ereyga muhiimka ah

Shidaal; Waxyaabaha lagu daro; Aniline; chromatography gaaska;

1. Horudhac Sababo la xiriira xaddidaadda tamarta batroolka gudaha iyo tignoolajiyada sifaynta, badeecadaha saliidda ee ay soo saaraan wershadaha caadiga ah ee suuqa ayaa gabaabsi noqday, taas oo ka dhigaysa tiro badan oo badeecado isku dhafan oo suuqa ku qulqulaya. Shidaal la isku daray oo joogto ah ayaa inta badan lagu qasaa nafta udgoonka (saliid fudud) oo isku qasan sida alaab ceeriin ah. Si kastaba ha ahaatee, asalka qiimaha alaabta ceeriin ee sarreeya iyo sare u qaadida faa'iidada, xeryahooda aniline waxaa badanaa loo isticmaalaa wax lagu daro gaaska aan caadiga ahayn. Si loo sameeyo tusmada tayada shidaalka ee lagu daro waxyaabahan oo kale ah inay buuxiyaan heerka qaran ee shidaalka baabuurta, tusaale ahaan, ku darida 1% (jajabka tirada badan) N-methylaniline waxay kordhin kartaa tirada octane by 2-4 unug [1]. Si kastaba ha ahaatee, daroogooyinka aniline waxay leeyihiin khataro suurtagal ah dhaqdhaqaaqa iyo badbaadada baabuurta, iyo N-methylanilines waa xeryahooda nitrogen-ku jira, taas oo horseedi doonta korodhka maadada nitrogen oxides ee qiiqa baabuurta, taasoo keenta saameyn waxyeello leh deegaanka jawiga iyo caafimaadka aadanaha. . Qaybaha ugu muhiimsan ee lagu daro aniline waxaa ka mid ah aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline iyo N, n-dimethylaniline. Waqtigan xaadirka ah, hababka caadiga ah ee la soo sheego ee lagu ogaanayo xeryahooda methylaniline waxaa ka mid ah naphthalene diethylamine spectrophotometry, gaaska chromatography-nitrogen chemiluminescence detection, chromatography dareeraha waxqabadka sare, iwm. [2-4]. Naphthalene diethylamine spectrophotometry dhaqameed ayaa farageliya natiijada go'aaminta sababtoo ah dhacdada falcelinta dhinaca, iyo habka HPLC waxaa si lama filaan ah u saameeya faragelinta matrixka gaaska.

Habka ogaanshaha chemiluminescence gaaska chromatograph-nitrogen wuxuu u baahan yahay diyaarinta kiimikooyinka kiimikada ee nitrogen-ka qaaliga ah kaas oo si xushmad leh u ogaan kara nitrogen. Heerarka qaran ee dhowaan la diyaariyey (wali aan la daabicin) "Gas Chromatography ee Go'aaminta Oxycompounds iyo Aniline Compounds ee Shidaalka" sidoo kale wuxuu qeexayaa habka falanqaynta iyadoo la adeegsanayo Deans ku beddelo laba tiir oo ka soo horjeeda oo ka soo horjeeda iyadoo la adeegsanayo qalabka caadiga ah iyo kuwa aan qaali ahayn ee hydrogen ion. Habkan, ThermoFisher Scientific ayaa daabacday warqad Codsi ah (Codsiga Qoraallada C GC-50). Fududeynta ahaan, warqadani waxay soo bandhigaysaa hab tiir degdeg ah oo ku salaysan heerka maxalliga ah ee DB37/T-2650 ee uu soo saaray Gobolka Shandong ee 2015 [5]. Natiijooyinku waxay muujinayaan in habkani yahay mid fudud in lagu shaqeeyo, oo leh ku celcelin wanaagsan iyo saxnaan sare. Isla mar ahaantaana, habka ayaa la hagaajiyay si loo xalliyo dhibaatada faragelinta qiyaasta aniline ee ka kooban matrix gaaska.

2. Dulmar guud ee mabda'a habka Tiirka polyetylen glycol (PEG), xeryahooda aniline ee gaaska baabuurta ayaa laga soocay matrixka gaaska, iyo acetophenone ayaa loo isticmaalay heerka gudaha. Waxyaabaha ku jira aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine iyo N, n-dimethylaniline ee gaaska baabuurta waxaa lagu go'aamiyay chromatograph gaas oo ku qalabaysan qalabka ionization flame (FID), iyo xoojinta qayb kasta lagu xisaabiyaa iyadoo la tixraacayo heerka gudaha.

3. Qalabka

3.1 Raad 1300E Chromatograph gaas oo leh meel shunt/aan-shunt ahayn,

AS1310 muunad otomaatig ah, Qalabka ionization Flame (FID);

3.2 Chameleon Software

3.3 Microsyringe: awoodiisu waa 10uL.

4. Reagents iyo alaabta

4.1 Tiirka: Tiirka Polar, TG-Wax, tiirka dhererka 60m,

Dhexroorka gudaha 0.25mm, dhumucda filimka dareeraha ah 0.25μm

4.2 Ilaa si kale loo cayimin, reage-yaasha lagu isticmaalo habkan waa falanqeyn ahaan saafi ah oo la ogol yahay

Isticmaal reagents kale oo nadiif ah.

Reagents loo isticmaalo ujeeddooyin tayo leh iyo tiro, oo ay ku jiraan 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) iyo N, n-dimethylaniline (CAS # 121-69-7), heerka gudaha wuxuu ahaa phenylene

Ketone (CASA # 96-86-2).

5. Hababka tijaabada ah

5.1 Samaynta qalooca caadiga ah

5.1.1 Diyaarinta xalka caadiga ah: Dhammaan walxaha caadiga ah waa isooctane (chromatographically saafi ah)

Kala-saar, siday u kala horreeyaan loogu habeeyey lix walxood oo aniline ah oo ku jira 0.1%, 0.2%, 0.5%, 1%,

Muunada caadiga ah ee heerarka 1.5% iyo 2%, eeg Shaxda 1 si aad u hesho macluumaad xog-uruurin oo faahfaahsan.

Shaxda 1. Miisaska muunadda caadiga ah

5.1.2Muunadaha caadiga ah waxaa loo falanqeeyay si waafaqsan habka GC ee Jadwalka 2

Shaxda 2. Habka GC

5.1.3 Tayada: Qaybuhu waa tayo marka loo eego wakhtiga haynta qayb kasta, iyo chromatogram-ka muunadda caadiga ah ee nooca caadiga ah (0.1% heerka fiirsashada) ayaa lagu muujiyay sawirka 1.

Jaantuska 1. Chromatogram ee muunadda caadiga ah

5.1.4 Samee qalooca caadiga ah. Wax ka beddel habka cabbiridda habka xogta ee software Chameleon, nooca cabbirku waa toosan (aan lagu khasbin asalka), nooca qiimayntu waa aagga ugu sarreeya, heerka gudahana waa isbeddel. Isla'egta qalooca caadiga ah iyo isku xidhka toosan ee qayb kasta waxa lagu muujiyay shaxda 3, iyo qalooca caadiga ah ee qayb kasta waxa lagu muujiyay sawirka 2-7.

miiska 3. xogta qalooca calibration

5.1.5 Xisaabinta natiijada: Saamiga aagga ugu sarreeya ee qayb kasta iyo meesha ugu sarreysa ee acetophenone ayaa la xisaabiyay. Jajabka tirada guud ee qayb kasta oo u dhiganta saamiga waxa laga akhriyay qalooca sixitaanka ee ku habboon, natiijaduna waa sax ilaa 0.01%.

6. Natiijooyinka iyo doodaha

6.1 Qalooca caadiga ah: Qalooca caadiga ah waxaa lagu dejiyay 6 badeecooyin caadi ah, kala duwanaanta fiirsashada mugga waa 0.01% ilaa 2.0%, iyo isku xidhka toosan ee R2 ayaa ka weyn 0.999, siday u kala horreeyaan (fiiri shaxda 3 wixii faahfaahin ah).

6.2 Xaqiijinta habka iyo hagaajinta: Marka la barbar dhigo habka beddelka Deans, habka tiirka kaliya ee lagu soo bandhigay warqadan wuxuu leeyahay faa'iidooyinka qiimo jaban, hawlgal fudud iyo soo saarid sare. Si kastaba ha ahaatee, qaybo ka mid ah matrixka gaaska ayaa laga yaabaa inay saameeyaan xeryahooda aniline.

Tusaale ahaan, marka loo eego habka lagu sharraxay warqaddan, marka la tijaabinayo muunad matrix shidaal oo bannaan, waxaa la ogaaday in ka dib marka la barbar dhigo chromatogram-ka muunadda caadiga ah, uu jiro ugu sarreeya qiyaastii 0.04min (ballaca ugu sarreeya ee ugu sarreeya waa 0.07min) laga bilaabo qaybta aniline ee alaabta caadiga ah, taas oo faragelinaysa falanqaynta aniline. (fiiri sawirka 2)

3

FIG 2. Isbarbardhigga u dhexeeya aniline standard solution spectra iyo spectra matrix gaaska banaan

Si loo xaqiijiyo in walaxdani aanay ahayn aniline, oo meesha laga saaro faragelinta qiyaasta aniline. Habka warqadan ayaa la hagaajiyay, iyo habka kor u kaca heerkulka barnaamijka waa

Sharaxaada DB37/T-2650 ee 5℃/daqiiqo ayaa loo bedelay 4℃/daqiiqo. Muunada gaaska gaaska oo leh muunado caadi ah oo lagu daray habkan ayaa lagu lafaguray. Sida ka muuqata FIG. 3,

Habka la hagaajiyay ayaa ka sooci kara qaybtan aniline ee matrixka shidaalka, waxayna sii caddaynaysaa in saamiga saliidda lagu heli karo habka DB37/T-2650

Ugu sarreeya ee 21.905min ma ahayn aniline. Kooxda faragelinta waxaa lagu go'aamiyay inay yihiin naphthalene iyadoo la eegayo spectrometry mass qualitative iyo isbarbardhigga caadiga ah.

FIG 3. Isbarbardhigga shaybaarrada saliidda, shaybaarrada aniline-ka iyo matrixka shidaalka (habka la hagaajiyay)

6.2 Heerka soo kabashada iyo tijaabada saxda ah: Tijaabada heerka soo kabashada caadiga ah waxaa lagu sameeyay matrix shidaal banaan, iyo heerka soo kabashada caadiga ah ee heerka dheeriga ah ee 100ppm ayaa la sameeyay (n=5). Natiijooyinka waxaa lagu muujiyay shaxda 4.

shaxda 4. Heerarka soo kabashada iyo natiijooyinka imtixaanka soo celinta

7.gunaanad

Tijaabadani waxa ay tilmaamaysaa heerka deegaanka ee DB37/T-2650 ee Gobolka Shandong, oo waxa uu qaataa baadhitaha FID si loo ogaado xeryahooda aniline ee shidaalka. Habka waa mid fudud natiijaduna waa mid la isku halleyn karo. Inkasta oo faragelinta loo isticmaali karo falanqaynta dhabta ah, faragelinta naphthalene ee saliidaha shidaalka qaarkood ee falanqaynta aniline waa laga fogaan karaa iyada oo la wanaajinayo xaaladaha.

Tixraacyo:

［1］Zhong Shaofang, WEN Huan iyo al. Go'aaminta Waxyaabaha lagu daro Methylaniline ee Shidaalka Baabuurta ee Gas Chromatography [J]. Shaybaadhka Spectrum, 2012, Volume 29, Issue 6, 3564-3567.

2. Zhang Maolin, LI Baoding, ZHANG Yufa. Daraasad ku saabsan go'aaminta N-methylaniline ee Spectrophotometry [J]. Wargeyska Zhengzhou Grain University, 2000, 21 (2): 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong iyo al. Daraasad ku saabsan go'aaminta isku mar ee aniline, N-methylaniline iyo N, N-dimethylaniline ee hawada iyadoo la adeegsanayo koromografi dareere ah oo sarreeya [J]. Wargeyska Shiinaha ee Kormeerka Caafimaadka, 2009, 19 (8): 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng Chromatography,2010, 28(4): 336 - 340

DB37/T-2650, Go'aaminta xeryahooda aniline ee shidaalka gaaska