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Лаба №14

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File 14/lab-14.tex

+\documentclass[a4paper,10pt]{article}
+\usepackage[left=2cm,right=2cm,top=2cm,bottom=2cm,bindingoffset=0cm]{geometry}
+\usepackage[utf8]{inputenc}
+\usepackage[T2A]{fontenc}
+\usepackage[ukrainian]{babel}
+\usepackage{indentfirst,mathenv,amsmath,array}
+\usepackage[pdftex]{graphicx}
+\graphicspath{{images/}}
+\usepackage[pdftex,unicode,colorlinks]{hyperref}
+\hypersetup{
+    pdftitle={Лабораторна робота №14},
+    pdfauthor={Ульяницький Олександр}
+}
+\title{\emph{Лабораторна робота №14}\\Флуориметричне визначення Цирконію морином}
+\author{Ульяницький Олександр}
+
+\begin{document}
+\maketitle
+\section*{Теоретичні відоиості}
+Для визначення Цирконію використовують природні барвники,
+зокрема оксипохідні флавону. З них найбільше застосування знайшов
+морин (3,5,7,2',4'-пентаоксифлавон) (рис. \ref{fig:morin}), що утворює із цирконієм у
+сильнокислих розчинах комплексну сполуку, яка характеризується
+яскраво-зеленою флуоресценцією з $\lambda_\mathrm{max}=520$ нм.
+
+У 2~М розчині НСl максимальна інтенсивність флуоресценції
+комплексу досягається через 10 - 15 хв. після введення морину в
+аналізований розчин і не змінюється протягом 1 год. Визначенню
+цирконію не заважають 100-кратні кількості Cd, As(III), Bi(IІІ), Сг(ІІІ),
+Fе(ІІ,ІІІ), Со, Ni, Cu, Mg, Zn, Ag. Заважають визначенню цирконію Al, Ge,
+Sb, Sc, Th, U. У їх присутності цирконій визначають, вимірюючи
+інтенсивність флуоресценції досліджуваного розчину до та після
+додавання трилону Б. В останньому випадку флуоресценція комплексу
+цирконію з морином зникає, а флуоресценція комплексів заважаючих
+елементів, які не утворюють у сильнокислих розчинах комплексонатів,
+зберігається. Такий розчин використовують як ``холостий'' дослід. У
+такому випадку градуювальник графік будують в координатах $\Delta І,~\textrm{відн.од.} = f(C),~\textrm{мг/л}$.
+Межа виявлення цирконію дорівнює 1,0 мкг/л.
+\begin{figure}[htp!]
+ \centering
+ \includegraphics[height=2.4cm]{morin.png}
+ % morin.png: 324x200 pixel, 96dpi, 8.57x5.29 cm, bb=0 0 243 150
+ \caption{Структурна формула морину}
+ \label{fig:morin}
+\end{figure}
+
+\section*{Мета роботи}
+Ознайомитись із можливостями флуоресцентних
+методів, що базуються на першому правилі Стевенса.
+\section*{Розчини}
+\begin{enumerate}
+    \item Стандартний розчин ZrOCl$_2$ із вмістом цирконію 1 мкг/мл.
+    \item Морин, 0,04\%-ний розчин в ацетоні.
+    \item Хлороводнева кислота, 2 моль/л розчин.
+\end{enumerate}
+\section*{Посуд}
+\begin{enumerate}
+    \item Мірні колби ємністю 25,0 мл (10 шт.) та 50,0 мл (1 шт.).
+    \item Піпетки з поділками ємністю 1,00, 2,00, 5,00 мл та 10,00 мл.
+    \item Кювети прямокутні скляні з $l=1,0$ (2 шт.).
+\end{enumerate}
+\section*{Обладнання}
+\begin{enumerate}
+    \item спектрофлуорометр ``UNICO LS55''
+\end{enumerate}
+\section*{Порядок виконання роботи}
+Для побудови градуювального графіка в
+п'ять мірних колб вводять по 0,50; 1,00; 1,50; 2,00 й 2,50 мл стандартного
+розчину Цирконію, по 10,00 мл кислоти, 1,00 мл розчину морину і доводять
+до мітки хлороводневою кислотою. Інтенсивність флуоресценції отриманих
+розчинів вимірюють через 15 хв. Результати вимірювань заносять до табл. \ref{tab:GG}
+\begin{figure}[htp!]
+ \centering
+ \includegraphics{excitation_spectrum.pdf}
+ % exitation_spectrum.pdf: 442x308 pixel, 72dpi, 15.59x10.87 cm, bb=0 0 442 308
+ \caption{Спектр збудження морину.}
+ \label{fig:excitation}
+\end{figure}
+\begin{figure}[htp!]
+ \centering
+ \includegraphics{emission_spectrum.pdf}
+ % emission_spectrum.pdf: 448x310 pixel, 72dpi, 15.80x10.94 cm, bb=0 0 448 310
+ \caption{Спектр флуорисценції морину при $\lambda_\textrm{збудж.}=420$ нм.}
+ \label{fig:emission}
+\end{figure}
+
+Із застосуванням програми Origin (версія 5.0 і вище) будують
+градуювальний графік в координатах І, відн. од. --- концентрація Zr, мг/л (рис. \ref{fig:GG}).
+Лінеаризують отриману залежність (з використанням наступних опцій у
+зазначеній програмі: Analysis: Fit Polinomial: Order=1), отримують рівняння
+ГГ вигляду \eqref{eq:lin}:
+\begin{equation}
+\label{eq:lin}
+    І = (a \pm \Delta a)+(b \pm \Delta b) \cdot C_\mathrm{Zr},~\textrm{мг/л},~(R^2=\dots),
+\end{equation}
+де $\Delta a$ та $\Delta b$ – похибки розрахунку вільного члена та тангенса кута нахилу прямої відповідно.
+\begin{table}[htp!]
+\centering
+\caption{Дані для побудування градуювального графіка для визначення Цирконію морином. $\lambda_\textrm{збудж.}=420$ нм, $\lambda_\textrm{флуор.}=510$ нм, $l=1,0$ см.}
+\label{tab:GG}
+\begin{tabular}{|c|c|c|}
+\hline
+    $V$, мл & $C_{Zr}$, мкг/мл & $I$ \\
+\hline
+    1,0 & 0,04 & 127,810\\
+    1,5 & 0,06 & 198,816\\
+    2,0 & 0,08 & 233,615\\
+    2,5 & 0,10 & 316,194\\
+    4,0 & 0,16 & 507,128\\
+    6,0 & 0,24 & 755,089\\
+\hline
+\end{tabular}
+\end{table}
+\begin{figure}[htp!]
+ \centering
+ \includegraphics{GG.pdf}
+ % GG.pdf: 449x310 pixel, 72dpi, 15.84x10.94 cm, bb=0 0 449 310
+ \caption{Градуювальний графік для визначення Цирконію морином. $\lambda_\textrm{збудж.}=420$ нм, $\lambda_\textrm{флуор.}=510$ нм, $l=1,0$ см.}
+ \label{fig:GG}
+\end{figure}
+
+Рівняння градуювального графіку для визначення Цирконію морином:
+\begin{equation}
+\label{eq:GG}
+    I = (-4,405 \cdot 10^{-1} \pm 8,397) + (3,149 \cdot 10^{3} \pm 6,353 \cdot 10^{1}) \cdot C_\mathrm{Zr},~\textrm{мкг/мл},~(R^2=0,9984),
+\end{equation}
+
+\section*{Визначення цирконію в задачі}
+Задачу отримують в мірній колбі ємністю 25,0 мл.
+Розбавляють хлороводневої кислотою до риски та ретельно
+перемішують. Відбирають аліквотні частини розчину (по 5,00 мл) в чотири
+мірні колби, додають всі реактиви, як при побудові градуювального
+графіка, і через 15 хв. вимірюють інтенсивність флуоресценції розчинів. За
+рівнянням ГГ розраховують концентрацію цирконію в розчинах ($C_i$, мг/л),
+перераховують на вміст його в розчині задачі ($m_i$, мг) за формулою \eqref{eq:mass}:
+\begin{equation}
+\label{eq:mass}
+m_i,~\textrm{мг} = \frac{C_i \cdot 0,025 \cdot V_\textrm{зад}}{V_\textrm{ал}}
+\end{equation}
+де $V_\textrm{зад}$ -- об'єм розчину задачі, мл (25,0 мл), $V_\textrm{ал}$---об'єм алiквотної частини (5,00 мл), а результати заношу до таблиці \ref{tab:probe}.
+\begin{table}[!htp]
+\centering
+\caption{Результати визначення Силіцію в задачi. $\lambda = 400$ нм, $l=5,0$}
+\label{tab:probe}
+\begin{tabular}{|c|c|c|}
+    \hline
+    $I$ & $C_{\mathrm{Zr}}$, мкг/мл & $m_\mathrm{Si}$, мг \\
+    \hline
+    358,607 & 0,114 & 0,0143\\
+    351,138 & 0,112 & 0,0140\\
+    \hline
+\end{tabular}
+\end{table}
+Отримані дані обробляють, як зазначено в розділі Статистична обробка
+результатів визначення (табл. \ref{tab:stat}). Результати отримують у формі:
+$m(\mathrm{Zr}),~\textrm{мг} = \bar m \pm \Delta m$.
+\begin{table}[htp!]
+\centering
+\caption{Статистична обробка результатів визначення Цирконію  морином. $n = 2; P = 0,95; t_{P=0,95, n=2} = 12,706; \varepsilon = 9,52\%$}
+\label{tab:stat}
+\begin{tabular}{|c|c|c|c|c|c|c|}
+    \hline
+    $m(\mathrm{Zr})$, мг & $S_{m(\mathrm{Zr})}$ & $S_{r}$ & $S^2$ & $S$ & $\Delta m(\mathrm{Zr})$, мг & $\bar{m}(\mathrm{Zr})$, мг\\
+    \hline
+    $1,40 \cdot 10^{-2}$ & $1,06 \cdot 10^{-4}$ & $1,06 \cdot 10^{-2}$ & $2,25 \cdot 10^{-8}$ & $1,50 \cdot 10^{-04}$ & $1,35 \cdot 10^{-3}$ & $1,42 \cdot 10^{-2}$\\
+    $1,43 \cdot 10^{-2}$ & & & & & &\\
+    \hline
+\end{tabular}
+\end{table}
+\section*{Висновки}
+На лабораторній роботі було визначено Цирконій моином методом люмінесцентної спектрометрії.
+Маса Циркониію в задачі становить:
+\begin{displaymath}
+  m_\mathrm{Zr}~\textrm{мг} = 1,42 \cdot 10^{-2} \pm 1,35 \cdot 10^{-3}
+\end{displaymath}
+
+\end{document}
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