Course Syllabus for English-Taught Majors

Analytical Chemistry Laboratory Part ICourse Syllabus

 

Course Code09041007

Course CategoryMajor Basic

MajorsChemistry

SemesterFall

Total Hours72 Hours         Credit2

Lecture Hours72 Hours

InstructorsJilin Yan

Textbooks

Handout by instructor /孙尔康 张剑荣 《分析化学实验》 南京大学出版社 2015 第二版

References

1.  Irene Mueller-Harvey, Richard M Baker, Steve Hill, Chemical Analysis in the Laboratory: A Basic Guide, Royal Society of Chemistry 1st Edition 2002

2. 武汉大学 《分析化学实验-上册》 高等教育出版社 2011年第5

3. Abrams Binyomin Analytical Chemistry Lab Manual Kendall Hunt Publishing; 1 edition , 2011

4. 华中师范大学,东北师范大学,陕西师范大学 《分析化学实验》 高等教育出版社 2015年第四版

5. 金谷 《定量分析化学实验》 中国科学技术大学出版社 2005年第一版

 

Teaching Aim

Quantitative chemical analysis laboratory is the very basic of chemical analysis. This course is designed for professionally oriented students in the majors’ program in chemistry; its aim is to develop competence in areas of quantitative chemical analysis. These topics include both training in the laboratory, and additional expertise interpreting and communicating the data from these experiments to a panel of reviewers. Through this course, the students will obtain related training one basic operations on analytical instruments, how to file out a valid lab report, and this course will help in developing the ability to resolve practical analytical problems. Each session will take approximately four hours, the students are required to finish the lab session and submit the report before leaving the laboratory.

 

Experiment 1: Laboratory glassware: the cleaning     

课时:1周,共4课时

Clean glassware is essential in chemistry. The problem is that the tolerance for impurities varies with the work you are doing, and sometimes a chemist does not know how important clean glassware is to an experiment until it has failed. 

 

Experiment 2: Analytical Balance & Volumetric Glassware    

课时:1周,共4课时

This laboratory session is designed to introduce some of the apparatus and operations required during the lab sessions, including the treatment of data using spreadsheets. While some of the procedures may seem trivial and the results obvious, this is a chance for you to develop good laboratory technique.

 

Experiment 3: Basic operations in volumetric titration

课时:1周,共4课时

In this section, the students will get some basic training on how to use analytical glassware, such as burrets, pipets, for quantitative measurements

1. Practice on basic operations for quantitative analysis

2. Learn the application of indicators

Problems

1. What are the indicators used for the titration? How do the colors change?

2. In order to prepare 1 L 0.1mol L HCl standard solution, how much concentrated HCl should be measured?

 

Experiment 4: Determination of total alkalinity of soda ash

课时:1周,共4课时

A standard HCl solution is prepared and calibrated with Na2CO3 as the primary substance, and it is then applied for the determination of total alkalinity of a soda ash sample through an acid-base titration

1. Learn the molecular formula and chemical properties of primary standard substance sodium carbonate.

2. Learn the process of preparation and calibration of HCl standard solution.

3. Master the titration process, transition range and the indicator selection for titrating of a weak base with a strong acid.

Problems

1. What is the indicators used for this titration?

2. What are the advantages and disadvantages of Na2CO3 and Na2B4O7•10H2O when they are used respectively as the primary standard substances for the calibration of HCl solution?

 

Experiment 5: Determination of nitrogen amount in ammonium sulfate fertilizer

课时:1周,共4课时

Ammonium in the fertilizer is converted to much stronger acid and then titrated with a NaOH standard.

1.Understand the basic principles of the strengthening of a weak acid;

2.Grasp the principle and operation for the determination of nitrogen in ammonia with the formaldehyde method;

3.  Grasp the criteria for choosing an acid-base indicator.

Problems

1.  NH4+ is the conjugate acid of NH3, why it can not be titrated directly with a NaOH standard solution?

2. Can we determine the nitrogen in NH4NO3, NH4Cl or NH4HCO3 thourgh the formaldehyde method mentioned in this experiment?

3.Phenolphthalein is used as indicator in the neutralization of free acid of the formaldehyde, but methyl red is chosen in the neutralization of free acid of (NH4)2SO4, try explain this?

Experiment 6: Analysis of mixed alkali    

课时:1周,共4课时

A stepwise titration is performed with two indicators.

1. Learn the principle of analysis of mixed alkali with dual-indicator method

2.  Learn the application of pH indicators

Problems

If a mixed alkali sample is analyzed with the method here and volumes as following conditions are obtained, tell the components of the samples.

(1) V1>V2>0

(2) V2>V1>0

(3)V1=V20

(4)V1=0, V20

(5)V20, V2=0

 

Experiment 7: Determination of total water hardness

课时:1周,共4课时

An EDTA standard is prepared and calibrated, it is then applied for the determination of the total amount of calcium and magnesium in tap water.

1. Learn the principle and application of complexometric titration.

2. Master the direct titration in complexometric titration.

Problems

1. What kind of indicator should be adopted to calibrate the EDTA used in this lab session? What is the most suitable primary standard substance?

2. Write the calculation formula of total hardness of water expressed by (unit as mg/L), and calculate total hardness of water sample in this experiment.

 

Experiment 8: Sequential titration of bismuth and lead ions

Acidic effect is applied to obtain a selective titration of bismuth and lead respectively.

1. Understand the principle of improving the selectivity of EDTA by regulating the acidity

2. Sequential titration using EDTA

Problems

1.Describe the conditions and the reasons for the color change in the Erlenmeyer flask during the sequential titration of Bi3+ ,Pb2+ 

2. Why hexamethylene tetramine was chosen to adjust the pH to 56 rather than NaOH, NaAc or NH3·H2O?

 

Experiment 9: Determination of the content of hydrogen peroxide

课时:1周,共4课时

A potassium permanganate standard is applied for the titration of hydrogen peroxide under acidic condition.

1.Learn the preparation of KMnO4 solution and the calibration process.

2.Learn the principles and methods of the titration of H2O2 with permanganate.

Problems

1. In the preparation of KMnO4 solution, a microporous glass funnel is applied for filtering step. Can we use a quantitative filter paper instead? and why?

2. What should be paid attention to in the preparation of KMnO4 solution? When calibration of the KMnO4 solution with Na2C2O4, why does the purple color of KMnO4 fade slowly at the initial period, but much faster later until a stable red appears at the end point of titration?

3. Can we use HNO3, HCl or HAc to control acidity in the determination of H2O2 by permanganate titration?

 

Experiment 10: Determination of total iron in iron ore

课时:1周,共4课时

An iron ore sample is dissolved and reduced to Fe2+ with SnCl2 as the reducing agent, a K2Cr2O7 standard solution is then applied for the titration of F2+ for the measurement of iron.

1.Master the preparation and application of K2Cr2O7 standard solution.

2.Learn acid dissolve method of ore sample.

3.Learn the principle and method of determine iron with K2Cr2O7.

4.Learn the mercury-free method for the determination of iron.

5.Learn the mechanism of the sodium diphenylamine sulfonate indicator.

Problems

1.Why K2Cr2O7 can be weighed directly to prepare the solution of accurate concentration?

2.Why should the decomposition of iron ore be performed at low temperature? What will impact on the result if heat it to boiling?

3.What is the condition of reducing Fe3+ with SnCl2? How to control the amount of SnCl2?

4.What is the function of adding H3PO4 during the titration of Fe2+ with the K2Cr2O7 solution?

5.What is the function of methyl orange in this experiment?

 

Experiment 11: Determination of copper content in copper alloys 

课时:1周,共4课时

Copper (II) oxidizes iodide into iodine, and the so-produced iodine is titrated with a sodium thiosulfate standard for an indirect measurement of copper.

1.Master preparation and calibration points of Na2S2O3 solution.

2.Learn the action principle of starch indicator.

3.Learn the principle of indirect iodometric method for the determination of copper.

4.Learn the decomposition of copper alloy samples.

5.Master the operation of iodometry to determine copper.

Problems

1.In the calibration of Na2S2O3 solution, HCl and H2O2 are used to decompose solid copper. What will happen if H2O2 isn't used up during that stepr?

2.What is the primary standard substance used to calibrate Na2S2O3 solution? What is the substance that shows brilliant green at the end point when calibrating Na2S2O3 with K2Cr2O7?

3.Why is NH4HF2 always added in when determining copper by iodimetry? Why NH4SCN (or KSCN) is added in only close to the end point?

 

 

Experiment 12: Determination of Barium content in BaCl2•2H2O

课时:3周,共12课时

Barium is precipitated into BaSO4, and the precipitate is collected and weighed for the measurement of Ba.  

1. Learn the principle and method of determining Ba in BaCl2•2H2O.

2. Master the basic operations as preparation, filtration, washing, ignition and constant weight of crystalline precipitate.

Problems

1.Why should the precipitate reagent for the precipitation of BaSO4 be added dropwize in the hot dilute HCl solution and under constant stirring? What will the result be if too much HCl solution was added?

2.Why precipitate BaSO4 in the hot solution, but filter it after cooling down to room temperature? Why ageing is required for crystalline precipitate?

 

Experiment 13: Determination of calcium oxide in lime stone

课时:2周,共8课时

Calcium is precipitated into calcium oxalate, and the precipitate is then dissolved in acid and measured through a redox titration with a KMnO4 standard solution.

1, Understand the basic principle and basic operations of potassium permanganate method

2, Practice of the operation on titration and gravimetric determination

Problems

1.Can we apply the KMnO4 standard directly onto the filter paper? What would happen if we do so?

2.Why should NH3H2O be slowly introduced to adjust the pH value?

 

Final exam

Standardization of a HCl solution with Na2CO3 as the primary substance.

 

Assessment Methods

Exams (final 40%), In class performance and lab reports (60%)

 

 

                                Made by Jilin Yan

                      

Date 10.28. 2016