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1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
1.- Introduction
CH3
that selectively precipitates Ni2+ and Pd2+, led to an improved analytical
method for the quantitative analysis of nickel.4 The resulting analysis, as
Analytical Chemistry II HO
N
N
OH
shown in Figure 1.2, requires fewer manipulations and less time after com-
pleting the sample’s dissolution. By the 1970s, flame atomic absorption
CH3 spectrometry replaced gravimetry as the standard method for analyzing
Chapter 1 Introduction to Analytical Chemistry 3
dimethylglyoxime nickel in ores,5 resulting in an even more rapid analysis. Today, the standard
analytical method utilizes an inductively coupled plasma optical emission
Original Sample Start spectrometer.
Solids 1:3 H2SO4/HNO3, 100°C for 8-10 hrs
dilute w/H2O, digest for 2-4 hr A more appropriate description of analytical chemistry is “the science
Solutions of inventing and applying the concepts, principles, and…strategies for
key PbSO4; Sand Cu2+, Fe3+, Co2+, Ni2+ 14 hours measuring the characteristics of chemical systems.”6 Analytical chemists
dilute; bubble H2S(g)
4 Kolthoff, I. M.; Sandell, E. B. Textbook of Quantitative Inorganic Analysis, 3rd Ed., The Mac-
millan Company: New York, 1952.
Fe3+, Co2+, Ni2+ CuS 16 hours 5 Van Loon, J. C. Analytical Atomic Absorption Spectroscopy, Academic Press: New York, 1980.
cool, add NH3 6 Murray, R. W. Anal. Chem. 1991, 63, 271A.
digest 50o-70o for 30 min
1.- Introduction
Analytical Chemistry II
Problem Requirements
1.- Introduction
Analytical Chemistry II
Feedback
Loop
Qualitative Analysis
give information about species (atomic, molecular, functional group)
present in a sample
Quantitative Analysis
are used to obtain information about the relative amount of one or several
species
Characterization
Determinations of chemical structure, equilibrium constants, particle size, and
surface structure
1.- Introduction
Analytical Chemistry II
Matrix
the remainder of the sample
Analysis
determination of the physical properties or chemical composition of samples
Determination
What is being stablished
Measurement
the process of associating numbers with physical/chemical quantities and
phenomena
Techniques
chemical or physical principle used to study an analyte
Methods
application of a technique for a specific analyte in a specific matrix
Procedures
set of written directions telling us how to apply a method to a particular
sample
Protocols
set of stringent guidelines specifying a procedure that must be followed
if an agency is to accept the results
1.- Introduction
in Figure 3.2, the American Public Health Agency and the American Soci-
ety for IITesting Materials publish separate procedures for determining the
Analytical Chemistry
concentration of lead in water.
1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
Developing a Procedure
1.- Introduction
Analytical Chemistry II
Developing a Procedure
1.- Introduction
Analytical Chemistry II
Developing a Procedure
Determining the relation between the measured signal and the analyte
concentration, usually done measuring one or more standard samples,
each containing a known concentration of analyte
1.- Introduction
Analytical Chemistry II
Developing a Procedure
1.- Introduction
Analytical Chemistry II
Developing a Procedure
1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
Methods Properties
• Accuracy
• Precision
• Sensitivity
• Specificity and Selectivity
• Robustness and Ruggedness
• Scale of Operation
• Equipment, Time, and Cost
1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
1.- Introduction
Analytical Chemistry II
Instrumental Analysis
Treated Sample
Instrument
Signal
1.- Introduction
Analytical Chemistry II
Calibration
Operation that, under specified conditions, in a first step, establishes a relation
between the quantity values with measurement uncertainties provided by
measurement standards and corresponding indications with associated
measurement uncertainties (of the calibrated instrument or secondary standard)
and, in a second step, uses this information to establish a relation for
obtaining a measurement result from an indication
(BIPM JCGM 200:2008 International vocabulary of metrology )
1.- Introduction
Analytical Chemistry II
Calibration
1.- Introduction
Analytical Chemistry II
Calibration
1.- Introduction
Analytical Chemistry II
Calibration
• External Calibration
Sample Standard
• Internal Standard
Sample+Internal Standard Standard+Internal Standard
1.- Introduction
Analytical Chemistry II
Calibration
Further Reading:
1.- Introduction