7.3.2: Instrumentation
- Page ID
- 424808
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\(\newcommand{\avec}{\mathbf a}\) \(\newcommand{\bvec}{\mathbf b}\) \(\newcommand{\cvec}{\mathbf c}\) \(\newcommand{\dvec}{\mathbf d}\) \(\newcommand{\dtil}{\widetilde{\mathbf d}}\) \(\newcommand{\evec}{\mathbf e}\) \(\newcommand{\fvec}{\mathbf f}\) \(\newcommand{\nvec}{\mathbf n}\) \(\newcommand{\pvec}{\mathbf p}\) \(\newcommand{\qvec}{\mathbf q}\) \(\newcommand{\svec}{\mathbf s}\) \(\newcommand{\tvec}{\mathbf t}\) \(\newcommand{\uvec}{\mathbf u}\) \(\newcommand{\vvec}{\mathbf v}\) \(\newcommand{\wvec}{\mathbf w}\) \(\newcommand{\xvec}{\mathbf x}\) \(\newcommand{\yvec}{\mathbf y}\) \(\newcommand{\zvec}{\mathbf z}\) \(\newcommand{\rvec}{\mathbf r}\) \(\newcommand{\mvec}{\mathbf m}\) \(\newcommand{\zerovec}{\mathbf 0}\) \(\newcommand{\onevec}{\mathbf 1}\) \(\newcommand{\real}{\mathbb R}\) \(\newcommand{\twovec}[2]{\left[\begin{array}{r}#1 \\ #2 \end{array}\right]}\) \(\newcommand{\ctwovec}[2]{\left[\begin{array}{c}#1 \\ #2 \end{array}\right]}\) \(\newcommand{\threevec}[3]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \end{array}\right]}\) \(\newcommand{\cthreevec}[3]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \end{array}\right]}\) \(\newcommand{\fourvec}[4]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \\ #4 \end{array}\right]}\) \(\newcommand{\cfourvec}[4]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \\ #4 \end{array}\right]}\) \(\newcommand{\fivevec}[5]{\left[\begin{array}{r}#1 \\ #2 \\ #3 \\ #4 \\ #5 \\ \end{array}\right]}\) \(\newcommand{\cfivevec}[5]{\left[\begin{array}{c}#1 \\ #2 \\ #3 \\ #4 \\ #5 \\ \end{array}\right]}\) \(\newcommand{\mattwo}[4]{\left[\begin{array}{rr}#1 \amp #2 \\ #3 \amp #4 \\ \end{array}\right]}\) \(\newcommand{\laspan}[1]{\text{Span}\{#1\}}\) \(\newcommand{\bcal}{\cal B}\) \(\newcommand{\ccal}{\cal C}\) \(\newcommand{\scal}{\cal S}\) \(\newcommand{\wcal}{\cal W}\) \(\newcommand{\ecal}{\cal E}\) \(\newcommand{\coords}[2]{\left\{#1\right\}_{#2}}\) \(\newcommand{\gray}[1]{\color{gray}{#1}}\) \(\newcommand{\lgray}[1]{\color{lightgray}{#1}}\) \(\newcommand{\rank}{\operatorname{rank}}\) \(\newcommand{\row}{\text{Row}}\) \(\newcommand{\col}{\text{Col}}\) \(\renewcommand{\row}{\text{Row}}\) \(\newcommand{\nul}{\text{Nul}}\) \(\newcommand{\var}{\text{Var}}\) \(\newcommand{\corr}{\text{corr}}\) \(\newcommand{\len}[1]{\left|#1\right|}\) \(\newcommand{\bbar}{\overline{\bvec}}\) \(\newcommand{\bhat}{\widehat{\bvec}}\) \(\newcommand{\bperp}{\bvec^\perp}\) \(\newcommand{\xhat}{\widehat{\xvec}}\) \(\newcommand{\vhat}{\widehat{\vvec}}\) \(\newcommand{\uhat}{\widehat{\uvec}}\) \(\newcommand{\what}{\widehat{\wvec}}\) \(\newcommand{\Sighat}{\widehat{\Sigma}}\) \(\newcommand{\lt}{<}\) \(\newcommand{\gt}{>}\) \(\newcommand{\amp}{&}\) \(\definecolor{fillinmathshade}{gray}{0.9}\)APPARATUS: Parr 6755 Solution Calorimeter; Parr 6772 Calorimetric Thermometer; PC computer; lead donut; 100 mL pipet; pipet bulb; Analytical Balance (check uncertainty); and, flask of room temperature DI water.
REAGENTS: KCl(solid); CH3COONa (solid); CH3COONa.3H2O (solid); NaCl (solid).
NOTE: All solid samples (with the exception of CH3COONa.3H2O) should be ground to a fine powder, oven dried and cooled in a desiccator prior to use.
The Parr 6755 Solution Calorimeter
The solution calorimeter consists of a rotating sample cell and an insulated Dewar flask (see Figure 3). The rotating cell holds 20 mL of liquid sample or up to one gram of solid powder sample. Chemical reaction is initiated by pressing the glass push-rod against the bottom of the rotating cell and dropping the reactant in the rotating cell into the Dewar. The rotating cell is stirred vigorously and the reaction proceeds to completion. The rotating cell and push-rod assembly is extremely fragile and should be handled and used with care at all times.
PRECISION: The precision obtainable with the 6755 Solution Calorimeter will be a function of the amount of heat liberated by the reactants and the temperature at which the test is conducted. The best precision will be obtained when working with reactions that release between 200 and 600 calories, producing a temperature rise of 1.5° to 5°C at or near room temperature. Under these conditions a standard deviation of less than 0.4% of the determined value can be obtained in repetitive tests. If the total heat release produces a rise of less than 0.5° or more than 6°C, or if the test is conducted at higher working temperatures with significant heat leak, the relative standard deviation may increase to 1.0% of the determined value.
Specifications For The 6755 Solution Calorimeter | |
---|---|
Working temperature range |
10° to 50°C |
Temperature sensitivity |
0.0002°C |
Energy measurement range |
2 to 1000 calories |
Detectability limit |
0.1 calorie |
Energy equivalent |
100-145 calories/°C |
Maximum volume, solute |
20 mL |
Required volume, solvent |
90 to 120 mL |
Specifications For The 6772 Calorimetric Thermometer | |
---|---|
Range: |
0-70°C |
Resolution: |
0.0001°C |
Absolute accuracy: Without calibration With calibration |
+/- 0.100°C +/- 0.050°C |
Repeatability: Single point |
+/- 0.002°C |
Linearity: 10°C span |
+/- 0.002°C |