The Analytical Challenge
Chapter 1, pp. 1-22, #1,7,8,9,10
X, Y and Z X Y Z
Individual volume zones
Complex Sample
of each analyte
Very few analytical methods provide both qualitative and
quantitative analysis of complex mixtures. Some form of
SEPARATION is needed up front.
Analysis of Chocolate
How would one analyze different chocolate bars for their
caffeine and theobromine content? These are the analytes.
***There are many parts to this answer***
The Analytical Process
Analysis
Replicate measurements
Sample preparation is often the key step in the analytical process!
Sample Types
• Homogeneous sample (same composition
throughout)
• Heterogeneous sample (different composition from
region to region)….Random and segregated materials
Heterogeneous samples (materials) need a different
strategy for sampling than do homogeneous
samples.
Types of Analytical Analyses
• Qualitative analysis (identifying
what is in an unknown sample)
• Quantitative analysis (identifying
how much analyte is present in an
unknown sample)
Distillation
Process by which mixtures are separated based on differences in
component volatilities.
Filtration
Process by which solids are separated from fluids (liquids or
gases) by interposing a medium through which only the fluid
can pass.
Pressure difference between feed and permeate
Membrane Filtration
Powerful methods for analyte separation/isolation.
Liquid-Liquid (Solvent) Extraction
Process by which components in a liquid mixture are
separated based on their relative solubilities (partitioning) in
two immiscible liquids (organic – water).
K = Cphase 1/Cphase2
Partition coefficient
Sample Preparation
Weighing the chocolate
and extracting the fat.
Maximize extraction
with small particles
Liquid extraction used to remove fat from the solid chocolate.
Caffeine and theobromine are insoluble in the ether.
Sample Preparation
Caffeine and theobromine dissolved into the water. Sample
is then filtered and made ready for the real analysis.
Analysis – Separation and Detection
Analysis – Separation and Detection
Calibration curve = Standard curve = Response curve
The Data
Average ± std. dev.
Values for theobromine are reproducible (<1%)
Values for caffeine are less reproducible (6%)
General Steps in Chemical Analysis
• Formulating the question (Is the water safe to drink?)
• Selecting the analytical method(s) (instrument) to be used.
• Sampling (properly selected sample - garbage in, garbage out)
• Sample preparation (convert sample into form suitable for analysis)
• Analysis (reproducibility, sensitivity, stability)
• Reporting and Interpretation (verbal and written communication)
• Drawing conclusions (What do the results mean?)