CHM260

BASIC INSTRUMENTAL ANALYSIS

LABORATORY SUMMARY WRITTEN

REPORT

Name :CASSY LUGAK

ID No. :2018433928
Programme :AS1205D
Instructor :DR YANTI YANA BINTI
HALID
INTRODUCTION
To determine the concentration of an element in the solution, atomic absorption
spectroscopy is used. The AAS theory relies on the assumption that the flame allows
the atom to undergo a transition from a ground state to the first state. This radiation is
absorbed in the form of a wavelength with each element corresponding to its
wavelength. This gives AAS a broad degree of selectivity.

METHODOLOGY
Preparations of Standard Solution
1. 5.00 ml of 1000 ppm stock solution was pipette into 50 ml volumetric flask and
diluted with deionized water until the mark.The solution was labelled as
‘100ppm’.
2. By used the 100 ppm solution and a 50 ml volumetric flask,a series of standard
solutions have been prepared by having the following concentrations:
1ppm,3ppm,5ppm,7ppm,9ppm
3. The unknown solutions was obtained.
4. The absorbance of the standard solutions in (2) were measured,followed by the
unknown.

Operation of the AAS

Instrument:Perkin Elemer AAnalyst 700
Safety infromation
1. Do not leave flammable/combustible material near the AA!!
2. Do not let acetylene tank level drop below 70 psi!!
3. Do not stare into the lamp!!

Igniting and optimizing the flame(air/acetylene operation)

1. The burner height was adjusted by turning the horizontal adjustment knob until the
light beam(which can be seen by placing a piece of white paper perpendicular to the
burner head) is centered over the burner slot.
2. The vertical positioning of the burner head was adjusted by routing the knob until
the light is near but not hitting the top of the burner head.
3. The acetylene tank was opened and the flow was checked from 85-100kpa.
4. The air valve(on the wall) was opened and the flow was checked from 50-65kpa.
5. The oxidant switch was turn on to Air.
6. The ignite button was pressed.
7. The blank(water) were aspirate for 60-90 seconds.Press [A/Z].
8. A mid-concentration standard was aspirated and the horizontal and vertical adjusts
were rotated to obtain maximum absorbance.
9. A blank was aspirated and the aspiration hose was leave in the water or blank
unless running samples.

Measurement of atomic absorbance

1. A blank was aspirated and pressed [Cont],[A/Z].
2. The standards was aspirated and the absorbance for each one was recorded.
3. The samples was aspirated and the absorbance for each one was recorded.

Shut down procedure

1. The water was aspirated for a few minutes to clean the burner head.
2. The gas control switch was turned on the Pneumatics Control Panel to off.
3. All gas source valves was closed.
4. The gas control switch was turned to Air to allow the gasses to bleed.Then the gas
control switch was turned to Off.
5. The instrument was turned Off.

How to Run the AAS

1. The air compressor,stock cock air,acetylene regulator and acetylene tank was
opened.
2. The compressed air between 5-6 kg/cm3 and the acetylene pressure is 100 kpa.
3. The exhaust fan and isolating switch was been switch on.
4. Make sure the aspiration hose is in the water or blank unless running samples.
5. The instrument and computer was been switch on.
6. Double click at WinLab 32;wait until the calibrating equipment is ready.
7. To create your method,click file→new→method→starting condition:Element Ca.
8. Method Editor:untitled (Type in the Date)
Method description :To determine the concentration of Ca
Calibration equation:linear through zero
Change unit(for standards and unknown)
9. Standard concentration
Blank:DI water
Standard: Std 1,Std 2,Std 3,Std 4 and Std 5
Concentration : 1ppm,3ppm,5ppm,7ppm,9ppm
10. File→save as→method
Name:
Method:
11. File→new→sample info file→ok
Sample ID:unknown Ca
12. File→save as→method
File name→save
13. Click workspace(Workspace)-highlight whatever is in the box→open→type in
your name.
14. Click burner switch→analyze standard→analyze blank→analyze
sample(unknown).
15. Switch off burner.
16. Click tools→edit calibration
17. To point→click file→active window preview
18. To open the file (for future reference),click
‘file’→open→workspace→Filename→ok→analyze→Recall Calibration.
Note:Aspirate deionised water(DI) between each sample measurement to clean the
nebulizer chamber of the previous solution.

You will see the calibration graph being constructed within the Calibration
window;the correlation should be better than 0.999.Otherwise repeat the dilution
steps for the standards.
RESULTS
Solution Volume of Added Concentration of Absorbance
of Standard,ml added
standard,ppm
Standard 1 0 0 0.0006
Standard 2 5 10 0.0077
Standard 3 10 20 0.0118
Standard 4 15 30 0.0225
Standard 5 20 40 0.0232
Unknown Unknown ? 0.0103
Fig 1.1
1. Calculate the concentration of added standard in ppm.
M1V1=M2V2
Standard 1 : M1(50)=(100)(0)
M1 = 0
Standard 2 : M1(50)=(100)(5)
M1 = 10 ppm
Standard 3 : M1(50)=(100)(10)
M1 = 20 ppm
Standard 4 : M1(50)=(100)(15)
M1 = 30 ppm
Standard 5 : M1(50)=(100)(20)
M1 = 40 ppm
2. Plot standard calibration curve.

Absorbance versus Concentration of standard

0.03
f(x) = 0 x + 0
0.02 R² = 0.95
Absorbance

0.02
0.01
0.01
0
0 5 10 15 20 25 30 35 40
Concentration

3. Find out the concentration of unknown.

Concentration of unknown ,x = ?
When y=0
 y = 0.0006x + 0.0012
0 = 0.0006x + 0.0012
-0.0012=0.0006x
x = -2
x = |-2|
x = 2 ppm
Concentration of unknown = 2 ppm
A.Pre-Laboratory Question
a) Explain how you will dilute a 100ppm stock solution to the following
concentration in a 50 mL flask. Show complete working calculation.
1ppm, 5ppm, and 9ppm
M1V1=M2V2
(1)(50)=(100)(V2)
V2 = 0.5 ml
(5)(50)=(100)(V2)
V2 = 2.5 ml
(9)(50)=(100)(V2)
V2 = 4.5 ml
0.5 ml of 100 ppm stock solution was pipet and diluted it into 50 ml volumetric flask.
2.5 ml of 100 ppm stock solution was pipet and diluted it into 50 ml volumetric flask.
4.5 ml of 100 ppm stock solution was pipet and diluted it into 50 ml volumetric flask.
b ) Sketch and label the following graph. Indicate and explain how you can determine
the concentration of an unknown from the graph.
i. The standard calibration curve absorbance vs. concentration of the standard.

ii ) The standard addition method of absorbance against the concentration of

the standard solution.
B.Post-laboratory Questions
a ) Using any available software, plot a standard calibration curve of
absorbance versus concentration of Ca standard solution.

Solutions Concentration (ppm) Absorbance

Standard 1 1.5 x 10-3 0.215
Standard 2 3.2 x 10-3 0.445
Standard 3 4.4 x 10-3 0.599
Standard 4 6.3 x 10-3 0.856
Standard 5 8.2 x 10-3 1.252

Absorbance vs Concentration of Ca solution

1.4

1.2
f(x) = 0.25 x − 0.07
1 R² = 0.97
Absorbance

0.8

0.6

0.4

0.2

0
0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5
Concentration,ppm (x 10^-3)

b ) In a standard addition method, you will prepare a series of solutions to add

different increments of standard solutions to fixed aliquots of unknown sample
 X (10.0 mL). All solutions were prepared using a 50 mL volumetric flask.
Suppose that the analysis of the standard solution of X gave the following
results:
Solutions Concentration (ppm) Absorbance
Standard 1 0.00 0.201
Standard 2 2.44 0.292
Standard 3 4.88 0.378
Standard 4 7.32 0.467
Standard 5 9.76 0.554
1.Plot the standard Addition graph

Absorbance vs Concentration of Added Standard

0.6
0.5 f(x) = 0.04 x + 0.2
R² = 1
Absorbance

0.4
0.3
0.2
0.1
0
0 2 4 6 8 10 12
Concentration of added standard,ppm
2. Determine the concentration of X (in ppm) in the unknown sample.
Concentration ,x = ?
When y=0
y = 0.0361x + 0.2022
0 = 0.0361x + 0.2022
-0.2022=0.0361x
x = -5.6
x = |-5.6|
x = 5.6 ppm
Concentration of X = 5.6 ppm

C.Complete the table of added volume and concentration of the diluted

standard
 Solution The volume of added The concentration of added
standard, mL standard, ppm
1 0.5 1
2 1.5 3
3 2.5 5
4 3.5 7
5 4.5 9
Fig 1.2

DISCUSSION
In this experiment, atomic absorption spectroscopy (AAS) is one of the
techniques based on the idea that ground state metal absorbs light at a particular
wavelength. In addition, flame atomic absorption is a very precise quantitative
technique and a good qualitative technique as well. This is one of the key reasons why
atomic absorption techniques are most commonly used.

From the table fig 1.1,the concentration of the added standard in ppm can be
calculated by used formula M1V1=M2V2 .From all the calculation have done the
concentration obtained were 0 ppm,10 ppm,20 ppm,30 ppm and 40 ppm.After all the
value of the concentration of added standard obtained,we can plot the calibration
curve.From the calibration curve,we can find the value of unknown concentration
which is 2 ppm.The value of unknown concentration has been calculated by using the
equation from the calibration curve.The R2 value from this graph was 0.9538.The
reading was quite not far from the theoretical value.

CONCLUSION
In short, if we use it which is the absorption, the flame AAS has limitations
depending on the number of atoms in the optical path of the spectrometer of a given
instant. Next, the sample inserted into the flame is resident for only a fleeting moment
in the light path as it propelled up through the flame.

REFERENCES
 https://www.slideshare.net/tejasrigopi/atomic-absorption-
spectrophotometer-38678151
 https://www.slideshare.net/sharmasuriti/atomic-absorption-spectroscopy-
15185397