izwi guru

Petroli; Zvinowedzerwa; Aniline; Gas chromatography;

1. Sumo Nekuda kwekudziviswa kwesimba remafuta emuno uye tekinoroji yekunatsa, zvigadzirwa zvemafuta zvinogadzirwa nemakambani ekuchenesa mafuta ari mumusika hazviwanikwe, izvo zvinoita kuti huwandu hwakawanda hwezvigadzirwa zvemafuta akasanganiswa hufashukire mumusika. Mafuta akasanganiswa akajairika anonyanya kusanganiswa nemafuta akasanganiswa (mafuta akareruka) sezvinhu zvekugadzira. Zvisinei, nekuda kwemitengo yepamusoro yezvinhu zvekugadzira uye kuwedzera purofiti, macompounds eaniline anowanzo shandiswa sezvinowedzera mafuta zvisina kujairika. Kuti huwandu hwemafuta ane zvinowedzerwa zvakadaro husvike padanho renyika remafuta emotokari, semuenzaniso, kuwedzera 1% (chikamu chikuru) N-methylaniline inogona kuwedzera nhamba yeoctane nemayuniti 2-4 [1]. Zvisinei, zvinowedzerwa zveaniline zvine njodzi pakufamba nekuchengetedzeka kwemotokari, uye N-methylanilines zvinhu zvine nitrogen, izvo zvinotungamira mukuwedzera kwehuwandu hwenitrogen oxides muutsi hwemotokari, zvichikonzera mhedzisiro yakaipa pamamiriro ekunze neutano hwevanhu. Zvikamu zvikuru zvezvinowedzera zveaniline zvinosanganisira aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline uye N, n-dimethylaniline. Parizvino, nzira dzinozivikanwa dzekuona methylaniline compounds dzinosanganisira naphthalene diethylamine spectrophotometry, gas chromatography-nitrogen chemiluminescence detection, high performance liquid chromatography, nezvimwewo [2-4]. Naphthalene diethylamine spectrophotometry yechinyakare inokanganisa mhedzisiro yekuona nekuda kwekuitika kwe side reaction, uye nzira yeHPLC inokanganiswa zvachose nekupindira kwe petrol matrix.

Nzira yekuongorora gas chromatograph-nitrogen chemiluminescence inoda kugadzirira nitrogen chemiluminescence detector inodhura inogona kuona nitrogen nenzira yakasarudzwa. Muyero wenyika we "Gas Chromatography for the Determination of Oxycompounds and aniline Compounds in Gasoline" wakanyorwa nguva pfupi yadarika (usati waburitswa) unotsanangurawo nzira yekuongorora uchishandisa Deans switch pamakona maviri epolar akatarisana uchishandisa hydrogen ion flame detector yakajairika uye isingadhuri. Panzira iyi, ThermoFisher Scientific yakaburitsa bepa reApplication (Application Notes C GC-50). Senzira yekurerutsa, bepa iri rinounza nzira yekolamu imwe inokurumidza yakavakirwa padanho remunharaunda DB37/T-2650 rakaburitswa neShandong Province muna 2015 [5]. Mhedzisiro yacho inoratidza kuti nzira iyi iri nyore kushandisa, ine kugona kudzokororwa zvakanaka uye kunyatsorurama. Panguva imwe chete, nzira iyi yakagadziriswa kugadzirisa dambudziko rekupindira kweaniline quantification ne petrol matrix composition.

2. Pfupiso yepfungwa yenzira iyi. Pakoramu yepolar polyethylene glycol (PEG), macompounds eaniline mupeturu yemotokari akaparadzaniswa kubva kumafuta epeturu, uye acetophenone yakashandiswa sechiyero chemukati. Zviri mukati meaniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine uye N, n-dimethylaniline mupeturu yemotokari zvakaongororwa negasi chromatograph ine flame ionization detector (FID), uye huwandu hwechikamu chimwe nechimwe hwakaverengerwa nekutarisa chiyero chemukati.

3. Zviridzwa

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

AS1310 otomatiki sampler, Flame ionization detector (FID);

3.2 Software yeChameleon

3.3 Microsyringe: kugona kwayo i10uL.

4. Zvinogadzirisa zvinhu uye zvinhu

4.1 Koramu: Koramu yePolar, TG-Wax, kureba kwekoramu 60m,

Dhayamita yemukati 0.25mm, ukobvu hwefirimu remvura 0.25μm

4.2 Kunze kwekunge zvataurwa neimwe nzira, ma reagents anoshandiswa nenzira iyi akachena uye anobvumirwa kuongorora.

Shandisa mamwe ma reagents ane kuchena kwakanyanya.

Zvinoshandiswa pakuongorora huwandu hwezvinhu, kusanganisira 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 chaive phenylene

Ketone (CASA #96-86-2).

5. Nzira dzekuedza

5.1 Kugadzwa kwegwara rakajairwa

5.1.1 Kugadzirwa kwemushonga wakajairika: Zvinhu zvese zvakajairika zvakachena kubva muchromatographically)

Kusanganiswa, kwakagadzirwa nezvinhu zvitanhatu zveaniline mu 0.1%, 0.2%, 0.5%, 1%, zvichiteerana.

Kune mienzaniso yakajairika pamazinga e1.5% ne2%, ona Tafura 1 kuti uwane ruzivo rwakadzama rwekuwanda kwemasero.

Tafura 1. Tafura yekuenzanisa yemuenzaniso wakajairika

5.1.2Mienzaniso yakajairwa yakaongororwa zvichienderana nenzira yeGC iri muTafura 2

Tafura 2. Nzira yeGC

5.1.3 Hunhu: Zvikamu izvi zvine hunhu zvichienderana nenguva yekuchengeta chikamu chimwe nechimwe, uye chromatogram yemuenzaniso wakajairika werudzi rwakajairika (0.1% concentration level) inoratidzwa muMufananidzo 1.

Mufananidzo 1. Chromatogram yemuenzaniso wakajairika

5.1.4 Gadzira curve yakajairwa. Gadzirisa nzira yekuenzanisa mumethodi yekugadzirisa data musoftware yeChameleon, mhando yekuenzanisa iri linear (haisi kumanikidzwa kupfuura kwakabva), mhando yekuongorora inzvimbo yepamusoro, uye standard yemukati inoshanduka. Standard curve equation uye linear correlation coefficient yechikamu chimwe nechimwe zvinoratidzwa muTafura 3, uye standard curve yechikamu chimwe nechimwe inoratidzwa muMufananidzo 2-7.

tafura 3. Data reCalibration curve

5.1.5 Kuverengwa kwemhedzisiro: Chiyero chenzvimbo yepamusoro pechikamu chimwe nechimwe nenzvimbo yepamusoro yeacetophenone chakaverengerwa. Chikamu chehukuru hwechikamu chimwe nechimwe chinoenderana nechiyero chinoverengwa kubva pakoridho yakakodzera yekugadzirisa, uye mhedzisiro yacho yakarurama kusvika ku0.01%.

6. Mhedzisiro nehurukuro

6.1 Mutsetse wakajairwa: Mutsetse wakajairwa unowanikwa nezvigadzirwa zvitanhatu zvakajairika, huwandu hwehuwandu hwehuwandu hunobva pa0.01% kusvika 2.0%, uye mutsetse wekubatana kwemutsara R2 wakakura kupfuura 0.999, zvichiteerana (ona Tafura 3 kuti uwane rumwe ruzivo).

6.2 Kuongororwa uye kugadziriswa kwenzira: Kana tichienzanisa neDeans switch method, nzira ye single column yakaunzwa mupepa rino ine zvakanakira zvekudhura kwakaderera, kushanda kuri nyore uye kudzokororwa kwakanyanya. Zvisinei, zvimwe zvikamu zviri mu gasoline matrix zvinogona kukanganisa aniline compounds.

Semuenzaniso, zvichienderana nenzira yakatsanangurwa mupepa rino, pakuyedza sampuro isina peturu, zvinowanikwa kuti mushure mekuenzanisa nechromatogram yesample yakajairika, pane peak painenge 0.04min (upamhi hwepeak i0.07min) kubva kuchikamu cheaniline chechigadzirwa chakajairika, izvo zvinokanganisa kuongororwa kweaniline. (ona Mufananidzo 2)

3

Mufananidzo 2. Kuenzanisa pakati peaniline standard solution spectra neblank gasoline matrix spectra

Kuti tisimbise kuti chinhu ichi hachisi aniline, uye kubvisa kukanganiswa kwehuwandu hweaniline. Nzira iri mupepa rino yakagadziriswa, uye maitiro ekuwedzera tembiricha yepurogiramu ari

Tsananguro yeDB37/T-2650 ye5℃ /min yakachinjwa kuita 4℃ /min. Samples dzematrix epeturu dzine sampuro dzakajairwa dzakaongororwa nenzira iyi. Sezvinogona kuonekwa kubva kuMufananidzo 3,

Nzira yakagadziriswa inogona kuparadzanisa chikamu ichi kubva kuaniline mu gasoline matrix, uye inoratidza zvakare kuti sampuro yemafuta inogona kuwanikwa nenzira yeDB37/T-2650.

Nguva yekusvika pa21.905min yakanga isiri aniline. Boka rekupindira rakaonekwa kuti raiva naphthalene kuburikidza ne qualitative mass spectrometry uye standard comparison.

Mufananidzo 3. Kuenzanisa kwemaspectra emasampuli emafuta, masampuli eaniline uye matrix yepeturu (nzira yakagadziriswa)

6.2 Kuedza kwekudzoreredza simba uye kunyatsoongorora: Kuedza kwekudzoreredza simba kwakaitwa nemafuta asina chinhu, uye kudzoreredza simba kwakaitwa nekuwedzera kwe100ppm (n=5). Mhedzisiro yacho yakaratidzwa muTafura 4.

tafura 4. Mwero wekupora uye mhedzisiro yebvunzo yekudzokorora

7.mhedziso

Kuedza uku kunoreva chiyero chemunharaunda cheDB37/T-2650 cheShandong Province, uye kunoshandisa FID detector kuona aniline compounds mupeturu. Nzira yacho iri nyore uye mhedzisiro yacho yakavimbika. Kunyangwe kupindirana kungashandiswa mukuongorora chaiko, kupindirana kwenaphthalene mune mamwe mapeturu ekuongorora aniline kunogona kudzivirirwa nekugadzirisa mamiriro acho ezvinhu.

Mareferensi:

［1］Zhong Shaofang, WEN Huan nevamwe. Kuongororwa kweMethylaniline Additives muMotor Petroline neGas Chromatography [J]. Spectrum Laboratory, 2012, Vhoriyamu 29, Chinyorwa 6, 3564-3567.

［2］Zhang Maolin, LI Baoding, ZHANG Yufa. Chidzidzo pamusoro pekuonekwa kweN-methylaniline neSpectrophotometry [J]. Journal of Zhengzhou Grain University, 2000, 21(2): 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong nevamwe. Chidzidzo pamusoro pekuongororwa panguva imwe chete kweaniline, N-methylaniline uye N, N-dimethylaniline mumhepo ne high performance liquid chromatography [J]. Chinese Journal of Health Inspection, 2009, 19(8): 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng. Kugoverwa kwemakonzo ane nitrogen mu catalytic peturu ne gas chromatography-Nitrogen chemiluminescence detection [J]. Chromatography,2010, 28(4): 336 — 340

DB37/T-2650, Kuongororwa kwemakomponi eaniline mupeturu yemotokari nekushandisa gasi chromatography