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This document outlines the course information for an elementary quantitative analysis chemistry course. It includes the following key points:
- The course has 1000 total points divided among exams, a final exam, laboratory work, and a lab notebook. Exams and the final are worth 100-200 points each.
- Required materials include a textbook, lab manual, and bound laboratory notebook.
- The course covers topics like measurement, tools, error, statistics, equilibrium, titrations, and separations through lectures and laboratory experiments.
- The tentative lab schedule lists 15 experiments worth 400 total points to be completed over the semester, scaled from 1100 total experiment points. Good lab techniques and notebook documentation are emphasized.
This document outlines the course information for an elementary quantitative analysis chemistry course. It includes the following key points:
- The course has 1000 total points divided among exams, a final exam, laboratory work, and a lab notebook. Exams and the final are worth 100-200 points each.
- Required materials include a textbook, lab manual, and bound laboratory notebook.
- The course covers topics like measurement, tools, error, statistics, equilibrium, titrations, and separations through lectures and laboratory experiments.
- The tentative lab schedule lists 15 experiments worth 400 total points to be completed over the semester, scaled from 1100 total experiment points. Good lab techniques and notebook documentation are emphasized.
This document outlines the course information for an elementary quantitative analysis chemistry course. It includes the following key points:
- The course has 1000 total points divided among exams, a final exam, laboratory work, and a lab notebook. Exams and the final are worth 100-200 points each.
- Required materials include a textbook, lab manual, and bound laboratory notebook.
- The course covers topics like measurement, tools, error, statistics, equilibrium, titrations, and separations through lectures and laboratory experiments.
- The tentative lab schedule lists 15 experiments worth 400 total points to be completed over the semester, scaled from 1100 total experiment points. Good lab techniques and notebook documentation are emphasized.
CHEM 221 Course Work: Exam 1: 100 pts (Thurs., Sept. 14) Exam 2: 100 pts (Thurs., Oct. 26) Exam 3: 100 pts (Tues., Nov. 21) Final: 200 pts (10am-12pm, Monday, Dec. 11) Laboratory: 400 pts (due at end of each lab) Lab Notebook: 100 pts (due at end of semester) Total: 1000 pts Required Items:
(i) Text: "Quantitative Analysis" 7/e Daniel C. Harris, Freeman & Co., New York (ii) Lab Manual: "Laboratory Manual for Quantitative Chemical Analysis", J.D.Carr (2005) (iii) Laboratory Notebook: bound (not spiral), use one with grids instead of lined pages for graphs. (iv) Padlock for lab station and lab deposit card Homework problem sets will not be collected or graded, but will aid your preparation for the exams. COURSE OUTLINE Lecture Topics Date Chapter Topic Problems Aug 22 Chap 0 & 1 Measurement 0-5,6 & 1-5,7,22,24,26 Aug 24 Chap 2 & 3 Tools 2-D,10,12,15, & 3-A,5,9,11 Aug 29 Chap 3 Error 3-12,13,15,18,21,23 Aug 31 Chap 27 Gravimetry 27-2,3,7,14,18,25,26 Sept 5 Chap 4 Statistics 4-A,B,2,3,6 Sept 7 Chap 4 Statistics (cont) 4-9,11,13,14,15,18,22 Sept 12 Chap 5 Calibration 5-A,B,C,22,23 Sept 14 EXAM 1 Sept 19 Chap 6 Equilibrium (Intro) 6-A,B,G,I,K,1,2,3,5,13 Sept 21 Chap 6 Equilibrium (cont) 6-16,21,37,40,54 Sept 26 Chap 7 Titrations 7-A,B,D,1,2,4,8,11,13 Sept 28 Chap 8 Activity 8-A,C,1,4,8,14 Oct 3 Chap 8 Equilibrium (systematic) 8-F,G, H,10,16 Oct 5 Chap 8 Equilibrium (more) 8-18,8-21,8-23 Oct 10 Chap 8 Equilibrium (even more) 8-26, 28 Oct 12 Chap 9 Monoprotic acid/base 9-B,C,G,H,4,6,10,13,19 Oct 16-17 Fall Break Oct 19 Chap 9 Monoprotic (again) 9-24,26,27,29,30,36,37 Oct 24 Chap 10 Polyprotic acid/base 10-A,1,2,4,7,9,16,23,29,31,33,38 Oct 26 EXAM 2 Oct 31 Chap 11 Acid/base Titrations 11-A,B,F,G,I,3,5,6,7,13,16 Nov 2 Chap 11 Acid/base Titrations (cont) 11-23,27,34,36,45,46,54,64 Nov 7 Chap 12 EDTA Titrations 12-B,2,4,5,6,13,22,28 Nov 9 Chap 14 Electrochemistry 14-B,D,I,2,3,15,18,25,41 Nov 14 Chap 15 Potentiometry 15-E,6,7,8,10,13,17,23,24 Nov 16 Chap 16 Redox Titrations 16-A,C,1,2,7,14,15,16,24 Nov 21 EXAM 3 Nov 22-24 Thanksgiving Nov 28 Chap 18 Spectrophotometry 18-A,C,D,1,6,8,16,18,19 Nov 30 Chap 23 Separations 23-B,1,2,3,11,29 Dec 5 Chap 23 Separations Dec 7 Chap 24 Gas Chromatography 24-A,B,C Dec 11 FINAL EXAM 10:00-12:00 Date Experiment Value Aug 21-25 Check-in, Safety, Introduction to Analytical Chemistry 0 Aug 28-Sep 1 Statistics (Exp 2) 50 Sep 5-8 Gravimetric Aluminum (Exp 3) 150 Sep 11-15 Gravimetric Aluminum (cont) Sep 18-22 Volumetric Soda Ash (Exp 4) 200 Sep 25-29 Volumetric Soda Ash (cont) Oct 2 6 Titration of Weak Acid & pK Determination (Exp 5) 100 Oct 9-13 Complexometric Titration for Water Hardness (Exp 6) 100 Oct 18-24 Potentiometric Titration of Iron (Exp 7 ) 100 Oct 25-31 Coulometric Analysis of Vitamin C (Exp 14 ) 100 Nov 1 7 Spectrophotometric Determination of Chromium and Cobalt (Exp 10 ) 100 Nov 8-14 Spectrophotometric Determination of Iron (Exp 11 ) 100 Nov 15-21 Gas chromatography of Aromatic Hydrocarbons (Exp 15 ) 100 Nov 27-Dec 1 Lab Make-up Dec 5-8 Check out of lab TOTAL 1100 Tentative Lab Schedule Due to equipment limitations, experiments # 7, 10, 11, 14 & 15 will be taken in different order by portions of the students. NOTE: Students having a Monday lab should make up Sept 4 lab on Sept 8 (Friday) Scaled to 400 for final grade COURSE OUTLINE Lectures:
ALL lecture notes are available online (http://bionmr-c1.unl.edu/) before the scheduled class as a PowerPoint file.
!!!!The Lectures Notes Are Not Meant To Replace Attending Class!!!!! Laboratory:
50% of your grade in CHEM 221 is based on your laboratory effort. You will be furnished samples whose composition is unknown to you. You will be asked to determine how much of a given analyte is present. You will be graded on how well you agree with the correct answer. You will also be graded on how well you keep and maintain your lab notebook.
Good Lab Practice and Techniques are Essential Lab Notebook Techniques The Lab Notebook Must: State what was done. State what was observed Be understandable to someone else
Include Complete Description of Experiment: Purpose Methods Results Conclusions
Include Balanced Chemical Equations for Every Reaction Used
Paste Hardcopies of Important Data in Notebook
Include locations Where other Data is stored (computer files)
Notebooks are Legal Documents and Routinely Used for Patent Litigation
Laboratory Notebook should be bound (not spiral), use one with grids instead of lined pages for graphs. Lab Notebook Techniques This Notebook Page Has Precise Description with Adequate Detail This Notebook Page is incomplete and a Useless Document. Limited Detail. How to Read and Use a Buret When reading a buret, it is important that your line of sight be in a direction perpendicular to the buret column. All buret reading should be done using a buret card. How to Read and Use a Buret A constant dark reflection against a white background enables higher precision in determining relative titrant volumes. Read volume associated with bottom of meniscus.
A 50 mL buret can be read to 0.01 ml. Upper limit of the black streak ought to be placed just under the meniscus, so that the bottom of the meniscus can be seen distinctly against a narrow zone of white. How to Read and Use a Buret A bubble in the nozzle of a buret will produce an inaccurate volume reading if the bubble escapes during a titration The quickest way to get rid of bubbles is to fill the buret with titrant and open the valve.
Some bubbles may require light tapping to dislodge them. Microsoft Excel Demo Introduction to Analytical Chemistry CSI: Crime Scene Investigation Identifying an Unknown Is Not As Easy as Portrayed by the CSI TV Show.
Typically Requires More Than One Experiment and > 45 Minutes of Analysis with corresponding high cost (single DNA analysis ~$10,000) Background
1.) Definition:
ANALYTICAL CHEMISTRY: The Science of Chemical Measurements.
2.) Types of Questions Asked in Analytical Chemistry a.) What is in the sample? (qualitative analysis) b.) How much is in the sample? (quantitative analysis)
3.) Techniques used in Analytical Chemistry: a.) Wet Chemical Methods: titrations, color-forming reactions, precipitations, etc. b.) Instrumental Methods: spectrometry, chromatography, etc. Introduction to Analytical Chemistry What is it ? How much is there? How pure is it? What are the impurities? Introduction to Analytical Chemistry The Analytical Process
1.) Formulating the Question:
Translate General Question into Specific Question Is this water safe to Drink? What is the concentration of Arsenic in the water sample?
2.) Selecting Analytical Procedures: a.) Choose procedure to measure Arsenic in water (i) Uncertainty in measurement (ii) Limit of detection (iii) Destroy sample (iv) Availability, time, cost b.) If necessary, develop new procedure
3.) Sampling: a.) Select representative material to analyze (i) dont use the entire sample (ii) consistency in sample collection
4.) Sample Preparation: a.) convert sample into form suitable for chemical analysis (i) Dissolve sample (ii) Concentrate sample
(iii) Remove species that interfere with analysis Introduction to Analytical Chemistry Introduction to Analytical Chemistry The Analytical Process
4.) Sample Preparation: a.) Example: M. Dahan et al., Science (2003) 302:442-445 How do you prepare samples for Drug Discovery? What we want to know: Is the drug active? Does it cure the disease/illness? How is the drug taken? (Pill, injection) How often does the drug need to be taken? Does the drug have side-effects?
How these Questions are Typically Addressed: Treat animal (rat, mice, etc) with drug Monitor drug duration in animal Monitor location of drug accumulation Monitor animal health
How do you treat the animal with the drug? How do you monitor the drug concentration in the Animal? How do you determine the drug location? How do you determine the animals health? Tumor size is measured by fluorescence through the mouse skin using quantum dots as a function drug dosage Introduction to Analytical Chemistry The Analytical Process
4.) Sample Preparation: a.) Example: How do you prepare samples for Drug Discovery? Regulatory Toxicology and Pharmacology 31, S57S62 (2000) Tissue plug from mouse kidney Cross-section of sacrificed mouse showing tissue removal Chromatography indicates presence of drug an metabolites in tissue sample Determine drug quantity and distribution Inject mouse with drug Introduction to Analytical Chemistry The Analytical Process
5.) Analysis: a.) measure concentration of analyte in several identical aliquots (portions) (i) Replicate measurements uncertainty in the analysis Avoid large errors Reliability of measurement (ii) Calibration Curve Measure response for known samples
6.) Report and Interpretation of Results 7.) Drawing Conclusions a) How the Report is used 0 10 20 30 40 50 60 k g / p e r s o n A u s t r i a B e l g i u m C a n a d a C z e c h
R e p u b l i c D e n m a r k F i n l a n d F r a n c e G e r m a n y I s r a e l N o r w a y P o l a n d S l o v a k
R e p u b l i c S p a i n S w e d e n U K R u s s i a Sugar Consumption 1970 1980 1990 Units and Concentrations Units of Measurement
1.) SI Units: a.) international units of measurement (metric units) b.) ALL SI units are based on certain fundamental quantities Quantity Unit (Symbol) Length Meter (m) Mass Kilogram (kg) Time Second (s) Electric current Ampere (A) Temperature Kelvin (K) Luminous intensity Candela (cd) Amount of substance Mole (mol) Plane angle Radian (rad) Solid angle Steradian (sr) To a large extent, analytical chemistry is a science of measurement and measurement implies minimizing errors Units and Concentrations Standards of length were once represented by the distance between two marks on a solid metal bar. Copies of these standards were displayed in public places so that people could check the accuracy of the rules they were using. In 1588, Elizabeth I issued a new standard yard which remained the legal British yard for over 300 years. Standards Of Length (1876) Trafalgar Square Units of Measurement Units and Concentrations Units of Measurement
History of the meter Origins of the meter go back to at least the 18th century Two competing approaches to the definition of a standard unit of length. define the meter as the length of a pendulum having a half-period of one second define the meter as one ten-millionth of the length of the earth's meridian along a quadrant
(1791) French Academy of Sciences chose the meridian force of gravity varies slightly over the surface of the earth, affecting the period of the pendulum. meter equal 10 -7 of the length of the meridian through Paris from pole to the equator. prototype was short by 0.2 millimeters because researchers miscalculated the flattening of the earth due to its rotation.
(1960) used a definition based upon a wavelength of krypton-86 radiation
(1983) meter replaced by the following definition: The meter is the length of the path traveled by light in vacuum during a time interval of 1/299 792 458 of a second.
International Prototype Meter standard bar made of platinum-iridium Units and Concentrations Units of Measurement
The Saga of Claude mile Jean-Baptiste Litre International System of Units uses the character "l" (lower-case L) to denote the metric unit of volume litre (liter). It is often difficult to distinguish between the character "l" and the digit "1" in certain fonts or when handwritten. International System of Units only permits the use of a capital letter when the unit is named after a person.
Kenneth Woolner of the University of Waterloo perpetuated a hoax in the April 1978 issue of CHEM 13 News Woolner created the fictional character of Claude mile Jean-Baptiste Litre with a distinguished scientific career where he purportedly proposed a unit of volume measurement.
since no such person existed for "L", it seemed reasonable that one should be invented. Reg suggested that I should write a "biography" for the April issue of CHEM 13 NEWS, and over the course of an evening (which included, I think I recall, most of a bottle of scotch) we generated much of the substance of an 18th century life, full of drama, revolution and romance. Dr. Woolner , 1988 1 liter Units and Concentrations Units of Measurement
1.) SI Units: d.) To indicate multiples or fractions of units, various prefixes are used Prefix Symbol Factor Mega M 10 6 Kilo k 10 3 Hecto h 10 2 Deca da 10 1 Deci d 10 -1 Centi c 10 -2 Milli m 10 -3 Micro m 10 -6 Nano n 10 -9 Pico p 10 -12 Femto f 10 -15 Atto a 10 -18 Example: 3.2x10 -11 s = 32 x10 -12 s = 32 ps Units and Concentrations Units of Measurement
1.) SI Units: e.) conversions to SI units f.) Liter is commonly used for volume instead of m 3 Quantity Unit Symbol SI equivalent Volume liter L *10 -3 m 3 milliliter mL *10 -6 m 3 Length angstrom *10 -10 m inch In. *0.0254 m Mass pound lb *0.45359237 kg metric ton *1000 kg Force dyne dyn *10 -5 N Pressure bar bar *10 5 Pa atmosphere atm *101325 Pa torr Torr 133.322 Pa pound/in 2 psi 6894.76 Pa Energy erg erg *10 -7 J electron volt eV 1.602176462x10 -19 J calorie, thermochemical cal *4.184 J Calorie (British) Cal *1000 cal = 4.184 kJ British thermal unit Btu 1055.06 J Power horsepower 745.700 W Temperature Centigrade (= Celsius) o C *K - 273.15 Fahrenheit o F *1.8(K 273.15) + 32 Units and Concentrations Units of Measurement
2.) Expressions of Concentration: a.) Molarity (moles/L, or M): (i) Most common unit of concentration Gives number of moles of a substance in 1 liter of the given solvent. Recall: 1 mole (mol) of a substance = 6.022 x 10 23 units (atoms, molecules, ions, etc). Molecular weight (MW): the mass of a substance that contains 1 mole. Example:
Find the concentration in Molarity (M) of 12.00g of benzene (C 6 H 6 ) dissolved up to a total volume of 250.00 ml in hexane.
No. Cs at. wt. C No. Hs at. wt. H 0.2500L ) 78.114g 1mol (12.00g)( Make Sure Units Cancel! Units and Concentrations Units of Measurement
2.) Expressions of Concentration: b.) Formality (F): (i) Concentrations expressed in M describe the actual concentration of a given chemical species in solution.
(ii) Some chemicals when placed in solution will dissociate or converted to multiple forms Example:
(iii) Not convenient to refer to the concentrations of each individual form. (iv) Instead, concentration of total substance originally added to the solution is used. Formal concentration or Formality given in (mol/L) Note: For compounds with a single form in solution, M = F Acetic Acid: Units and Concentrations Units of Measurement
2.) Expressions of Concentration: b.) Percent Composition: (i) Weight Percent (wt/wt or w/w): Concentration expressed in terms of mass of substance versus the total mass of the sample.
(ii) Volume Percent (vol/vol or v/v): Concentration expressed in terms of volume of substance versus the total volume of the sample.
(iii) Weight-Volume Percent (wt/vol or w/v): Concentration expressed in terms of mass of substance versus the total volume of the sample.
) 100 ( tan x sample total or solution total of mass ce subs of mass percent Weight ) 100 ( x sample total or solution total of volume ce tan subs of volume percent Volume ) 100 ( x sample total or solution total of volume ce tan subs of mass percent volume weight Units and Concentrations Units of Measurement
2.) Expressions of Concentration: b.) Percent Composition: (iv) Instead of expressing concentrations as a percentage, express in terms of: parts per thousand (ppt) x10 3 parts per million (ppm) x10 6 Parts per billion (ppb) x10 9
3.) Solution Preparation: a.) Dilution of a Solution:
M c V c = M d V d
where: M c = Molarity of substance in the concentrated solution V c = volume of concentrated solution used M d = desired Molarity of the diluted solution V d = total volume of final diluted solution