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Determination of Mn in Steel (Standard Addition)
Sample Calculations of Determination of Mn in Steel (Standard Addition) Vikram Sharma
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Initial Values Find the mass of your steel for each trial, in this calculation it will be .5091g, in a mL flask Mn Standard concentration (Cs) = mg/mL Absorbance data Absorbance Blank 0.031 Sample 0.198 Sample+5mL 0.631 Sample+10mL 1.082
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Why are we using the standard addition calculation?
We have to use the standard addition calculation because we have to take into account the matrix effect Matrix effect- the change in the analytical signal (absorbance in this case) because of all the stuff other than the analyte (Mn) in the solution.
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Part I, 2 equation 2 unknowns
Use aliquots 2 and 3 1.082 Sample+10mL 0.631 Sample+5mL 0.198 Sample 0.031 Blank Absorbance Remember to subtract your blank!!!
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Defining Variables Ax,T=Corrected Absorbance of aliquot 2 = .167
Ax+s,T=Corrected Absorbance of aliquot 3 = .600 Vs=Volume Standard mg/mL Mn= L Vx=Volume Unknown with conc. Cx = L Cx= Concentration Mn in sample
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The Numbers… Cx = [.167/(.600-.167)]* [(.00500L*.1025mg/mL)/.02000L]
Cx= mg/mL Cx*100mL=.988mg .988mg/1000mg/g= g Mn gMn/.5091gSample*100%= .194%
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Part II, Graphical Procedure
The X axis equation Xn=[S]i*(Vs/Vo) Where [S]i= Original Conc. Std Mn (.1025 mg/mL) Vs = Volume standard (0, 5, 10 mL) Vo = Volume unknown (20 mL)
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Graphical Procedure The Y axis equation Yn=IS+X*(V/Vo) Where:
IS+X= Absorbance value V = Total volume (50 mL) Vo = Volume unknown (20 mL)
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Graphical analysis X values Y Values Sample 0.4175 Sample+5mL 0.025625
0.4175 Sample+5mL 1.5 Sample+10mL 2.6275
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Find the conc. of unknown, [X]f
[X]f is the magnitude of the X-intercept value Therefore Y=0, so find X in the calculated equation from the least squares line: y=43.1[X]f+.410 0=43.1[X]f+.410 -.410/43.1= [X]f [X]f =| |=.00951mg/mL
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Finding %(wt/wt) [X]f *100mL=.951mg .951mg/1000mg/g=.000951g Mn
gMn/.5091gSample*100%= .187% Compare .194% to .187%
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Question In the graphing procedure, is the x intercept supposed to be positive or negative? Negative. If it’s positive, you screwed up.
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