mawu ofunikira

Mafuta; Zowonjezera; Aniline; Chromatography ya mpweya;

1. Chiyambi Chifukwa cha kuchepetsa mphamvu ya mafuta m'nyumba ndi ukadaulo woyenga mafuta, mafuta opangidwa ndi mafakitale oyenga mafuta nthawi zonse pamsika ndi ochepa, zomwe zimapangitsa kuti mafuta ambiri osakanikirana azidzaza msika. Mafuta osakanikirana nthawi zonse amasakanizidwa ndi mafuta onunkhira osakanikirana (mafuta opepuka) ngati zinthu zopangira. Komabe, chifukwa cha mitengo yokwera ya zinthu zopangira komanso phindu lalikulu, mankhwala a aniline nthawi zambiri amagwiritsidwa ntchito ngati zowonjezera zamafuta zosazolowereka. Pofuna kuti mafuta abwino okhala ndi zowonjezera zotere azikwaniritsa muyezo wa mafuta agalimoto, mwachitsanzo, kuwonjezera 1% (gawo lalikulu) N-methylaniline ikhoza kuwonjezera chiwerengero cha octane ndi mayunitsi 2-4 [1]. Komabe, zowonjezera za aniline zimakhala ndi zoopsa pakuyenda ndi chitetezo cha magalimoto, ndipo N-methylanilines ndi mankhwala okhala ndi nayitrogeni, zomwe zingayambitse kuwonjezeka kwa kuchuluka kwa nayitrogeni oxides mu utsi wa magalimoto, zomwe zimayambitsa mavuto pa chilengedwe ndi thanzi la anthu. Zigawo zazikulu za zowonjezera za aniline ndi aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline ndi N, n-dimethylaniline. Pakadali pano, njira zomwe zimafotokozedwa kawirikawiri zopezera mankhwala a methylaniline ndi monga naphthalene diethylamine spectrophotometry, kuzindikira gas chromatography-nitrogen chemiluminescence, high performance liquid chromatography, ndi zina zotero [2-4]. Njira yachikhalidwe ya naphthalene diethylamine spectrophotometry imasokoneza zotsatira zodziwira chifukwa cha kuchitika kwa side reaction, ndipo njira ya HPLC imakhudzidwa mosalekeza ndi kusokoneza kwa matrix ya petrol.

Njira yodziwira mpweya wa chromatograph-nitrogen chemiluminescence imafuna kukonzekera chowunikira cha nitrogen chemiluminescence chokwera mtengo chomwe chingathe kuzindikira nayitrogeni mosankha. Muyezo wadziko lonse wolembedwa (wosasindikizidwa) wa "Gas Chromatography for the Determination of Oxycompounds and aniline Compounds in Petroline" umafotokozanso njira yowunikira pogwiritsa ntchito Deans switch pa mizati iwiri yotsutsana ya polarity pogwiritsa ntchito chowunikira cha hydrogen ion chodziwika bwino komanso chotsika mtengo. Pa njira iyi, ThermoFisher Scientific yafalitsa pepala la Application (Application Notes C GC-50). Pofuna kuphweka, pepalali likuwonetsa njira yofulumira ya mizati imodzi kutengera muyezo wapafupi wa DB37/T-2650 woperekedwa ndi Shandong Province mu 2015 [5]. Zotsatira zake zikuwonetsa kuti njira iyi ndi yosavuta kugwiritsa ntchito, yokhala ndi kubwerezabwereza bwino komanso kulondola kwambiri. Nthawi yomweyo, njirayi idakonzedwa bwino kuti ithetse vuto la kusokoneza kwa kuchuluka kwa aniline ndi kapangidwe ka matrix a petrol.

2. Chidule cha mfundo ya njira imeneyi Pa mzere wa polar polyethylene glycol (PEG), mankhwala a aniline mu mafuta a magalimoto adalekanitsidwa ndi mafuta a petulo, ndipo acetophenone idagwiritsidwa ntchito ngati muyezo wamkati. Zomwe zili mu aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine ndi N, n-dimethylaniline mu mafuta a magalimoto zidatsimikiziridwa ndi chromatograph ya gasi yokhala ndi chowunikira cha flame ionization (FID), ndipo kuchuluka kwa gawo lililonse kudawerengedwa potengera muyezo wamkati.

3. Zida

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

AS1310 choyezera chokha, chowunikira ma ionization a malawi (FID);

3.2 Mapulogalamu a Chameleon

3.3 Microsyringe: mphamvu yake ndi 10uL.

4. Zothandizira ndi zipangizo

4.1 Mzati: Mzati wa polar, TG-Wax, kutalika kwa mzati 60m,

M'mimba mwake wamkati 0.25mm, makulidwe a filimu yamadzimadzi 0.25μm

4.2 Pokhapokha ngati tatchula mwanjira ina, ma reagents omwe amagwiritsidwa ntchito mu njira iyi ndi oyera komanso ololedwa.

Gwiritsani ntchito zinthu zina zoyera kwambiri.

Ma reagents omwe amagwiritsidwa ntchito pazinthu zodziwika bwino komanso zowerengera, kuphatikizapo 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 Kukhazikitsa njira yokhazikika

5.1.1 Kukonzekera njira yokhazikika: Zinthu zonse zokhazikika ndi za isooctane (zopanda chromatographically)

Kusungunuka, komwe kumapangidwa motsatana ndi zinthu zisanu ndi chimodzi za aniline mu 0.1%, 0.2%, 0.5%, 1%,

Kuti mudziwe zitsanzo zokhazikika pamlingo wa 1.5% ndi 2%, onani Gome 1 kuti mudziwe zambiri za kuchuluka kwa madzi m'thupi.

Gome 1. Tebulo lokhazikika la zitsanzo

5.1.2Zitsanzo zokhazikika zinasanthulidwa motsatira njira ya GC mu Table 2

Gome 2. Njira ya GC

5.1.3 Mkhalidwe: Zigawozi ndi zamtundu malinga ndi nthawi yosungira ya gawo lililonse, ndipo chromatogram ya chitsanzo chokhazikika cha mtundu wamba (mlingo wa 0.1% wa kuchuluka) ikuwonetsedwa mu Chithunzi 1.

Chithunzi 1. Chromatogram ya chitsanzo chokhazikika

5.1.4 Khazikitsani kapitolo kokhazikika. Sinthani njira yowerengera mu njira yogwiritsira ntchito deta mu pulogalamu ya Chameleon, mtundu wa kapitolo ndi wolunjika (osati wokakamizidwa kuposa woyambira), mtundu wowunikira ndi dera la peak, ndipo muyezo wamkati ndi wosinthasintha. Equation yokhazikika ya kapitolo ndi coefficient yolumikizana yolunjika ya gawo lililonse ikuwonetsedwa mu Table 3, ndipo kapitolo kokhazikika ka gawo lililonse kakuwonetsedwa mu Chithunzi 2-7。

tebulo 3. Deta ya calibration curve

5.1.5 Kuwerengera zotsatira: Chiŵerengero cha dera la nsonga ya gawo lililonse ndi dera la nsonga ya acetophenone chinawerengedwa. Gawo la kuchuluka kwa voliyumu ya gawo lililonse logwirizana ndi chiŵerengerocho limawerengedwa kuchokera ku curve yoyenera yokonza, ndipo zotsatira zake ndi zolondola mpaka 0.01%.

6. Zotsatira ndi zokambirana

6.1 Mzere wokhazikika: Mzere wokhazikika umakhazikitsidwa ndi zinthu 6 zokhazikika, kuchuluka kwa voliyumu kumakhala kuyambira 0.01% mpaka 2.0%, ndipo coefficient ya kulumikizana kwa mzere R2 ndi yayikulu kuposa 0.999, motsatana (onani Gome 3 kuti mudziwe zambiri).

6.2 Kutsimikizira ndi kukonza njira: Poyerekeza ndi njira ya Deans switch, njira ya single column yomwe yatchulidwa mu pepalali ili ndi ubwino wa mtengo wotsika, ntchito yosavuta komanso kubwerezabwereza kwakukulu. Komabe, zigawo zina mu petrol matrix zingakhudze ma aniline compounds.

Mwachitsanzo, malinga ndi njira yomwe yafotokozedwa mu pepalali, poyesa chitsanzo chopanda mafuta cha matrix, zapezeka kuti poyerekeza ndi chromatogram ya chitsanzo chokhazikika, pali nsonga pafupifupi 0.04min (m'lifupi mwake ndi 0.07min) kuchokera ku gawo la aniline la chinthu chokhazikika, zomwe zimasokoneza kusanthula kwa aniline. (onani Chithunzi 2)

3

CHITHUNZI 2. Kuyerekeza pakati pa aniline standard solution spectra ndi blank gasoline matrix spectra

Pofuna kutsimikizira kuti chinthuchi si aniline, ndikuchotsa kusokoneza kwa kuchuluka kwa aniline. Njira yomwe ili mu pepalali ndi yabwino kwambiri, ndipo njira yowonjezerera kutentha kwa pulogalamuyo ndi

Kufotokozera kwa DB37/T-2650 kwa 5℃/min kwasinthidwa kukhala 4℃/min. Zitsanzo za matrix a petulo zokhala ndi zitsanzo zokhazikika zomwe zawonjezeredwa zidasanthulidwa ndi njira iyi. Monga momwe zikuonekera kuchokera pa Chithunzi 3,

Njira yabwino kwambiri imatha kulekanitsa gawoli ndi aniline mu mafuta, ndipo imatsimikiziranso kuti chitsanzo cha mafuta chingapezeke pogwiritsa ntchito njira ya DB37/T-2650.

Chiwopsezo chachikulu pa mphindi 21.905 sichinali aniline. Gulu losokoneza linapezeka kuti ndi naphthalene pogwiritsa ntchito qualitative mass spectrometry ndi standard comparison.

CHITHUNZI 3. Kuyerekeza kwa ma spectra a zitsanzo za mafuta, zitsanzo za aniline ndi matrix ya petulo (njira yabwino kwambiri)

6.2 Kuyesa kwa kuchira ndi kulondola: Kuyesa kwa kuchira kwachizolowezi kunachitika ndi matrix yopanda mafuta, ndipo kuchira kwachizolowezi komwe kunali ndi mulingo wowonjezera wa 100ppm kunachitika (n=5). Zotsatira zake zawonetsedwa mu Gome 4.

tebulo 4. Zotsatira za mayeso obwezeretsa ndi kubwerezabwereza

7.mapeto

Kuyesera kumeneku kukutanthauza muyezo wa DB37/T-2650 wa m'chigawo cha Shandong, ndipo kumagwiritsa ntchito chowunikira cha FID kuti chizindikire mankhwala a aniline mu petulo. Njirayi ndi yosavuta ndipo zotsatira zake ndi zodalirika. Ngakhale kusokoneza kungagwiritsidwe ntchito pakusanthula kwenikweni, kusokoneza kwa naphthalene m'magawo ena a petulo pa kusanthula aniline kungapewedwe mwa kukonza bwino zinthu.

Maumboni:

［1］Zhong Shaofang, WEN Huan ndi ena. Kuzindikira Zowonjezera za Methylaniline mu Petroli Yoyendetsa ndi Gas Chromatography [J]. Spectrum Laboratory, 2012, Voliyumu 29, Nkhani 6, 3564-3567.

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

［3］Liu Baomin, LIU Minghong, XU Hong ndi ena. Kafukufuku wokhudza kutsimikiza kwa aniline, N-methylaniline ndi N, N-dimethylaniline mumlengalenga pogwiritsa ntchito chromatography yamadzimadzi yogwira ntchito bwino [J]. Chinese Journal of Health Inspection, 2009, 19(8): 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng. Kugawa kwa mankhwala okhala ndi nayitrogeni mu mafuta oyambitsa pogwiritsa ntchito mpweya wa chromatography-Kuzindikira kwa nayitrogeni chemiluminescence [J]. Chromatography,2010, 28(4): 336 — 340

DB37/T-2650, Kuzindikira mankhwala a aniline mu mafuta a injini pogwiritsa ntchito chromatography ya gasi