isiokwu

mmanụ ụgbọala; Ihe mgbakwunye; Aniline; chromatography gas;

1. mmeghe N'ihi mmachi nke ike mmanụ ala na teknụzụ nnụcha, ngwaahịa mmanụ ndị a na-emepụta mgbe niile n'ahịa dị ụkọ, nke na-eme ka ọnụ ọgụgụ dị ukwuu nke ngwaahịa mmanụ a gwakọtara ọnụ na-ejupụta ahịa. A na-agwakọta mmanụ ụgbọala a na-agwakọta mgbe niile yana naphtha aromatic (mmanụ ọkụ) agwakọta dị ka akụrụngwa. Otú ọ dị, na ndabere nke ọnụ ahịa akụrụngwa dị elu na ịba ụba nke uru, a na-ejikarị ogige aniline eme ihe dị ka ihe mgbakwunye mmanụ ụgbọala na-adịghị mma. Iji mee ka index dị mma nke mmanụ ụgbọala na ihe mgbakwunye ndị dị otú ahụ zute ọkọlọtọ mmanụ ụgbọala ụgbọ ala, dịka ọmụmaatụ, ịgbakwunye 1% (nkpịsị uka) N-methylaniline nwere ike ịbawanye ọnụọgụ octane site na nkeji 2-4 [1]. Otú ọ dị, ihe mgbakwunye aniline nwere ihe ize ndụ na njem na nchekwa nke ụgbọ ala, na N-methylanilines bụ ogige ndị nwere nitrogen, nke ga-eduga n'ịba ụba nke ọdịnaya nke nitrogen oxides na mkpochapụ ụgbọala, na-akpata mmetụta na-emerụ ahụ na gburugburu ikuku na ahụike mmadụ. . Ihe ndị bụ isi nke ihe mgbakwunye aniline gụnyere aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-methylaniline na N, n-dimethylaniline. Ugbu a, ụzọ a na-akọkarị maka nchọpụta nke ogige methylaniline gụnyere naphthalene diethylamine spectrophotometry, gas chromatography-nitrogen chemiluminescence detection, chromatography mmiri mmiri dị elu, wdg [2-4]. Omenala naphthalene diethylamine spectrophotometry na-egbochi nsonaazụ mkpebi n'ihi mmeghachi omume nke akụkụ, yana nnyonye anya nke mmanụ ụgbọala matriks na-emetụta usoro HPLC nke enweghị atụ.

Usoro nchọpụta gas chromatograph-nitrogen chemiluminescence chọrọ nkwadebe nke ihe nchọpụta chemiluminescence nitrogen dị oke ọnụ nke nwere ike ịhọrọ nitrogen. The na nso nso a depụtara (ka na-ebipụta) ọkọlọtọ mba “Gas Chromatography maka Mkpebi nke Oxycompounds na aniline Compounds na mmanụ ụgbọala” na-akọwakwa a usoro nke analysis na iji Deans ịgbanwee na abụọ na-emegide polarity kọlụm na-eji nkịtị na dịtụ ọnụ ala hydrogen ion ọkụ detector. Maka usoro a, ThermoFisher Scientific ebipụtala akwụkwọ anamachọihe (Ngwa ngwa C GC-50). Dị ka ọ dị mfe, akwụkwọ a na-ewebata usoro otu kọlụm ọsọ ọsọ dabere na ọkọlọtọ mpaghara DB37/T-2650 nke Shandong Province nyere na 2015 [5]. Nsonaazụ na-egosi na usoro a dị mfe iji rụọ ọrụ, yana ezigbo nkwughachi na oke ziri ezi. N'otu oge ahụ, a na-emezi usoro ahụ iji dozie nsogbu nke nnyonye anya nke aniline quantification site na mmanụ ụgbọala matriks mejupụtara.

2. Nleba anya nke ụkpụrụ nke usoro Na kọlụm polar polyethylene glycol (PEG), ogige aniline na mmanụ ụgbọala ụgbọala na-ekewapụ na mmanụ ụgbọala matriks, na acetophenone na-eji dị ka n'ime ọkọlọtọ. Ihe dị n'ime aniline, N-methylaniline, o-methylaniline, p-methylaniline, m-toluidine na N, n-dimethylaniline na mmanụ ụgbọala na-ekpebi site na chromatograph gas nke nwere ihe nchọpụta ọkụ ionization (FID), na ntinye nke akụkụ ọ bụla bụ. gbakọọ site n'ịtụ aka na ụkpụrụ ime.

3. Ngwa

3.1 Chọpụta 1300E Gas Chromatograph nwere ntinye shunt / enweghị shunt,

AS1310 akpaka sampler, ọkụ ionization detector (FID);

3.2 Chameleon Software

3.3 Microsyringe: ike bụ 10uL.

4. Reagents na ihe

4.1 Ogidi: kọlụm polar, TG-Wax, ogologo kọlụm 60m,

N'ime dayameta 0.25mm, mmiri mmiri film ọkpụrụkpụ 0.25μm

4.2 Ọ gwụla ma akọwapụtara n'ụzọ ọzọ, reagents eji na usoro a bụ nyocha nke ọma na ikike

Jiri ndị ọzọ reagents nke elu ịdị ọcha.

Reagents eji maka qualitative na quantitative ebumnuche, gụnyere 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) na N, n-dimethylaniline (CAS # 121-69-7), ụkpụrụ ime bụ phenylene.

Ketone (CASA # 96-86-2).

5. Ụzọ nnwale

5.1 Ntọala nke ọkọlọtọ ọkọlọtọ

5.1.1 Nkwadebe nke ọkọlọtọ ọkọlọtọ: All ọkọlọtọ bekee bụ isooctane (chromatographically dị ọcha)

Dilution, nke ahaziri ya na ihe aniline isii na 0.1%, 0.2%, 0.5%, 1%,

Maka ihe atụ ọkọlọtọ na ọkwa 1.5% na 2%, lee Tebụl 1 maka ozi ntinye uche zuru oke.

Isiokwu 1. Standard sample table ịta

5.1.2A tụlere ụkpụrụ ọkọlọtọ dịka usoro GC siri dị na Tebụl 2

Tebụl 2. Usoro GC

5.1.3 Qualitative: Ihe mejupụtara ya bụ qualitative dị ka oge njigide nke akụkụ ọ bụla, na chromatogram nke ọkọlọtọ ọkọlọtọ nke ụdị ụdị (0.1% ntinye uche) na-egosi na Figure 1.

Ọgụgụ 1. Chromatogram nke ụdị ọkọlọtọ ọkọlọtọ

5.1.4 Mepụta ọkọlọtọ ọkọlọtọ. Dezie usoro nhazi n'ime usoro nhazi data na ngwanrọ Chameleon, ụdị nhazi ahụ bụ ahịrị (anaghị amanye ya n'isi mmalite), ụdị nleba anya bụ mpaghara kachasị elu, na ụkpụrụ dị n'ime na-agbanwe agbanwe. E gosiputara nha nhata ọkọlọtọ na ọnụọgụ njikọ linear nke mpaghara ọ bụla na Tebụl 3, na akara ọkọlọtọ nke akụrụngwa ọ bụla ka egosiri na eserese 2-7.

okpokoro 3. data nhazi nhazi

5.1.5 Ngụkọta nsonaazụ: A na-agbakọ ọnụ ọgụgụ kachasị elu nke mpaghara ọ bụla na mpaghara elu nke acetophenone. A na-agụpụta akụkụ dị ukwuu nke akụkụ nke ọ bụla dabara na nha ya site na usoro mgbazi kwesịrị ekwesị, nsonaazụ ya ziri ezi ruo 0.01%.

6. Nsonazụ na mkparịta ụka

6.1 Standard curve: A na-emepụta usoro ọkọlọtọ site na ngwaahịa ọkọlọtọ 6, oke ntinye uche sitere na 0.01% ruo 2.0%, yana ọnụọgụ ọnụọgụ R2 karịrị 0.999, n'otu n'otu (lee tebụl 3 maka nkọwa).

6.2 Usoro nkwenye na njikarịcha: E jiri ya tụnyere usoro mgbanwe Deans, otu usoro kọlụm ewepụtara n'akwụkwọ a nwere uru nke ọnụ ala dị ala, ọrụ dị mfe na nrụpụta dị elu. Otú ọ dị, ụfọdụ ihe ndị dị na mmanụ ụgbọala matriks nwere ike imetụta ogige aniline.

Dịka ọmụmaatụ, dịka usoro akọwara n'akwụkwọ a si dị, mgbe ị na-anwale ihe nlele matriks petrol na-enweghị ihe ọ bụla, a na-achọpụta na mgbe atụnyere chromatogram nke ọkọlọtọ ọkọlọtọ, a na-enwe ọnụ ọgụgụ kasị elu n'ihe dịka 0.04min (obosara kachasị elu nke elu bụ 0.04min). 0.07min) sitere na akụkụ aniline nke ngwaahịa ọkọlọtọ, nke na-egbochi nyocha nke aniline. (lee foto 2)

3

FIG. 2. Tụnyere n'etiti aniline ọkọlọtọ ngwọta ụdịdị na oghere mmanụ ụgbọala matrix spectra

Iji gosi na ihe a abụghị aniline, ma kpochapụ nnyonye anya nke aniline quantification. A na-eme ka usoro dị na akwụkwọ a dịkwuo mma, na usoro mmemme okpomọkụ ịrị elu bụ

DB37/T-2650 nkọwa nke 5 ℃ / min gbanwere 4 ℃ / min. A tụlere ihe nlele matriks mmanụ ụgbọala nwere ọkọlọtọ ọkọlọtọ agbakwunyere site na usoro a. Dị ka a pụrụ ịhụ na FIG. 3,

The kacha usoro nwere ike ikewapụ a akụrụngwa si aniline na mmanụ ụgbọala matrix, na n'ihu na-egosi na mmanụ sample nwere ike nweta site DB37/T-2650 usoro.

Ọnụ kacha elu na 21.905min abụghị aniline. Ekpebiri otu nnyonye anya ka ọ bụrụ naphthalene site na qualitative mass spectrometry na ntụnyere ọkọlọtọ.

FIG. 3. Ntụle nke ụdịdị dị iche iche nke mmanụ samples, aniline samples na mmanụ ụgbọala matriks (kachasị usoro)

6.2 Ọnụego mgbake na nnwale ziri ezi: A na-eji matriks mmanụ ụgbọala efu mee nnwale nke mgbake ọkọlọtọ, na ọnụego mgbake ọkọlọtọ na ọkwa mgbakwunye nke 100ppm mere (n=5). E gosipụtara nsonaazụ ya na tebụl 4.

tebụl 4. Iweghachite ọnụego na repeatability ule results

7.mmechi

Nnwale a na-ezo aka na ọkọlọtọ mpaghara DB37/T-2650 nke Shandong Province, ma nakwere ihe nchọpụta FID iji chọpụta ogige aniline na mmanụ ụgbọala. Usoro dị mfe na nsonaazụ a pụrụ ịdabere na ya. Ọ bụ ezie na enwere ike iji nnyonye anya na nyocha n'ezie, nnyonye anya nke naphthalene na ụfọdụ mmanụ mmanụ na nyocha aniline nwere ike ịzere site n'ịkwalite ọnọdụ ahụ.

Ntụaka:

［1］Zhong Shaofang, WEN Huan et al. Mkpebi nke mgbakwunye Methylaniline na mmanụ ụgbọala site na Gas Chromatography [J]. Ụlọ nyocha Spectrum, 2012, Mpịakọta 29, mbipụta 6, 3564-3567.

2. Zhang Maolin, LI Baoding, ZHANG Yufa. Ọmụmụ na mkpebi nke N-methylaniline site Spectrophotometry [J]. Akwụkwọ akụkọ nke Mahadum Grain Zhengzhou, 2000, 21 (2): 86-88.

［3］Liu Baomin, LIU Minghong, XU Hong et al. Ọmụmụ na mkpebi nke otu oge nke aniline, N-methylaniline na N, N-dimethylaniline na ikuku site na arụmọrụ chromatography mmiri dị elu [J]. Akwụkwọ akụkọ China nke nyocha ahụike, 2009, 19 (8): 1804-1807.

4］Yang Yongtan, Wu Ming-qing, WANG Zheng. Nkesa ogige nwere nitrogen na mmanụ ụgbọala catalytic site na gas chromatography-Nitrogen chemiluminescence detection [J]. Chromatography,2010,28(4): 336 — 340

DB37/T-2650, Mkpebi nke ogige aniline na mmanụ ụgbọala site na gas chromatography