Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

Introduction

A PURPORTED DEBATE AMONG MIDDLE AGE PHILOSOPHERS AND THEOLOGIANS REVOLVED AROUND, "HOW MANY ANGELS CAN DANCE ON THE HEAD OF A PIN?"

 

THE OBJECTIVE OF THIS PROJECT WAS MUNDANELY ANALOGOUS: "HOW MANY ACTIVITIES OR EXPERIMENTS RELEVANT TO THE CHEMISTRY CLASSROOM CAN BE ENVISIONED ON THE HEAD OF A STEEL NAIL?

ANSWER MANY MORE THAN ARE INCLUDED HERE!

 

          No matter what conceptual real-life analogies we choose, what mathematics we apply, what media we use, which experiments we routinely conduct, or even what degree of sophistication our approach, as high school chemistry teachers we normally cover the same broad topics of study in our classrooms.

            Why not try a fresh approach to your standard analogies and experiments using

 

Steel

 

an alloy of particular interest to students living in a city that calls its football team the "Steelers" ; a city with an economic and historical development that revolved around this very substance for many years!

 

 

 

 

 

 


 

 


 

Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

Objective

The overall purpose of this set of laboratory activities is to use a specific material, steel, in meaningful high school chemistry experiences. The corrosion of steel is an electrolytic process that can be studied easily within the parameters of a high school chemistry classroom. The experiments described herein provide some very tangible applications of; experimental design, phases of matter, crystal structures, oxidation/reduction reactions, Standard Reduction Potential, electrochemistry, LeChatlier's Principle, G, Free Energy and others as discussed throughout this study.

            How many of theses concepts are drawn upon and taught with the following experiments, depends on the objectives which the teacher desires to fulfill. From the simplest perspective, the following experiment can function as no more than good practice in experimental design; practice observing steel corrosion, hypothesizing as to the underlying factors responsible for corrosion, setting up a multivariable experiment and gathering the data The data is analyzed for evidence of "trends" without interpretation of results in terms of any underlying causal factors.

A more complex treatment of the experiment would require that the student have a good grasp on electrolytic processes and the function of an electrochemical cell; mechanisms by which corrosion of steel occurs. This would enable the student to more effectively identify and "interpret" data trends in light of a known mechanism.

            The most complex treatment of the experiment would include all of the above plus knowledge of the composition of the different steels being used (SAE # 1008, 1045, 4140, 4340) and some knowledge of the various microstructures that may occur in these steels. This would allow for interpretation of data trends in light of the microstructure of the steels involved (how the various alloying elements in the crystal structure or the %C phase mix might possibly interact with the electrolytic mechanism of steel corrosion.)

 

 

 

 

 

 

 

 


 

 

 


 

Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

Background

 

Initial discussion with students will likely indicate that many know steel contains the element iron. Also, from everyday life, many will no doubt be familiar with the "corrosion" of iron appearing as a red, low-density substance commonly called "rust." A few students may even suggest that rust is the compound, iron (III)oxide (under most conditions rust is actually iron(III) hydroxide.) When it comes to hypothesizing what it is that causes steels to rust, a few students should know that moisture definitely plays a part (if they've ever left their bike out in the rain, etc.)

               To hypothesize about corrosion, students must first be familiar with the simplest definition of steel as an iron-based carbon alloy (containing up to approx. 2% carbon.) Let them examine firsthand some partially corroded iron and steel objects; demo objects should be drawn from a variety of environmental conditions (rust on an "indoor" object such as scissors; rust on an object often left "outdoors," such as a garden tool; a picture of cars rusting in a junkyard etc.) After examining the objects, students should at least be able to hypothesize that rust might be related to the environmental conditions surrounding a steel object.

Experimenting with steel requires comprehension of the term alloy. According to the Metals Handbook, 8th ed., published by the American Society for Metals it is," A substance having metallic properties and being composed of two or more chemical elements of which at least one is an elemental metal." Have several examples of alloys available for students to examine, such as a brass ring. Steel is "iron-based" so that is its dominant metal; and carbon up to 2% is the other most common alloying element in steel.

            Do students think that "steel" always means the same substance? Go back to the term "alloy." An alloy is a "mixture" of substances; not a compound! Chemistry students should be able to differentiate a compound from a mixture. Calling on what they know about mixtures

(constituents can be mixed in any proportion, separable by physical means), have them conjecture whether or not all steels are the same (of course, they are not.) There are many types of steel containing different proportions of the alloying elements; that is, steels vary widely in composition.

            For students who have no difficulty with the above ideas, go on and build on their knowledge of mixtures, introducing them to the concept of the "microstructure" of steels. Students should be aware of two mixture types, heterogeneous and homogeneous, from their previous study of the Composition of Matter. They know that a heterogeneous mixture is "multi-phased" and that a homogeneous mixture is termed a "solution" which is the same phase throughout. Do students think these ideas also apply to the mixtures called alloys; particularly the alloy steel? Indeed, they do! Not only do steels vary in chemical composition; the same steel can have either single-phased or multi-phased forms depending on ( among other things) its thermodynamic history. According to Noel F. Kennon in a recent book edited by Leonard E. Samuels called Light Microscopy of Carbon Steels , at normal temperatures many steels are heterogeneous two-phased mixtures of ferrite (iron atoms arranged in a body-centered cubic crystal structure) mixed with cementite ( carbon in the form of the compound, iron carbide, Fe3C). At higher temperatures, the same steel can transform into a homogeneous mixture, that is a solid solution, of carbon atoms dissolved in austenite (iron atoms arranged in a face-centered cubic crystal structure.) (6-9, 29)

After students realize that steels have many different compositions and microstructures, explain that steels can be classified according to their compositions by a Society of American Engineers (SAE) number such as 1008, 1045, etc. If teaching a more advanced course, if enrichment is desired, or if your students can handle the material, at this point the body-centered cubic crystal structure and the face-centered cubic crystal structure can be illustrated with models and associated with the phase of steel to which they apply. (Van Vlack 59 -84)

            Building on these ideas; that steels are alloys containing iron, that iron "corrodes" into iron (III) hydroxide, that steel objects seem to corrode more when moisture (water) is present, and that not all steels are the same, have students "hypothesize" factors they think play a role in the corrosion of steel and to what degree (do some factors have a greater effect on steel corrosion than others?) Have them "brainstorm" an experimental set-up designed to test their ideas about steel corrosion. Any experimental design should include the above ideas. For mainstream chemistry classes, the foregoing ideas will be enough to handle and test. The discussion on steel microstructure and crystal structure should be eliminated.

            Advanced Chemistry Classes and Gifted Chemistry Classes, however, should be required to understand the "mechanism" by which steel corrodes. They should call upon the equations for the corrosion of steel when designing any experiment on corrosion. Activities or discussions on these topics should be conducted in second and third lab sessions or during regular classes.

            "The Selection of Mild Steel for Corrosion Service," (Metals Handbook 1:257 ) states, "the corrosion of iron and steel has become accepted as a phenomenon that is essentially electrolytic, especially where attack depends on the simultaneous presence of moisture and oxygen." This means that for corrosion to occur, moisture (water)containing charged particles, an electrolyte, must be present. Electrons are carried away from the neutral Fe atoms in steel, forming iron (II) ions, Fe2+ to a substance with a higher potential to gain electrons. In a sense, this forms a local "electrochemical cell" on the surface of the steel. (Corrosion in Action 15) Students who understand the function of and the nomenclature associated with the electrochemical cell will have a much better grasp on the corrosion process. Unless students are very comfortable with electrochemistry and the electrochemical cells, it would be good to spend several class periods diagramming electrochemical cells; building several simple cells in the lab. (Petrucci 471 - 490)

            Students must at least know that oxidation, electron loss, occurs at the electrode in a cell called the anode (Fe functions as an anode when it gives up electrons from a steel surface and corrodes.) Reduction ,electron gain, occurs at the electrode in a cell called the cathode and normally O2Ý functions in this capacity on the steel surface. Knowing the process is electrolytic, students hypothesize that water solutions containing ions, such as salt water, will have a greater effect on the speed of corrosion than will pure water. Solution type, as well as steel type, now becomes a factor to be considered in the corrosion experiment.

            Consider the electrochemical equations associated with corrosion. Even in the absence of O2, it has been demonstrated that ferrous metals will go into solution in water until a state of equilibrium is reached according to the following equation

                           Fe   +    2 H2O = Fe2+  + 2OH-         + H2

                          Iron         water  ferrous hydroxide hydrogen gas

                                                       ions     ions

 

The ferrous and hydroxide ions result from the single displacement reaction that reduces H+ in the water to hydrogen gas; which is sometimes "plated out" on the surface of the metal. If the conditions are such that the equilibrium constant for this reaction is low enough and the vapor space small enough, the reaction will stop before there is saturation with respect to ferrous hydroxide. ("The Selection of Mild Steel for Corrosion Service" Metals Handbook 8th 1: 257) Chemistry students should be very familiar with single replacement reactions and recognize the ions involved. (However, be careful here! My students normally learn that Fe does not replace hydrogen ion from water at room temp...and indeed the kinetics are against it...but then it is not customary to use water devoid of oxygen in the high school chemistry lab.)

            The corrosion of steel is an excellent application of LeChatelier's Principle. LeChatelier was a French industrial chemist and professor particularly interested in problems related to metallurgy. His principle states that a system in dynamic equilibrium subjected to a stress will shift in such a way as to remove that stress. (Wilbraham 502) The presence of iron and water will push the reaction to the right (in order to use up the reactants) and enhance corrosion; whereas the excess presence of either product, hydroxide ions, OH -, or H2 gas, should cause the above corrosion reaction to go into reverse, and thus slow down the corrosion. (The reaction shifts left to remove the excess OH- ions or hydrogen gas.) Applying LeChatelier's principle, students can now hypothesize that "basic" conditions around the iron, such as the presence of CaCO3 should retard corrosion. Likewise, if acid is present, the H+ will neutralize the OH- ion, effectively reducing it and driving the reaction to the right; restoring the OH- ion and enhancing corrosion. Hypotheses as to the same concerning basic and acidic solutions should be tested when designing any corrosion experiment.

            If O2 is in the water (as it most always is), then it normally enhances corrosion. Recall, if Fe acts as the "anode," giving up electrons in the local electrochemical cell that enables corrosion, then O2Ý can function as the "cathode," taking on those electrons, because a potential difference exists between them.(Corrosion in Action 20) Oxygen is reduced according to the following equation;O2 + 2H2O + 4e- = 4OH- (Petrucci 484)

 

            Oxygen present in solution also can enhance corrosion in other ways. "Oxygen, if present, reacts with the hydrogen film (that may build up on the steel surface), removes it from the surface of the metal in the formation of water and also reacts with the ferrous ions to form ferric ions in such a concentration as to exceed the solubility product of ferric hydroxide, and hence a precipitate of ferric hydroxide is formed. Both reactions are involved in the corrosion process." ("The Selection of Mild Steel for Corrosion Service" 1:257). An additional equation shows why, as corrosion progresses, the water around the corrosion turns from yellow to orange to red. As mentioned, the O2 goes on to convert the ferrous ions (yellow in solution) to the characteristic ferric ions (orange/red in solution) associated with "rust" :

 4 Fe2+ + O2+ 2H2 O = 4 Fe3+ + 4 OH-  (Metals Handbook 8th 1: 257)

 

Students apply LeChatelier's Principle and postulate that any O2 present in solution will drive the reaction forward, enhancing corrosion. Oxygen level is indeed an important variable in any experiment on the corrosion of steel!

            Finally, good experimental design often incorporates indicators as to the reactions being tested. Evidence that OH- is a product of the reduction of oxygen during corrosion can be tested by the presence of phenolphthalein near the surface of the iron or steel; any place where the reduction of O2 is occurring on the surface of ferrous metals should become "basic" and turn that indicator pink. Likewise, when corrosion initially begins, iron(II) or ferrous ions build up on the surface of the steel where the oxidation of iron atoms occurs; this site should turn the indicator for ferrous ions, hexacyanoferrate(III), blue. If the iron is held in a gel medium, as with the experiments found in Appendix B of this study, these colors develop nicely showing the electrolytic nature of corrosion (Corrosion in Action 17) The following experiment on the corrosion of steel was conducted during the summer months, and should be similar to the experiments generated by students who have undergone the previous discussions and activities. The experiment is best run by making each lab group responsible for setting up and monitoring one set of solutions throughout the course of the experiment. Joint sets of data could be pooled for a final evaluation of experimental results. The experiment can also be subdivided into a series of smaller experiments that limit the number of variables tested simultaneously. THIS EXPERIMENT DEFINITELY LENDS ITSELF TO AN "OPEN-ENDED APPROACH" IN WHICH EACH LAB GROUP RECEIVESÝ 4 TYPES OF STEEL WITH WHICH TO DESIGN THEIR OWN EXPERIMENT TESTING THE VARIABLES THAT AFFECT STEEL CORROSION

 

 

 

 

 


 

 

 

 


 

Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

What will you Need?

 

Materials:

            Steel Samples (cut in rectangular solids 1/2" x 1/2" x 1and 1/2")

            13 samples of Low Carbon Steel SAE# 1008

            13 samples of Medium Carbon Steel SAE# 1045                    

            13 samples of Medium Alloy Steel SAE# 4140

            13 samples of Medium Alloy Steel SAE# 4340

            (Suggestion; Mark each block with Steel SAE# using magic marker)

            13 1000mL beakers

            26 glass rods (cut to fit bottom of above beakers)

            2 Liters Distilled H2O

            2 Liters Saline Solution ( 1M NaCl, .01 M KBr, .01M KI)

            2 Liters .005M H2SO4 (pH =2)

            2 Liters 100ppm CaCO3 solution

            4 wash bottles (one for each solution above)

            4 berol pipets (one for each solution above)

 

 

 

 

 

 

 


 

 

 

 

 


 

Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

Procedures:

 

See Pictures #1 & 2 Appendix A

 

1. Mark 3 beakers "Distilled Water"        (A Freshwater Environment)

Additionally, label the first beaker "Minimum O2", second "Dissolved O2", and a third "Max O2."

 

2. Mark 3 beakers "Saline Solution" (A Marine Environment)

Additionally, label the first beaker "Minimum O2", second "Dissolved O2", and a third "Max O2."

 

3. Mark 3 beakers "H2SO4 solution, pH =2" ( A Heavy Industrial Environment)

Additionally, label the first beaker "Minimum O2", second "Dissolved O2", and a third "Max O2."

 

4. Mark 3 beakers " 100 ppm CaCO3 solution" (A Hard water Area)

Additionally, label the first beaker "Minimum O2", second "Dissolved O2", and a third "Max O2."

 

5. Mark the last beaker "Open to the Atmosphere/ Dry Conditions."

 

6. Arrange beakers on a table in groups by solution type ( Distilled, Saline, H2SO4, 100ppm CaCO3.)

Additionally arrange beakers within each group by increasing O2 level: Minimum O2, Dissolved O2, Maximum O2 The effect of both solution type and oxygen level will be tested.

7. Sit the "Dry Conditions/ Atmospheric Exposure" beaker by itself.

 

8. Place two of the glass rods horizontally in the bottom of the "Dry Conditions" beaker and arrange the four types of steel in order of increasing SAE # 1008, 1045, 4140, 4340. * See Picture #3

These will serve as the experimental control. Any corrosion due to interaction between normal atmospheric conditions and specific steel type should show up here.

 

            Also, sure that the initial depth of each sample or the initial mass of each sample is marked on a folder assigned to each beaker prior to the experiment if you plan to use initial values in the calculation of extent corrosion. * See Measurement of Variables                                                                                    

                                                                                                           

9. Place two glass rods horizontally in the bottom of each remaining beaker.

 

10. As mentioned, prepare a manila folder marked "Distilled Water/ Minimum O2." Remove the four steel samples from this folder. In the beaker marked "Distilled Water/Minimum O2" arrange these samples in order of increasing SAE # 1008, 1045, 4140, 4340.

 

11. Proceed in the same manner as # 8 and #10 above for each of the remaining beakers, making sure to match the proper set of steel samples from the manila folders to the correct conditions under which they shall be tested as marked on the beaker.

 

 

 

 

 

 

 

 

 

 

 


 

 


 

Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

Learning Outcomes

 

          At the conclusion of these laboratory experiences (dependent on sophistication of approach) students should be able to do some or all of the following:

 

1. set up and conduct a multivariable experiment with appropriate control, systematically gather and classify data, and analyze data for any dominant trends therein.

 

2. describe steel as an iron-carbon alloy containing up to approx. 2% carbon (and always traces of manganese). It can also contain several other elements, called alloying elements, added to affect its properties. (Samuels 29-30).

 

3. indicate that there are many types of steel with great variations in their microstructures; these being dependant on the initial composition of the steel and how the steel was processed both thermodynamically and mechanically. ("Compositions of Standard Steels." and "Hot Finished Carbon Steel." Metals Handbook. 8th ed., Vol 1: 61-63)

 

4. show a general awareness of the range of microstructures that can occur in steels and be able to describe several of these.

 

5. describe, using a body-centered cubic crystal model, the most common microstructure of many steels at normal temperatures. This is essentially a two-phased heterogeneous system consisting of ferrite ( iron atoms arranged in a bcc array) mixed with carbon In some from of an iron carbide compound, Fe3C, called cementite.              (Samuels 6-9)

 

6. describe, using a face-centered cubic crystal model, another microstructure that can occur in steels (at elevated temperatures.) This is a one phase, homogenous mixture or a "solid solution" of carbon atoms "dissolved" in austenite (iron atoms arranged in a fcc array.)Ý The carbon atoms are found in the interstitial spaces (spaces in the crystal structure between the iron atoms.) ( 6, 29)

 

7. explain that the corrosion of steel is an electrolytic process in which electrons are transferred away from the Fe in steel through a solution containing charged particles, called electrolytes. ("The Selection of Steel for Mild Corrosion Service." 1: 257)

 

8. define an oxidation half reaction as one in which electrons are lost

 

9. define reduction half reaction as one in which electrons are gained

 

10. describe an electrolytic process as one in which electrons will flow from an area of high charge density to an area of low charge density through an electrolyte; a moist interface containing charged particles.

 

11. describe the components of a "half-cell" as a metal strip called an electrode immersed in a solution of its own ions

 

12. construct a simple electrochemical cell (also called a voltaic or galvanic cell) by connecting two "half-cells" to a voltmeter ( after placing a salt bridge between them.) Give evidence that electrons are flowing between the two half cells.

               

13. identify the parts of the electrochemical cell ( anode where oxidation occurs) and cathode (where reduction occurs), electrolyte, salt bridge, etc.

 

14. use the Standard Reduction Potential Table to explain why electrons flow between the anode and the cathode in the electrochemical cell constructed. Connect this to emf.

                                               

15. explain corrosion on the surface of a piece of steel in terms of an electrochemical cell.

 

16. give the equations which define corrosion in steels and explain how each reactant and product affects the corrosion reaction in terms of LeChatelier's Principle.

 

17. explain the design of an experiment to test the environmental factors that affect the rate of corrosion in steels and tell why each environmental factor is included in the experiment.

 

18. in terms of what is known about steel corrosion, hypothesize as to the results of this corrosion experiment; both as to steel type and as to specific environmental conditions.

 

19. define "galvanic couple" in terms of the electrochemistry of metals.

 

20. explain what is meant by steel acting "anodic" and what is meant by steel acting "cathodic."

 

21. explain how steel can be made to act "cathodic" and what is meant by "cathodic" protection.

 

22. tell what indicator you would use to test for steel areas acting "anodic" and forming Fe2+ ions; and what color you expect

 

23. tell what indicators you would use to show that steel is acting "cathodic" and what color to expect

 

24. explain why the potential on stainless steel should differ from that on low carbon steel, and describe an experiment that would show this

                            

 

 

 

 

 


 

 

 



 

Carnegie Mellon

NSF Grant DMR 079996

High School Teachers Summer Internship

 

 

 

 

 

 

 

Sample Results

EXPERIMENTAL RESULTS

                                Qualitative

                                                                                Data Grid (Observations)

 

Corrosion of Steels                                   SAE#   1008,  1045,  4140,   4340

                                                                                Observations

                                                   7/29/03  Day 14                                                                   3:00 PM

                                Date______________________             Time _____________

 

Solution

Type                       Minimum O2                                                             Dissolved O2                                          Max O2

                                (sealed)                                                                                                  (wet/dry)

Saline                     orange/red deposit                   thick red deposit                                   film of red/org

                                 on bottom (1mm)                     on bottom (5-6mm)                               susp on bott

                                thick(3mm) dep on                 thick, furry ,drk red                              1008(blk pts

                                top of all blks, furry                 corr 1008(most)-1045                          4140-1045-

                                red/orange on sides                  4340-4140(least)                                   4340(least)

                                solution: yell/or particles         solution:org/ ppt red

Acidic__________________________________________________________________

pH=2                       bottom clear                              orange deposit                                     slight

H2SO4                               4140 bubbles on surface         bottom (1mm)                                       org chnk

                                 no corr-4340 few bub            blks covered thin or                              under 1008

                                slight corr-1045(no bub         film 1008 (most) 4340-

                                top (sl corr)-1008 lght            1045-4140(least)                                 Orang cor

                                yell top (most corr)                  solution: clear/or                                 top 1008-

                                solution: clear/yell tinge         fine or deposit on top                                           4140-4340

_                                                                                                                                                          -1045 (no)

Basic___________________________________________________________________

100ppm                    white/or deposit                     deep or/red depost                                    white/org

CaCO3                               bottom                                                      bottom                                                                                under 1008

                                thk org "icing"                      thk corr 1008-                                         4140 most cor

                                all blk, esp 4140                     4140-1045-4340                                      then 1008

                                 clear yellow sol                       clear or sol                                              white powder                                                                                                                                   (suspended org part top)         top1045,4340         

Distilled________________________________________________________________

Water                     fine or powder                        thick red deposit                                     flecks of 4140        

                                mold-like furry                       furry or needles                                       most, then1008                                       1008,4140 most                     4140 most, oth                                       medium

                                                                                                                                                                               

                                                Quantitative

Ultrasound Measurements

Index  to Corrosion: 

                          Sum of depth lost on a 3-Point Test         Instrumental        Uncertainty

                                                                                                      

                                                 Values x  10-4  in                                                         +/-  3 x 10-4 in

 

                                                Minimum Oxygen Level  ( Immediately Sealed)

 

 

                                                1008                        1045                        4140                        4340

 

Saline                                       13                         8                              22                           7

 

pH =2                                           4                         11                            4                             4

Sulfuric Acid

 

Basic       ppm 100                      9                         9                              6                              17

Calcium

Carbonate

 

Distilled                                    12                       28                            0                              7

 

 

Ultrasound Measurements