ChE 3090-02 2016 Fall

Instrumental Analysis

Instructor: Ying-Ling Liu,

Office: CHE Building Room #404
E-mail: liuyl@mx.nthu.edu.tw

RequiredTextBook
PrinciplesofInstrumentalAnalysis,6thEd.,
byDouglasA.Skoogetal.
ThomsonBrooks/Cole,CA
Grading
Exam #1 (35%), Exam #2 (35%), Laboratory
(25%), Homework + Attendance (5%)
MakeUpExam:
Ifyoumissanexamformedicalreasons,youwillneedadescriptionfroma
doctor inordertotakeamakeup.
Examsmissedforpersonalreasonswillbejudgedbasedupon situations.
Anyoneunabletotakeanexammustmakeeveryefforttocontactme
beforethetest (includingmedicalreasons) throughphoneoremailtobe
consideredforamakeup.
2

Courseintroduction
PartI
Chapter1,6:AnIntroductiontoSpectrometricMethods
Chapter9:AtomicAbsorptionSpectrometry
Chapter12:AtomicXraySpectrometry
Chapter13,14:UltravioletMolecularAbsorptionSpectrometry
Exam#1
PartII
Chapter16,17:InfraredSpectrometry
Chapter19:NuclearMagneticResonanceSpectrometry
Chapter20:MolecularMassSpectroscopy
Chapter26:ChromatographicSeparation;
(TAcomesinforlabarrangement)
Chapter27,28:GasChromatography/LiquidChromatography
Exam#2
PartIII
WetLab

Instrumental analysis for the cases of

Melamine issue
Plasticizer issue
Radiation-polluted food
Heavy metal in water and foods
Water/air quality
Industrial product quality control
Reverse engineering
5

Qualitative analysis
- The measurements to know what
species/analytes the samples contains.
Semi-Quantitative analysis
- The measurements to know the relative
amounts/concentrations of the interested
analytes in the samples.
Quantitative analysis
- The measurements to know the absolute
amounts/concentrations of the interested
analytes in the samples.
6

Selection of instruments
- for measurements
- for purchase
(price, performance, optional equipments,
extending ability, customer service, reputation)

Selection of analytical method

- what accuracy is required?

- How much sample is available?

- What is the concentration range of the analyte?
- What components of the samples might cause
interference?
- What are the physical and chemical properties
of the sample matrix?
- How many samples are to be analyzed?
7
p.1718

Performance characteristics of instruments

- Precision: the precision of analytical

data is the degree of mutual agreement
among data that have been obtained in
the same way. error>>>>
- Bias: providing a measure of the

sytematic, or determinate, error of an

analytical method.
- Sensitivity: the sensitivity of an
instrument or a method is a measure of
its ability to discriminate between small
difference in analyte concentration.
- Detection limit: the minimum
concentration or mass of analyte that can
be detected at a known confident level.
p.1921

Performance characteristics of instruments

- Dynamic range
the range of the instrument
linearly response to the
concentration of the
analyte (5% deviation)
LOQLOL

- Selectivity: referring to the degree to

which the method is free from interference
by other species contained in the sample
matrix.
analyle

p.1921

Performance characteristics of instruments

p.19

10

Performance characteristics of instruments

p.19

11

Othercharacteristicstobeconsidered

p.19

12

Calibrationandstandardizationprocess
Calibration determines the relationship between the
analytical response and the analyte concentration.
An external standard is prepared separately from the
sample.
An internal standard is added to the sample itself.

13

External standard calibration

External standard Calibration

preparationofstandardindifferent
concentrationsofinterestedanalytein
thedynamicrangeoftheinstrument.
Measurementsoftheinstrument
responsetoeachstandard
Makingaplotofinstrumentresponse
tostandardconcentration,gettingthe
calibrationcurveusingtheleastsquare
method
measurementoftheinstrument
responsetotheunknownsamples
Obtainingthesampleconcentration
withthecalibrationcurve

P.12

14

Standard addition method

FIGURE 1-10 Linear calibration plot for the method of standard additions.
The concentration of the unknown solution may be calculated from the slope
m and the intercept b, or it may be determined by extrapolation, as explained
in the text.
15
P.14

The internal-standard method

An internal standard (concentration known) is added to the
samples, blanks, and calibration standards in the analysis.
Calibration involves plotting the ratio of the analyte signal to
the internal-standard signal as a function of the analyte
concentration of the standards. The ratio for the samples is
then used to obtain their analyte concentration from a
calibration curve.
An internal-standard can compensate for several types of both
random and systematic errors.
-The internal-standard should provide a signal that is similar to
the analyte signal in most ways but sufficiently difference so
that the two signals are distinguishable by the instrument.
-The internal-standard must be known to be absent from the
sample matrix.
16