Chapter 1

Introduction
What is Analytical Chemistry?
Analytical Chemistry
Divided into two main categories
Classical methods
Instrumental methods
Both can be broken down into three subcategories
Separations
Compound identification
Quantitative analysis
Analytical Chemistry
Analytical Chemistry
Classical Methods Instrumental Methods
Separations
Compound
identification
Quantitative
analysis
What is an instrument?
See Table 1-1 for list of various properties and
instrumental methods
Examples:



What is an instrument?

What is an Instrument? (cont.)
Instrument Components
Energy source
Information sorter
Input transducer
Signal processor/readout

Example: gas chromatograph with FID
Flame column electrodes
digitizer/computer
Figures of Merit
When selecting methods must consider

Figures of Merit
Precision absolute std dev, relative std dev
Bias accuracy
Sensitivity slope of calibration curve
Detection limit minimum conc @ known confid.
Conc range linear dynamic range (LDR)
Selectivity how free of interferences
Figures of Merit (cont.)
Standard deviation



LDR

Std dev
x
i
x

2

N 1

RSD
s
x
Concentration
I
n
s
t
r
u
m
e
n
t

R
e
s
p
.

Figures of Merit (cont.)
Detection limits
Minimum concentration or mass of analyte that can be
detected at a known confidence level
Determined in different ways depending on analytical
method
Spectroscopy
Analyze blank 10 times and determine concentration for
each analysis
Detection limit = 3 x std dev of blank
Chromatography
Analyze lower and lower concentration solutions until find
one that has peak height three times that of noise
Calibration
Calibration of Methods
Relates instrument signal to analyte concentration
External Calibration curve y = mx + b
Make solutions of known concentration
Analyze with instrument
Plot concentration vs instrument response
Get equation of line using computer
Use equation to find concentration of unknowns
Standard additions
Add known amounts of analyte to separate samples
Analyze with instrument
Calibration (cont.)
Standard additions (cont.)
Plot amount added (or concentration added ) vs instrument
response
X-intercept is concentration in unknown
c
x
= unknown conc. = (bc
s
)/(mV
x
)
c
s
is conc in spike soln and V
x
is volume unknown
Internal standards calibration curve
Add same amount of additional species to all samples and
standards (called internal standard)
Analyze samples and standards for analyte and internal
standard
Plot ratio of std conc/IS conc vs ratio of std signal/IS signal
Corrects for matrix effects and changes in sample volume