ebangela imiphumo eyingozi kwindawo yomoya kunye nempilo yabantu. . Iinqununu eziphambili zezongezo ze-aniline ziquka i-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-methylaniline kunye ne-N, i-n-dimethylaniline. Okwangoku, iindlela ezichazwe ngokuqhelekileyo zokufumanisa i-methylaniline compounds ziquka i-naphthalene diethylamine spectrophotometry, i-gas chromatography-nitrogen chemiluminescence discovery, i-high performance liquid chromatography, njl njl. [2-4]. I-spectrophotometry ye-naphthalene ye-diethylamine iphazamisa umphumo wokuzimisela ngenxa yokwenzeka kwempendulo yecala, kwaye indlela ye-HPLC ichaphazeleka ngokungathandabuzekiyo ngokuphazanyiswa kwe-matrix ye-petroli.

Indlela yokufumanisa igesi yechromatograph-nitrogen chemiluminescence ifuna ukulungiswa kwe-nitrogen chemiluminescence ebiza kakhulu ekwazi ukubona initrogen. Umgangatho wesizwe osandula ukuyilwa (okusaza kupapashwa) "I-Chromatography yeGesi yokuMiselwa kwee-Oxycompounds kunye ne-aniline Compounds kwi-Gasoline" ikwachaza indlela yohlalutyo kusetyenziswa i-Deans switch kwikholamu ezimbini ezichaseneyo ze-polarity usebenzisa i-hydrogen ion flame detector eqhelekileyo nengabizi kakhulu. Kule ndlela, i-ThermoFisher Scientific ipapashe iphepha leSicelo (Amanqaku eSicelo C GC-50). Njengokwenza lula, eli phepha lizisa indlela ekhawulezayo yekholomu enye esekelwe kumgangatho wendawo weDB37 / T-2650 okhutshwe yiPhondo laseShandong kwi-2015 [5]. Iziphumo zibonisa ukuba le ndlela ilula ukuyisebenzisa, ngokuphindaphinda okulungileyo kunye nokuchaneka okuphezulu. Kwangaxeshanye, indlela yalungiselelwa ukusombulula ingxaki yokuphazamiseka kwenani le-aniline ngokubunjwa kwe-matrix yepetroli.

2. Isishwankathelo somgaqo wendlela Kwikholamu ye-polar polyethylene glycol (PEG), i-aniline compounds kwi-petroli ye-automotive yahlukaniswa ne-petroli matrix, kwaye i-acetophenone isetyenziswe njengomgangatho wangaphakathi. Imixholo ye-aniline, i-N-methylaniline, i-o-methylaniline, i-p-methylaniline, i-m-toluidine kunye ne-N, i-n-dimethylaniline kwi-petroli yemoto igqitywe yi-chromatograph yegesi exhotyiswe nge-flame ionization detector (FID), kunye nokuxinwa kwecandelo ngalinye. ibalwa ngokubhekisele kumgangatho wangaphakathi.

3. Izixhobo zomculo

3.1 Landela i-1300E yegesi yeChromatograph ene-shunt/non-shunt inlet,

I-AS1310 i-sampler ezenzekelayo, i-FID ionization detector (FID);

3.2 Isoftware yeChameleon

3.3 Microsyringe: umthamo yi-10uL.

4. Ii-reagents kunye nezixhobo

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

I-diameter yangaphakathi 0.25mm, ubukhulu befilimu yolwelo 0.25μm

4.2 Ngaphandle kokuba kucaciswe ngenye indlela, ii-reagents ezisetyenziswe kule ndlela zihlalutya kwaye zivumelekile

Sebenzisa ezinye ii-reagents zokucoceka okuphezulu.

Ii-reagents ezisetyenziselwa iinjongo zomgangatho kunye nobungakanani, kubandakanywa i-aniline (Ca #62-53-3), N-

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

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

1) kunye N, n-dimethylaniline (CAS # 121-69-7), umgangatho wangaphakathi wawuyiphenylene

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

5. Iindlela zovavanyo

5.1 Ukusekwa kwegophe elisemgangathweni

5.1.1 Ukulungiswa kwesisombululo esisemgangathweni: Zonke izinto eziqhelekileyo ziyi-isooctane (i-chromatographically pure)

I-Dilution, ngokulandelanayo ilungiselelwe izinto ezintandathu ze-aniline kwi-0.1%, 0.2%, 0.5%, 1%,

Ukufumana iisampulu ezisemgangathweni kwi-1.5% kunye ne-2% yamanqanaba, jonga iThebhile 1 ngolwazi oluthe kratya logxininiso.

Itheyibhile 1. Itheyibhile yogxininiso yesampula eqhelekileyo

5.1.2Iisampuli eziqhelekileyo zahlalutywa ngokwendlela yeGC kwiThebhile 2

Itheyibhile 2. Indlela yeGC

5.1.3 Umgangatho: Amacandelo asemgangathweni ngokwexesha lokugcinwa kwecandelo ngalinye, kunye ne-chromatogram yesampuli eqhelekileyo yohlobo oluqhelekileyo (i-0.1% yezinga lokugxininiswa) iboniswe kwi-Figure 1.

Umzobo 1. I-Chromatogram yesampuli eqhelekileyo eqhelekileyo

5.1.4 Misela igophe elisemgangathweni. Hlela indlela yokulinganisa kwindlela yokucubungula idatha kwi-software ye-Chameleon, uhlobo lokulinganisa luyilayini (alunyanzeliswanga phezu kwemvelaphi), uhlobo lokuvavanya luyindawo ephezulu, kwaye umgangatho wangaphakathi uyaguquguquka. I-equation ye-curve equation kunye ne-linear coefficient coefficient yecandelo ngalinye iboniswe kwiThebhile 3, kwaye i-curve esemgangathweni yecandelo ngalinye iboniswe kuMfanekiso 2-7.

itheyibhile 3. Idatha yegophe yolungelelaniso

5.1.5 Ubalo lweziphumo: Umlinganiselo wendawo ephakamileyo yecandelo ngalinye ukuya kwindawo ephakamileyo ye-acetophenone ibalwe. Iqhezu lomthamo wobuninzi becandelo ngalinye elihambelana nomlinganiselo lifundwa kwi-curve yokulungisa efanelekileyo, kwaye umphumo uchanekile kwi-0.01%.

6. Iziphumo neengxoxo

I-6.1 I-curve esemgangathweni: I-curve esemgangathweni isungulwe ngeemveliso eziqhelekileyo ze-6, uluhlu lwe-volume concentration luvela kwi-0.01% ukuya kwi-2.0%, kunye ne-coefficient ye-linear coefficient R2 inkulu kune-0.999, ngokulandelanayo (jonga iThebhile 3 ngeenkcukacha).

6.2 Indlela yokuqinisekisa kunye nokuphucula: Xa kuthelekiswa nendlela yokutshintsha i-Deans, indlela enye yekholomu efakwe kweli phepha ineenzuzo zeendleko eziphantsi, ukusebenza okulula kunye nokuveliswa okuphezulu. Nangona kunjalo, amanye amacandelo kwi-matrix yepetroli inokuchaphazela iikhompawundi ze-aniline.

Ngokomzekelo, ngokwendlela echazwe kweli phepha, xa kuhlolwa isampula ye-matrix ye-petroli engenanto, kufunyenwe ukuba emva kokuthelekisa kunye ne-chromatogram yesampulu eqhelekileyo, kukho incopho malunga ne-0.04min (incopho yobubanzi be-peak 0.07min) ukusuka kwinxalenye ye-aniline yemveliso eqhelekileyo, ephazamisa uhlalutyo lwe-aniline. (jonga umfanekiso 2)

3

IKHIWANE. 2. Uthelekiso phakathi kwe-aniline yesisombululo esiqhelekileyo se-spectra kunye ne-blank petroli matrix spectra

Ukuze kuqinisekiswe ukuba le nto ayikho i-aniline, kwaye isuse ukuphazamiseka kwi-aniline quantification. Indlela kweli phepha iphuculwe, kwaye inkqubo yokunyuka kobushushu benkqubo

I-DB37/T-2650 inkcazo ye-5℃ / min itshintshelwe kwi-4℃ / min. Iisampulu ze-matrix yepetroli ezineisampulu ezisemgangathweni ezongeziweyo zahlalutywa ngale ndlela. Njengoko kunokubonwa kwiFIG. 3,

Indlela ephuculweyo inokwahlula eli candelo kwi-aniline kwi-matrix yepetroli, kwaye ingqina ngakumbi ukuba isampulu yeoli inokufunyanwa ngendlela ye-DB37/T-2650.

Incopho kwi-21.905min yayingekho i-aniline. Iqela lokuphazamiseka linqunywe ukuba libe yi-naphthalene nge-qualitative mass spectrometry kunye nokuthelekisa okusemgangathweni.

IKHIWANE. 3. Ukuthelekiswa kwe-spectra yeesampulu zeoli, iisampuli ze-aniline kunye ne-matrix yepetroli (indlela ephuculweyo)

6.2 Izinga lokubuyisela kunye novavanyo oluchanekileyo: Uvavanyo lwezinga lokubuyisela lwenziwa nge-matrix yepetroli engenanto, kunye nezinga lokubuyisela umgangatho kunye nenqanaba lokongeza le-100ppm lenziwe (n = 5). Iziphumo zaboniswa kwiTheyibhile yesi-4.

itheyibhile 4. Izinga lokubuyisela kunye neziphumo zovavanyo lokuphindaphinda

7.isiphelo

Olu vavanyo lubhekiselele kumgangatho wendawo we-DB37/T-2650 wePhondo laseShandong, kwaye yamkela i-FID detector ukufumanisa iikhompawundi ze-aniline kwipetroli. Indlela ilula kwaye umphumo unokuthenjwa. Nangona ukuphazamiseka kungasetyenziselwa uhlalutyo lwangempela, ukuphazamiseka kwe-naphthalene kwezinye i-petroli substrates kuhlalutyo lwe-aniline kunokuphetshwa ngokulungisa iimeko.

IiReferensi:

［1］Zhong Shaofang, WEN Huan et al. Ukumiselwa kwezongezo zeMethylaniline kwiGasoli yeMoto ngeChromatography yeGesi [J]. Spectrum Laboratory, 2012, Volume 29, Issue 6, 3564-3567.

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

［3］ULiu Baomin, LIU Minghong, XU Hong et al. Uphononongo lokumiselwa kwangexesha elinye i-aniline, i-N-methylaniline kunye ne-N, i-N-dimethylaniline emoyeni ngokusebenza okuphezulu kwechromatography yolwelo [J]. Ijenali yaseTshayina yoHlolo lweMpilo, i-2009, i-19 (8): 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng. Ukuhanjiswa kweekhompawundi ezinenitrogen kwi-catalytic petroli ngegesi chromatography-Nitrogen chemiluminescence ubhaqa [J]. I-Chromatography, i-2010, i-28 (4): 336 - 340

I-DB37/T-2650, Ukumiselwa kweekhompawundi ze-aniline kwipetroli yemoto ngechromatography yerhasi