تهیه نانوسلولز اصلاح شده با 5-Br-PADAP جهت پیش تغلیظ و اندازه گیری مقادیر ناچیز یون های کبالت در نمونه آب های طبیعی

محورهای موضوعی : فلزات سنگین

سکینه گنجی جویباری ¹ , علی میرابی ² , علی شکوهی راد ³

1 - دانشجوی کارشناسی ارشد، دانشگاه آزاد اسلامی، واحد قائم شهر، گروه شیمی، قائم شهر، ایران.
2 - دانشیار شیمی تجزیه، دانشگاه آزاد اسلامی، واحد قائم شهر، گروه شیمی، قائم شهر، ایران.* (مسوول مکاتبات).
3 - دانشیار مهندسی شیمی، دانشگاه آزاد اسلامی، واحد قائم شهر، گروه مهندسی شیمی، قائم شهر، ایران.

تاریخ دریافت : 1396/11/14 تاریخ پذیرش : 1397/06/14 تاریخ انتشار : 1400/07/01

کلید واژه: استخراج, پیش تغلیظ, اندازه گیری کبالت, نانو سلولز,

چکیده مقاله :

زمینه و هدف: جداسازی و اندازه گیری مقادیر ناچیز یون های کبالت در نمونه های حقیقی به جهت سمیت آن، برای انسان اهمیت زیادی دارد که در تحقیق حاضر از نانو سلولز اصلاح شده به عنوان جاذب استفاده شده است. نانو سلولز به روش هیدرولیز اسیدی سنتز و با 2- ( 5- برمو -2- پیریدیل آزو ) 5- ( دی اتیل آمینو ) فنل) Br-PADAP 5-) اصلاح شد. به کمک میکروسکوپ الکترونی عبوری (TEM) اندازه نانو فیبرهای سلولزی تعیین شد. بعد از اصلاح نانو جاذب با PADAP 5-Br-، از نانوکامپوزیت اصلاح شده آنالیز وزن سنجی حرارتی (TGA) صورت گرفت و همچنین برای تعیین مقدار سطح قبل و بعد از اصلاح جاذب از تکنیک BET استفاده شد. در کار حاضر هدف اصلاح سطح نانو سلولز با لیگاند 5-Br-PADAP جهت استفاده از آنها برای استخراج و پیش تغلیظ مقادیر ناچیز یون های کبالت قبل از اندازه گیری آن توسط طیف سنجی جذب اتمی شعله ای در نمونه های حقیقی می باشد.روش بررسی: حجم معینی از یون کبالت را داخل لوله آزمایش حاوی نانو جاذب اصلاح شده ریخته و به آن محلول بافر با 9pH= اضافه کرده و به مدت 15 دقیقه درون شیکر و سپس سانتریفیوژ قرار داده و در مرحله بعد محلول رویی را دور ریخته و 1 میلی لیتر HCl جهت بازیابی یون کبالت افزوده و 10دقیقه داخل شیکر و سپس سانتریفیوژ قرار داده و جذب محلول رویی توسط دستگاه جذب اتمی شعله ای خوانده شد.نتایج به دست آمده نشان می دهد که نانو سلولز اصلاح شده، برای اندازه گیری یون کبالت در غلظت های پایین بسیار حساس و گزینش پذیر عمل می کند و تحت تاثیر پارامتر های مختلفی مانند pH، مقدارجاذب، زمان استخراج و نوع حلال شوینده قرار می گیرد.یافته ها: منحنی کالیبراسیون در گستره 500-10 نانو گرم بر میلی لیتر خطی بود و حد تشخیص روش 3/4 نانوگرم بر میلی لیتر و انحراف استاندارد نسبی (RSD) روش 8/1 % به دست آمد. همچنین دارای فاکتور پیش تغلیظ و غنی سازی بالا می باشد.بحث ونتیجه گیری: روش پیشنهادی جهت اندازه گیری مقادیر ناچیز یون های کبالت با روش افزایش استاندارد در نمونه آب های طبیعی نظیر آب دریا، رودخانه، آب چاه ، آبندان و آب شهری توسط دستگاه طیف سنجی جذب اتمی با نتایج رضایت بخش مورد استفاده قرار گرفت.

چکیده انگلیسی:

Background and Objective: Separation and determination of trace amounts of cobalt ions in real samples due to their toxicity to humans is very important. In the present study, a nanocellulose was synthesized by the acid hydrolysis and then modified with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol (5-Br-PADAP). The size of cellulose nanofibers was determined using transmission electron microscope (TEM). After modification of the nano-sorbent with the 5-Br-PADAP, the thermogravimetric analysis (TGA) of the modified nanocomposite was carried out, and the BET technique was used to determine the surface area of the nano-sorbent before and after modification. In the present work, the aim is to modify the surface of nanocellulose with ligand of 5-Br-PADAP to use them to extraction and pre-concentration of trace amounts of cobalt ions before determination it by flame atomic absorption spectroscopy in real samples.Material and Methodology: Certain volume of cobalt ion into the test tube containing the modified nanosorbent was Poured and buffer solution with pH = 9 was added and place it in a shaker and finally centrifuged for 15 minutes and then discard the top solution and 1 mL HCl was added to recover cobalt ions and placed in a shaker for 10 minutes and then centrifuged, and the absorption of the supernatant was determined by FAAS. The results showed that the modified nanocellulose is very sensitive and selective towards the determination of cobalt ions which could be affected by several parameters such as pH, adsorbent amount, sample volume, extraction time, and type of eluetion.Findings: The calibration curve is linear in the range of 10-500 ng/mL, and the detection limit and the relative standard deviation (RSD) are calculated to be 4.3 ng/mL and 1.8 %, respectively, that result in a high preconcentration and enrichment factor.Discussion and Conclusions: By using the flame atomic absorption spectrometry and applying the standard addition method, the proposed method was used to determination of the trace amounts of cobalt ions in the natural water samples such as seawater, river water, well water, lake water and tap water, with satisfactory results.

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