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    CHM260 Basic Instrumental Analysis Laboratory Summary Written

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    1. The document describes a laboratory experiment to determine the concentration of calcium (Ca) in an unknown solution using atomic absorption spectroscopy (AAS). Standard solutions of known Ca concentrations were prepared and their absorbances measured. 2. A calibration curve of absorbance versus standard concentration was plotted, showing a linear relationship with R2 of 0.95. The unknown sample's absorbance of 0.0103 corresponded to a Ca concentration of 2 ppm based on the calibration curve. 3. The standard addition method involves preparing solutions by adding known increments of standard to a fixed aliquot of sample and measuring absorbances. This allows determining the sample's initial concentration.

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    CHM260 Basic Instrumental Analysis Laboratory Summary Written

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    105 views12 pages
    1. The document describes a laboratory experiment to determine the concentration of calcium (Ca) in an unknown solution using atomic absorption spectroscopy (AAS). Standard solutions of known Ca concentrations were prepared and their absorbances measured. 2. A calibration curve of absorbance versus standard concentration was plotted, showing a linear relationship with R2 of 0.95. The unknown sample's absorbance of 0.0103 corresponded to a Ca concentration of 2 ppm based on the calibration curve. 3. The standard addition method involves preparing solutions by adding known increments of standard to a fixed aliquot of sample and measuring absorbances. This allows determining the sample's initial concentration.

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    1. The document describes a laboratory experiment to determine the concentration of calcium (Ca) in an unknown solution using atomic absorption spectroscopy (AAS). Standard solutions of known Ca concentrations were prepared and their absorbances measured. 2. A calibration curve of absorbance versus standard concentration was plotted, showing a linear relationship with R2 of 0.95. The unknown sample's absorbance of 0.0103 corresponded to a Ca concentration of 2 ppm based on the calibration curve. 3. The standard addition method involves preparing solutions by adding known increments of standard to a fixed aliquot of sample and measuring absorbances. This allows determining the sample's initial concentration.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    105 views12 pages

    CHM260 Basic Instrumental Analysis Laboratory Summary Written

    Uploaded by

    Cassy
    1. The document describes a laboratory experiment to determine the concentration of calcium (Ca) in an unknown solution using atomic absorption spectroscopy (AAS). Standard solutions of known Ca concentrations were prepared and their absorbances measured. 2. A calibration curve of absorbance versus standard concentration was plotted, showing a linear relationship with R2 of 0.95. The unknown sample's absorbance of 0.0103 corresponded to a Ca concentration of 2 ppm based on the calibration curve. 3. The standard addition method involves preparing solutions by adding known increments of standard to a fixed aliquot of sample and measuring absorbances. This allows determining the sample's initial concentration.

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    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

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