kalmar maɓalli

Fetur; Ƙari; Aniline; Chromatography na iskar gas;

1. Gabatarwa Saboda takaita amfani da makamashin man fetur na cikin gida da fasahar tacewa, kayayyakin mai da matatun mai na yau da kullun ke samarwa a kasuwa suna cikin ƙarancin wadata, wanda ke sa adadi mai yawa na kayayyakin mai da aka haɗa suka mamaye kasuwa. Ana haɗa man fetur da aka haɗa akai-akai da naphtha mai ƙanshi mai laushi (mai sauƙi) a matsayin kayan masarufi. Duk da haka, a bayan hauhawar farashin kayan masarufi da haɓaka riba, galibi ana amfani da mahaɗan aniline azaman ƙarin man fetur marasa tsari. Domin tabbatar da ingancin man fetur tare da irin waɗannan ƙari sun cika ƙa'idar man fetur na ƙasa, misali, ƙara 1% (ƙasa mai yawa) N-methylaniline na iya ƙara adadin octane da raka'a 2-4 [1]. Duk da haka, ƙarin aniline yana da yuwuwar haɗari ga motsi da amincin ababen hawa, kuma N-methylanilines mahaɗan ne masu ɗauke da nitrogen, wanda zai haifar da ƙaruwar abun ciki na nitrogen oxides a cikin hayakin mota, yana haifar da illa ga muhallin yanayi da lafiyar ɗan adam. Babban abubuwan da ke cikin ƙarin aniline sun haɗa da aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline da N, n-dimethylaniline. A halin yanzu, hanyoyin da aka fi ruwaitowa don gano mahaɗan methylaniline sun haɗa da naphthalene diethylamine spectrophotometry, gano gas chromatography-nitrogen chemiluminescence, high performance liquid chromatography, da sauransu. [2-4]. Naphthalene diethylamine spectrophotometry na gargajiya yana tsoma baki ga sakamakon tantancewa saboda faruwar amsawar gefe, kuma babu makawa hanyar HPLC tana shafar ta hanyar tsangwama na matrix na fetur.

Hanyar gano gas chromatograph-nitrogen chemiluminescence tana buƙatar shirya na'urar gano nitrogen mai tsada wacce za ta iya gano nitrogen a zahiri. An tsara kwanan nan (wanda ba a buga ba) ma'aunin ƙasa "Gas Chromatography don Tabbatar da Oxycompounds da aniline Compounds a cikin Gasoline" kuma ya bayyana hanyar bincike ta amfani da maɓallin Deans akan ginshiƙai biyu masu adawa da juna ta amfani da na'urar gano harshen hydrogen ion na yau da kullun kuma mai araha. Don wannan hanyar, ThermoFisher Scientific ta buga takardar Aikace-aikace (Bayanan Aikace-aikacen C GC-50). A matsayin sauƙaƙawa, wannan takarda ta gabatar da hanyar ginshiƙi ɗaya mafi sauri bisa ga ma'aunin DB37/T-2650 na gida wanda lardin Shandong ya bayar a 2015 [5]. Sakamakon ya nuna cewa wannan hanyar tana da sauƙin aiki, tare da kyakkyawan maimaitawa da babban daidaito. A lokaci guda, an inganta hanyar don magance matsalar tsangwama na ƙididdigar aniline ta hanyar haɗa matrix na gasoline.

2. Bayani kan ƙa'idar hanyar A kan ginshiƙin polyethylene glycol (PEG), an raba mahaɗan aniline a cikin man fetur na mota daga matrix na man fetur, kuma an yi amfani da acetophenone a matsayin ma'aunin ciki. An tantance abubuwan da ke cikin aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine da N, n-dimethylaniline a cikin man fetur na mota ta hanyar amfani da na'urar gano ionization ta gas (FID), kuma an ƙididdige yawan kowane sashi ta hanyar la'akari da ma'aunin ciki.

3. Kayan kida

3.1 Gilashin Gas Chromatograph na 1300E tare da hanyar shiga shunt/non-shunt,

AS1310 samfurin atomatik, na'urar gano ionization ta harshen wuta (FID);

3.2 Manhajar Hawainiya

3.3 Microsyringe: ƙarfinsa shine 10uL.

4. Masu sake haɗawa da kayan aiki

4.1 Ginshiƙi: Ginshiƙin polar, TG-Wax, tsawon ginshiƙi mita 60,

Diamita na ciki 0.25mm, kauri na fim ɗin ruwa 0.25μm

4.2 Sai dai idan an ƙayyade wani abu daban, abubuwan da ake amfani da su a cikin wannan hanyar suna da tsarki kuma an yarda da su ta hanyar nazari.

Yi amfani da wasu sinadaran da ke da tsarki sosai.

Magungunan da ake amfani da su don dalilai na inganci da adadi, gami da 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) da N, n-dimethylaniline (CAS#121-69-7), ma'aunin ciki shine phenylene

Ketone (CASA #96-86-2).

5. Hanyoyin gwaji

5.1 Kafa lanƙwasa na yau da kullun

5.1.1 Shirya maganin da aka saba amfani da shi: Duk abubuwan da aka saba amfani da su suna da isooctane (tsaftace a tsarin chromatographic)

Narkewa, an tsara shi da sinadarai shida na aniline a cikin 0.1%, 0.2%, 0.5%, 1%,

Don samfuran da aka saba da su a matakan 1.5% da 2%, duba Tebur 1 don cikakken bayani game da yawan tattarawa.

Tebur 1. Teburin tattara bayanai na misali

5.1.2An yi nazarin samfuran da aka saba bisa ga hanyar GC a cikin Tebur 2

Tebur na 2. Hanyar GC

5.1.3 Inganci: Abubuwan da aka haɗa suna da inganci gwargwadon lokacin riƙewa na kowane sashi, kuma an nuna chromatogram na samfurin da aka saba amfani da shi na nau'in da aka saba amfani da shi (matakin tattarawa 0.1%) a cikin Hoto na 1.

Hoto na 1. Chromatogram na samfurin yau da kullun

5.1.4 Kafa lanƙwasa ta yau da kullun. Gyara hanyar daidaitawa a cikin hanyar sarrafa bayanai a cikin manhajar Chameleon, nau'in daidaitawa yana layi (ba a tilasta shi akan asalin ba), nau'in kimantawa shine yankin kololuwa, kuma ma'aunin ciki yana canzawa. An nuna daidaiton lanƙwasa na yau da kullun da ma'aunin haɗin layi na kowane sashi a cikin Jadawali na 3, kuma an nuna lanƙwasa ta yau da kullun na kowane sashi a Hoto na 2-7.

Tebur 3. Bayanan lanƙwasa na daidaitawa

5.1.5 Lissafin Sakamako: An ƙididdige rabon yankin kololuwar kowanne sashi zuwa yankin kololuwar acetophenone. An karanta ɓangaren girman taro na kowane sashi wanda ya dace da rabo daga lanƙwasa mai dacewa, kuma sakamakon ya yi daidai da 0.01%.

6. Sakamako da tattaunawa

6.1 Layin Daidaitacce: An kafa layin daidaitacce ta hanyar samfura 6 na yau da kullun, kewayon yawan ƙarar yana daga 0.01% zuwa 2.0%, kuma ma'aunin haɗin kai na layi R2 ya fi 0.999, bi da bi (duba Tebur 3 don ƙarin bayani).

6.2 Tabbatar da hanyoyin da ingantawa: Idan aka kwatanta da hanyar canza Deans, hanyar ginshiƙi ɗaya da aka gabatar a cikin wannan takarda tana da fa'idodin ƙarancin farashi, sauƙin aiki da kuma yawan sake samarwa. Duk da haka, wasu abubuwan da ke cikin matrix na fetur na iya shafar mahaɗan aniline.

Misali, bisa ga hanyar da aka bayyana a cikin wannan takarda, lokacin gwada samfurin matrix na gas mara komai, an gano cewa bayan kwatantawa da chromatogram na samfurin da aka saba, akwai kololuwa a kusan minti 0.04 (faɗin kololuwar kololuwar shine minti 0.07) daga ɓangaren aniline na samfurin da aka saba, wanda ke tsoma baki ga nazarin aniline. (duba Hoto na 2)

3

FIG. 2. Kwatanta tsakanin siginar maganin aniline na yau da kullun da siginar matrix na gas mara komai

Domin tabbatar da cewa wannan sinadari ba aniline ba ne, da kuma kawar da tsangwama ga ƙididdige aniline. An inganta hanyar da ke cikin wannan takarda, kuma tsarin hauhawar zafin shirin shine

Bayanin DB37/T-2650 na 5℃ /min an canza shi zuwa 4℃ /min. An yi nazarin samfuran matrix na fetur tare da samfuran yau da kullun da aka ƙara ta wannan hanyar. Kamar yadda za a iya gani daga Hoto na 3,

Hanyar da aka inganta za ta iya raba wannan bangaren da aniline a cikin matrix na fetur, kuma ta ƙara tabbatar da cewa ana iya samun samfurin mai ta hanyar hanyar DB37/T-2650.

Kololuwar da aka samu a minti 21.905 ba aniline ba ce. An tabbatar da cewa rukunin tsangwama ya zama naphthalene ta hanyar amfani da na'urar auna mass spectrometry da kuma kwatancen da aka saba.

FIG. 3. Kwatanta spectra na samfuran mai, samfuran aniline da matrix na fetur (hanyar da aka inganta)

6.2 Gwajin Matsakaici da Daidaito: An gudanar da gwajin matsakaici na ma'aunin ma'aunin man fetur mara komai, kuma an gudanar da gwajin ma'aunin ...

Tebur 4. Sakamakon gwajin dawowa da maimaitawa

7.ƙarshe

Wannan gwajin yana nufin daidaitaccen DB37/T-2650 na lardin Shandong, kuma yana amfani da na'urar gano FID don gano mahaɗan aniline a cikin fetur. Hanyar tana da sauƙi kuma sakamakon abin dogaro ne. Kodayake ana iya amfani da tsangwama a cikin ainihin binciken, ana iya guje wa tsangwama na naphthalene a cikin wasu abubuwan da ke cikin mai zuwa binciken aniline ta hanyar inganta yanayin.

Nassoshi:

［1］Zhong Shaofang, WEN Huan da sauransu. Tantance Ƙarin Methylaniline a cikin Man Fetur ta hanyar Gas Chromatography [J]. Dakin Gwaji na Spectrum, 2012, Juzu'i na 29, Fitowa ta 6, 3564-3567.

［2］Zhang Maolin, LI Baoding, ZHANG Yufa. Nazari kan tantance N-methylaniline ta hanyar Spectropphotometry [J]. Mujallar Jami'ar Hatsi ta Zhengzhou, 2000, 21(2): 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong da sauransu. Bincike kan tantance aniline, N-methylaniline da N, N-dimethylaniline a cikin iska ta hanyar amfani da chromatography na ruwa mai aiki sosai [J]. Mujallar Nazarin Lafiya ta Sin, 2009, 19(8): 1804-1807.

［4］Yang Yongtan, Wu Ming-qing, WANG Zheng. Rarraba mahaɗan da ke ɗauke da nitrogen a cikin man fetur mai narkewa ta hanyar amfani da chromatography na gas-Gano sinadarin nitrogen [J]. Chromatography, 2010, 28(4): 336 — 340

DB37/T-2650, Tantance mahaɗan aniline a cikin man fetur ta hanyar amfani da chromatography na gas