keyword

peturu; Additives; Aniline; Gasi chromatography;

1. sumo Nekuda kwekudziviswa kwesimba remagetsi epetroleum uye tekinoroji yekunatsa, zvigadzirwa zvemafuta zvinogadzirwa neanogara achinatsa pamusika zviri kushomeka, izvo zvinoita kuti huwandu hukuru hwezvigadzirwa zvemafuta akasanganiswa zvifashukire pamusika. Yenguva dzose yakasanganiswa peturu inonyanya kusanganiswa neyakasanganiswa inonhuhwirira naphtha (mafuta akareruka) semidziyo. Nekudaro, kumashure kwemitengo yakakwira yezvigadzirwa uye kuwedzera purofiti, aniline makomputa anowanzoshandiswa seasina kujairika ekuwedzera peturu. Kuti uite kuti mhando yemhando yepeturu ine zviwedzere zvakadaro zvienderane neyakajairwa mota yemotokari peturu, semuenzaniso, kuwedzera 1% (chikamu chezhinji) N-methylaniline inogona kuwedzera nhamba yeoctane ne2-4 mayunitsi [1]. Zvisinei, aniline additives ane ngozi dzinogona kuitika pakufamba uye kuchengeteka kwemotokari, uye N-methylanilines iine nitrogen-containing compounds, iyo inotungamira kuwedzera kwehuwandu hwe nitrogen oxides mumhepo inopera, zvichikonzera zvinokuvadza pamhepo yemhepo uye hutano hwevanhu. . Izvo zvikamu zvikuru zveaniline additives zvinosanganisira aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline uye N, n-dimethylaniline. Parizvino, nzira dzinowanzotaurwa dzekuonekwa kwemakemikari emethylaniline anosanganisira naphthalene diethylamine spectrophotometry, gas chromatography-nitrogen chemiluminescence discovery, high performance liquid chromatography, etc. [2-4]. Iyo yechinyakare naphthalene diethylamine spectrophotometry inokanganisa mhedzisiro yekutsunga nekuda kwekuitika kwedivi rekuita, uye nzira yeHPLC inokanganisika nekukanganiswa kwepeturu matrix.

Iyo gasi chromatograph-nitrogen chemiluminescence yekuongorora nzira inoda kugadzirwa kweinodhura nitrogen chemiluminescence detector inogona kusarudza nitrogen. Iyo ichangobva kunyorwa (ichiri kuzoburitswa) chiyero chenyika "Gas Chromatography yeKutemerwa kweOxycompounds uye aniline Compounds muGasoline" inotsanangurawo nzira yekuongorora uchishandisa Deans switch pamakoramu maviri akatarisana nepolarity uchishandisa yakajairwa uye isingadhure hydrogen ion flame detector. Kune iyi nzira, ThermoFisher Sayenzi yakaburitsa bepa reKushandisa (Manotsi eKushandisa C GC-50). Sekurerutsa, bepa rino rinounza inokurumidza nzira imwe chete yekoramu zvichibva pane yenzvimbo chiyero DB37/T-2650 yakapihwa neShandong Province muna 2015 [5]. Mhedzisiro yacho inoratidza kuti iyi nzira iri nyore kushanda, ine yakanaka kudzokorora uye yakakwirira kunyatso. Panguva imwecheteyo, iyo nzira yakagadziridzwa kugadzirisa dambudziko rekukanganiswa kweaniline quantification ne peturu matrix kuumbwa.

2. Mhedziso yenheyo yenzira Pamusoro pepolar polyethylene glycol (PEG) column, aniline compounds mumotokari yemotokari yakaparadzaniswa kubva kune peturu matrix, uye acetophenone yakashandiswa seyero yemukati. Zviri mukati me aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine uye N, n-dimethylaniline mumotokari peturu zvakatemwa negasi chromatograph yakashongedzerwa nemoto ionization detector (FID), uye kusangana kwechikamu chimwe nechimwe kwaive. yakaverengerwa nekutarisa kune yemukati mwero.

3. Zviridzwa

3.1 Tsvaira 1300E Gasi Chromatograph ine shunt/isina-shunt inlet,

AS1310 otomatiki sampler, Flame ionization detector (FID);

3.2 Chameleon Software

3.3 Microsyringe: simba i10uL.

4. Reagents uye zvinhu

4.1 Koramu: Polar column, TG-Wax, kureba kwembiru 60m,

Inner dhayamita 0.25mm, mvura firimu ukobvu 0.25μm

4.2 Kunze kwekunge zvatsanangurwa neimwe nzira, mareagents anoshandiswa mune iyi nzira akachena uye anotenderwa

Shandisa mamwe ma reagents ekuchena kwepamusoro.

Zvishandiso zvinoshandiswa kuita zvemhando yepamusoro uye zvehuwandu zvinangwa, zvinosanganisira aniline (Ca #62-53-3), N-

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

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

1) uye N, n-dimethylaniline (CAS#121-69-7), chiyero chemukati chaiva phenylene.

Ketone (CASA #96-86-2).

5. Nzira dzokuedza

5.1 Kugadzwa kwestandard curve

5.1.1 Kugadzirira kweyakajairwa mhinduro: Zvese zvakajairwa zvinhu isooctane (chromatographically pure)

Dilution, zvakateerana zvakagadzirirwa nezvinhu zvitanhatu zveaniline mu 0.1%, 0.2%, 0.5%, 1%,

Kuti uwane masampuli akajairwa pa1.5% uye 2% mazinga, ona Tafura 1 yeruzivo rwakadzama rwekusungwa.

Tafura 1. Standard sampuli yekufungisisa tafura

5.1.2Iwo akajairwa samples akaongororwa zvinoenderana neGC nzira muTafura 2

Tafura 2. GC nzira

5.1.3 Hunhu: Izvo zvikamu zvine hunhu zvinoenderana nenguva yekuchengetedza yechikamu chimwe nechimwe, uye chromatogram yeyakajairwa sampu yeyakajairika mhando (0.1% yekumisikidza level) inoratidzwa muFigure 1.

Mufananidzo 1. Chromatogram yemuenzaniso wakajairika

5.1.4 Gadzira mwero wecurve. Rongedza nzira yecalibration mune iyo data processing nzira muChameleon software, iyo calibration mhando ndeyemutsara (isina kumanikidzwa pamusoro pekwakabva), mhando yekuongorora inzvimbo yepamusoro, uye chiyero chemukati chinosiyana. Iyo yakajairwa curve equation uye mutsara wekubatanidza coefficient yechikamu chimwe nechimwe inoratidzwa muTafura 3, uye mwero wepakati wechikamu chimwe nechimwe unoratidzwa muFigure 2-7.

tafura 3. Calibration curve data

5.1.5 Mhedzisiro yekuverenga: Chiyero chechikamu chepamusoro chechikamu chimwe nechimwe kusvika kunzvimbo yepamusoro yeacetophenone yakaverengwa. Huremu vhoriyamu chikamu chechikamu chega chega chinoenderana nereshiyo inoverengwa kubva kune yakakodzera kugadzirisa curve, uye mhedzisiro yacho ndeyechokwadi kusvika 0.01%.

6. Migumisiro uye nhaurirano

6.1 Yakajairwa curve: Iyo yakajairwa curve inotangwa ne6 zvigadzirwa zvakajairwa, huwandu hwehuwandu hwehuwandu hunobva pa0.01% kusvika 2.0%, uye mutsara wekubatanidza coefficient R2 yakakura kupfuura 0.999, zvichiteerana (ona Tafura 3 yeruzivo).

6.2 Method verification uye optimization: Kana ichienzaniswa neDeans switch nzira, iyo imwechete column nzira yakaunzwa mubepa rino ine zvakanakira mutengo wakaderera, kushanda kuri nyore uye kubereka kwakanyanya. Nekudaro, zvimwe zvikamu mu peturu matrix zvinogona kukanganisa aniline makomisheni.

Semuyenzaniso, zvinoenderana nenzira yakatsanangurwa mubepa rino, kana uchiyedza sampu yepeturu matrix isina chinhu, zvinoonekwa kuti mushure mekuenzanisa nechromatogram yemuenzaniso wakajairika, pane peak ingangoita 0.04min (hupamhi hwepamusoro hwepamusoro 0.07min) kubva kune aniline chikamu cheyakajairwa chigadzirwa, icho chinokanganisa kuongororwa kweaniline. (ona Mufananidzo 2)

3

FIG. 2. Kuenzanisa pakati peaniline standard solution spectra uye blank peturu matrix spectra

Kuti uone kuti chinhu ichi hachisi aniline, uye kubvisa kupindira kune aniline quantification. Iyo nzira iri mubepa iri yakagadziridzwa, uye chirongwa chekukwira kwekushisa kwechirongwa chiri

DB37/T-2650 tsananguro ye5℃/min yakashandurwa kuita 4℃/min. Iwo peturu matrix samples ane standard samples akawedzerwa akaongororwa neiyi nzira. Sezvinoonekwa kubva kuFIG. 3,

Iyo yakagadziridzwa nzira inogona kuparadzanisa chikamu ichi kubva kune aniline mune peturu matrix, uye zvakare inoratidza kuti sampu yemafuta inogona kuwanikwa neDB37/T-2650 nzira.

Iyo yepamusoro pa21.905min yakanga isiri aniline. Iro boka rekupindira rakatemwa kuve naphthalene nemhando yepamusoro spectrometry uye yakajairwa kuenzanisa.

FIG. 3. Kuenzanisa kwe spectra yemafuta samples, aniline samples uye peturu matrix (yakagadziridzwa nzira)

6.2 Kudzoreredza mwero uye kuyedza kwakaringana: Iyo yakajairwa kudzoreredza mwero kuyedza yakaitwa isina blank peturu matrix, uye mwero wekudzoreredza mwero nekuwedzera kwe100ppm wakaitwa (n=5). Mibairo yakaratidzwa muTable 4.

tafura 4. Recovery rate uye repeatability bvunzo mhinduro

7.mhedziso

Chiyedzo ichi chinoreva chiyero chemunharaunda DB37/T-2650 yePurovhinzi yeShandong, uye inotora detector yeFID kuti ione makomisheni eaniline mupeturu. Nzira yacho iri nyore uye chigumisiro chakavimbika. Kunyange zvazvo kupindira kunogona kushandiswa mukuongorora chaiko, kupindira kwe naphthalene mune mamwe peturu substrates kune aniline kuongorora kunogona kudziviswa nekugadzirisa mamiriro acho ezvinhu.

References:

［1］Zhong Shaofang, WEN Huan et al. Kutemerwa kweMethylaniline Additives muMotor Gasoline neGasi Chromatography [J]. Spectrum Laboratory, 2012, Vhoriyamu 29, Chinyorwa 6, 3564-3567.

［2］Zhang Maolin, LI Baoding, ZHANG Yufa.Chidzidzo pamusoro pekugadziriswa kweN-methylaniline neSpectrophotometry [J]. Nyaya yeZhengzhou Grain University, 2000, 21(2) : 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong et al. Kudzidza paSimultaneous kutsunga kweaniline, N-methylaniline uye N, N-dimethylaniline muMhepo nepamusoro pekuita liquid chromatography [J]. Chinese Journal of Health Inspection, 2009, 19 (8) : 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng.Kugoverwa kwenitrogen-containing compounds mu catalytic peturu negasi chromatography-Nitrogen chemiluminescence kuwanikwa [J]. Chromatography,2010, 28(4): 336 - 340

DB37/T-2650, Kutemerwa kweaniline makomisheni mumotokari peturu negasi chromatography