mawu ofunika

Petroli; Zowonjezera; Aniline; chromatography ya gasi;

1. chifukwa chakuletsa kwaukadaulo wamafuta amafuta am'nyumba komanso ukadaulo woyenga, mafuta omwe amapangidwa ndi oyenga nthawi zonse pamsika akusowa, zomwe zimapangitsa kuti zinthu zambiri zosakanikirana zamafuta zisefukire pamsika. Mafuta osakanizidwa nthawi zonse amaphatikizidwa ndi naphtha (mafuta opepuka) ngati zopangira. Komabe, kumbuyo kwa mitengo yamtengo wapatali yamtengo wapatali komanso kuwonjezereka kwa phindu, mankhwala a aniline amagwiritsidwa ntchito ngati zowonjezera zosagwirizana ndi mafuta. Pofuna kuti khalidwe index wa mafuta ndi zina kukumana dziko galimoto mafuta muyezo Mwachitsanzo, kuwonjezera 1% (misa kachigawo) N-methylaniline akhoza kuonjezera chiwerengero octane ndi mayunitsi 2-4 [1]. Komabe, zowonjezera za aniline zimakhala ndi zoopsa zomwe zingawonongeke pakuyenda ndi chitetezo cha magalimoto, ndipo N-methylanilines ndi mankhwala omwe ali ndi nayitrogeni, zomwe zingapangitse kuwonjezeka kwa nitrogen oxides mu utsi wa galimoto, zomwe zimapangitsa kuti pakhale zotsatira zovulaza pamlengalenga ndi thanzi laumunthu. . Zigawo zazikulu za zowonjezera za aniline zimaphatikizapo aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline ndi N, n-dimethylaniline. Pakalipano, njira zodziwika bwino zodziwira mankhwala a methylaniline zimaphatikizapo naphthalene diethylamine spectrophotometry, gas chromatography-nitrogen chemiluminescence discovering, high performance liquid chromatography, etc. [2-4]. Naphthalene diethylamine spectrophotometry yachikhalidwe imasokoneza zotsatira zake chifukwa cha zochitika za mbali, ndipo njira ya HPLC imakhudzidwa mosapeŵeka ndi kusokoneza kwa matrix a mafuta.

Njira yodziwira gasi ya chromatograph-nitrogen chemiluminescence imafuna kukonza chojambulira chokwera mtengo cha nayitrogeni chemiluminescence chomwe chimatha kuzindikira nayitrogeni mwa kusankha. Muyezo wapadziko lonse womwe walembedwa posachedwa (oyenera kusindikizidwa) "Gas Chromatography for the Determination of Oxycompounds and aniline Compounds in Gasoline" umafotokozanso njira yowunikira pogwiritsa ntchito ma Dean switch pamizati iwiri yosiyana ya polarity pogwiritsa ntchito chowunikira chamoto wamba komanso chotsika mtengo cha hydrogen ion flame. Panjira iyi, ThermoFisher Scientific yatulutsa pepala la Application (Zolemba Zofunsira C GC-50). Monga kuphweka, pepalali limayambitsa njira yofulumira imodzi yotengera DB37/T-2650 yoperekedwa ndi Province la Shandong mu 2015 [5]. Zotsatira zikuwonetsa kuti njirayi ndi yosavuta kugwiritsa ntchito, yobwerezabwereza bwino komanso yolondola kwambiri. Panthawi imodzimodziyo, njirayo idakonzedwa kuti ithetse vuto la kusokoneza kwa aniline quantification pogwiritsa ntchito mafuta a masanjidwewo.

2. Mwachidule pa mfundo ya njira Pa chigawo cha polar polyethylene glycol (PEG), mankhwala a aniline mu mafuta a galimoto anasiyanitsidwa ndi matrix a petulo, ndipo acetophenone inagwiritsidwa ntchito ngati muyezo wamkati. Zomwe zili mu aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine ndi N, n-dimethylaniline mu petulo yamagalimoto zidatsimikiziridwa ndi chromatograph ya gas yokhala ndi chowunikira chamoto cha ionization (FID), ndipo kuchuluka kwa chigawo chilichonse chinali. kuwerengeredwa potengera mulingo wamkati.

3. Zida

3.1 Tsatani 1300E Gas Chromatograph yokhala ndi shunt/non-shunt inlet,

AS1310 automatic sampler, Flame ionization detector (FID);

3.2 Pulogalamu ya Chameleon

3.3 Microsyringe: mphamvu ndi 10uL.

4. Reagents ndi zipangizo

Mzere wa 4.1: Mzere wa Polar, TG-Wax, kutalika kwa 60m,

M'mimba mwake 0,25mm, madzi filimu makulidwe 0,25μm

4.2 Pokhapokha ngati tafotokozedwa mwanjira ina, ma reagents omwe amagwiritsidwa ntchito munjirayi ndi aulytically oyera komanso ovomerezeka

Gwiritsani ntchito ma reagents apamwamba kwambiri.

Ma reagents omwe amagwiritsidwa ntchito pazolinga zabwino komanso kuchuluka, kuphatikiza 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) ndi N, n-dimethylaniline (CAS # 121-69-7), muyezo wamkati unali phenylene

Ketone (CASA # 96-86-2).

5. Njira zoyesera

5.1 Kukhazikitsidwa kwa curve yokhazikika

5.1.1 Kukonzekera yankho lokhazikika: Zinthu zonse zokhazikika ndi isooctane (chromatographically pure)

Dilution, motsatana kukhazikitsidwa ndi zinthu zisanu aniline mu 0.1%, 0.2%, 0.5%, 1%,

Pazitsanzo zokhazikika pamiyezo ya 1.5% ndi 2%, onani Table 1 kuti mudziwe zambiri.

Tebulo 1. Tebulo lokhazikika lachitsanzo

5.1.2Zitsanzo zokhazikika zidawunikidwa molingana ndi njira ya GC mu Gulu 2

Table 2. GC njira

5.1.3 Mkhalidwe Woyenera: Zigawozo ndi zamtengo wapatali malinga ndi nthawi yosungira gawo lililonse, ndipo chromatogram ya chitsanzo chodziwika cha mtundu wamba (0.1% mlingo wa ndende) ikuwonetsedwa mu Chithunzi 1.

Chithunzi 1. Chromatogram ya chitsanzo chodziwika bwino

5.1.4 Khazikitsani njira yokhotakhota. Sinthani njira yowerengera mu njira yopangira ma data mu pulogalamu ya Chameleon, mtundu wa calibration ndi mzere (osakakamizika pa chiyambi), mtundu wowunikira ndi malo apamwamba, ndipo muyezo wamkati umasinthasintha. Ma curve equation wokhazikika ndi mzere wolumikizana ndi mzere wa chigawo chilichonse akuwonetsedwa mu Gulu 3, ndipo mayendedwe okhazikika a gawo lililonse akuwonetsedwa Chithunzi 2-7.

tebulo 3. Data yokhotakhota

5.1.5 Kuwerengera kwa zotsatira: Chiŵerengero cha chigawo chapamwamba cha chigawo chilichonse ndi malo apamwamba a acetophenone chinawerengedwa. Gawo lalikulu la gawo lililonse lolingana ndi chiŵerengerocho limawerengedwa kuchokera pamapindikira oyenera, ndipo zotsatira zake ndi zolondola mpaka 0.01%.

6. Zotsatira ndi zokambirana

6.1 Mzere wokhotakhota: Mzere wokhotakhota umakhazikitsidwa ndi zinthu 6 zokhazikika, kuchuluka kwa ndende ya voliyumu kumachokera ku 0.01% mpaka 2.0%, ndipo mzere wolumikizirana R2 ndi wamkulu kuposa 0.999, motsatana (onani Gulu 3 kuti mumve zambiri).

6.2 Njira yotsimikizira ndi kukhathamiritsa: Poyerekeza ndi njira yosinthira a Deans, njira imodzi yokha yomwe idayambitsidwa mu pepalali ili ndi zabwino zake zotsika mtengo, zophweka komanso zopangana zambiri. Komabe, zigawo zina mu petulo matrix zingakhudze mankhwala aniline.

Mwachitsanzo, molingana ndi njira yomwe yafotokozedwa mu pepalali, poyesa chitsanzo cha petulo chopanda kanthu, chimapezeka kuti tikayerekeza ndi chromatogram ya chitsanzo chodziwika bwino, pali chiwongoladzanja cha pafupifupi 0.04min (chiwongoladzanja cha nsonga yake ndi 0.07min) kuchokera ku gawo la aniline la chinthu chokhazikika, chomwe chimasokoneza kusanthula kwa aniline. (onani Chithunzi 2)

3

CHITH. 2. Kuyerekeza pakati pa mawonekedwe a aniline solution ndi matrix opanda kanthu a petulo

Pofuna kutsimikizira kuti chinthu ichi si aniline, ndi kuthetsa kusokoneza kwa aniline quantification. Njira yomwe ili mu pepalali imakongoletsedwa, ndipo ndondomeko yowonjezereka ya kutentha ndi

Kufotokozera kwa DB37/T-2650 kwa 5 ℃ /mphindi kusinthidwa kukhala 4 ℃ / min. Zitsanzo za matrix a petulo okhala ndi zitsanzo zokhazikika zomwe zidawonjezeredwa zidawunikidwa ndi njira iyi. Monga momwe zikuwonekera kuchokera ku FIG. 3,

Njira yowongoleredwa imatha kulekanitsa gawo ili kuchokera ku aniline mu matrix amafuta, ndikutsimikiziranso kuti chitsanzo chamafuta chikhoza kupezedwa ndi njira ya DB37/T-2650.

Pamwamba pa 21.905min sanali aniline. Gulu losokoneza lidatsimikiziridwa kukhala naphthalene ndi qualitative mass spectrometry ndi kuyerekezera kofanana.

CHITH. 3. Kuyerekeza kwa zitsanzo za mafuta, zitsanzo za aniline ndi matrix a petulo (njira yowongoka)

6.2 Mlingo wochira komanso kuyesa kolondola: Kuyesa kwanthawi zonse kwa kuchira kunachitika ndi matrix opanda kanthu a petulo, ndipo mulingo wamba wochira ndi mulingo wowonjezera wa 100ppm udachitika (n = 5). Zotsatira zawonetsedwa mu Table 4.

tebulo 4. Kuchira mlingo ndi zotsatira repeatability mayeso

7.mapeto

Kuyesera uku kumatanthauza DB37/T-2650 ya m'chigawo cha Shandong, ndipo imatenga chowunikira cha FID kuti chizindikire mankhwala a aniline mu petulo. Njirayi ndi yosavuta ndipo zotsatira zake ndi zodalirika. Ngakhale kusokonezedwa kungagwiritsidwe ntchito pakuwunika kwenikweni, kusokoneza kwa naphthalene mu magawo ena a petulo ku kusanthula kwa aniline kungapewedwe mwa kuwongolera mikhalidwe.

Zolozera:

［1］Zhong Shaofang, WEN Huan et al. Kutsimikiza kwa Methylaniline Additives mu Motor Gasoline ndi Gas Chromatography [J]. Spectrum Laboratory, 2012, Volume 29, Issue 6, 3564-3567.

［2］Zhang Maolin, LI Baoding, ZHANG Yufa.Kafukufuku wokhudza kutsimikiza kwa N-methylaniline ndi Spectrophotometry [J]. Journal ya Zhengzhou Grain University, 2000, 21 (2): 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong et al. Phunzirani pa kutsimikiza munthawi yomweyo aniline, N-methylaniline ndi N, N-dimethylaniline mu Air ndi high performance liquid chromatography [J]. Chinese Journal of Health Inspection, 2009, 19 (8) : 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng.Kugawidwa kwa mankhwala okhala ndi nayitrogeni mu mafuta othandizira ndi gas chromatography-Nitrogen chemiluminescence discovery [J]. Chromatography, 2010, 28(4): 336 - 340

DB37/T-2650, Kutsimikiza kwa mankhwala a aniline mu petulo yamagalimoto ndi gasi chromatography