Lecture 1 - Intro of Anal Chem (Compatibility Mode)

VNU University of Science – VNU, Hanoi
Analytical chemistry
Lecture’s notes
Spring 2020
Assoc. Prof. Dr. Ta Thi Thao
Head of Dept. of Anal. Chem.

Faculty of chemistry
Lecture 1
Introduction of analytical chemistry

1.1. Introduction of analytical chemistry
1.1.1. What is anal. Chem. (old definition)
1.1.2. New definitions of Anal. Chem.
(Source: Miguel. V. Trends in anal. Chem. Vol. 16, No. 3, (1997), 125- 131).
“Analytical chemistry is a metrological

science that develops, optimizes and
applies measuring processes
intended to derive quality chemical
information of both global and partial
type in order to solve the measuring
problems posed.”
What is analytical chemistry?
(according to the new definitions)
• Analytical chemistry is not a separate
branch of chemistry, but simply the
application of chemical knowledge.
 The craft of analytical chemistry is not in
performing a routine analysis on a routine
sample, but in improving established
methods, extending existing methods to
new types of samples, and developing new
methods for measuring chemical
phenomena.
1.1.3. Revolutions of Analytical
chemistry
• Anal. Chem. has devoloped through 3
revolutions.
+ First revolution was in early 20th century:
quantitave detn. of big amount - titration
and gravimetry.
+ Second revolution was the instrumental
beginning in 1930s
+ Now is the third revolution: represents the
broadening and depending the meaning of
analysis
1.1.4. Roles of analytical chemistry
1.1.5.The Analytical Perspective
1. What is the analytical problem?
2. What type of information is needed to solve the
problem?
3. How will the solution to this problem be used?
4. What criteria were considered in designing the
experimental procedure?
5. Were there any potential interferences that had to be
eliminated? If so, how
were they treated?
6. Is there a plan for validating the experimental method?
7. How were the samples collected?
8. Is there evidence that steps 2, 3, and 4 of the analytical
approach are repeated more than once?
9. Was there a successful conclusion to the problem?
1.2.The analytical process
1. Definition problems
2. Choose analytical methods
3. Sampling
4. Sample preparation
5. Chemical Separation
6. Analysis
7. Data processing and Report Results

1.2.The analytical process (cont.)
1. Define the problem (eg.: determination of phosphate in lake)
 What need to be found?
 Qualitative or quantitative?
 What will the information be used for? Who will be
used?
 When will it be needed?
 How accurate and precise does it have to be?
 What is the fund?
 The analysts should consult with the clients to
plan the useful and efficient analysis, including
how to obtain a useful sample.
1.2. The analytical process (cont.)
2. Choose methods
 Sample type; - Size of sample;
 Sample preparation needed;
 Concentration and range (sensitivity needed)
 Selectivity needed (interferences)
 Accuracy and precision needed
 Tools/ instruments available
 Expertise/ experience
 Cost - Speed
 Does it need to be automated?
 Are method available in the chemical literature?
 Are standard methods available?
• Chemical analysis: for detn. of major and
minor amount of analytes
- Volumetric methods: based on 4 equilibria
- Gravimetrics
• Instrumental analysis: spectrochemical
analysis, electrochemical analysis
Comparison of Different analytical methods
Approx. Appro Selectivit Speed Cost Principle uses
Method range xpreci y
sion
( mol/L) (%)
Gravimetry 10-1-10-2 0.1 Poor- mod. Slow Low Inorg.
Titrimetry 10-1-10-4 0.1-1 Poor- mod. Mod. Low Inorg., Org.
Potentionmetry 10-1 -10-6 2 Good Fast Low Inorg.
Electrogravimetry, 10-1-10-4 0.01-2 Moderate Slow-mod. Mod. Inorg., org.
coulometry
Good Moderate Mod.
Voltammetry 10-3 -10-10 2-5 Inorg., org.
2 Good-mod. Fast- mod. Low- Mod. Inorg., org.

Spectrophotometry 10-3-10-6
2-5 Moderate Moderate Mod. Org.
Fluorometry 10-6-10-9
Good Fast Mod.- High Inorg- Multiele.
Atomic spectrometry 10-3 -10-9 2-10
Fast-Mod. Mod.-high
Chromatography 10-3 -10-9 2-5 Good Org. Multicom.
Kinetic methods 10-2-10-10 2-10 Good-Mod. Fast- Mod. Mod. Inorg.,org,enzyme

3. Sampling
6. Analysis

3. Sampling
Sample type
Representative/ random sample
Sample size
Minimum sample number
Sampling statistics/ error
Sampling matrix: - The matrix is the type of bulk
material that is to be sampled, example are:
Soil; water; sediment; sludge, air…
- The sample matrix can be homogeneous or
heterogeneous
3. Sampling
6. Analysis

(cont.)
 Samples are solid, liquid or gas?
Dissolve?
Ash or digest?
Chemical separation or masking of
interferences needed?
Need to be concentrate the analysts?
Need to change analyst for detection?
Need to adjust solution conditions (pH, add
reagent…)
• Preparation of the lab sample
• filtering
• drying (to remove water)
• eliminate interferences (chemical
separations)
• replicates
3. Sampling
6. Analysis

5. Chemical Separation if necessary

Distillation
Precipitation
Solvent Extraction
Solid phase extraction May be done as part of the
Chromatography measurement step
Electrophoresis
3. Sampling
6. Analysis

6. Analysis
- Chemical analysis
- Calibration in instrumental analysis
- Validation/controls/ blanks
- Replicates
* Quality assurance (QA) and quality control

(QC)
- Quality Control ensure the quality of results
 reagent, method, and field blanks
 calibration
 control charts
Quality assurance (QA) and
quality control (QC)
Method Validation (performance of the instrument)
- Selectivity and Specificity
- detection limit, limit of quantitation
- Calibration
- Bias and Recovery using matrix spikes and -
standard reference materials (SRM)
- Uncertainty
- Repeatability and reproducibility
Method Verification (performance of a standard anal.
method)
- Bias, Recovery, Precision using matrix spikes,
standard reference materials (SRM)
- Uncertainty Regression Detection limit
3. Sampling
6. Analysis

The analytical process (cont.)
• Data reliability (estimate of error)
• Comparing results (statistical analysis)
• Reporting results (Figures or Tables)
based on using statistics

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VNU University of Science – VNU, Hanoi

Head of Dept. of Anal. Chem.

Introduction of analytical chemistry

“Analytical chemistry is a metrological

7. Data processing and Report Results

Gravimetry 10-1-10-2 0.1 Poor- mod. Slow Low Inorg.

Titrimetry 10-1-10-4 0.1-1 Poor- mod. Mod. Low Inorg., Org.

Potentionmetry 10-1 -10-6 2 Good Fast Low Inorg.

Electrogravimetry, 10-1-10-4 0.01-2 Moderate Slow-mod. Mod. Inorg., org.

2 Good-mod. Fast- mod. Low- Mod. Inorg., org.

Kinetic methods 10-2-10-10 2-10 Good-Mod. Fast- Mod. Mod. Inorg.,org,enzyme

7. Data processing and Report Results

7. Data processing and Report Results

7. Data processing and Report Results

5. Chemical Separation if necessary

7. Data processing and Report Results

* Quality assurance (QA) and quality control

7. Data processing and Report Results

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