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Analytical Chemistry - I
Syllabus
Subject Title

Analytical Chemistry I

Prof. Name

3hrs / week

Myeong Hee Moon

2123 - 5634

Text: Quantitative Chemical Analysis 8th ed. Harris. Must Use English Version Textbook Reference: Analytical Chemistry (Christian) 7th Lecture Fundamentals of Analytical Chemistry (Skoog) 8th Info.
Lecture note can be obtained from homepage http://chem.yonsei.ac.kr/~mhmoon

1st exam: 25% 2nd exam: 25% Final: 25% Attendance Evaluation (including Quiz) 25 %

Total 100 %

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Syllabus
Week 1 2 3 4 5 6 7 8 Days 3. 43.8 3.113.15 CONTENTS
Introduction The Analytical Process/chemical measurements Experimental Error/Statistics

Remark

3.18 3.22 Statistics/Quality Assurance & Calibration 3.253.29 4.14.5 4.84.12 4.154.19 4.224.26
Quality Assurance & Calibration Chemical Equilibrium Activity & Systematic treatment of Equilibrium Monoprotic Acid-Base Equilibria

04.02: 1st exam

Midterm

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Syllabus

9 10 11 12 13 14 15 16

4.295.3 5.65.10

Polyprotic Acid-base Equiilibria Acid-base Titrations 05.7 2nd exam

5.135.17 EDTA Titrations 5.205.24 Advcanced Topics in Equilibrium 5.275.31 Fundamentals of Electrochemistry 6.36.7
Electrodes and Potentiometry

6.106.14 Electrodes and Potentiometry 6.176.21 Final Exam 06.11

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Ch 0. Fundamentals in Analytical Chemistry

Topics :

Stages in Chemical Analysis Concentrations Stoichiometric Calculations Titrations

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Analytical Chemistry Applied to:

Chemistry, Biology Medicine (hospital), Geology (geological survey) Oceanography, Material Science Forensic Science, Archeology Farming, Food Science Environmental Science, etc (Government regulations on pollution)

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ANALYZE ? What is it (chemical elements) ? Qualitative analysis How much is present ? Quantitative analysis Development of New Products ? want to know composition of mixtures or giving possibility of impurities

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0-2. analytical Chemists Job

analyte : the species being measured in a chemical analysis (chemical substance)

Stages in chemical analysis Decide First Level of Results needed. Level of accuracy Economical Aspect

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How much caffeine is in a chocolate bar ?

1. Sampling

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Sample preparation

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Steps in chemical analysis

1. Formulating the question 2. Selecting analytical procedure: literature survey 3. Sampling 4. Sample Preparation : converting sample into a form suitable for chemical analysis - drying, sample weighing, mixing 3. Chemical Analysis 4. Calibration Curves 5. Interpreting the Results 6. Draw conclusions

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Ch 1. Chemical Measurements
1-1 SI Units (Systeme International d'Unites)

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Conversion between Units

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1-2. Chemical Concentrations

1) Molarity (M)
# of moles per a liter of solution moles of solute (1 mole = g/fw) Molarity 1 Liter=103cm3 = 1000cc

molecular weight - for moles formula weight - for electrolytes (since no molecule exists in electrolyte sol.)

2) Molality (m)
# of moles per a kg of solvent. temp. independent

# of moles kg (solvent )

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3) Percent Composition
wt (%) mass of solute 100 mass of total mixtures
volume of solute 100 volume of total solution

vol (%)

4) ppm & ppb

ppm mass of substituent 10 6 mass of sample mass of substituent 10 9 mass of sample

ppb

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1-3. Preparing Solutions

Dilution Mconc Vconc = Mdil Vdil

ex) A solution of ammonia in water is called "ammonium hydroxide" because of the equilibrium : NH3 + H2O NH4+ + OHThe density of concentrated ammonium hydroxide, which contains 28.0 wt% NH3, is 0.899 g/mL. What volume of this reagent should be diluted to make 500 mL of 0.250 M NH3 ? (Ans: 8.45mL)

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1-4. solutions & Stoichiometry

1) Volumetric calculation a A + b B products mol
A

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ex) In acid solution, potassium permanganate reacts with H2O2 to form Mn2+: 5H2O2 + 2 MnO4- + 6 H+ 5O2 + 2Mn2+ + 8 H2O In neutral solution, it reacts with MnSO4 to form MnO2: 3Mn2+ + 2 MnO4- + 4 OH- 5 MnO2 + 2 H2O Calculate the number of milliliters of 0.100 M KMnO4 that will react with 50.0 mL of 0.200 M H2O2 and 50.0 ml of 0.200 M MnSO4.

a mol b

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2) gravimetric calculation Cl2 2 AgCl (s)

mol cl2 =

1 mol AgCl 2

g cl 2

Gravimetric factor

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Additional Exercise in Stoichiometric Calculations

1. A 0.2638-g soda ash sample is analyzed by titrating the sodium carbonate with the standard 0.1288 M hydrochloric acid solution, requiring 38.27 mL. Calculate the percent sodium carbonate in the sample.

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2. A 0.200-g sample of pyrolusite is analyzed for manganese content as follows. Add 50.0 mL of a 0.100 M solution of ferrous ammonium sulfate to reduce the MnO2 to Mn2+. After reduction is complete, the excess ferrous ion is titrated in acid solution with 0.0200 M KMnO4, requiring 15.0 mL. Calculate the percent manganese in the sample as Mn3O4 (only part or none of the manganese may exist in this form, but we can make calculations on the assumption that it does). (Ans: 66.7%)

2 Fe2+ + MnO2 + 4 H+ 2 Fe3+ + Mn2+ + 2 H2O 5 Fe2+ + MnO4- + 8 H+ 5 Fe3+ + Mn2+ + 4 H2O

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1.5 Titrations titration

acid-base redox precipitation Spectrophotometric biochemistry : Addition of titrant to analyte for calculation of conc. Calculate conc. of analyte from how much it is consumed.

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1.5 Titrations
Calculation of analyte conc. from how much titrant is consumed. By HOW to DETECT ? 1. detecting sudden change in V or I 2. color change (indicator) 3. change in Absorbance

* Equivalence Point : ideal, stoichiometric. : occurs when the quantity of titrant added is the exact amount necessary for stoichiometric rxn with analyte.

* End Point : actually observable point. Sudden change in color or voltage.

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1.5 Titrations In case of titration, conc. of titrant should be known first. Is it accurate ? Use primary standard. 99.9 % or better in purity. Stable when dried by heating or vacuum

* In case of titrant which is not primary std. Use standardization titrate a proper primary std with the titrant. Then calculate the conc. of titrant.

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1-6.

Titration Calculations

key step :

molestitrant

molesanalyte

ex) standardization of titrant - analysis of unknown - Determination of Ca content in Urine oxalate 1. Ca+2 + C2O42- Ca(C2O4)H2O (s) 2. precipitate in ice-cold water and wash (to remove free oxalate) then redissolve in acid 3. heat to 600C, and titrate with standardized KMnO4 until purple end.

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1-6.

Titration Calculations

Q1: standardization ? Suppose 0.3562 g Na2C2O4 (fw=134.00) in 250.0 mL flask. Calculate molarity of KMnO4 when 10.0 mL of the sol. consumes 48.36 mL of KMnO4. 5 C2O4-2 + 2 MnO4- + 16 H+ 10 CO2 + 2 Mn+2 + 8 H2O

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Q2: Analysis of unknown. Suppose Ca in 5.00 mL urine is precipitated and it requires 16.17mL of std. MnO4- solution. [Ca+] in urine ???

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Homework
In the Textbook: 1-19, 20, 30, 31, 34, 42, 45

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