CHEM 119-080,081,082 - University of Delaware



CHEM 119-

080 - 086

HONORS

QUANTITATIVE

CHEMISTRY I

DR. MUNSON

FALL, 2002

02F

CHEM 119-080-086

HONORS QUANTITATIVE CHEMISTRY I

Fall, 2002

Text: Daniel. C. Harris, Quantitative Chemical Analysis, 6th Ed.,

W. H. Freeman & Co.

Chapters: 0 – 10, 12, 27

Lecture: CHEM 120-080 9:30 – 10:45 TR Lecture 210 BRL

CHEM 120-081 11:00 – 12:15 TR Lecture 210 BRL

Laboratory: CHEM 120-082 3:35 - 6:35 W Lab 006 QDH

CHEM 120-083 7:00 -10:00 W Lab 006 QDH

CHEM 120-084 12:30 – 3:30 R Lab 006 QDH

CHEM 120-085 3:30 – 6:30 R Lab 006 QDH

CHEM 120-086 7:00 – 10:00 R Lab 006 QDH

Lab Lecture:

Theory of Analytical Chemistry

Quizzes during lab lecture

Possible small group homework problems

Previous quizzes, final exams, and solutions are included in notes. Work to numerical answer. Calculator use is essential.

Brief Discussions of lab experiments

The lab experiments will generally be discussed in class on Tuesday before the lab experiment begins on Wednesday. Read each experiment before then and be prepared to discuss the experiment in class.

Laboratory:

Attend your regular lab section. No changes in lab sections may be made without permission.

Labs can be done in the allotted time and may not require the entire period. You may bring and study other work in lab. You may come and go during lab periods. If you arrive late, do not expect the Lab Instructor to remain late because you have not completed the experiment. The lab sections are tightly scheduled. You may not routinely remain after your laboratory period is completed.

The labs may be open on Friday afternoons or Saturday mornings for catch up, make up, and re-doing experiments. If space is available (and with permission) you may work in another other lab period.

You may not work in lab without supervision. Reasonable care must be exercised in performing all of the experiments in the laboratory.

You must wear safety goggles in the laboratory at all times when anyone is doing any experiment.

No additional experiments may be done without Munson's permission.

No equipment or chemicals may be removed from the lab.

Notebook:

You are to keep a NEAT, WELL-ORGANIZED, BOUND LABORATORY NOTEBOOK. The introduction and detailed procedure for each experiment must be written in the notebook PRIOR TO the laboratory session and will be checked by the Laboratory Instructor. The procedure should be sufficiently detailed that you can follow it to do the experiment. You will use YOUR written procedure and not my lab write-up in lab. Notebooks are to be kept current and experiments are to be signed weekly by the Laboratory Instructor. Everything should be written in ink.

Laboratory grading:

Both the average value and the best value will be graded. Each result will be graded on a scale of 2.5 - 5, based on the relative error of your analysis, (Ri, compared with the historical average value of the relative standard error for that experiment, (R(avg). A grade will also be given for the precision of your results, also based on a comparison with results from students in previous years.

Laboratory results are to be reported to bmunson@udel.edu, no later than 7:00 pm on the designated days.

A deduction of 0.1 point will be made for each day (or fraction thereof) late.

A deduction of 0.1 point will be made if the unknown number or other essential datum is missing and the results can be graded.

A deduction of 0.3 point will be made for calculational errors.

A deduction of 0.5 point will be made if the required number of results is not reported. One value receives only one grade (5.0 max).

Accuracy

|( (Ri/(R(avg) |Grade |( (Ri/(R(avg) |Grade |

|0.10 |5.0 |0.80 |3.8 |

|0.15 |4.9 |0.87 |3.7 |

|0.20 |4.8 |0.94 |3.6 |

|0.23 |4.7 |1.00 |3.5 |

|0.27 |4.6 |1.25 |3.4 |

|0.30 |4.5 |1.50 |3.3 |

|0.35 |4.4 |1.70 |3.2 |

|0.40 |4.3 |1.90 |3.1 |

|0.47 |4.2 |2.00 |3.0 |

|0.54 |4.1 |2.50 |2.9 |

|0.60 |4.0 |3.00 |2.8 |

|0.70 |3.9 |>3.00 |2.5 |

Precision Grade

(Ri/(R(avg) ( 0.50 2.0

0.50 < (Ri/(R(avg) ( 0.80 1.8

0.80 < (Ri/(R(avg) ( 1.00 1.5

1.00 < (Ri/(R(avg) ( 1.30 1.3

1.30 < (Ri/(R(avg) ( 1.50 1.0

1.50 < (Ri/(R(avg) ( 1.80 0.8

1.80 < (Ri/(R(avg) ( 2.00 0.5

2.00 < (Ri/(R(avg) ( 2.50 0.3

(Ri/(R(avg) > 2.50 0.0

Repeat Work:

You may repeat a laboratory experiment once and submit for a grade. The higher of the two grades will be recorded.

Make-up quizzes will be available. The higher of the two grades will be recorded.

The grading in this course is the following

Laboratory 60 %

Experiments 50 %

Notebook 10 %

Lecture 40 %

Quizzes/Homework 20 %

Final Exam 20 %

The grading range is the following:

A ( 85

A- = 82 - 84

B+ = 78 - 81

B = 74 - 77

B- = 70 - 73

C+ = 65 - 69

C = 60 - 64

C- = 55 - 59

D+ = 50 - 54

D = 45 - 49

D- = 40 - 44

LAB POLICIES

CHEM119 Honors

1. Lab Notebooks

a. The Laboratory Instructor will check and sign your notebook each day at the beginning and at the end of the laboratory period.

b. Notebooks will be collected and graded during the semester and at the end of the term.

c. Notebooks are to be kept current.

d. Details of the experiment should be written in the notebook before beginning each experiment: Title, Purpose or Introduction, and enough of the procedures that you can do the experiment from the directions written in your notebook. Do not bring the written handout material from the notes to the lab with you.

e. Do not write data on the left hand page and then copy neatly on the right hand page. You should have your notebook sufficiently well organized that you have places on the right hand side to record all of the data in a neat and clearly legible fashion.

f. A neat, well-organized, and accurate notebook is beneficial to your grade (10%). The requirements of (d) and (e) above ensure that you know what you are doing when you begin each experiment.

g. Notebooks are to be kept in ink.

2. Analytical Balances

a. The balances must be clean and have readings removed and the doors closed when you have finished a weighing.

b. Hot materials should not be weighed on the balance: reliable weights cannot be achieved.

c. Do not weigh anything that has water on the outside of the container. Wet containers lose water rapidly and will not give accurate weights. Water also corrodes the balance pan.

d. Do not weigh any solid by transferring the sample to weighing paper on the balance pan. Weigh by difference and do all of your sample transfers outside the balance. If you spill any material on the balance table, clean up your mess!

e. The balance doors must be closed to obtain reliable results.

f. You should use the same balance for replicate and differential weighings in an experiment. You may use different balances for different experiments.

3. Unknowns

a. Record your unknown number! It is your responsibility to record and report your unknown number.

b. Remove the label with the unknown number and paste it on the first page of the experiment.

c. Return sample vials as soon as possible -- cleaned and with labels removed. It is not necessary to keep each unknown for the entire semester, just in case you decide to do another analysis.

d. If you dry the unknown in the oven prior to an experiment, put the unknown in a clearly marked small beaker (your name) to prevent spillage and confusion about samples.

e. Do not put the plastic cap in the oven.

4. Lab up-keep

a. Burets are to be rinsed with distilled water and returned at the end of each lab period.

b. Return glassware and equipment to the appropriate places.

c. Broken glassware should be reported to the Lab Instructor and put into the broken glass container.

d. We have boxes for each section that can also be used to store samples.

e. You are responsible for keeping your work area clean! Nothing is to be left on the bench tops

5. Other equipment

a. The pH meters are rugged, but should be handled with reasonable care. They are expensive.

b. The pH electrodes are not rugged, but fragile. Care should be taken to prevent anything from hitting the bottom surface of the electrode. The pH electrodes cost approximately $75 each. Rinse with distilled water. Don’t blot dry.

c. The pH electrodes should be immersed in distilled water when not in use. If they dry, they are ruined. The electrodes must be stored vertically with the right side up so that the tips are always under water.

d. The pH meters should be turned off and/or unplugged overnight. Leave them on “Stand by” for the next lab period during the day.

e. The spectrophotometers are rugged, but should be handled with reasonable care. They are expensive.

f. Keep the pair of cells with each spectrophotometer. The cells (test tubes) are not identical.

g. The laptop computers and the LabWorks stations are very expensive. Put them in plastic supports to keep them off the bench top in case solutions are spilled. Water (or acid or base) is not good for electronic equipment. Return the computer and the LabWorks station to the cabinet when you finish the experiment.

6. Safety

a. Goggles must be worn in the lab at all times when anyone is doing an experiment.

b. Shorts and sandals are not allowed. Bare feet in a chemistry lab are not allowed and demonstrate suicidal tendencies.

c. Report all spills and breakage to the Lab Instructor.

d. Report all accidents to the Lab Instructor immediately.

e. Laboratory Notebooks

CHEM 119 Honors

All data are to be recorded in the notebook during the laboratory period. Do not record data on separate pieces of paper and transfer them to your notebook later. Do not record data on the left hand page and transfer them to the right hand page.

Leave an extra few pages at the end of each experiment for additional information and corrections, or perhaps a re-done experiment.

Mistakes should be crossed out with one line only. Do not remove any pages from the lab notebook. Everything should be written in ink.

The organized and neatly written lab write-up goes on the right hand page. The left-hand page is for scrap and preliminary calculations. Nothing on the left-hand pages will be looked at or graded by the lab instructor, but very little should be written on the left-hand pages.

Set up a Table of Contents for the experiments.

All pages in the lab notebook should be numbered and the numbers along with the title of the experiment should appear in the Table of Contents.

The following should appear in ink in the bound notebook. The introduction and detailed procedure must be completed before you come to lab. You will use this written procedure in lab.

I. Heading

A. Title of experiment

B. Dates experiment was performed

II. Purpose or Introduction

A. A brief statement of what the experiment demonstrates

B. Do not restate title

C. Don't just copy from the lab handout

III. Experimental Section

A. Procedure

1. The procedure should be described in sufficient detail that you can follow it.

2. It is not necessary to copy the entire laboratory write up from the bound notes here.

B. Observations

1. Report data in tabular form.

2. Show balanced chemical equations.

3. Report any observable occurrences in the experiment (color changes, precipitation, gas evolution, etc.)

C. Calculations

1. All calculations may be included in this section, but at least one sample calculation of each type must be shown.

2. Include all units, with some regard to significant figures or relative accuracy.

3. Calculate the average value, absolute and relative standard deviations for each experiment.

D. Results

1. Report results from the calculations in tabular form.

2. Units must be given.

3. Some regard should be given for relative accuracy or significant digits in the calculations.

4. Always report the average value, the standard deviation, and the relative standard deviation for each set of results.

IV. Conclusions

A. A short paragraph describing likely sources of error should be included.

B. Weighing errors, misreading digits, balance inaccuracy, etc. should be included only if you believe that they are applicable to your work.

C. Include a short paragraph of general conclusions and comments

CHEM 119 H

Quantitative Chemistry

Course Outline

I. Introduction

A. Gravimetric vs Volumetric Analysis

B. Quantitative (~99.9 % Complete) Reactions

C. Concentration Units

D. Stoichiometric Calculations

II. Statistical Analysis of Data

A. Significant Figures and Relative Accuracy

B. Error or Uncertainty in Measurements

C. Mean, Deviation, Confidence Interval

D. Distribution Plots

E. Are Two Values Different?

F. Rejection of Data

G. Propagation of Uncertainty

III. Acids and Bases

A. Weak Mono-protic Acids

1. Standard Approximations

2. Rigorous Treatment

B. Conjugate Acids and Bases: KA, KW, KB

C. Weak Bases

1. Standard Approximations

2. Rigorous Treatment

IV. Buffers and Acid/Base Titrations

A. Standard Approximations

B. Rigorous Treatment

C. Titration Curves

D. Speciation

V. Gravimetric Analysis

A. Calculations

B. Precipitation and Properties of Precipitates

C. Thermogravimetric Analysis

D. Common Precipitating Agents

VI. Solubility of Precipitates

A. Ideal Solubility and KSP

B. Common Ion Effect

C. Effect of pH

D. Activity Coefficients

E. Complexation

F. Titration Curves

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