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   سنتز و کاربرد چارچوب فلز-آلی مغناطیسی عامل دارشده با ‏پلی‌ایندول برای استخراج و اندازه گیری ترکیب های فنلی در ‏نمونه های زیست‌محیطی ‏  
   
نویسنده منوچهری محبوبه ,نوری صبرعلی
منبع پژوهش هاي كاربردي در شيمي (jarc) - 1403 - دوره : 18 - شماره : 2 - صفحه:71 -85
چکیده    در اﻳﻦ ﭘﮋوﻫﺶ، ﻧﺎﻧﻮﺟﺎذﺑﻲ ﺟﺪﻳﺪ ﺑﺮ ﭘﺎﻳﻪ ﭼﺎرﭼﻮب ﻓﻠﺰ-آﻟﻲ ﻣﻐﻨﺎﻃﻴﺴﻲ ﭘﻮﺷﺶ داده ﺷﺪه ﺑﺎ ﭘﻠﻲ اﻳﻨﺪول ﺳﻨﺘﺰ و ﺑﺮای اﺳﺘﺨﺮاج، ﭘﻴﺶﺗﻐﻠﻴﻆ و ﺗﻌﻴﻴﻦ ﻣﻘﺎدﻳﺮ ﻧﺎﭼﻴﺰ ﻧﻴﺘﺮوﻓﻨﻞﻫﺎ در ﻧﻤﻮﻧﻪﻫﺎی آب، ﺑﻪﻛﺎر ﺑﺮده ﺷﺪ. ﺟﺎذب ﺳﻨﺘﺰﺷﺪه ﺑﺎ روش ﻫﺎی ﭘﺮاش ﭘﺮﺗﻮ اﻳﻜﺲ )xrd(، ﻃﻴﻒ ﺳﻨﺠﻲ ﻓﺮوﺳﺮخ ﺗﺒﺪﻳﻞ ﻓﻮرﻳﻪ )ftir(، ﻣﻐﻨﺎﻃﻴﺲ ﺳﻨﺠﻲ ﻧﻤﻮﻧﻪ ارﺗﻌﺎﺷﻲ )vsm(، ﻣﻴﻜﺮوﺳﻜﻮﭘﻲ اﻟﻜﺘﺮوﻧﻲ روﺑﺸﻲ )sem( و ﻣﻴﻜﺮوﺳﻜﻮﭘﻲ اﻟﻜﺘﺮوﻧﻲ ﻋﺒﻮری )tem( ﺷﻨﺎﺳﺎﻳﻲ ﺷﺪ. ﺗﺼﺎوﻳﺮ sem و tem ﻧﺎﻧﻮﺳﺎﺧﺘﺎرﺑﻮدن ﺟﺎذب را ﺗﺎﻳﻴﺪ ﻛﺮدﻧﺪ. اﻟﮕﻮی xrd ﺳﺎﺧﺘﺎر ﺟﺎذب را ﺑﺮرﺳﻲ ﻛﺮد. ﻧﺘﻴﺠﻪﻫﺎی vsm ﻧﺸﺎن دادﻧﺪ ﻛﻪ ﻧﺎﻧﻮﺟﺎذب ﺳﻨﺘﺰﺷﺪه وﻳﮋﮔﻲ اﺑﺮﭘﺎراﻣﻐﻨﺎﻃﻴﺴﻲ دارد. روش ﻃﺮاﺣﻲ ﻣﺨﺘﻠﻂ ﻣﺮﻛﺰی )ccd( ﺑﺮای ﺷﻨﺎﺳﺎﻳﻲ و ﺑﻬﻴﻨﻪﺳﺎزی ﻋﺎﻣﻞﻫﺎی ﻣﻮﺛﺮ ﺑﺮ ﭘﻴﺶ ﺗﻐﻠﻴﻆ ﺑﻪ ﻛﺎرﮔﺮﻓﺘﻪ ﺷﺪ. ﭘﺲ از ﺟﺬب و ﺷﻮﻳﺶ، ﻧﻴﺘﺮوﻓﻨﻞﻫﺎ ﺑﺎ دﺳﺘﮕﺎه ﺳﻮاﻧﮕﺎری ﻣﺎﻳﻊ ﺑﺎ ﻛﺎراﻳﻲ ﺑﺎﻻ ﻣﺠﻬﺰ ﺑﻪ آﺷﻜﺎرﺳﺎز ﻓﺮاﺑﻨﻔﺶ اﻧﺪازهﮔﻴﺮی ﺷﺪﻧﺪ. ph ﻣﺤﻠﻮل ﻧﻤﻮﻧﻪ، زﻣﺎن ﺟﺬب، ﻣﻘﺪار ﺟﺎذب و ﺣﺠﻢ ﻧﻤﻮﻧﻪ در ﺷﺮاﻳﻂ ﺑﻬﻴﻨﻪ ﺑﻪ ﺗﺮﺗﻴﺐ ﺑﺮاﺑﺮ ﺑﺎ 9/5، 3/7 دﻗﻴﻘﻪ، 27/5 میلی گرم، و 75 ﻣﻴﻠﻲﻟﻴﺘﺮ ﺑﻮدﻧﺪ. . ﻫﻤﭽﻨﻴﻦ در اﻳﻦ ﺷﺮاﻳﻂ ﻧﻤﻚ ﺑﻪ ﻣﺤﻠﻮل ﻧﻤﻮﻧﻪ، زﻣﺎن واﺟﺬب ﺑﺮاﺑﺮ ﺑﺎ 3 دﻗﻴﻘﻪ و 200 ﻣﻴﻜﺮوﻟﻴﺘﺮ ﻛﻠﺮﻳﺪرﻳﻚ اﺳﻴﺪ 0/01 0 ﻣﻮﻻر در اﺳﺘﻮﻧﻴﺘﺮﻳﻞ ﺑﻪ ﻋﻨﻮان ﺣﻼل ﺷﻮﻳﺶ، اﻧﺠﺎم ﺷﺪ. ﺗﺤﺖ ﺷﺮاﻳﻂ ﺑﻬﻴﻨﻪ ﺣﺪ ﺗﺸﺨﻴﺺﻫﺎ و ﮔﺴﺘﺮه ﺧﻄﻲ ﻣﻨﺤﻨﻲ واﺳﻨﺠﻲ ﺑﻪﺗﺮﺗﻴﺐ در ﮔﺴﺘﺮه 0/15 تا 0/25 و 0/300 تا 5/00 ﻣﻴﻜﺮوﮔﺮم ﺑﺮ ﻟﻴﺘﺮ ﺑﻪدﺳﺖ آﻣﺪ. اﻧﺤﺮاف اﺳﺘﺎﻧﺪارد ﻧﺴﺒﻲ روش ﺑﻪﻋﻨﻮان ﻣﻌﻴﺎری از دﻗﺖ در ﮔﺴﺘﺮه 4/5 تا 6/4 درصد به دست آمد.
کلیدواژه چارچوب فلز-آلی ,نانوجاذب مغناطیسی ,پلی ایندول ,پیش تغلیظ ,نیتروفنول ها
آدرس دانشگاه آزاد اسلامی واحد تهران ‌مرکز, گروه شیمی, ایران, دانشگاه آزاد ‏اسلامی واحد تهران ‌مرکز, گروه شیمی, ایران
پست الکترونیکی sand1385@gmail.com
 
   synthesis and application of metal-organic framework functionalized with poly‏)‏indole‏(‏‎ to ‎extract and measure phenolic compounds in environmental samples  
   
Authors manoochehri mahboobeh ,nouri sabrali
Abstract    in this research, a new nanoabsorbent was synthesized based on a metalorganic magnetic framework coated with polyindole. this nanoabsorbent was then used for the extraction, pre-concentration, and determination of small amounts ofnitrophenols in water samples. first, the synthesized adsorbent was identified using various methods including x-ray diffraction (xrd), fourie transform infrared spectroscopy (ftir), vibrating sample magnetometry (vsm), scanning electron microscopy (sem), and transmission electron microscopy (tem). the sem and tem images confirmed the nanostructure of the adsorbent, while the xrd pattern checked and confirmed its phase structure. additionally, the vsm results showed that thesynthesized nanoabsorbent has superparamagnetic properties. finally, all of these methods confirmed the successful synthesis of the nanoabsorbent. the central composite design (ccd) method was employed to identify and optimize the parametersthat affect pre-concentration. after adsorption and washing, nitrophenols were measured using a high-performance liquid chromatography device equipped with an ultraviolet detector. the optimal extraction conditions were as follows: ph of thesample solution, 9.5; absorption time, 3.7 minutes; amount of absorbent, 27.5 mg; sample volume, 75 ml; washing solvent, 200 μl of 0.01 m hydrochloric acid in acetonitrile; desorption time, 3 minutes without adding salt to the sample solution.under these optimal conditions, the limit of detection and the linear range of the calibration curve were obtained in the range of 0.15-0.25 and 5.0-300 μg/liter, respectively. the relative standard deviation of the method, as a measure of accuracy,was obtained in the range of 4.5-4.6%. finally, the desired adsorbent was used for rapid extraction and pre-concentration of nitrophenols in water samples.
Keywords metal-organic framework; magnetic nanosorbent ,polyindole ,preconcentration ,extraction ,measurement of nitrophenols
 
 

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