Course Name:: Volumetric and Gravimetric Analytical Chemistry: 4022133-3

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Course Name: Volumetric and Gravimetric

Analytical Chemistry

Course Code: 4022133-3


Learning is a collaborative activity
between
Students and Teachers

LEAR
NING
Volumetric and Gravimetric Analytical Chemistry
Learning Outcomes

➢ To Understand the volumetric analysis processes


and its principles.

➢ To gain knowledge on the principles of gravimetric


analysis.

➢ knowing the equipment that is used in volumetric


and gravimetric analysis
Course Grades
Midterm Paper sheet practical Final Exam Total
exam
20 10 30 40 100

References
1-Fundamentals of Analytical Chemistry, 9th Ed ,Douglas A. Skoog, Donald
M. West,F. James Holler ,Stanley R. Crouch .
2-Analytical Chemistry, 7th Ed,Gary D. Christian.
3- )‫ محمد أحمد آشي وآخرون‬.‫د‬.‫التحليل الكيميائي الكمي التقليدي لطالب الكليات والجامعات (تأليف أ‬
4- )‫ عبدالغني حمزة وآخرون‬.‫د‬.‫الحسابات في الكيمياء التحليلية (تأليف أ‬

For contact:
E-mail: manalkhoj@gmail.com
Lectures schedule
Weak Date Subject
1 22/12 The Language of Analytical Chemistry /Using statistical method

2 29/12 (Concentrations) Molarity and normality


3 06/01 (Concentrations) Molarity and normality
4 13/01 Principle of volumetric analysis/neutralization titrations theory
5 20/01 pH calculation
6 27/01 pH calculation

7 05l02 Midterm exam

8 12/02 Titration curve calculation

9 19/02 Oxidation-Reduction Titration (Redox)

10 26/02 Precipitation Titration

11 03/03 Complexometric titration

12 10/03 Gravimetric analysis


13 17/03 Gravimetric analysis
14 24/03
15 02/04 Revision
Lecture 1: contents
➢ The nature of analytical chemistry.
➢ Qualitative and quantitative analysis.
➢ statistical method
• Mean
• Range
• Precision
•Accuracy
•Standard deviation
•Variance
•Errors
What is Analytical Chemistry ??

➢It is a Measurements science consisting of


a set of powerful ideas and methods that
are useful in all field of science and
medicine.*

➢It is studies and uses instruments and


methods used to separate, identify
and quantify matter.*

*Fundamentals of Analytical Chemistry, 9th Ed ,Douglas A. Skoog, Donald M. West, F. James Holler,
Stanley R. Crouch.
Analytical Chemistry

Quantitative Analysis Qualitative Analysis

Gravimetric Analysis Instrumental Analysis

Volumetric Analysis
Qualitative Analysis (identification)
Provides information about the elements and
compounds in a sample.

“Identifying what is in unknown”

Quantitative Analysis
provides information about the amount of each
substance in a sample

“Identifying how much is present”


Quantitative Analysis
• Gravimetric Analysis:
Measure the mass of the analyte
or some compound chemically related to it.

• Volumetric analysis:
Measure the volume of a solution containing
sufficient reagent to react completely with
the analyte .
Where is Analytical Chemistry used?

1- Clinical laboratories.
2- Forensic laboratories.
3-Environmental laboratories.
4- Manufacturing /industry
5- Research.
6- Others.
Analytical chemistry and other branches of sciences
Important concepts

Analysis:
A process that provides chemical or physical
information about the constituents in the
sample or the sample itself.

Analytes:
Substances being measured in a given sample.
Important concepts

Interference :
A species that causes an error in an analysis by
enhancing or attenuating (making smaller) the
quantity being measured.

Matrix:
Everything else in the sample.
statistical
methods
Mean
Mean : average of a set of values.
It is obtained by dividing the sum of replicate
measurements by the number of measurements in
the set.


N
xi
i =1
x=
N
Where
xi = individual values of x and
N = number of replicate measurements
Results of 6 determinations of
the Fe(III) content of
a solution, known to contain 20 ppm:

Note: The mean value is 19.78 ppm (i.e. 19.8ppm)


Precision
Precision is how close replicate measurements on
the same sample are to each other.

Accuracy
Accuracy is the closeness of a measured value to the true
(accepted value).
Accuracy and Precision:

Is There a Difference?
Ways of Expressing precision

1- Deviation from the mean:

di = xi − x
Example

di = 20.00−19.78 = 0.22
Ways of Expressing precision

2-Sample Standard Deviation (s )


N
(xi − x)2

s= i=1
N −1
Ways of Expressing precision

3-Variance:
This is the square of the standard deviation

(x
N 2
− x) 2

s =
2 i =1 i

N −1
Ways of Expressing precision

Rang (R):

The difference between the lowest and highest


values.
Example
The normality of a solution is determined by four
separate titration, the results being 0.2014, 0.2049,
0.2039, and 0.2043.
Calculate the mean, range and standard deviation? ?
Answer:
1-(Mean)

X= 0. +
2041 0. +
2049 0. +
2039 0.2043= 0.2043
4
2- Range
R = 0.2049 – 0.2039 = 0.001
Example

3- Standard deviation:

S= (0.0002
)2
+ (0.0006
)2
+ (0.0004
)2
+ (0.0000
)2
= 0.0004
4−1
Ways of Expressing accuracy
1- Absolute error: The difference between the
measured value and the true value.
E = x i - xt
where
Xi = measured value
xt = true or accepted value

2-Relative error: The absolute error divided by the true value.


xi − xt
Er = 100%
xt
Example

The result of analysis are 36.97 g compared with


accepted value of 37.06 g. Calculate the absolute error
and relative error in part per thousand?

Solution
Absolute error= measured(observed) – true(accepted)
E = Xi – Xt

Absolute error =36.97g – 37.06g = - 0.09g

Relative error = - 0.09 X 100= -0.24 %


37.06
Example

Three student weigh a sample of known weight (4.5g),


four time each
Donovan : 4.56 g ,4.55 g, 4.76 g, 4.58 g
Mike :4.55 g ,4.56 g, 4.66 g, 4.53 g
Kevin : 4.77 g ,4.78 g, 4.76 g, 4.79 g
Who is the most accurate?
Who is the least precise?
Solution

Donovan: 4.56 g, 4.55 g, 4.76 g, 4.58 g


» Average = 4.6125 g
» Range 0.21, Standard Deviation = 0.099
Mike: 4.55 g, 4.56 g, 4.66 g, 4.53 g
» Average = 4.575 g
» Range 0.13, Standard Deviation = 0.058
Kevin: 4.77 g, 4.78 g, 4.76 g, 4.79 g
» Average = 4.775 g
» Range 0.03, Standard Deviation = 0.013
• Who is the most accurate?
– Mike is 0.08 g off, Donovan is 0.11 off, and Kevin is off by 0.28 g
– Mike is the most accurate because he is the closest to the true
value
• Who is the least precise?
– Donovan has the highest standard deviation and the largest range,
therefore he is the least precise.
Types of Errors in Experimental Data
1-Random or Indeterminate Errors
The errors that affect the precision of measurement.
Types of Errors in Experimental Data

2-Systematic or Determinate Errors


The errors that affect the accuracy of a result.
Sources of Systematic Errors
1. Instrumental errors
Caused by unideal instrument behavior,
by faulty calibrations, or by use under
inappropriate conditions.

2. Method errors
Arise from unideal chemical or physical
behavior of analytical systems.

3. Personal errors
Results from the carelessness, inattention,
or personal limitations of the experimenter.
homework
Q: Reproducibility of a Sample Selenium content
(mg/g) (xI)
method for determining
the % of selenium in 1 0.07
foods. 2 0.07
9 measurements were 3 0.08
made on a single batch 4 0.07
of brown rice. 5 0.07
6 0.08
Calculate the mean, 7 0.08
range and standard 8 0.09
deviation? 9 0.08

Mean = Sxi/N= 0.077 mg/g

Standard deviation: = 0.007


By the end of this lecture you should know

• The meaning of analytical chemistry.


• Difference between Qualitative and Quantitative
analysis.
• The importance of analytical chemistry.
• Basic statistical concepts in analytical chemistry (Mean,
Precision, Accuracy, Way of expressing
precision and accuracy, Errors in experimental
data and Source of systematic errors.
Prep. for next lecture
Prep. for next lecture

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