Chem 26 3rd LE Notes

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    Chem 26 Notes

    UPDShould only be a supplement to discussions

    Table of Contents*

    Part 2 Introduction to nalytical

    Chemistry

    !" Introduction

    !#" Stoichiometry!$" %olumetric nalysis

    !#" Introduction

    !2" cid&$ase Titration

    !'" Precipitation Titration

    !(" Comple)ometric Titration!" +edo) Titration

    !C" Introduction to Potentiometry

    !#" ,eneral Principles

    !2" +eference -lectrode

    !'" Indicator -lectrode!D" Introduction to bsorption

    Spectroscopy

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    !#" Interaction of +adiation and

    .atter

    !2" +adiation bsorption!'" Instrumentation

    !-" Introduction to Separation

    Techni/ues

    !#" Separation by -)traction

    !2" Chromato0raphic Separation!1" -/uations

    *Ctrl 3 1 the roman numeral to s4ip to

    that part5 -) !$5'"7

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    !5#" Stoichiometry

    Stoichiometry

    brance regarding quantities

    quantitative relationship of reactacts and products in reactions

    mole/mass relationship in chemical reactions

    Mole

    Avogadro (6.0 ! "0#$

    number of atoms% molecules% ions% etc in a given gram

    &ravimetric Analysis

    deals 'ith mass

    compared 'ith olumetric

    analyte

    converted to insoluble ppt

    isolated% and then 'eighed

    used in ppt method

    based on chemically related composition

    Steps

    )onvert

    *solate

    +eigh

    , analyte

    *f analyte is not precipitate

    but chemically related

    mass and composition of related to analyte can lead to analyte

    -!ample 'ould be a roc sample e1

    #(gotten$ e (desired$

    &ravimetric actor% &

    for converting mass parameters

    'here

    n is determined by related/same elements

    -!ample

    Sulfur in S1#2S1

    3

    *ron in e#1

    32e

    1

    #

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    olatili4ation Method

    quantitatively eliminate 'ater

    direct

    'ater collected over soliddessicant

    calculate mass gain

    indirect

    loss mass after being heated calculate mass loss

    Application

    5etermine moisture

    ractice

    correct to a dry basis

    compared to sample as received

    add/remove 'ater to some reproducible level

    -!ample7 "3.89, protein% "0.3, 'ater% etc

    -quation

    'here

    :M is non volatile matter

    roteins is the compound desired

    :ote

    :onvolatile Matter ; 5ry

    +ater ; olatile

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    !$5#" Introduction

    olumetric ac

    for slo' reactions

    use e!cess to speed up reaction

    amount of e!cess used to react 'ith analyte is determined by titration 'ith ndstandardi4ed solution

    5isplacement

    )omple!ometric

    -5

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    !$52" cid&$ase Titration

    Acid2>ase

    :eutrali4ation @eaction

    == 12 1

    fast

    'hich is ideal

    Ktitrant

    ; "/ "!"02"3

    *ndicators

    change in color% etc

    produces observable physical change at/near eq. pt.

    natural or synthetic

    +ea organic acid/base that differs in color from conBugate base/acid

    change color at a certain p

    determine p it changes at

    *deally% C*nD ; C*n2D

    if C*nD 'ere yello' and C*n2D 'ere red% then solution 'ould be orange

    5etermine p of solution

    at equivalence point

    p ; pKa

    ideally% if p ; 8% indicator pKa ; 8

    )olor

    ull acid color ; pKa = "

    ull base color ; pKa ? "

    -!ample

    if Ka; "!"023

    Acid color p ; #

    >ase color p ; 8

    )omplete change in color from # to 8

    p range ; 3 E "

    @eaction should occur bet'een # and 8

    Application

    construct graph

    @egions in )urve

    *nitial oint

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    olume ; 0

    re2equivalence oint

    p determined by !Fs =/12

    olume G -q oint

    -quivalence oint

    p is dissociation of 1

    ost -quivalence

    p determined by !Fs titrant

    olume H -q oint

    +ea >ase ? Strong Acid

    opposite graph of Strong >ase ? +ea Acid

    use Kb

    and related enderson 2 asselbalch equation

    ase 2 Strong Acid

    best change in p at equivalence point steep curve

    if Ka ; "02I

    titrationg is no longer feasible

    high error% curve not steep enough

    "026is the cutoff% though deliado pa rin

    5etermine appropriate indicator

    -asily pinpoint eq pt or p at eq pt

    KBeldahl Method

    determine organic nitrogen

    protein analysis

    fertili4er

    Steps

    Sample (>ound :$

    = )onc S1

    3% J

    :3

    =

    = !Fs Strong Acid

    :#% liberated

    = >ac titrated 'ith standardi4ed base

    Soda Ash

    double indicator

    lie in lab

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    !$5'" Precipitation Titration

    recipitation

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    5)2= )l2 :@

    Ag)l is a coloid% Ag)lO)l2! 5)2

    -nd point is Ag)lOAg=5)2

    :ame

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    !$5(" Comple)ometric Titration

    )omple! ormation

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    !$5" +edo) Titration

    @edo!

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    stronger the e

    ses

    )opper

    ero!ide

    14one

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    !C5#" ,eneral Principles

    otentiometry

    arts

    @eference -lectrode

    -ref

    Salt >ridge

    -B

    Analyte Solution

    *ndicator -lectrode

    -ind

    -quation

    -cell ; -in ? -ref = -B

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    !C52" +eference -lectrode

    @eference -lectrode

    accureately no'n

    independent of concentration

    anode

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    !C5'" Indicator -lectrode

    *ndicator -lectrode

    ighly specific

    potential depends on activity% concentration

    )athode

    )alomel

    S)-

    g/g% )l

    %

    Silver/ Silver )hloride

    responds to change of analyte

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    m; 0.08/n

    *nert

    carbon%etc

    Membrane *ndicators

    &lass

    for p% sensitive

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    !D5#" Interaction of +adiation and

    .atter

    Analytical )hemR

    !D52" +adiation bsorption

    Analytical )hemR

    !D5'" Instrumentation

    Analytical )hemR

    !-5#" Separation by -)traction

    Analytical )hemR

    !-52" Chromato0raphic Separation

    Analytical )hemR

    !1" -/uations

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    KSev