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جستجوی مقالات مرتبط با کلیدواژه "gas chromatography" در نشریات گروه "شیمی"

تکرار جستجوی کلیدواژه «gas chromatography» در نشریات گروه «علوم پایه»
  • رضوان عسکری بدویی، مریم کاظمی پور*، ندا محمدی، محمد مهدی پور

    با گسترش استفاده از مواد فسیلی، آلودگی مواد غذایی به هیدروکربن های آروماتیک چند حلقه ای (Polycyclic Aromatic Hydrocarbons: PAHs)ا به یک تهدید سلامتی در سراسر دنیا تبدیل شده به نحوی که بسیاری از مراجع نظارتی برای آنها حدود مجاز تعیین نموده اند. امروزه اندازه گیری این آلاینده ها در مواد غذایی یکی از زمینه های مهم تحقیقاتی به شمار می آید. در این پژوهش، پوشش نانوکامپوزیت ZnO /MWCNTs بر روی سیم استیل ساخته شد و به عنوان یک پوشش فیبر میکرو استخراج فاز جامد فضای فوقانی جدید (HS-SPME) برای استخراج مقادیر ناچیز آلاینده های زیست محیطی بررسی شد. مشخصات نانوکامپوزیت تهیه شده با استفاده از طیف سنجی مادون قرمز تبدیل فوریه (FTIR) و میکروسکوپ الکترونی روبشی (SEM) مورد ارزیابی قرار گرفت. پارامترهای موثر بر HS-SPME هیدروکربن ها (به عنوان مثال ، دما و زمان استخراج ، دما و زمان واجذب و غلظت نمک) با استفاده از روش یک متغیر در هر زمان، بررسی و بهینه سازی شدند. این پوشش برای اندازه گیری 4 PAHs شامل نفتالن، فلورن، آنتراسن و فنانترن در نمونه آب قلیان به دست آمده از تنباکوهای مختلف مورد استفاده قرار گرفت. نتایج به دست آمده در این کار نشان می دهد که نانوکامپوزیت تهیه شده می تواند ماده پوششی امیدوار کننده ای برای کاربردهای آینده SPME و تکنیک های تهیه نمونه مربوطه باشد. این روش در محدوده غلظت 1 تا 20 میکروگرم بر لیتر برای 4 PAHs مورد نظر خطی و انحراف استاندارد نسبی روش زیر 9 درصد بوده و حداقل تعیین مقدار به طور کلی حدود 3/0 میکروگرم بر لیتر به دست آمد.

    کلید واژگان: نانوذرات اکسید روی, نانولوله کربنی چند جداره, نانوکامپوزیت, روش میکرو استخراج فضای فوقانی, کروماتوگرافی گازی
    Rezvan Askari Badoee, Maryam Kazemipour *, Neda Mohammadi, Mohammad Mehdipour

    With the expansion Polycyclic Aromatic Hydrocarbons (PAHs), the contamination of food with these pollutants has become a health threat all over the world in such a way that many regulatory authorities have set permissible limits for them. Today, the measurement of these pollutants in food is one of the important research fields. In this research, ZnO/MWCNTs nanocomposite coating was fabricated on stainless steel and investigated as a new upper space solid phase microextraction (HS-SPME) fiber coating for extracting small amounts of environmental pollutants. The characteristics of the prepared nanocomposite were evaluated using Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The parameters affecting the HS-SPME of hydrocarbons (for example, extraction temperature, extraction time, desorption temperature, desorption time, and salt concentration) were investigated and optimized using the method of one variable at a time. The coating was used to measure 4 PAHs including naphthalene, fluorene, anthracene and phenanthrene in hookah water samples obtained from different tobaccos. The results show that the prepared nanocomposite can be a promising coating material for future applications of SPME and related sample preparation techniques. This method was linear in the concentration range of 1 to 20 μg/liter for the 4 PAHs, and the RSD% of the method was less than 9%, and the LOQ were generally around 0.3 μg/liter.

    Keywords: Zinc Oxide Nanoparticles, Multi-Walled Carbon Nanotube, Nanocomposite, Head Space Solid Phase Microextraction, Gas Chromatography
  • Ioryue Ijah Silas, Terngu Timothy Uzah

    The research presents a comparative analysis of the quality of locally produced groundnut oil (Arachis hypogaea) sold in the north-central zone of Nigeria markets (Benue, Nasarawa, Kogi, Kwara, Niger and Plateau S tates). The aim was to assess and compare the qualities of the oils and to know the safety of human consumption. The groundnut oil produced biodiesel, shampoo lubricants, and soap-making indus tries. The concentrations of the heavy metals were analyzed with atomic absorption spectrometry (AAS). It showed that the lead, zinc, and copper (Pb, Zn, Cu) were within the FAO/WHO recommended limit, while Cd (0.201-0.331 mg kg-1) was above the limit (0.07 mg kg-1). Also, the gas chromatography (GC-FID) results indicated that twelve fatty acids (linoleic > oleic > palmitic > s tearic > lignoceric > arachidic acid > behenic > erucic > arachidonic > margaric > linolenic > palmitoleic) were obtained in the groundnut oils in all markets and fatty acids include caprylic acid, capric acid, lauric acid, and myris tic acid were absent in oils. In addition, the magnitude of six phospholipids (phosphatidylcholine > phosphatidylethanolamine > phosphatidylinositol > phosphatidylserine > phosphatidic acid > lysophosphatidylcholine) were also achieved, respectively. The results showed that iodine, peroxide, saponification value and refractive index were below the FAO/WHO recommended level, and the acid value was higher than the normal range.

    Keywords: Analysis, Groundnut oil, Atomic absorption spectrometer, Fatty acid, Phospholipids, Gas chromatography
  • مهدی تقدیری*، ستاره ذاکری شهواری، حمیدرضا زارع مهرجردی

    در این کار تحقیقاتی یک روش چندباقیمانده سریع، دقیق و حساس و با هزینه مناسب بر مبنای روش کچرز برای اندازه گیری و پایش باقیمانده سموم در برنج ارائه می شود. جداسازی هم زمان آفت کش ها با دستگاه کروماتوگرافی گازی مجهز به آشکارساز اسپکترومتر جرمی با سرعت جریان گاز حامل 0/1 میلیلیتر بر دقیقه، دمای تزریق 250 درجه سانتیگراد با مد غیر انشعابی و ستون موئینه به طول 30 متر با سرعت جریان 0/1 میلی لیتر بر دقیقه انجام گرفت. در این تحقیق استونیتریل به عنوان حلال استخراجی به کار گرفته شد. آنالیت های استخراج شده در نهایت با روش استخراج فاز جامد پخشی پاک سازی شد. در شرایط بهینه منحنی درجه بندی برای تمامی آفت کش ها در محدوده غلظتی 0/1000-0/10 میکروگرم بر لیتر خطی بوده و مقادیر ضرایب همبستتگی بین 99/0 تا 999/0 بدست آمدند. مقادیر درصد بازیابی بین 79 تا 112 درصد با درصد انحراف استاندارد نسبی کمتر از 7 درصد بدست آمد. همچنین حد تشخیص و حد اندازه گیری کمی مناسبی برای تمامی آفت کش ها به دست آمد. مقادیر حد تشخیص بین 52/12-04/3 میکروگرم بر لیتر و حد اندازه گیری کمی بین 76/41-14/10 میکروگرم بر لیتر بدست آمدند.

    کلید واژگان: کروماتوگرافی گازی, طیف سنجی جرمی, آفت کش, روش چندباقیمانده, روش کچرز
    Mehdi Taghdiri *, Setareh Zakeri-Shahvari, Hamidreza Zare-Mehrjardi

    The principle of this research is based on the development of multi-residue method by QuEChERS sample preparation follow by gas chromatography with mass spectrometric detection in the selected ion monitoring mode (GC–MS-SIM) for the routine analysis of 42 pesticides in rice samples. The rice samples were initially extracted with acetonitrile, and the targeted pesticides were purified following the dispersive solid phase extraction (d-SPE) cleanup method. The calibration curve for each analyte quantified by matrix-matched calibration was linear over the concentration range of 10.0–1000.0 μg L−1 with a correlation coefficient range between 0.990 and 0.999. Mean recoveries from three replicates ranged from 79% to 112%, with satisfactory precision (RSD<7%). The limit of detection and the limit of quantification were in the range of 3.04–12.52 μg L−1 and 10.14–41.76 μg L−1 respectively, for all 42 pesticides.

    Keywords: Gas chromatography, Mass spectrometry, matrix-matched calibration, Multi-residue, Pesticide, QuEChERS
  • Ali Akbar Imani, MohammadReza Rezaei Khahkha, Rouhollah Parvari, Maryam Faraji, Ali Faghihi Zarandi *

    Toluene is one of the mos t dangerous and, simultaneously, the mos t consumed subs tances in various factories. Toluene s trongly affects the central nervous sys tem. The numerous side effects caused by exposure to toluene indicate the removal of toluene vapours from the air in the workplace. This s tudy aims to use the removal of toluene vapours from the air using a Fe-MOFs metal-organic subs trate for the firs t time in the world and to inves tigate efficient methods to increase the efficiency of removing toluene vapours from the air. This experimental s tudy was carried out on a laboratory scale. After the iron metal-organic framework (Fe-MOFs) was synthesized, the components affecting the adsorption rate, such as reaction time (5-20 min), initial concentration (100-400 mg L-1), adsorbent amount, and temperature (25-80oC) were analyzed and optimized. Then, the efficiency of removing toluene vapours from the air was determined using a gas chromatography device. The absorption capacity of toluene was obtained by the desired adsorbent, 337.2 mg g-1. Also, the effect of different parameters on toluene absorption was inves tigated and optimized. The maximum absorption for concentration (300 mg L-1), temperature (75oC), and contact time (160s) were obtained as 340 mg g-1, 331 mg g-1, and 325 mg g-1, respectively. The obtained results indicate the suitability of the Fe-MOFs for the absorption of toluene vapours from the air before being determined by gas chromatography (GC-FID).

    Keywords: Toluene, Removal, Adsorption, Iron metal-organic frameworks, Gas chromatography
  • Mohammad Gheshlaghi, Khalil Farhadi *, Rahele Tahmasebi

    Polycyclic aromatic hydrocarbons (PAHs) have been listed among the hazardous compounds according to the US environmental protection agency (USEPA) and the world health organization (WHO). Even low concentrations of PAHs have shown serious toxicity, highlighting the necessity of the measurement of these compounds which require highly sensitive and precise methods. In this study, for the first time, a solid phase microextraction (SPME) fiber was fabricated by a highly porous monolithic nanofiber nanocomposite based on polyethersulfone (PES)/multiwalled carbon nanotubes (MWCNTs) and used for direct sampling of indoor air before identification of polycyclic aromatic compounds by gas chromatography-flame ionization detector (GC-FID). A new homemade sampling chamber was also designed to increase the exposure of airborne PAHs to the proposed SPME fiber. The microextraction conditions were optimized. The correlation coefficients and the linear range (LDR) of the compounds ranged from 0.9991 to 0.9996 and from 0.02 to 10 mg/m3, respectively. In addition, the limit of detection (LOD) varied in the range of 0.014-0.032 mg/m3. The relative standard deviation (RSD) for single fiber and fiber to fiber was 2.95 and 5.95%, respectively. This method was successfully applied to measure some PAHs in indoor spaces.

    Keywords: Monolithic fibers, Polyethersulfone, Solid-phase microextraction, Polycyclic aromatic hydrocarbons, Gas chromatography, Indoor air
  • Mostafa jafarizaveh Jafarizaveh, Akram Tabrizi, Farideh Golbabaei

    As main air pollutants, volatile organic compounds (VOCs) must be paid special attention. In this study, the removal efficiency of xylene from the air was investigated by nano-activated carbons (NACs) as an efficient adsorbent and compared to commercial activated carbons (ACs). In the chamber, the xylene vapor in pure air was generated, stored in the airbag (5 Li), and moved to adsorbents. Then, the xylene vapor was absorbed on the NAC/AC adsorbents and desorbed from it by a heat accessory. The efficiency of xylene removal with NACs and ACs was investigated in the dynamic and static systems based on 100-700 mg L-1 of xylene, flow rates of 100 ml min-1, and 100 mg of adsorbent at a humidity of 32% (25°C). Xylene concentrations were determined by gas chromatography equipped with a flame ionization detector (GC-FID). In the batch system, the maximum absorption capacity for NACs and ACs was obtained at 205.2 mg g-1 and 116.8 mg g-1, respectively. The mean adsorption efficiency for NACs and ACs adsorbents was obtained at 98.5% and 76.55%, respectively. The RSD% for NACs ranged between 1.1-2.5% in optimized conditions. The characterizations of the NACs adsorbent showed that the particle-size range was between 35-100 nm. The results showed that the adsorption efficiency of NACs for removing xylene from the air was achieved more than ACs. The GC-MS validated the proposed procedure in real air samples.

    Keywords: Xylene, Adsorption, Air, Nano activated carbon, Dynamic system, Gas chromatography
  • Afsaneh Hajializadeh, Mehdi Ansari, Mohammad Mehdi Foroughi, Shohreh Jahani, Maryam Kazemipour *
    New Solid-Phase Microextraction (SPME) coating was made by electrodeposition of Zeolite Imidazolate Framework (ZIF-67) nanocrystals with the aid of polyaniline (PANI) on steel fiber. The SPME fiber was used to extract four Polycyclic Aromatic Hydrocarbons (PAHs) from the Head Space (HS) of tea infusions and determined by Gas Chromatography coupled with a Flame Ionization Detector (GC-FID). The coating of the SPME fiber was characterized by Fourier Transformed InfraRed (FT-IR) spectroscopy and Scanning Electron Microscopy (SEM). Vital parameters affecting extraction performance, including desorption conditions, salt concentration, extraction time, and temperature, have been evaluated and optimized. The validated method was specific for the PAHs analysis, with the Limit of Detection (LOD) as low as 20.0 to 50.0 ng/L. The linear range was relevant to 70.0-180.0 ng/L with a relative standard deviation (RSD) % of less than 12.8. The factor of enrichment was found to be 446.7-808.8. The synthesized coating was shown to be thermally and chemically stable. The recommended approach was successfully applied to quantify PAHs in some frequent tea infusions in the market. The fiber coating of ZIF-67 can be easily made and applied efficiently to detect PAHs pollution in the environment and food products.
    Keywords: Metal-organic framework, Solid-phase microextraction, ZIF-67, Gas chromatography, Tea infusion
  • Aknur Turgumbayeva, Nazym Tileuberdi, Kairat Zhakipbekov *, Saken Tulemissov, Galiya Umurzakhova, Gulnara Utegenova
    Polylactide based essential oil films were formulated by incorporating polyethylene glycol, nanopowder (zinc oxide), and essential oil by solvent casting method.The films were tested against pathogens for their antibacterial activity.The effectiveness of selected oil-nanomaterial based film was tested by performing the tests. In vitro antibacterial efficacies of nanopowders/essential oil were determined by the decimal reduction concentrations and the minimum bactericidal concentrations for the pathogens. In a typical process, Brassica napus extract was obtained from supercritical fluid extraction using pressurized carbon dioxide as solvent. The composition of the essential oil was analyzed by gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS).39 compounds were identified in the oil.Polylactide based essential oil films were formulated by incorporating polyethylene glycol, nanopowder (zinc oxide), and essential oil by solvent casting method.The films were tested against pathogens for their antibacterial activity. The effectiveness of selected oil-nanomaterial based film was tested by performing the tests. In vitro antibacterial efficacies of nanopowders/essential oil were determined by the decimal reduction concentrations and the minimum bactericidal concentrations for the pathogens.In a typical process, Brassica napus extract was obtained from supercritical fluid extraction using pressurized carbon dioxide as solvent.The composition of the essential oil was analyzed by gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). 39 compounds were identified in the oil. The major compounds of the oil were 1,3,6,10-Cyclotetradecatetraene, 3,7,11-trimethyl-14- (1-methylethyl) - 30,07%, Cyclohexanone, 5 -methyl-2- (1-methylethylidene) - 12.91%, 3,4-Methylenedioxypropiophenone - 9,67%, Hexadecanoic acid, ethyl ester - 8.28%, Octacosanol - 5,50%, 11,15-Tetramethylhexadeca-1,3,6,10,14-pentaene - 4,55% and 1,6,10,14-Hexadecatetraen-3-ol, 3,7,11,15-tetramethyl – 3,14 %.
    Keywords: Brassica napus, essential extract, gas chromatography, Oil-Nanomaterial film
  • Ali Faghihi Zarandi, Corresponding, MohammadReza Rezaei Kahkha, MohammadBagher Aghebatbekheir, Nasser Hasheminejad

    Benzene has a carcinogenic effect on the human body and adsorption from the air is the best way to control it. By this research, benzene vapor was removed from the air based on a tantalum metal-organic framework (Ta-MOF) by gas flow solid-phase interaction (GF-SPI). Benzene adsorption with Ta-MOF was studied in the static and dynamic systems at room temperature. The benzene concentration was analyzed by gas chromatography equipped with an FID detector (GC-FID). The factors affecting benzene removal efficiency like initial concentration of benzene, amount of adsorbent, exposure time, flow rate, and temperature were studied and optimized. The results showed us, the adsorption capacities range of Ta-MOF for benzene in the static and dynamic system were obtained between 90-160 mg g -1 and 65-135 mg g -1 , respectively. Also, the high removal efficiency was achieved by more than 95% at 45°C, 67.5 mg L -1 benzene concentration, 0.5 g of Ta-MOF, and the flow rate of 250 mL min -1 for a dynamic system. By dynamic system, the benzene is generated in the chamber, stored in a bag, and then moved on the surface of Ta-MOF. The GF-SPI method was validated by GC-MS and spiking real samples.

    Keywords: Adsorption, Gas flow solid-phase interaction, Tantalum metal-organic framework, Gas chromatography
  • محبوبه دهقانی، مریم کاظمی پور*، مهدی انصاری، مهدی شهیدی زندی
    در این پژوهش، یک جاذب کامپوزیتی از پلی پیرول، نانولوله های کربنی چند جداره اصلاح شده و کربن فعال اصلاح شده حاصل از پوسته سخت فندق، به روش الکتروشیمیایی سنتز و از آن برای تجزیه گروهی از هیدروکربن های آروماتیک فرار در نمونه های چای و سبزیجات استفاده شد. بهینه سازی پارامترهای موثر بر فرآیند پوشش دهی فیبر و هچنین پارامترهای موثر در مرحله واجذبی آنالیت ها به روش کلاسیک و مرسوم تغییر یک متغیر در یک زمان (OVAT)، انجام شد. بر اساس نتایج حاصله پتانسیل پوشش دهی 1 ولت، زمان پوشش دهی 1000 ثانیه، دمای واجذبی 280 درجه سانتی گراد و زمان واجذبی 5 دقیقه بعنوان مقادیر بهینه در نظر گرفته شدند. برای بهینه سازی پارامترهای موثر در مرحله استخراج از طراحی آزمایش استفاده شد که در نهایت دمای استخراج 25 درجه سانتی گراد، زمان استخراج 30 دقیقه و مقدار نمک 10 درصد بدست آمد. در روش پیشنهادی، منحنی کالیبراسیون بدست آمده برای نفتالن در محدوده غلظتی 8-5/0 میکروگرم بر لیتر، برای فلورن و فنانترن در محدوده غلظتی 15-2 میکروگرم بر لیتر و برای آنتراسن و پایرن در محدوده غلظتی10-2 میکروگرم بر لیتر خطی بود. در شرایط بهینه، حدود تشخیص برای آنالت های هدف 9/0-06/0 میکروگرم بر لیتر بود و تکرارپذیری (%RSD)، روش در محدوده 6/8-5/0 متغیر بود.
    کلید واژگان: جاذب کامپوزیتی, نانو لوله های کربنی, میکرواستخراج فاز جامد, کروماتوگرافی گازی, هیدروکربن های آروماتیک
    Mahboobeh Dehghani, Maryam Kazemipour *, Mehdi Ansari, Mehdi Shahidizandi
    In this study, a composite coating of polypyrrole/modified multiwalled carbon nanotubes/modified activated carbon prepared from hazelnut shells (PPy/MWCNTs/AC), was electrochemically synthesized and used for analyzing a group of volatile aromatic hydrocarbons in tea and vegetable samples. In order to obtain an adherent and stable composite coating, the effective parameters on electrodeposition process were optimized using the one-variable-at-a-time procedure, as well as the effective parameters in the desorption step of analytes was performed by this method. Based on the results, the deposition potential of 1 V, the deposition time of 1000 seconds, the desorption temperature of 280 ° C and the desorption time of 5 minutes were considered as the optimal values. To optimize the effective parameters in the extraction stage, the experimental design was used. Finally, the extraction temperature was 25 ° C, the extraction time was 30 minutes and the amount of salt was 10%. The calibration curve for each analyte in a range was linear as follows: 2 ̶ 15 µg ̸ L (fluorene and phenanthrene), 2 ̶ 10 µg ̸ L (anthracene and pyrene) and 0.5 ̶ 8 µg ̸ L (naphthalene). Under the optimized conditions, the amounts of the detection limits (LODs) calculated at S ̸ N proportion of 3, were varied from 0.06 to 0.9 µg ̸ L. The RSDs% of the peak areas ranged between 0.5 and 8.6%.
    Keywords: composite adsorbent, Carbon nanotubes, Aromatic Hydrocarbons, Solid phase microextraction, Gas Chromatography
  • Hamideh Assadollahzadeh*, Ebrahim Noroozian

    The analysis of organochlorine pesticides (OCPs) residues has received an increasing attention in the last decades. Thesolid-phase microextration (SPME) is a convenient and fast analytical method, which has been widely used for the determination of volatile and semivolatile organic compounds in aqueous samples. In this study, the multiwalled carbon nanotubes/polypyrrole composite (MWCNTs-PPy) coated on steel fiber was used for extraction OCPs from water samples by the SPME technique. The effects of various parameters on the efficiency of SPME process such as extraction time, extraction temperature, ionic strength, desorption time, and desorption temperature were studied. Under optimized conditions, the detection limits for the OCPs varied between 0.051 and 0.39 pg mL-1, the inter-day and intra-day relative standard deviations for various OCPs using a single fiber were 6.5-11.5% and 3.6-11.5, respectively. The linear ranges varied between 0.001 and 1 ng mL-1. The proposed method was successfully applied to the analysis of ground water samples with the recoveries from 86 to 110%

    Keywords: Organochlorine pesticides, Multiwalled carbon nanotubes, Polypyrrole composite, Solid phase microextraction, Gas chromatography
  • Mir Ali Farajzadeh *, Sakha Pezhhanfar, Ali Mohebbi, MohammadReza Afshar Mogaddam

    Migration of chemicals from plastic containers into drinks and liquids containing them, is supposed to be a hazardous phenomenon and results in many health problems. Sample preparation is of great importance due to trace amounts analysis of these compounds. In this research, dispersive liquid–liquid microextraction is applied for the extraction and preconcentration of the migrated compounds prior to their detection and determination by gas chromatography equipped with mass spectrometry or flame ionization detector. The method is on the basis of forming droplets of a water–immiscible organic solvent (extractant) into an aqueous phase by means of a disperser solvent. As a result, there would be a large contact area between the extractant and aqueous phase containing the analytes which boosts mass transfer. After centrifuging, the extractant is sedimented at the bottom of the aqueous phase and an aliquot of it is removed and injected into the separation system. Various experimental conditions which influence the extraction efficiency were optimized. Under the optimum conditions, the extraction recoveries were ranged from 52–63%. The relative standard deviations were ≤ 7.2% for intra– (n = 6) and inter–day (n = 4) precisions at a concentration of 20 µg L–1 of each analyte. The limits of detection were in the range of 0.18–0.38 µg L–1. Eventually the applicability of the proposed method for appraising the compounds migrated from the plastic containers was evaluated by analyzing the target compounds in different drinks and liquids stored in the plastic bottles.

    Keywords: Plastic bottles, Phthalate esters, antioxidants, endocrine disruptors, Dispersive liquid-liquid microextraction, Gas Chromatography
  • Mohammad Chahkandi *, Amirhassan Amiri

    In this study, we demonstrate the application of newly developed magnetic potassium substituted hydroxyapatite (KHA/Fe3O4) for the extraction of phthalate esters (PE) from water samples. Nanoparticles of KHA were synthesized through an easy alkoxide–based sol–gel technique. The structure of nanocomposite was characterized by X–ray diffraction (XRD), Fourier transform infrared (FTIR) analysis, and energy dispersive X–ray Analysis (EDXA). Moreover, the size of nanoparticle and micro–strain of synthesized KHA and KHA/Fe3O4 using Williamson–Hall (W–H) plots and transmission electron microscopy (TEM) were measured. The hexagonal and cubic structures of synthesized KHA and its nanocomposite having P63/m space group confirmed by XRD pattern. Also, the size of spherical particles of KHA in pure and nanocomposite, and Fe3O4 nanoparticles evaluated by W–H and TEM methods are in good agreement as 60, 65, and 18 nm. The PEs were analyzed by gas chromatography‒flame ionization detector (GC‒FID). Different parameters influencing the extraction efficiency including: sample pH, amount of sorbent, extraction time, desorption conditions, and salt effect, were optimized. The obtained optimal conditions were: sample pH, 7; amount of sorbent, 25 mg; extraction time, 8.0 min; desorption solvent and its volume, 200 μL dichloromethane; and desorption time, 5.0 min. Under optimum conditions, good linearity was achieved for all analytes in the 0.015–100 ng mL−1 concentration range. The limits of detection (at an S/N ratio of 3) are between 0.005 and 0.03 ng mL−1. The recoveries of PEs from spiked real water samples are between 86.3 and 99.2%, with relative standard deviations between 5.3 and 9.3 %.

    Keywords: Phthalate esters, Gas Chromatography, Potassium substituted hydroxyapatite, Magnetic nanoparticle, Sol-Gel, Transmission electron microscopy, Fourier transform infrared spectrometry, X-ray diffraction
  • پیمان معینی، احمد باقری*
    در کار حاضر به منظور بررسی و بهینه سازی دمای پراکنش ترکیب سیانو کربنی (اورتو کلروبنزیلیدین مالونونیتریل یا OCBM) ، سه روش آماده سازی نمونه با نام های میکرواستخراج فاز جامد، نمونه برداری با استفاده از تله خلاء دو جزئی و اسکن دمایی در پورت تزریق با دستگاه کروماتوگرافی گازی مورد استفاده قرار گرفته اند. از کاربردهای ترکیب سیانو کربنی OCBMبرای تست ماسک های محافظ عوامل شیمیایی بوده و بررسی ها نشان دهنده آن هستند که در بسیاری از مراکز به منظور پراکنده کردن این ترکیب در اتاقک های تست از قرار دادن آن به صورت پودر بر روی هیترهایی با دمای بالا استفاده می شود. فرض هایی مبنی بر اینکه این شیوه پراکنش در درجه حرارت های بالا ممکن است سبب تخریب ماده، تولید مواد سمی و یا ایجاد واکنش های ناخواسته شود وجود دارد. از این رو از دیگر اهداف مورد بررسی در این مقاله، آنالیز بخارات تولید شده از پراکنش ترکیب سیانو کربنی OCBM با شیوه مذکور و پاسخ به سوالات مطرح شده در این فرضیات بوده است. برای این منظور در ابتدا اطلاعات اولیه ای از اسکن دمایی ترکیب هدف در پورت تزریق دستگاه کروماتوگرافی حاصل شده، پس از آن برای ایجاد بیشترین مشابهت بین شرایط نمونه برداری و شرایط عملیاتی به کارگرفته در اتاقک های تست گاز، ترکیب بر روی هیتر قرار داده شده و با اعمال بیشترین دمای ممکن، ترکیب تبخیر و از آن نمونه برداری شده است. در بخش پایانی مقاله از روش میکرواستخراج فاز جامد به عنوان یک روش آماده سازی عاری از حلال آلی برای استخراج و تشخیص ترکیبات با غلظت ناچیز تولید شده در فرآیند پراکنش استفاده شده است.
    کلید واژگان: OCBM, سیانو کربنی, کروماتوگرافی گازی, میکرواستخراج فاز جامد, تله خلاء دو جزئی
    Peymnan Moeini, Ahmad Bagheri *
    Abstract In this work, in order to investigate and optimize the dispersion temperature of the cyanocarbon compound(O-Chlorobenzylidene Malononitrile or OCBM), three methods of preparation of the sample with solid phase micro extraction, sampling using two-component vacuum traps and temperature scanning in the injection port using the gas chromatography apparatus used are located. The use of the OCBM cyanocarbon compound for testing chemical masks has been tested and tests have shown that in many centers, in order to disperse this compound in test chambers, it is placed in powder form on heaters with temperature high is used. There are assumptions that this dispersal technique at high temperatures may cause material damage, producing toxic substances, or creating unwanted reactions. Therefore, the other objectives of this paper were to analyze the vapors generated by the distribution of the OCBM produced by the cyanocarbon in the country with the above-mentioned method and the answer to the questions posed by these assumptions. For this purpose, preliminary information was obtained from the objective target temperature scan at the chromatography injection port, and then, in order to create the most similarity between the sampling conditions and the operating conditions used in the gas test chambers, the combination was placed on the heater. The mixture is evaporated and sampled using the highest possible temperature. In the final section of the paper, the solid-state micro-extraction method is used as an organic solvent-free preparation method for the extraction and detection of low-concentration compounds produced in the dispersion process.
    Keywords: Cyanocarbon OCBM, Gas Chromatography, Solid Phase micro extraction, Two-component vacuum trap
  • Mir Ali Farajzadeh, Masoumeh Sattari Dabbagh, Adeleh Yadegari, Ali Akbar Alizadeh Nabil
    Two convenient sample preparation methods, air–assisted liquid–liquid microextraction (AALLME) and dispersive liquid–liquid microextraction (DLLME) have been developed for the simultaneous determination of multiclass pesticide residues in vegetable and fruit juice samples with gas chromatography–flame ionization detection and the advantages of each method were investigated. In AALLME, fine droplets of an extraction solvent were immediately formed by suction with a syringe and injection of the mixture of an aqueous sample solution and an extraction solvent into a test tube for several times. In DLLME, the cloudy solution was formed with the aid of a disperser solvent. The effect of main factors, such as type and volume of extraction solvent, salt addition, pH, etc was studied. Under the optimum conditions, enrichment factors and extraction recoveries were obtained in the ranges of 262–515, 52–103% and 45–438, 9.2–88% in AALLME and DLLME methods, respectively. Both methods are inexpensive, simple, fast, efficient, reliable, and sensitive. Therefore, the proposed methods are suitable for determination of trace levels of multiclass pesticide residues in fruit juice and vegetable samples.
    Keywords: Air-assisted liquid-liquid microextraction, Dispersive liquid-liquid microextraction, Fruit, vegetable samples, Gas chromatography, Multiclass pesticides
  • Hossein Hashempour *, Maryam Mehmannavaz, Mostafa Ebadi, Abdolreza Abri, Amir, Abbas Matin, Ali Reza Amani, Ghadim
    In this study, fatty acid (FA) composition of aerial parts of selected Salvia species from Iran was analyzed by Gas chromatography. The amount of FAs was quantified for leaf and shoot of species as mg per kg (mg/kg) of dry weight. The results showed that FA contents of aerial parts for studied plants varied significantly and changed between 73.05 and 739.50 mg/kg of dried weight. Caprylic (C8:0, 1.00-380.49 mg/kg), elaididc (C18:1n9t, 0.73-97.29 mg/kg), stearic (C18:0, 1.1-62.97 mg/kg), palmitic (C16:0, 1.19-36.48 mg/kg), and α-linoleic (C18:3n3, 1.34-19.36 mg/kg) acid were major identified FAs. The numerical analyze was applied on FA composition of shoot and leaf of specimens and the shoot FA composition was selected to identify the systematic position of studied species. The UPGMA (Unweighted Pair Group Method with Arithmetic Mean) dendrogram showed that the species were grouped in two clusters. Caprylic acid (C8:0), behenic acid (C22:0), and lignoceric acid (C24:0) were chief characters in the infrageneric grouping the species in the genus. S. chloroleuca and S. atropatanawere placed in cluster I and separated from other species based on shoot FA composition. The discrimination of Salvia species based on their botanical classification was supported by results. The results confirmed that FA composition of shoot are distinguishable and can be used as chemotaxonomic markers.
    Keywords: Salvia, Fatty Acid composition, Chemotaxonomy, Gas Chromatography
  • افسانه ملاحسینی*، سپیده عباسی
    در کار حاضر، برای اولین بار، نانو فیبر الکتروریسی شده پلی آکریلونیتریل به عنوان پوشش جدید در میکرو استخراج فاز جامد ((SPME و اندازه گیری فتالات ها از نمونه های آب معرفی شد. پارامترهای آزمایشگاهی موثر بر کارایی SPME، با استفاده از روش سطح پاسخ (RSM)، بر اساس طرح مرکب مرکزی (CCD) بهینه شدند. تحت شرایط بهینه، روش حاضر، دارای منحنی کالیبراسیون خطی در محدوده 1-100 ng/ml و ضریب همبستگی (r2) بیشتر از 0.998 است. تکرارپذیری و تجدید پذیری روش ارائه شده، به ترتیب در محدوده 3.8-4.3 و 7.7-8.5 بوده و حدود تشخیص برابر با 0.05-1.0 ng/ml بودند.روش توسعه داده شده به طور موفقیت آمیزی برای اندازه گیری فتالات ها در نمونه های آب به کاربرده شد و بازیابی های نسبی در این محیط ها93-105 درصد به دست آمد.
    کلید واژگان: نانوفیبر الکتروریسی شده, پلی آکریلونیتریل, میکرواستخراج فاز جامد, کروماتوگرافی گازی, فتالات, طرح مرکب مرکزی
    Afsaneh Mollahhosseini *, Sepideh Abbasi
    In the present work, for the first attempt, polyacrylonitrile electrospun nanofiber was introduced as a new sorbent in solid phase microextraction method for determining phthalates in various water samples. Affecting parameters on the performance of SPME were optimized using response surface methodology (RSM) based on central composite design (CCD). Under optimum conditions, the method yielded a linear calibration curve ranging from 1-100 ng/ml with correlation coefficients (r2) higher than 0.998. The repeatability and reproducibility of the proposed method were between 3.8-4.3 and 7.7-8.5, respectively. Limits of detection were 0.05-1.0 ng/ml. The newly developed method was successfully applied for the determination of phthalates in various water samples and relative recoveries in these matrices were 93-105%.
    Keywords: Polyacrylonitrile electrospun nanofibers, Solid phase microextraction, Gas-chromatography, Phthalates, Central composite design
  • آرزو قادی *، اسماعیل بابانژاد آریمی، علی معزی، ایمان محمدی
    کلرزنی به منظور ضدعفونی آب شرب به دلیل واکنش کلر با مواد آلی طبیعی موجود در آب مثل اسیدهای تانیک، فلویک و هیومیک موجب تشکیل محصولات جانبی نظیر تری هالومتان ها می شود. به علت سرطان زا بودن این ترکیبات، اندازه گیری سریع این ترکیبات در آب نیازمند روش های تجزی های سریع و حساس می باشد. در این تحقیق، روش میکرو استخراج فاز جامد، به عنوان یک تکنیک جداسازی و پیش تغلیظ عاری از حلال برای تعیین چهار تری هالومتان رایج در آب آشامیدنی و با استفاده از کروماتوگرافی گازی با طیف سنج جرمی مورد استفاده قرار گرفته است. در این تکنیک، فیبر پلی دی متیل سیلوکسان و به روش فضای فوقانی، برای پیش تغلیظ و استخراج آنالیت از نمونه آبی بهکار گرفته شد. شناسایی و اندازه گیری آنالیتهای استخراج شده به وسیله واجذب حرارتی در محفظه تزریق کروماتوگرافی گازی- طیف سنج جرمی انجام شد. پارامترهای مختلف موثر بر کارایی استخراج تری هالومتان ها از قبیل دمای استخراج و واجذب، زمان استخراج و واجذب و همچنین مقدار نمک بررسی و بهینه شدند. تحت شرایط بهینه، فاکتور تغلیظ حد تشخیص در محدوده 1/2 تا 4/4 میکروگرم بر لیتر و محدوده خطی از 20 تا 600 میکروگرم بر لیتر به دست آمد. انحراف استاندارد نسبی در سطح غلظت 30 میکروگرم بر لیتر تری هالومتان ها در آب در محدوده 1/3-5/2% بهدست آمد. روش به طور موفقیت آمیز برای استخراج و تعیین تری هالومتان ها در آب آشامیدنی شهرهای استان مازندران به کار برده شد.
    کلید واژگان: تری هالومتان ها, آب شرب, میکرو استخراج فاز جامد, کروماتوگرافی گازی, طیف سنج جرمی
    Arezoo Ghaderi *
    Chlorination for disinfection of drinking water leads to the formation of by-products like trihalomethanes, due to the reaction of chlorine with natural organic compounds like tannic acid, fulvic acid, and humic acid. Due to the carcinogenicity of these compounds, rapid measurement of these compounds in water requires rapid and sensitive analytical methods. In this study, solid-phase microextraction was used as a solvent-free separation and pre-condensation technique to determine four common halomethanes in drinking water using gas chromatography with mass spectroscopy. In this technique, polydimethylsiloxane fiber was used as headspace method for pre-condensation and extraction of the analyte from the aqueous sample. Detection and measurement of the extracted analytes was conducted using thermal desorption in the injection chamber of gas chromatography-mass spectroscopy. Various parameters affecting the efficiency of trihalomethane extraction, including the extraction and desorption temperature, the extraction and desorption time in addition to the amount of salt were investigated and optimized. Under optimal conditions, the concentration factor of detection limit was obtained in the range of 2.1 to 4.4 µg/l and the linear range of 20 to 600 µg/l. Relative standard deviation was obtained to be between 2.5% and 3.1% at the concentration of 30 µg/l trihalomethanes in water. The method was successfully applied to extract and determine trihalomethanes in drinking water in cities of Mazandaran Province.
    Keywords: Trihalomethanes, Drinking Water, Solid-Phase Microextraction, Gas Chromatography, Mass Spectroscopy
  • شیما مسقطی، سید محمد قریشی *
    پژوهش ها نشان می دهد، اسانس دارچین (به ویژه ماده سینامالدهید) می تواند در درمان بیماران مبتلا به دیابت موثر باشد درنتیجه هدف اصلی از انجام این پژوهش، بررسی آزمایشگاهی استخراج فوق بحرانی ترکیب سینامالدهید از پوست گیاه دارچین می باشد. نخست به مقایسه روش های سنتی استخراج اسانس دارچین با روش استخراج فوق بحرانی پرداخته شد سپس ماده موثره اسانس دارچین (سینامالدهید) با استفاده از کربن دی اکسید فوق بحرانی اصلاح شده با مقدارهای ثابتی از متانول (mL1) ، از پوست درخت دارچین استخراج و با روش استخراج با حلال آلی با دستگاه سوکسله مقایسه شدت. استخراج با سیال فوق بحرانی (SFE) با در نظر گرفتن زمان استاتیک 20 دقیقه و اندازه متوسط ذره ها (674/0 میلی متر) انجام شد. چهار متغیر موثر بر این فرایند، دما (°C40 تا80) ، فشار (Mpa30-10) ، شدت جریان کربن دی اکسید (mL/min5/2-5/0) و زمان استخراج دینامیک (120-40 دقیقه) می باشند که آزمایش ها بر اساس آن ها انجام گرفت و تاثیرشان بر میزان بازدهی مورد بررسی قرار گرفت.
    کلید واژگان: استخراج فوق بحرانی, استخراج سوکسله, سینامالدهید, کروماتوگرافی گازی, شرایط عملیاتی
    Shima Masghati, Seyed Mohammad Ghoreishi *
    Research shows that cinnamon essential oil (especially Cinnamaldehyde) can be effective on the treatment of diabetics. So the main purpose of this study was supercritical extraction and experimental investigation of Cinnamaldehyde from cinnamon bark. In this article, a comparison of traditional extraction methods versus the supercritical extraction of cinnamon essential oils was carried out. Then Cinnamaldehyde by using modified supercritical carbon dioxide with a fixed amount of methanol (1ml) was extracted and compared with Soxhlet extraction. Supercritical fluid extraction (SFE) with a static time of 20 minutes and the average particle size (0/674 mm) was used. The effects of variables on the process such as temperature (40- 80 ˚C), pressure (10-30Mpa), carbon dioxide flow rate (1/5 – 2/5 ml/min) and dynamic extraction time (40-120 min) were investigated on yield.
    Keywords: Supercritical extraction, Soxhlet extraction, Cinnamaldehyde, Gas chromatography, Operating conditions
  • Mehrdad Shahpar *, Sharmin Esmaeilpoor
    Water pollution is a major global problem which requires ongoing evaluation and revision of water resource policy at all levels (international down to individual aquifers and wells. It has been suggested that it is the leading worldwide cause of deaths and diseases, and that it accounts for the deaths of more than 14,000 people daily. Genetic algorithm-partial least square (GA-PLS), Kernel partial least square (GA-KPLS) and Levenberg-Marquardt artificial neural network (L-M ANN) techniques were used to investigate the correlation between retention time (RT) and descriptors for 150 organic contaminants in natural water and wastewater which obtained by gas chromatography coupled to high-resolution time-of-flight mass spectrometry (GC-TOF MS). The L-M ANN model gave a significantly better performance than the other models. This indicates that L-M ANN can be used as an alternative modeling tool for quantitative structure–retention relationship (QSRR) studies.
    Keywords: Water Pollution, Hazardous chemicals, Organic pollutants, Gas Chromatography, Time-of-flight mass spectrometry, chemometrics, Levenberg-Marquardt artificial neural network
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