سنتز و کاربرد چارچوب فلز-آلی مغناطیسی عامل¬دارشده با پلی‌ایندول برای استخراج و اندازه¬گیری ترکیب¬های فنلی در نمونه¬های زیست‌محیطی
محورهای موضوعی : شیمی معدنی
محبوبه منوچهری
1
,
صبرعلی نوری
2
1 - دانشیار شیمی معدنی گروه شیمی، واحد تهران‌مرکز، دانشگاه آزاد اسلامی، تهران، ایران.
2 - دانشجوی دکترای شیمی کاربردی گروه شیمی، واحد تهران‌مرکز، دانشگاه آزاد اسلامی، تهران، ایران.
کلید واژه: چارچوب فلز-آلی, نانوجاذب مغناطیسی, پلی ایندول, پیش تغلیظ, نیتروفنول ها,
چکیده مقاله :
در این پژوهش، نانوجاذبی جدید بر پایه چارچوب فلز-آلی مغناطیسی پوشش داده‌شده با پلی‌ایندول سنتز و برای استخراج، پیشتغلیظ و تعیین مقادیر ناچیز نیتروفنلها در نمونههای آب، بهکار برده شد. جاذب سنتزشده با روشهای پراش پرتو ایکس (XRD)، طیف‌سنجی فروسرخ تبدیل فوریه (FTIR)، مغناطیس‌سنجی نمونه ارتعاشی (VSM)، میکروسکوپی الکترونی روبشی (SEM) و میکروسکوپی الکترونی عبوری (TEM) شناسایی شد. تصاویر SEMو TEM نانوساختاربودن جاذب را تایید کردند. الگوی XRD ساختار جاذب را بررسی کرد. نتیجههای VSM نشان دادند که نانوجاذب سنتزشده ویژگی ابرپارامغناطیسی دارد. روش طراحی مختلط مرکزی (CCD) برای شناسایی و بهینهسازی عاملهای موثر بر پیشتغلیظ به‌کارگرفته شد. پس از جذب و شویش، نیتروفنلها با دستگاه سوانگاری مایع با کارایی بالا مجهز به آشکارساز فرابنفش اندازهگیری شدند. pH محلول نمونه، زمان جذب، مقدار جاذب و حجم نمونه در شرایط بهینه بهترتیب برابر با 5/9، 7/3 دقیقه، 5/27 میلیگرم، و 75 میلیلیتر بودند. همچنین در این شرایط، استخراج بدون افزودن نمک به محلول نمونه، زمان واجذب برابر با 3 دقیقه و 200 میکرولیتر کلریدریک اسید 01/0 مولار در استونیتریل بهعنوان حلال شویش، انجام شد. تحت شرایط بهینه حد تشخیصها و گستره خطی منحنی واسنجی بهترتیب در گستره 15/0 تا 25/0 و 300/0 تا 00/5 میکروگرم بر لیتر بهدست آمد. انحراف استاندارد نسبی روش بهعنوان معیاری از دقت در گستره 5/4 تا 4/6 درصد بهدست آمد.
In this research, a new nanoabsorbent was synthesized based on a metal-organic magnetic framework coated with polyindole. This nanoabsorbent was then used for the extraction, pre-concentration, and determination of small amounts of nitrophenols 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 the synthesized 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 parameters that 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 the sample 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
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