ENVIRONMENTAL ANALYSIS

Concern over the current and future

quality of the environment
Environmental Analysis

 Transport of Pollutants in the

Environment
 Water Analysis
 Analysis of Solids and Lands
 Atmospheric Analysis
 Sampling Methods
ENVIRONMENT
ENVIRONMENT POLLUTION

Pollution:
The addition of a substance by human activity to the
environment which can cause injury to human health
or damage to natural ecosystem
ENVIRONMENTAL ANALYSIS

Aims:
Pollution Monitoring
Evaluation:
• Investigate trends in pollution and identity future
problems
• Develop computer models which simulate
environmental process
• Inform the quality of environment
• etc
ANALYTICAL PROCEDURES
 Sampling: is process by which a sample is
obtained

When and where should the sample be taken?

How many samples should be taken?
How much sample is required?
How to transport and store the sample?
etc
Macam-macam Sampling
Batch, continues, composite and representative

 Batch: taking a sample and analysis either on site or

in lab, these sample are collected specific time and
place and also called grab sampel
 Continues, continuously monitoring.
 Composite: mixing several batch sampel, usually
collected at the same place but at different time
 Representative samples. Important that the sample is
representative of the whole system to achieve.
Storage
 Sometimes it is possible to carry out in situ analysis. Most often
the sample has to be transported some distance, need stored
and transported. Important to preserve the integrity of the
sample.
 Risk: chemical, biological reaction and interaction with bottle
sample.
 Once collection: store at refrigerator 4°C
 Pyrex glass bottle for organic analysis and plastic bottle
(polyethilene or polypropylene) for inorganic samples.
 Teflon (PTFE) is the most unreactive material but also most
expensive
 Sample Treatment

Aims:
 To convert the sample and analyte into a form
suitable for analysis by the chosen method
 To eliminate interfering substances
 To concentrate the sample
A variety of sample treatment methods depend on:
 Type of sample
 The analyte to be determined
 The kind of analytical method to be used

Typical sample treatment methods:

 Dissolution/digestion: acid, refluxing, UV and MW digestion
 Filtration
 Solvent extraction, organic analyte must extracted to
organic solvent
 Drying, sieving, etc
Analytical Method

Selectivity
 Expected concentration of analyte in the sample
 Number of samples to be analyzed
 Analysis time
 Cost of the analysis
 Classified as specific, selective or universal.
Analysis Methods

 Classical Analysis: titimetry (> 1 mg/L,

limited use for trace analysis),
gavimetry (minimum lab
eq.,inexpensive, accurate but tedious
and slow.
 Instrumental Analysis
 Portable Laboratories
Test kits and portable Lab.
 to avoid any changes in the sample
composition due to chemical or
biological reactions during transport to
the lab.
 to obtain results immediately as, for example, during
an emergency following a spillage of hazardous
chemicals, when a delay in analysis could have gave
consequences
Standardisation & calibration
 Standardisation. Titration needs to standardize the
titrant. Water hardness, standard EDTA is used as a
titrant. EDTA must be standardize using CaCO3
 Calibration • Standart Addition

• Blanko
 Accuracy

Accuracy refers to the difference (error

or bias) of the measured value with the
true value
(using standard reference materials)
Precision

Precision refers to the reproducibility

and repeatability of measurement
 Accuracy and
precision
The dictionary definition of both ‘accuracy’ and ‘precision’ are
roughly the same, indicating that these words may be used
synonymously. However in ‘Analytical Science’ they have two
separate meanings, the difference between them is best
illustrated by using target diagrams

Poor precision Good precision Good mean accuracy Good accuracy

poor accuracy poor accuracy poor precision good precision
 Accuracy and
precision (2)
You saw from the previous slide, a set of results can be
either accurate and/or precise or can be neither accurate
nor precise. Thus accuracy may be defined as:
The closeness of the mean value from a replicate set of results to the
true or accepted value
Precision may be defined as:
The spread of results from a replicate set of measurements

The difference between the true value and the mean

measured value is termed bias. The spread of replicate data is
measured in terms of standard deviation (s) or variance (s2)
Mean : x   xi / n

 (x
2
Standard deviation :  x)
s
i

n 1
RSD (relative standard deviation) :

RSD%  ( s x)  100%
 Bias and variance
Cu by AAS

10.4
A solution containing copper was

Cu in ppm
10.2
analysed 10 times using atomic 10
absorption spectroscopy. 9.8
9.6
The results obtained in ppm were: 0 2 4 6 8 10 12
10.08, 9.80, 10.10, 10.21, 10.14, Replicate sample
9.88, 10.02, 10.12, 10.11, 10.09
Bias = Mean value - true value
We can now calculate the precision
= 10.06 - 10.00
of the data as standard deviation
= 0.06 ppm
If the true value is known to be
10.00 ppm, we can also calculate Standard deviation (SD) = 0.12(4)
the bias
Relative SD = 100 X SD/10.00 = 1.2%

Conclusion - the method gives both good accuracy (low bias) and
acceptable precision (RSD of 1.2%)
 Repeatability &
Reproducibility
 Repeatability — is determined by analyzing replicate
samples on the same day under the same condition
(using the same instrument and operator, and
repeating during a short time period)
Reproducibility — is determined by analyzing
replicate samples under the condition may vary
(different instruments and operators, and over longer
time periods)

Two different operators

analysing milk
using different pieces of
equipment at different
times. The laboratory is
the same.
Error
 Gross errors; due to human negligence
 (misreading instrument, mislabelling sample, errors in calculation,
spillage, contaminations, etc)

 Systematic errors; relate to the inaccuracy of the

method, produced a bias in the method. Can be eliminated (eg
removal of interfering substance) , my result in a method exhibiting
good precision but poor accuracy

 Random errors; are inherent in all measurement, even

under the best condition using best instrumens. Random errors are
generally small and have equal probability of being positive and
negative. Cannot be eliminated, can be determined by replicate
measurements and reported as an uncertainty in the result.
Linear Regression

Correlation coeffisient
 Correlation coefisient, r, can be used to
test wheather there is significant linear
relationship between x and y
 Between -1 and 1
 Detection Limits

 Smallest value that can be distinguished

from a blank and there are various
ways to calculate this.
 d.l.= 3xstandard deviation of the baseline noise/

Reference Materials

Actual samples (e.g. river water, sediment, soil) which they can analysed
by government lab.
CRM (certifed reference materials) and can be purchased from
government. LGC in UK, BCR in USA.
The refernce material can be then be analysed and the determined coc
compared with that quoted on the certified accompanying the material to
get analytical error.
Concentration Unit
Problems of Environmental Analysis
 Low concentration of analyte; below the detection limit of
many analytical methods.

 Complex matrix, with numerous other compound (known and

unknown) present in the sample and the could lead to several other
problem on this list.

 Contamination, due to the low concentration of analyte.

 No suitable method, for analyte may be e a new previously

considered, and the analyst may have to develop a satisfactory
method.

 Reaction of analyte, which could eiither increase or decrease its conc.

 Speciation, since a substance (e.g. Heavy metal) may be pty of the present
in different forms, and toxicity of sbstance may depend on its form.