keyword

Man fetur; Additives; Aniline; Gas chromatography;

1. Gabatarwa Sakamakon takaita makamashin man fetur na cikin gida da fasahar tace man fetur da matatun mai na yau da kullum ke samarwa a kasuwa sun yi karanci, wanda ya sa dimbin man da aka hada da su ya mamaye kasuwa. Man fetur da aka haɗe na yau da kullun ana haɗe shi da gauraye nafita mai kamshi (man mai haske) azaman ɗanyen kayan aiki. Duk da haka, a bayan manyan farashin albarkatun kasa da haɓakar riba, ana amfani da mahadi aniline a matsayin abubuwan da ba a saba da su ba. Domin tabbatar da ingancin index na man fetur tare da irin wannan additives ya dace da daidaitattun man fetur na motoci, misali, ƙara 1% (mass juzu'i) N-methylaniline zai iya ƙara lambar octane ta raka'a 2-4 [1]. Duk da haka, abubuwan da ke tattare da aniline suna da haɗari masu haɗari ga motsi da amincin motocin, kuma N-methylanilines sune mahadi masu dauke da nitrogen, wanda zai haifar da karuwa a cikin abun ciki na nitrogen oxides a cikin sharar mota, haifar da illa ga yanayin yanayi da lafiyar ɗan adam. . Babban abubuwan da ke tattare da additives aniline sun hada da aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline da N, n-dimethylaniline. A halin yanzu, hanyoyin da aka fi ba da rahoto don gano mahaɗan methylaniline sun haɗa da naphthalene diethylamine spectrophotometry, gas chromatography-nitrogen chemiluminescence detection, high yi water chromatography, da dai sauransu [2-4]. Naphthalene diethylamine spectrophotometry na al'ada yana tsoma baki tare da sakamakon ƙaddara saboda abin da ya faru na halayen gefe, kuma hanyar HPLC ba makawa ya shafe shi ta hanyar tsangwama na matrix gasoline.

Hanyar gano sinadarin chromatograph-nitrogen chemiluminescence na iskar gas yana buƙatar shirya na'urar gano sinadarin nitrogen mai tsada wanda zai iya zaɓar gano nitrogen. Kwanan nan da aka tsara (har yanzu ba a buga ba) daidaitattun ƙasa "Gas Chromatography don Ƙaddamar da Oxycompounds da Aniline Compounds a Gasoline" kuma ya bayyana hanyar bincike ta amfani da Deans canza a kan ginshiƙai masu adawa da polarity guda biyu ta amfani da na kowa kuma mai rahusa mai gano harshen wuta na hydrogen ion. Don wannan hanyar, ThermoFisher Scientific ya buga takardar Aikace-aikacen ( Bayanan kula C GC-50). A matsayin sauƙi, wannan takarda ta gabatar da hanyar ginshiƙi mai sauri guda ɗaya bisa ƙa'idar gida ta DB37/T-2650 da lardin Shandong ya bayar a cikin 2015 [5]. Sakamakon ya nuna cewa wannan hanyar yana da sauƙi don aiki, tare da maimaitu mai kyau da daidaito mai girma. A lokaci guda, an inganta hanyar don magance matsalar tsangwama na ƙididdige adadin aniline ta hanyar haɗin matrix na man fetur.

2. Bayyani na ka'idar hanyar A kan ginshiƙin polyethylene glycol (PEG), mahaɗan aniline a cikin man fetur na mota sun rabu da matrix na man fetur, kuma an yi amfani da acetophenone a matsayin daidaitattun ciki. Abubuwan da ke cikin aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine da N, n-dimethylaniline a cikin iskar gas an ƙaddara su ta hanyar chromatograph gas sanye take da mai gano ionization na harshen wuta (FID), kuma ƙaddamarwar kowane bangare ya kasance. ƙididdiga ta hanyar tunani zuwa daidaitattun ciki.

3. Kayan aiki

3.1 Trace 1300E Gas Chromatograph tare da shunt / mara shunt,

AS1310 samfurin atomatik, Mai gano ionization Flame (FID);

3.2 Hawainiya Software

3.3 Microsyringe: iya aiki shine 10uL.

4. Reagents da kayan aiki

4.1 Rukunin: Shagon Polar, TG-Wax, Tsawon shafi 60m,

Inner diamita 0.25mm, ruwa film kauri 0.25μm

4.2 Sai dai in an kayyade, reagents da aka yi amfani da su a wannan hanyar suna da tsafta da halal

Yi amfani da sauran reagents na mafi girma tsarki.

Reagents da aka yi amfani da su don dalilai masu ƙima da ƙididdiga, 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), daidaitattun ciki shine phenylene.

Ketone (CASA #96-86-2).

5. Hanyoyin gwaji

5.1 Kafa daidaitattun lankwasa

5.1.1 Shiri na daidaitaccen bayani: Duk daidaitattun abubuwa sune isooctane (mai tsarki na chromatographically)

Dilution, bi da bi da aka saita tare da aniline abubuwa shida a cikin 0.1%, 0.2%, 0.5%, 1%,

Don daidaitattun samfurori a matakan 1.5% da 2%, duba Table 1 don cikakkun bayanai na tattara bayanai.

Tebur 1. Daidaitaccen samfurin taro

5.1.2An bincika daidaitattun samfuran bisa ga hanyar GC a cikin Table 2

Tebur 2. Hanyar GC

5.1.3 Qualitative: Abubuwan da aka gyara suna da inganci bisa ga lokacin riƙe kowane bangare, kuma chromatogram na daidaitaccen samfurin nau'in nau'in (0.1% maida hankali matakin) yana nunawa a cikin Hoto 1.

Hoto 1. Chromatogram na misali misali misali

5.1.4 Kafa madaidaicin lankwasa. Shirya hanyar daidaitawa a cikin hanyar sarrafa bayanai a cikin software na Chameleon, nau'in daidaitawa na layi ne (ba a tilasta shi akan asalin ba), nau'in kimantawa yanki ne kololuwa, kuma daidaitaccen ciki yana canzawa. Ana nuna ma'auni na ma'aunin lanƙwasa da madaidaicin haɗin kai na kowane bangare a cikin Tebur na 3, kuma ana nuna daidaitaccen madaidaicin kowane ɓangaren a cikin Hoto 2-7.

tebur 3. Calibration curve data

5.1.5 Sakamakon ƙididdigewa: An ƙididdige ma'auni na yanki mafi girma na kowane bangare zuwa mafi girman yanki na acetophenone. Matsakaicin juzu'in juzu'i na kowane ɓangaren da ya dace da rabo ana karanta shi daga madaidaicin gyaran da ya dace, kuma sakamakon daidai yake zuwa 0.01%.

6. Sakamako da tattaunawa

6.1 Standard Curve: An kafa madaidaicin madaidaicin ta samfuran daidaitattun 6, kewayon maida hankali daga 0.01% zuwa 2.0%, kuma madaidaicin daidaitawar R2 ya fi 0.999, bi da bi (duba Table 3 don cikakkun bayanai).

6.2 Tabbatar da hanyar da ingantawa: Idan aka kwatanta da hanyar sauya Deans, hanyar ginshiƙi guda ɗaya da aka gabatar a cikin wannan takarda yana da fa'idodin ƙananan farashi, aiki mai sauƙi da haɓakawa mai girma. Koyaya, wasu abubuwan da ke cikin matrix na man fetur na iya shafar mahaɗan aniline.

Misali, bisa ga hanyar da aka bayyana a cikin wannan takarda, lokacin da aka gwada samfurin matrix na man fetur mara kyau, an gano cewa bayan kwatanta da chromatogram na daidaitaccen samfurin, akwai kololuwa a kusan 0.04min (mafi girman nisa na kololuwa shine mafi girman nisa). 0.07min) daga sashin aniline na daidaitaccen samfurin, wanda ke tsangwama tare da nazarin aniline. (duba Hoto na 2)

3

FIG. 2. Kwatanta tsakanin aniline misali bayani bakan da kuma man fetur matrix bakan

Don tabbatar da cewa wannan abu ba aniline ba ne, kuma ya kawar da tsangwama ga ƙididdigar aniline. Hanyar a cikin wannan takarda an inganta shi, kuma tsarin hawan zafin jiki na shirin shine

DB37/T-2650 bayanin 5℃ /min canza zuwa 4℃ /min. An yi nazarin samfuran matrix na man fetur tare da daidaitattun samfuran da aka ƙara ta wannan hanya. Kamar yadda ake iya gani daga FIG. 3,

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

Kololuwar a 21.905min ba aniline bane. Ƙungiya ta tsangwama an ƙaddara ta zama naphthalene ta ƙwaƙƙwarar ƙira mai ƙima da daidaitattun kwatance.

FIG. 3. Kwatanta nau'ikan samfuran mai, samfuran aniline da matrix na man fetur (hanyar ingantawa)

6.2 Matsakaicin farfadowa da gwajin madaidaici: An gudanar da gwajin ƙimar dawo da ma'auni tare da matrix na man fetur mara kyau, kuma an yi daidaitaccen adadin dawo da ƙarin matakin 100ppm (n=5). An nuna sakamakon a Table 4.

tebur 4. Maidowa kudi da repeatability gwajin sakamakon

7.ƙarshe

Wannan gwajin yana nufin daidaitaccen gida na DB37/T-2650 na lardin Shandong, kuma yana ɗaukar na'urar gano FID don gano mahaɗan aniline a cikin mai. Hanyar yana da sauƙi kuma sakamakon abin dogara ne. Ko da yake ana iya amfani da tsangwama a cikin ainihin bincike, tsoma bakin naphthalene a cikin wasu man fetur na man fetur zuwa nazarin aniline za a iya kauce masa ta hanyar inganta yanayin.

Magana:

［1］Zhong Shaofang, WEN Huan et al. Ƙaddamar da Methylaniline Additives a cikin Motar Gas ta Gas Chromatography [J]. Laboratory Spectrum, 2012, juzu'i na 29, fitowa ta 6, 3564-3567.

2.Zhang Maolin, LI Baoding, ZHANG Yufa.Nazari akan ƙaddarar N-methylaniline ta Spectrophotometry [J]. Jaridar Jami'ar hatsi ta Zhengzhou, 2000, 21 (2): 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong et al. Nazari akan ƙayyadaddun lokaci guda na aniline, N-methylaniline da N, N-dimethylaniline a cikin iska ta babban aikin ruwa chromatography [J]. Jaridar Sinawa na Binciken Lafiya, 2009, 19 (8): 1804-1807.

4.Yang Yongtan, Wu Ming-qing, WANG Zheng.Rarraba mahalli masu dauke da nitrogen a cikin man fetur mai kara kuzari ta hanyar chromatography na iskar gas-Ganewar sinadarai na Nitrogen [J]. Chromatography, 2010, 28 (4): 336 - 340

DB37/T-2650, Ƙaddamar da mahaɗan aniline a cikin motar motar ta hanyar chromatography gas