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5-Introduction - Part 2

This document provides an overview of quantitative methods of chemical analysis. It discusses different types of analysis based on (1) the type of final measurement including gravimetric, volumetric/titrimetric, and instrumental analysis, (2) the calculation method including absolute and relative methods, (3) the sample size, (4) the number of constituents determined, (5) concentration of the analyte, and (6) nature of the analyte. It also provides examples of calculations for determining the percentage of magnesium in a sample and percentage of sodium benzoate in catsup. Finally, it outlines the typical steps in a chemical analysis including defining the problem, selecting a method, obtaining and preparing samples, performing separations,

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557 views

5-Introduction - Part 2

This document provides an overview of quantitative methods of chemical analysis. It discusses different types of analysis based on (1) the type of final measurement including gravimetric, volumetric/titrimetric, and instrumental analysis, (2) the calculation method including absolute and relative methods, (3) the sample size, (4) the number of constituents determined, (5) concentration of the analyte, and (6) nature of the analyte. It also provides examples of calculations for determining the percentage of magnesium in a sample and percentage of sodium benzoate in catsup. Finally, it outlines the typical steps in a chemical analysis including defining the problem, selecting a method, obtaining and preparing samples, performing separations,

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nids
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© © All Rights Reserved
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Classification of Quantitative

Methods of Analysis
A. Type of Final Measurement

1. Gravimetric Analysis - usually involves the selective


separation of the analyte by precipitation, followed by the
very nonselective measurement of mass (of the
precipitate)

2. Volumetric or Titrimetric Analysis - the analyte


reacts with a measured volume of reagent of known
concentration ; a change in some physical or chemical
property signals the completion of the reaction ; more
rapid than gravimetric analysis
3. Instrumental Analysis - based on the measurement
of a physical property (e.g. an electrical property or the
absorption of electromagnetic radiation) ; generally
more sensitive and selective than the classical techniques
but less precise ; usually much more expensive, capital
wise ; usually more rapid, may be automated and may be
capable of measuring more than one analyte at a time ;
some perform the separation and measurement step
simultaneously
B. Calculation of Amount of Analyte

1. Absolute Methods - rely upon accurately known


fundamental constants for calculating the amount of
analyte ( e.g. atomic weights )

2. Relative Methods - require comparison against some


solution of known concentration or signal due to some
property of the solution
C. Size of the Sample
Method Sample Weight (mg) Sample Volume (uL)

Meso greater than 100 greater than 100


Semi-micro 10 - 100 50 - 100
Micro 1 - 10 less than 50
Ultra-micro less than 1
N.B.
Micro and Ultra-micro are often classified as TRACE
ANALYSIS.
Special handling techniques and microbalances for weighing
are required for micro and ultra-micro operations.
D. Number of Constituents 1. Complete Analysis
Determined 2. Partial Analysis
E. Concentration of Analyte 1. Major Analysis - greater than
1%
2. Minor Analysis - 0.1% to 1%
3. Trace Analysis - less than
0.1%
4. Ultra-trace Analysis - a few
ppm or less
F. Nature of Analyte 1. Elemental Analysis

2. Molecular Analysis
Exercise 3

A 0.7406-g sample of impure magnesite, MgCO3, was


decomposed with HCl; the liberated CO2 was collected on
absorbent and found to weigh 0.1881-g. Calculate the percentage
of magnesium in the sample.
Molar Masses : MgCO3 = 84.32 Mg = 24.312 CO2 = 44.01

The benzoic acid extracted from 106.3-g of catsup required a


14.76-mL titration with 0.0514-M NaOH. Express the results of
this analysis in terms of percent sodium benzoate.
Molar Masses:
HC7H5O2 = 122.12 NaOH = 40.00 NaC7H5O2 = 144.10

Answers: 14.03% -Mg 0.103% -NaC7H5O2


Steps in Chemical Analysis
1. Define the Problem Factors
What is the problem what needs to be
found? Qualitative and/or
quantitative?
What will the information be used for?
Who will use it?
When will it be needed?
How accurate and precise does it have
to be?
What is the budget?
The analyst should consult with the
client to plan useful and efficient
analysis, including how to obtain a
useful sample.
Steps in Chemical Analysis
2. Select a Method Factors
Sample type
Size of sample
Sample preparation needed
Concentration and range (sensitivity
needed)
Selectivity needed (interferences)
Accuracy/precision needed
Tools/instruments available
Expertise/experience
Cost
Speed
Does it need to be automated?
Are methods available in the chemical
literature?
Are standard methods available?
Steps in Chemical Analysis
3. Obtain a Representative Factors
Sample Sample type/homogeneity/size
Sampling statistics/errors
4. Prepare the Sample for Factors
Analysis Solid, liquid or gas?
Dissolve?
Ash or digest?
Chemical separation or masking of
interferences needed?
Need to concentrate the analyte?
Need to change (derivatize) the analyte for
detection?
Need to adjust solution conditions (pH, add
reagents)?
Steps in Chemical Analysis
5. Perform Any Necessary Distillation
Chemical Separation Precipitation
Solvent extraction
Solid phase extraction
Chromatography (may be done as part of
the measurement step)
Electrophoresis (may be done as part of
the measurement step)

6. Perform the Factors


Measurement Calibration
Validation/controls/ blanks
Replicates
7. Calculate the Results Statistical analysis (reliability)
and Report Report results with limitations/accuracy
information
Analysis of Butter

A 500.0-mg sample of butter was warmed and shaken


vigorously with water. The undissolved material was
removed by filtering and the aqueous portion was made 1.0
M in HNO3 and 0.025 M in Fe(NO3)3. This acidified
solution was treated with 10.00-mL of 0.1755-M AgNO 3 to
precipitate the chloride ion and after the addition of a small
amount of nitrobenzene, 14.22-mL of 0.1006-M KSCN was
required to back titrate the excess Ag+. Calculate the
percent NaCl in the butter.
Molar Masses : NaCl = 58.45 AgNO3 = 169.87 KSCN = 97.18
Answers: 3.793% -NaCl

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