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● Analytical process
WEEK 2: THE NATURE OF ANALYTICAL PROCESS ○ Is the structures steps in chemical
I. ANALYTICAL PROCESS analysis
II. STEPS OF THE ANALYTICAL PROCESS
A. PROBLEM DEFINITION ○ It involves sample preparation,
B. METHOD SELECTION separation, and measurement
C. SAMPLING (SAMPLE
PREPARATION)
D. ANALYSIS (SEPARATION)
E. CALCULATION AND REPORTING
(MEASUREMENT)
III. AN INTEGRAL FOR CHEMICAL ANALYSIS:
FEEDBACK CONTROL SYSTEMS
IV. DEER KILL ANALYTICAL PROCESS
A. THE PROBLEM
B. THE METHOD
C. SAMPLE
D. SAMPLE PREPARATION
E. ANALYSIS
F. CALCULATION AND REPORTING
V. ERRORS IN THE LABORATORY
VI. ERRORS IN ANALYSIS - TYPES OF ERROR
A. DETERMINATE OR SYSTEMATIC ● The analytical process in the broader
ERROR
1. TYPES OF SYSTEMATIC sense is represented by the whole
ERRORS figure
B. INDETERMINATE
● The analytical process in the strictest
VII. EFFECTS OF SYSTEMATIC ERRORS
VIII. QUANTIFYING EXPERIMENTAL ERRORS sense is only the lower part shown in
IX. ASSESSMENT OF RELIABILITY OF RESULTS gray boxes
X. ANALYTICAL MEASUREMENTS
XI. ACCURACY AND PRECISION
A. ACCURACY
B. PRECISION
C. COMPUTING ACCURACY STEPS OF ANALYTICAL PROCESS (6 BASIC
D. COMPUTING PRECISION
MAIN STEPS)
XII. MEASURES OF CENTRAL VALUE OF
TENDENCY - BASIC STATISTICAL
TREATMENTS 1. Problem definition - identify the
XIII. SIGNIFICANT NUMBERS
A. RULES IN DETERMINING problem and formulate questions
SIGNIFICANT FIGURES 2. Method selection - select method of
XIV. SIGNIFICANT NUMBERS IN NUMERICAL
COMPUTATIONS analysis
A. ADDITION AND SUBTRACTION 3. Sampling - obtain bulk sample and
B. MULTIPLICATION AND DIVISION extract smaller laboratory sample
XV. SIGNIFICANT FIGURES LOGARITHMS AND
ANTILOGARITHMS from bulk
XVI. RULES FOR ROUNDING OFF NUMBERS 4. Sample preparation - prepare
sample for analysis
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
● Obtaining a Representative
Samples
B. METHOD SELECTION Factors
○ Sample type/homogeneity/
● Methods size
○ Qualitative method ■ size : macro, semi-
○ Quantitative Methods micro, micro, ultra
■ Type: major, minor,
● Select a method trace, ultra
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
0
E. CALCULATION AND REPORTING
(MEASUREMENT)
Facts:
● Dead whitetail deer near pond in the
Land Between the Lakes State Park
Hypothetical Case Study: in south central Kentucky
The incident began when a park ● Observation: grass around nearby
ranger found a dead white tailed deer near a power-poles was wilted and
pond in the Land between the Lakes National discolored
Recreation Area in western Kentucky. The
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
0
4. SAMPLE PREPARATION
5. ANALYSIS
A. Measuring the Amount of Analyte
● Arsenic in the kidney tissue of
● Spectrophotometer:
animals is toxic at levels above about
○ Highly colored
10 ppm.
complex of arsenic
● Grass samples showed about 600
was found to absorb
ppm arsenic
light at a wavelength
of 535 nm.
B. Reliability of the Data
● The data from these experiments
were analyzed using statistical
methods found in the manual.
ACCURACY
● Describes the nearness of an experimental
value or a mean to the true value.
○ Although true value can never
known exactly, accepted
value, is often used
● Statistically measured through: COMPUTING ACCURACY
absolute or relative error
A. Absolute Error
0
● The absolute error of a system is
PRECISION (CONSISTENCY) equal to the difference between
the actual reading, xi , and the
true (or accepted) value xt ; bears
● Refers to the agreement between
a sign.
values in a set of data (closeness of
data)
● Describes the reproducibility and
repeatability of measurements
B. Relative Error
● The relative error describes
the error in relation to the
magnitude of the true value,
and may, therefore, be more
useful than considering the
absolute error in isolation.
○ Xi = actual reading
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
Example 2.6
COMPUTING PRECISION
● Calculate the relative error in ● Precision can be computed
percentage terms for an iron analysis using Range, Average deviation
that gives a value of 115 ppm Fe or Standard Deviation.
content when the true value is, in fact,
110 ppm. ● Standard Deviation - The
standard deviation is perhaps the
Method: most recognized measure of
precision. Standard deviation
may be used to calculate the
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
● Degrees of Freedom
○ For sample = N - 1
Method:
MEAN/AVERAGE
● Sum of numbers divided by numbers
of measurements RANGE
● Highest value – Lowest Value =
x(max) – x(min)
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
EXAMPLE 2
AVERAGE DEVIATION
● The temperature of a laboratory is
● Ʃ|x-x̅| n | x - x̅ | = absolute deviation = known to be a constant 25.23°C. A
|value – mean| student uses an alcohol thermometer
to measure the temperature of the
laboratory three times and records
the temperatures in the table below:
STANDARD DEVIATION
b.) Median
= 68.8 + 69.1
2
= 68.95 Interpretation:
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
For Precision:
a) Determine the Range
● Find the range of the student's
thermometer readings:
○ Hv, Highest recorded
temperature is 23.91°C
○ Lv, Lowest recorded
temperature is 23.24°C
○ Range = Hv – Lv = 23.91 C –
23.24 C = 0.67
SUMMARY
b) Calculate Precision.
Precision = Mean ± Range = 23.68 ± 0.67 • Knowing the analytical process can make
one be able to do his work efficiently and
Interpretation: effectively
● The range of values is closer to 1 • Learning the “types of errors” can make us
than it is to 0 so we can decide that more aware of its impact and be able to
the student's measurements are minimize them
NOT precise. They are imprecise. • Understanding the concept of accuracy and
precision is as important as knowing how bad
Conclusion: equipment, poor data processing or human
● The student's temperature error can lead to a disaster of inaccurate
readings are both inaccurate and results
imprecise.
SIGNIFICANT NUMBERS
EXAMPLE 3
● The following results were obtained
in the replicate determination of the ● Laboratory investigations usually
lead content of a blood sample: involve the taking of and
0.752, 0.756, 0.752, 0.751, and 0.760 interpretation of measurements.
ppm Pb. Find the mean and the ● All physical measurements obtained
standard deviation of this set of data. by means of instruments (meter
sticks, thermometers, electrical
SAN PEDRO COLLEGE – MAIN CAMPUS
BACHELOR OF SCIENCE IN MEDICAL LABORATORY SCIENCE
ANALYTICAL CHEMISTRY FOR MLS (LEC)
LECTURER: RONALD FLORALDE
meters, clocks, etc.) are to some Rule 3: Leading zeros (zeros at the
extent uncertain. beginning of a number) are NOt significant
● The amount of uncertainty depends
both upon the skill of the measurer ● 0.008 has 1 significant figure
and the quality of the measuring tool. ● 0.000416 has 3 significant figures
● The degree of uncertainty in physical
measurements can be indicated by Trailing zeros (zeros at the end of the
means of significant figures. number):
● Significant figures - consists of all ● Are significant if and only if there is a
certain digits in a measurement plus decimal point present in the number OR
the first uncertain digit. they carry overbars.
figures in the original number digit is increased by one if it is odd, but left
which is 4.000 x 10-5 , retain as it is if even.
the 4 significant figures to the ● 12.5 is rounded to 12
right of the decimal point ● 11.5 is rounded to 12
resulting in -4.3979 (which
has 4 significant figures to the This rule means that if the digit to be dropped
right of the decimal point). is 5 followed only by zeroes, the result is
○ Since 4 is a non-zero number always rounded to the even digit. The
and the three zeroes are rationale is to avoid bias in rounding; half of
trailing zeroes. Hence, - the time we round up, half the time we round
4.3979 down.
● For (b), apply rule two (2): keep as
many digits as there are digits to the
right of the decimal point in the
original number.
○ Antilog 12.5 has only one digit
at the right of the decimal
point. The number of
significant numbers on the
right of the decimal point must
reflect on the answer. Hence,
3 x 1012 which has one
decimal digit.