Chapter 1: Introduction to

Environmental
1
Measurements
Dr Norhusna Mohamad Nor
2 Course Learning Outcomes
 At the end of this chapter, students should be able to:

 Understand the design of environmental studies and

classification of analytical methods
 Describe techniques, methods and procedures for
environmental measurements
 Perform basic statistical analysis of data
 Identify standards and calibration methods of environmental
measurement
3 What is Instrumental Analysis?
Instrumental analysis is a field of analytical
chemistry that investigates analytes using
scientific instruments.

What is Environmental Analysis?

Environmental analysis is a study of the
composition of the atmosphere, water
and soil by means of scientific
instruments.
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 The relationship between

analytical, chemistry, other
branches of chemistry and
the other sciences.
 5
 Instrument - Convert physical or chemical properties that
we cannot directly observe into information that we can
interpret.
6 Introduction
 All environmental studies on scientific research
ultimately depends on the results of chemical
analysis of samples of air, water, soil and biological
organisms.
 Accurate and reliable methods is required.
 Few problems in measuring the pollutants:
 The analytes of the present in extremely low quantities
 The matrix of analytes normally can be very complex
 The material to be sampled is usually very non-homogeneous

Note: An analyte, component, or chemical species is a substance or chemical constituent

that is of interest in an analytical procedure.
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 Commonly used units of measurement is SI units.

 Conversion of units is important in handling the
environmental measurement.
 Significant figures is related in accuracy of the
reported experimental data.

Note:
• In chemical analysis, matrix refers to the components of a sample other than the analyte
of interest.
• A homogeneous sample is required for the quantification process to correctly measure its
composition.
8 Common units of measurement

Unit Meaning Usual Use

µg/g Micrograms of analyte per gram of Concentration in solid samples
sample
µg/m3 Micrograms of analyte per 1000 L of Concentration of particulate matter in
sample air
µl/l Microliter of analyte per liter of sample Concentration of liquid analyte in
liquid sample
ppmv Volumes (or moles) of analyte per 106 Concentration of gaseous analyte in
air or other gases
ppmw Grams of analytes per 106 g of sample Solid or liquid analyte in solid samples
ppbw Grams of analytes per 109 of sample Solid of liquid analyte in solid samples
9 Concentration Units
 Classification of Analytical Method
10
ANALYSIS
QUALITATIVE
Qualitative analysis provides
information about the identity
of species.(i.e: functional
groups in the sample,
composition, structural
information).
QUANTITATIVE
Quantitative analysis
provides numerical
information of analyte
(quantitate the exact
amount or concentration).
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14 Techniques, Methods and Procedures
INSTRUMENTAL TECHNIQUES

SPECTROSCOPY CHROMATOGRAPHY CHROMATOGRAPHY-

SPECTROSCOPY
1. UV AND VISIBLE 1. GAS CHROMATOGRAPHY 1. GAS CHROMATOGRAPHY –
SPECTROSCOPY 2. LIQUID CHROMATOGRAPHY MASS SPECTROSCOPY
2. INFRARED 2. LIQUID CHROMATOGRAPHY –
SPECTROSCOPY (FTIR) MASS SPECTROSCOPY
3. MASS SPECTROSCOPY 3. GAS CHROMATOGRAPHY –
4. ATOMIC FOURIER TRANSFORM
SPECTROSCOPY (AAS, INFRARED SPECTROSCOPY
ICP, AFS)
 Analytical Methodology
15 1. DEFINE THE PROBLEM
- What need to be found? Qualitative and/or quantitative
- How accurate and precise does it have to be?
- What will the information be used for?
- What is the budget?
- When will it be needed?
- i.e: For liquid chromatography technique, the sample must be
presented as a dilute component in a solution.

2. SELECT THE TECHNIQUE

- Type and size of sample
- Sample preparation required
- Accuracy/precision needed
- Tools/instruments available
- Cost
- Are methods available in the chemical literature?
 3. PREPARATION OF SAMPLING & PRESERVATION
- Proper sampling and good sample handling – prevent loss or
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contamination
- Proper storage
4. PREPARATION SAMPLE FOR ANALYSIS
- Instrument chosen influence the procedures needed to prepare a
sample:
# dissolution of solid sample
# dilution
# concentrate the sample
# filtration to remove particulate matter
# extraction to remove analyte from complex matrix
5. PERFORM MEASUREMENT
- Calibration
- Replicates
6. CALCULATE AND REPORT THE RESULTS
 Calibration of Instrumental Methods
17
 All types of analytical methods require
calibration for quantitation.
 Calibration is a process that relates the measured
analytical signal to the concentration of analyte.
 The three most common calibration methods
are:
# Calibration curve
# Standard addition method
# Internal standard method
 Calibration Curve Method

1. Most convenient when a large

number of similar samples are to be
analyzed.

2. Most common technique.

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3. Facilitates calculation of Figures of

Merit.
 Calibration Curve Procedure

1. Prepare a series of standard solutions

(analyte solutions with known
concentrations).

2. Plot [analyte] vs. Analytical Signal.

19

3. Use signal for unknown to find

[analyte].
 Calibration Curves
20

Detection Limit (Limit of detection, LOD): The minimum concentration of

analyte that can be detected with a specific method at a known
confidence level.
Dynamic Range: The lowest concentration at which quantitative
measurements can be made (limit of quantitation, or LOQ) to the
concentration at which the calibration curve departs from linearity (limit of
linearity, or LOL).
 Standard Addition Method
1. Most convenient when a small number of
samples are to be analyzed.

2. Useful when the analyte is present in a

complicated matrix and no ideal blank is
available.

21 3. Standard addition is frequently used in

atomic absorption spectroscopy and gas
chromatography.
 Standard Addition Procedure
22
 Standard Addition Procedure
23

The absolute value of the x-intercept is the concentration of the analyte.

 Internal Standard Method
1. Most convenient when variations in
analytical sample size, position, or matrix
limit the precision of a technique.
2. A substance known as an “internal
standard” is added to samples and
standards (chemically similar to analyte).
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3. Used to correct for certain types of noise.
 Internal Standard Procedure
1. Prepare a set of standard solutions for analyte (A)
as with the calibration curve method, but add a
constant amount of a second species (B) to each
solution.
2. Prepare a plot of SA/SB versus [A].
Notes
1. The resulting measurement will be independent of sample size
25 and position.

2. Species A & B must not produce signals that interfere with

each other. Usually they are separated by wavelength or
time.
 Example: Pb by ICP Emission
Each Pb solution contains
100 ppm Cu.

Signal

[Pb]
(ppm) Pb Cu Pb/Cu

26 20 112 1347 0.083

40 243 1527 0.159
60 326 1383 0.236
80 355 1135 0.313
100 558 1440 0.388
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 No Internal Standard Correction Internal Standard Correction

600 0.450

0.400
500
0.350

Pb Emission Signal
Pb Emission Signal

400 0.300

0.250
300
0.200

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200 0.150

0.100
100
0.050

0.000
0
0 20 40 60 80 100 120
0 20 40 60 80 100 120
[Pb] (ppm)
[Pb] (ppm)
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Replication
 Replication is the repetition of an experimental condition so
that the variability associated with the phenomenon can be
estimated.

 Replicate samples or replicates, are portions of a material of

approximately the same size that are carried through an
analytical procedure at the same time and in the same way.

 Replication improves the quality of the results and provides a

measure of their reliability.

 Quantitative measurements on replicates are usually

averaged, and various statistical tests are performed on the
results to establish their reliability.
 Calculate and Report the Results
30
Figures of Merit
 Precision: How close the same measurements are to
one another.

 Accuracy: How close the measurement approaches

the real value.

 Sensitivity: Sensitivity of an instrument is a measure of

its ability to discriminate between small differences in
analyte concentration.
 Illustrating the difference between “accuracy” and “precision”
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Low accuracy, Low accuracy,

low precision high precision

High accuracy, High accuracy,

low precision high precision
32 Mean
Defined as follows: N

∑ xi
i = 1
x =
N

Where xi = individual values of x and N is number of

replicate measurements
 Precision
33
Relates to reproducibility of results..
How similar are values obtained in exactly the same way?

Useful for measuring standard deviation from the mean.

A smaller SD
represents data
where the results
are very close in
value to the mean.
The larger the SD
the more variance
in the results.
34 Accuracy

Measurement of agreement between experimental mean and

true value (which may not be known!).
Measures of accuracy:

Absolute error: E = xi - xt (where xt = true or accepted value)

Relative error: x −x
E = i t × 100%
r x
t
(latter is more useful in practice)
 Reproducibility of a method for determining the % of selenium in
foods. 9 measurements were made on a single batch of brown rice.
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Sample Selenium content (µg/g) (xI) xi2

1 0.07 0.0049
2 0.07 0.0049
3 0.08 0.0064
4 0.07 0.0049
5 0.07 0.0049
6 0.08 0.0064
7 0.08 0.0064
8 0.09 0.0081
9 0.08 0.0064

Σxi = 0.69 Σxi2= 0.0533

Mean = Σxi/N= 0.077µg/g (Σxi)2/N = 0.4761/9 = 0.0529

0.0533 − 0.0529
Standard deviation: s = = 0.00707106 = 0.007
9 −1
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THANK YOU!