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    Introduction To Analytical Chem

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    - Analytical chemistry examines the composition of matter and determines the elements, molecules, ions, atoms or groups that make up a substance and in what proportions. - It uses quantitative measurement and analysis to obtain this information. Common quantitative analysis methods include gravimetric analysis, volumetric analysis, electroanalytical methods, spectrophotometric methods, and chromatographic methods. - A typical quantitative analysis involves selecting an appropriate method, taking a representative sample, preparing and processing the sample, measuring some property of the analyte, calculating results while accounting for errors and interferences, and evaluating the reliability of the results.

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    Introduction To Analytical Chem

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    Alex
    42 views25 pages
    - Analytical chemistry examines the composition of matter and determines the elements, molecules, ions, atoms or groups that make up a substance and in what proportions. - It uses quantitative measurement and analysis to obtain this information. Common quantitative analysis methods include gravimetric analysis, volumetric analysis, electroanalytical methods, spectrophotometric methods, and chromatographic methods. - A typical quantitative analysis involves selecting an appropriate method, taking a representative sample, preparing and processing the sample, measuring some property of the analyte, calculating results while accounting for errors and interferences, and evaluating the reliability of the results.

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    Analytical Chemistry

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    Introduction to Analytical Chem

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    - Analytical chemistry examines the composition of matter and determines the elements, molecules, ions, atoms or groups that make up a substance and in what proportions. - It uses quantitative measurement and analysis to obtain this information. Common quantitative analysis methods include gravimetric analysis, volumetric analysis, electroanalytical methods, spectrophotometric methods, and chromatographic methods. - A typical quantitative analysis involves selecting an appropriate method, taking a representative sample, preparing and processing the sample, measuring some property of the analyte, calculating results while accounting for errors and interferences, and evaluating the reliability of the results.

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    42 views25 pages

    Introduction To Analytical Chem

    Uploaded by

    Alex
    - Analytical chemistry examines the composition of matter and determines the elements, molecules, ions, atoms or groups that make up a substance and in what proportions. - It uses quantitative measurement and analysis to obtain this information. Common quantitative analysis methods include gravimetric analysis, volumetric analysis, electroanalytical methods, spectrophotometric methods, and chromatographic methods. - A typical quantitative analysis involves selecting an appropriate method, taking a representative sample, preparing and processing the sample, measuring some property of the analyte, calculating results while accounting for errors and interferences, and evaluating the reliability of the results.

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    of 25

    KIM2301

    Analytical Chemistry
    Assoc. Prof. Dr. Şule DİNÇ ZOR
    Analytical Chemistry
    Analytical chemistry is a branch of chemistry that examines the
    composition of matter from which components and in what
    proportions. In short, it is the science that provides explanation of the
    structure of matter.
    Explanation can be the knowledge of the elements, molecules, ions,
    atoms or groups in the substance.

    Analytical chemistry is a measurement science consisting of a set of


    powerful ideas and methods that are useful in all fields of science,
    engineering, and medicine.

    Analytical chemistry is related with all sciences.

    Biology, medicine, physics, agriculture, engineering, environmental


    science, material science, geology, social sciences, space science
    • Qualitative Analysis is performed to find the answer of the question; What does it
    contain?

    • Quantitative Analysis is done to find the answer of the question; What is the
    concentration of XX?

    Quantitative Analysis Methods


    1- Gravimetric Analysis: It is a method based on the formation of a hardly soluble
    compound of the desired element, weighing it after necessary procedures, and
    calculating the amount of the element.
    Aranan elementin genellikle güç çözünen bir bileşiğinin oluşturulup, gerekli
    işlemlerden sonra tartılıp, elementin miktarının hesaplanmasına dayanan bir
    yöntemdir.

    2-Volumetric Analysis: It is the measurement of the volume of a solution containing


    enough reagent to fully react with the analyte. The equivalance point is found with
    the help of an indicator or potentiometrically.

    Analit ile tamamen reaksiyona girecek yeterli miktarda reaktif içeren bir çözeltinin
    hacminin ölçülmesidir. Ekivalens (dönüm) noktası bir indikatör yardımıyla veya
    potansiyometrik olarak bulunur.
    3-Elektroanalytical Methods: Measure of electrical properties such as
    potential, current, resistance, and quantity of electrical charge.

    4- Spectrophotometric Methods: the interaction between electromagnetic


    radiation and analyte atoms or molecules or the emission of radiation by
    analytes.

    5- Chromatographic methods: Separation method. The components in the


    mixture with a flowing gas or liquid phase (mobile phase) are passed over
    the stationary phase. A distinction is made according to the migration rate
    of the components.
    6- Other methods: It is based on measuring some of its properties such as
    mass/ charge rate (mass spectrophometry), radioactive decay rate, reaction
    heat, reaction rate, thermal conductivity, optically active and refractive
    index
    • A Typical Quantitative Analysis
    Quantitative Analysis Steps
    •Method selection
    •Representative Sampling
    • Preparation of Laboratory Sample
    •Re-Sampling
    •Dissolving Samples
    •Elimination of Disturbing Effects
    •Measurement of Analyte Property
    • Calculation of Results
    • Determining the Reliability of Results
    Selection of a Method
    We should consider;
    • Level of accuracy (Blood lead..)
    • Time (Proper length of time)
    • Money (as cheap as possible)
    • Complexity of the sample
    • Number of samples
    The most suitable methods (what we desire);
    • High accuracy,
    • 0 second,
    • No money
    Accuracy indicates the closeness of the measurement to the true
    or accepted value and is expressed by the error.
    Precision, on the other hand, describes the agreement among
    several results obtained in the same way. We can determine
    precision just by measuring replicate samples. Accuracy is often
    more difficult to determine because the true value is usually
    unknown. An accepted value must be used instead.
    Collection of the Sample
    • Sampling process is very important.
    • Sampling is a the process of collecting a small mass of a material whose
    composition represents the bulk of the material being sampled.
    • Analyte should not be converted to each other in the sampling (As(III), As(V))
    Processing the Sample
    • We have to prepare sample before analysis
    • Solid Sample should be grounded (Homogeneity, particle size…).
    • Sample should be protected from humidity (extra weight)
    • Liquid Sample should be protected from evaporation (open vessel)
    • Gas Sample should be protected in closed vessel to eliminate the contamination by
    atmospheric gases.
    • CONTAMINATION!!!!
    • Chemical analysis should be performed on replicate samples (same amount….)
    • At least three replicates for statistical analysis
    • Accuracy
    • Precision: Standard Deviation (SD), Relative Standard Deviation (RSD)
    • Samples should be dissolved in most cases.
    • Selection of solvent is important. Solvent should dissolve sample including analyte
    without conversion.
    • Concentration of analyte is important. It should be in the level that instrument can
    detect.
    • Some preconcentration technique we can need (Adsorption, column, extraction….)
    Elimination of Interferences
    An interference or interferent is a species that cause an error in an analysis by
    enhancing and/or attenuating (make smaller) the quantity being measured.
    Analyte is the species we determine
    Matrix or sample matrix is the collection of all the components present in the
    sample including analyte.
    Interference possibilities;
    • Reaction with analyte (Determination of Analyte with UV-VIS)
    • Absorption of the analyte wavelength (Determination of lead with AAS)
    • Emission of analyte wavelength (Determination of calcium with ICP-OES)
    • Elimination of interference is very important for accuracy of the results
    Calibrating and Measuring Concentration
    • We need calibration in quantitative analysis
    • Calibration is the process to determine the proportionality between
    analyte concentration and a measured quantity.
    • Measurement of the property (absorption, emission, fluorescence…)
    should be proportional to the concentration of analyte.
    CA=kX
    Calibration standards vs responses

    Linear calibration plot;


    Limit of Detection (LOD): Smallest concentration in which you can get response
    Limit of Quantitation (LOQ): Smallest concentration you can quantitatively
    determine
    Limit of Linearity (LOL): The point where the linearity is over
    Calculation of the Results
    Sample amount, final volume….should be considered
    Dilution factor is important.
    Thanks to computers 
    Evaluation of the Results
    Statistical tests (ANOVA, Student T Test….)
    Analysis of Certified or Standard Reference Materials (CRM or SRM)
    Certified Reference Materials are ‘controls’ or standards used to check the quality
    and traceability of products.
    It contains known concentration of analyte.
    Some Important Units of Measurement
    Scientists have adopted to use a standardized system of units known as the
    International System of Units (SI).
    • Mass and Weight
    • Mass is an invariant measure of quantity of
    matter in an object.
    • Weight is the force of attraction between an
    object and its surroundings, principally the earth.
    • Gravitational attraction varies with geographical
    location, so the weight of object depends on
    where you weigh it.
    • w=m x g (m: mass, g: acceleration due to gravity)
    A chemical analysis is always based on the mass so
    that results will not depend on locality.
    The Mole
    The mole (mol) is the SI unit for the amount of a chemical substance.
    It is the amount of the specified substance that contains the same
    number of particles as the number of carbon atoms in exactly 12
    grams of 12C. This important number is the Avogadro’s number (NA:
    6.022x1023)
    A mole of a chemical species is 6.022x1023 atoms, molecules ions,
    electrons, ion pairs, or subatomic particles.

    The molar mass (M) of a substance is the mass in grams of 1 mole of


    that substance. We can calculate molar masses by summing atomic
    masses of all atoms appearing in the chemical formula.

    The number of moles nx of a substance (X) having molar mass Mx

    nx: mx/Mx

    The millimole is 1/1000 of a mole


    Solutions and Their Concentrations
    We use number of methods for expressing concentration.
    Molar Concentration
    Number of moles of solute species that is contained in 1.0 liter of the
    solution.
    Molar concentration: number of moles solute/volume in liters,
    • Cx= Mx= nx / V (mol/L, mol L-1)

    Molar analytical concentration of a solution gives the total number of moles


    of a solute in 1 liter of solution. Solution can be prepared regardless of what
    might happen to solute during the solution process

    Molar equilibrium concentration is the molar concentration of a particular


    species in a solution. We have to know how the solute behaves when it is
    dissolved in solvent.
    Percent Concentration
    There are three common methods regarding the percent
    representation;

    Weight percent (w/w): weight solute/weight solution x 100 %


    This is used to express the concentration of commercial aqueous
    reagents (65% HNO3, 37% HCl)
    Volume percent (v/v): volume solute/volume solution x 100 %
    This is used to specify the concentration of a solution prepared by
    diluting a pure liquid with another liquid (25 % Methanol)
    Weight/volume percent (w/v): weight solute/volume solution x 100 %
    It is used to indicate the composition of dilute aqueous solution
    including solute (3.0 % AgNO3)
    50 % (w/w) NaOH= 76.3 % (w/v) NaOH

    Not: Volume of solvent is not used in all these formulas. We have to


    use volume of solution.
    Parts per Million (ppm), Parts per Billion (ppb) and Part per
    Trillion (ppt)

    It is proper to use ppm, ppb or ppt for very dilute solution


    ppmx = mgx /kgsample ppmx ≠ mgx /Lsample
    ppbx = µgx /kgsample ppbx ≠ µgx /Lsample
    pptx =ngx /kgsample pptx ≠ ngx /Lsample

    Detection limits expressions by ppm, ppb, ppt

    • AAS
    • ICP-MS
    • ICP-OES
    • ICP-MS << ICP-OES ≤ AAS (For the elemental determination).
    p-Functions
    • p-value is the negative logarithm (to the base 10) of the molar
    concentration of that species.
    • Scientist frequently express the concentration of a species in
    terms of its p-function or p-value.
    • pX= -log [X]
    • Best known p-value is pH which is the negative logarithm of
    [H3O+].
    • [H+] or [H3O+]
    Density and Specific Gravity
    Density of a substance is its mass per unit volume
    Specific gravity is the ratio of its mass to the mass of
    an equal volume of water at 4.0 oC.
    In metric system,
    d=m/V (g/mL)
    There is no particular system of units for specific
    gravity. Hence, this is commonly used to describe
    items of commerce
    Since the density of water is approximately 1.00
    g/mL, we can use density and specific gravity
    interchangeably.
    Chemical Stoichiometry
    Stoichiometry is the quantitative relationship among the
    amounts reacting chemical species.
    Number of moles of reactants and products can be expressed by
    Stoichiometry.

    Stoichiometric Calculations
    Example 4-1 (Page 66): Find the number of moles and millimoles of benzoic acid (M: 122.1
    g/mol)that are contained in 2.00 g of the pure acid.

    Example 4-2 (Page 66): What is the mass in grams of Na+ (23 g/mol) in 25.0 gram of Na2SO4 (142
    g/mol).

    Example 4-3 (Page 68): Calculate the molar concentration of ethanol in an aqueous solution that
    contains 2.3 g of C2H5OH (46.07 g/mol) in 3.50 L of solution.
    Example 4.5 (Page 70): Describe the preparation of 2.00 L of 0.108 M BaCl2 from BaCl2.2H2O (244.3
    g/mol).

    Example 4.6. (Page 70): Describe the preparation of 500 mL of 0.074 M Cl- solution from solid
    BaCl2.2H2O (244.3 g/mol).

    Example 4.7. (Page 71): What is the molar concentration of K+ in a solution that contains 63.3 ppm
    of K3Fe(CN)6 (329.3 g/mol)?

    Example 4.8. (page 72): Calculate the p value for each ion in a solution that is 2.00x10-3 M in NaCl
    and 5.4x10-4 M in HCl.

    QUE: In the bottle of HNO3, following information is given;


    d: 1.19 g/mL, 65%, M.W.: 63 g/mol.
    What is the volume of HNO3 we have to take to prepare 120 mM of 250 mL diluted HNO3 solution.

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