GEOEE 404W:

SURFACE AND INTERFACIAL PHENOMENA IN GEO-ENVIRONMENTAL SYSTEMS

 

Syllabus Fall 2011

 

Grade scale:

A         >93

A-             90-93

B+       85-89

B         80-84

B-        75-79

C+       70-74

C         60-69

D         50-59

F          <50

 

Lab Schedule (updated!):

Note 1: Lab sessions will start during the week of 9/12 (Mark Klima and Tom Motel, supervisors).

Note 2: During class between 9/1 and 9/22 we shall cover the basics of each one of the lab experiments, so that you can ‘digest’ them with more ‘gusto’!

 

Lab Content:

Important note: Before you begin each experiment, you should prepare a spreadsheet with tables that clearly identify the independent variables to be measured and the parameters to be used. Devote special care to the analysis of consistency of units for both the measured and the calculated quantities. You should also know which graph(s) you will need to construct on the basis of these tables; the best way to do this is to enter hypothetical (and hopefully realistic!) values into the relevant tables and construct representative graphs. If you need help in developing such a spreadsheet, be sure to contact me 24/7.

Here is an example for the RO experiment.

 

EXPRERIMENT #1: Adsorption in packed columns (basic phenomena: L/S equilibrium and mass transport)

            -Analysis of breakthrough time: Use one of your experimental results (say, tB at C/Co=0.5) to back-calculate the MTC, and then confirm (?) the validity of the Wheeler equation by using this MTC to obtain the correct tB values at your other two C/Co levels (see In-lieu-of-class activity #4).

            -Do you agree (see relevant class handout) that a = (We D2 p)/(4 Co Q) and b = (We rad Q)/(Co Q Ka) ln(Ce/Co)? Do you also agree that, if a=129 h/m (see HW2-5), the actual amount adsorbed (We) is only about 23% of what one would expect from the isotherm constructed in HW1-4?

-Can you confirm, from the intercept of the ax+b line (see Table 1 in the Lab manual), that the MTC should indeed be of the order of 10-5 m/s. (Remember the class handout “Transport phenomena (2)”?) What does that say about the relationship between adsorbent particle size and thickness of boundary layer that surrounds the particle? Perhaps the diffusivity of MB, which is a relatively large molecule, is LESS than the ‘typical’ liquid-phase diffusivity of ca. 10-9 m2/s…

            -Key graph and its message: Should the C/Co vs. t graph be a straight line? (When might it be?)

 

EXPERIMENT #2: Reverse osmosis or ‘ultrafiltration’ (basic phenomena: mass and momentum transport)

            -osmotic pressure (see relevant class handouts): equal volumes of solutions showing the same osmotic pressure contain equal numbers of molecules of solute (“extended Avogadro’s law”)

            -mass/mole balance of solutions: a rudimentary example.

            -solutions of electrolytes: why does, say, a 0.1N solution of NaCl produce an effect (say, on vapor pressure suppression) that is 10% less than expected on the basis of complete ionization? Debye-Hückel theory provides a simple and elegant explanation (see below).

            -The key fundamental issues in this experiment are to understand (i) whether indeed a “typical value [of parameter A] is 0.255 gal/day/ft2/psi”, and (ii) whether a reasonable value of parameter B can be ‘extracted’ from the results.

            -key graph and its message?

 

EXPERIMENT #3: Soil washing (basic phenomena: L/L equilibrium and ‘detergent’ effect of the surfactant)

            -presumably the concentration of the added surfactant is close to CMC…

            -key graph and its message?

 

EXPERIMENT #4: Pressure filtration (basic phenomenon: momentum transport)

            -basic momentum transport equation

            -Hagen-Poiseuille equation

            -key graph and its message?

 

EXPERIMENT #5: Surface charge and settling of suspensions (basic phenomenon: electrostatic repulsion)

            -electrophoretic mobility vs. pH curve

            -double-layer compression

            -mass titration curve

            -key graph and its message?

 

Format of Lab Reports

 

In-lieu-of-class activity for August 23 (due in Angel dropbox by midnight 8/24): The attached Excel spreadsheet contains information about the use of the classical BET equation to determine the specific surface area of an adsorbent on the basis of its adsorption isotherm. (Can you retrieve the original 1938 article, by Stephen Brunauer and coworkers, from the PSU library’s electronic database?) Based on this information do the following: (i) Construct the graph of the amount adsorbed (in cm3/g) vs. gas pressure (in atm) at the two temperatures shown. (ii) Determine the surface area of the silica gel adsorbent.

Does your graph at 77 K look like this? Why is 77 K a convenient temperature for this adsorption experiment? Is 90.1 K a more or less convenient temperature? Why is it informative (with respect to 77 K)? Hint: Remember Le Chatelier’s principle?

 

Note: This analysis illustrates the importance of having reliable experimental results over a reasonable range of values of the independent variable (x-axis)… something to keep in mind when we start doing the lab exercises! (If the results at 90 K do not “make sense”, and if your reading of the 1938 article does NOT help, we’ll ‘resolve’ these issues in class discussions and HW #1.)

 

 

In-lieu-of-class activity for August 25 (due in Angel dropbox by midnight 8/26): The attached Excel spreadsheet contains information about the use of the classical Langmuir and Freundlich equations to rationalize the process of liquid purification, by transfer (adsorption) of, say, a pollutant from solution onto the surface of a solid ‘substrate’ (or adsorbent). The original article is cited there as well; can you retrieve it from the library’s online database?

Based on this information do the following.

(i)               Construct the adsorption isotherm: uptake (in g/g) vs. equilibrium concentration (in mg/L).

(ii)             Construct the linearized Langmuir plot and determine its two characteristic parameters.

(iii)           Construct the linearized Freundlich plot and determine its two characteristic parameters.

(iv)       Compare your numbers with those listed in the original article, and comment on their degree of (dis)agreement.

            Does your Langmuir plot look like this? If you can’t find the original article, does google (say, wikipedia) help in finding the relevant information (e.g., Langmuir eqn, Freundlich eqn)? And the textbook?

 

Constituents of matter: atoms (ca. 10-10 m), molecules (ca. 10-10-10-8 m), colloids (10-9-10-7 m), particles (ca. 10-9-10-3 m), bulk ‘materials’.

Note: ‘colloid’ means glue-like (in Greek), because Thomas Graham (Trans Roy Soc London 151, 183, 1861) noted that amorphous solutes such as starch and caramel diffused very slowly.

 

INTERATOMIC/INTERMOLECULAR FORCES:

There are four fundamental forces in nature: (a) strong and weak (short-range) interactions between sub-atomic particles (in the ‘microscopic’ world); (b) electromagnetic and gravitational (longer range) forces between atoms and molecules (and also between sub-atomic particles). The electromagnetic (together with gravitational) forces determine the properties of gases, liquids and solids and therefore the behavior of atoms and molecules in the ‘macroscopic’ world; a convenient, though somewhat arbitrary classification of these forces is the following:

-‘physical’ (e.g., condensation)

-‘chemical’ (e.g., ionic or covalent bonding)

-‘electrical’ (e.g., coulombic interactions, Debye-Hückel theory of electrolyte solutions): Here is a summary (review?) of key physics/math concepts.

 

States of aggregation of matter: gases, liquids, solids.

 

See Table 1.4 (p10) in textbook.

 

 

SURFACE (G/S, L/S) AND INTERFACIAL (e.g., G/L, G/L, S/S) PHENOMENA IN ENVIRONMENTAL ENGINEERING:

-partition coefficient (e.g., Henry’s law constant)

-asymptotic behavior: surface coverage, monolayer

-surface tension, surfactants, critical micelle concentration

-affinity vs. capacity: quantification using adsorption isotherm parameters (e.g., BET, Langmuir, Freundlich, …)

 

Problem 1.1 (textbook)

 

Problem 1.7 (textbook)

 

Example 7.5 (textbook)

 

Example 11.1 (textbook)

 

 

Homework 1 (average grade=60%).

(1)    (a) A simple but powerful method that takes into account the fact that intermolecular forces may be important (even for gases) in real (vs. idealized) situations is the venerable van der Waals equation of state. Use the attached spreadsheet to show how the compressibility factor (Pv/(RT)) depends on pressure.

-Does your graph look like this? (Do you agree that a reasonable range of v values is 0.05-25 L/mol?)

(b) A dilute solution of an electrolyte is not ideal, i.e., its activity coefficients deviate significantly from 1.0. Show this to be the case by using the Debye-Hückel theory to complete the attached table for an aqueous solution of NaCl whose molality (at, say, 298 K and 1 atm) varies between 0.01 and 0.1.

(2)   Complete Problem 1.7 (see above). In particular, verify (and explain!) the meaning of the (n=0,d=0.401) data point, by consulting the original source of information. Do the answers change if you remove this point from the data set?

-Do you get (again?) that the number-, surface- and volume-mean are 293, 297 and 302 nm, respectively?

(3)   Make a graph of the Debye length vs. solution concentration for NaCl, CaCl2 and MgSO4. (Extra credit: Does it matter whether the relevant geometry is spherical (e.g., potential vs. radial distance surrounding a spherical particle) or ‘linear’ (e.g., potential vs. thickness of the electric double layer)?]

-Does your graph for NaCl look like this? And the final one like this? (Do you agree that m=Im/3 for CaCl2 and m=Im/4 for MgSO4? And for Na3PO4, Im=0.5(3m+9m) – see handout “Ionic strength: exercises” – so m would be Im/6… Right?)

(4)   Compare the uptakes of benzene and methylene blue on a GAC and evaluate the effect that this difference has on the breakthrough time under otherwise comparable (but representative!) conditions.

-Does your MB graph look like this? If you have difficulty finding Langmuir or Freundlich parameters for benzene on GAC (similar to the one used to adsorb MB?), let me know!

 

 

Here is the JChemEduc article that we shall analyze carefully in class, as an important exercise (also carried out in the labs!) in learning methodology:

(i)               use a calibration curve to construct a graph that contains “raw data”,

(ii)             use such a graph to establish a trend in the relevant dependent variable over a reasonable range of values of the independent variable, and

(iii)           identify (and understand!) the behavior of a key concept that governs the observed phenomenon.

And here is its “supporting information”, which contains key elements of a typical (and excellent!) lab report. Let’s develop a spreadsheet to ‘digest’/reproduce this exercise!

 

Using this same methodology, can you find this (very recent) article? Do its figures 2c and 2d resemble the results you obtained in your soil washing experiment? (Should they? If not, why not?)

 

http://www.ems.psu.edu/~radovic/CMC_2a.nb

 

Homework #2 (average preliminary grade=63%):

Note: If (you are of the opinion that) more points can be squeezed out of your answers, let’s discuss them in more detail! (In particular, let’s analyze whether and how you used the class handouts and/or the various ‘templates’ to simplify your tasks.)

1.     Complete the handout “CMC: a closer look” by constructing a series of graphs like the one shown, using n as the parameter (say, n = 25, 50, 75 and 100).

-Here is a template based on the handout “Surfactants”. Note that it requires solving an implicit equation, which can be done using, say, Solver in Excel or Mathematica (attached).

-Note: If values of n that are very different from 20 (using the same equilibrium constant) give you (only mathematical?) problems (or physical as well?), try using values of n that are NOT very different from 20; for example, n=22 with cT between 0.6e-4 and 2.2e-4… This shows you that, upon changing n (while keeping K constant), the range of cT values has to be adjusted ‘accordingly’!

2.     Solve at least one problem in the handout “Contact angle/surface tension”.

3.     Solve at least two problems in the handout “Surface tension & capillarity exercises”.

4.     Complete the exercise summarized in the handout “Methodology of learning (1)”.

-Does your key graph look like this? And the supporting “calibration curve” (actually a straight line) like this?

5.     Complete the exercsie summarized in the handout “Adsorption 2”. For gas-phase adsorption, select two adsorbates whose isotherm data are readily available. Be sure to select and document carefully your source(s) of information! Can you ‘extract’ a reasonable value for the methylene blue uptake from the slope of the breakthrough curve obtained in the lab experiment?

      -Do you agree that the equilibrium uptake ‘extracted’ from the slope (129 min/cm?) is obtained when the slope is multiplied by the pollutant concentration and flow rate and divided by the cross-sectional area and density of the packed adsorbent column? (Note: Doesn’t the relevant table in your Lab ‘manual’ indicate that the slope is actually 129 h/m? Does that help you to obtain a reasonable value for the equilibrium uptake of MB?)

6.     Following up on our discussion of the handout “Adsorption 2”, use the data that we were able to locate with the help of the Web of Knowledge to analyze the relative effectiveness of an adsorbent in removing a pollutant (e.g., benzene) from the gaseous vs. the liquid phase. Construct a meaningful graph and comment on the degree of (dis)agreement of these results and the ability to compare ‘apples’ and ‘apples’.

-Does your graph look like this? (If it does, be sure to document clearly HOW you obtained it! And then show that it is actually ‘easier’ to remove this pollutant from the gas phase than from the liquid phase!? Why?)

 

In-lieu-of-class activity #3 (week of 10/10): In preparation for the midterm exam (to be scheduled during the week of 10/24), review as many of the class handouts as necessary/possible. If not completed/clear, e-mail me specific questions about them, and/or about HW1 or HW2.

            -For example, does your BET plot for benzene and toluene vapors look like this? And do you agree that the analogous results shown in Chapter 9 of the textbook imply that the heat of adsorption (of nitrogen) is 2.9 kJ/mol higher than the heat of condensation (of nitrogen)?

 

Midterm exam (average grade=57%).

 

Experimental design: from ‘scratch’ or extension of a familiar experiment… tbd in consultation with Prof. Klima.

 

In-lieu-of-class activity #4 (due in Angel dropbox before class on 11/3): Show schematically and discuss briefly the key graphs and the key equations in the soil washing and reverse osmosis lab experiments. Be prepared to discuss them in class on 11/3.

 

In-lieu-of-class activity #5 (only two of us showed up for class of 11/3; due in Angel dropbox before class on 11/8): Complete the attached class handout and be prepared to discuss it in class on 11/8!

            -Here is one version of the completed class handout.

 

 

Homework #3: Experimental design exercises  (and not just “electrokinetic phenomena”), due 11/20 in Angel dropbox, accepted (without penalty) at the same time as the experimental design project (during the finals week, at the latest).

1. Complete the in-lieu-of-class #5 handout and discuss its relevance to the SW experiment.

-To obtain a variety of CMC values (including those of Triton X-100 and Dispersit SPC 1000?), can you find in the Knovel database (PSU library) Chapter II-19 of the  “Handbook of Applied Surface and Colloid Chemistry”?

2. Complete the 11/10 class handout and discuss its relevance to the PF experiment.

            -Here it is. And here is one completed version.

3. Complete the 11/15 class handout #1 and discuss its relevance to the RO experiment.

            -In order for 0.255 gpd/ft^2/psi to indeed be a “typical value” of the water permeability coefficient, the membrane area should be ?? ft^2, and this is (or is not?) a realistic number… Etc.

            -Can you find ‘typical’ values of the water permeability coefficient in units of m/s? How is this related to the liquid-phase mass transfer coefficient? Should it be similar to the kL value that we ‘back-calculated’ from the results of the GAC experiment (3e-5 m/s)?

4. Complete the 11/15 class handout #2 and discuss its relevance to the GAC experiment.

            -Do you agree that a column whose diameter is 1 m (and is 1.5 m long) will remove 95% of the pollutant with a breakthrough time of ca. 189 h?

5. Complete the 11/17 class handout and discuss its relevance to the SC experiment.

-See, for example, the double-layer compression graphs in ZetaMater’s brochure coag.pdf; see Experiment #5 above.

 

Class of 11/29: general discussion of experimental design assignments.

‘Classes’ of 12/1, 12/6 and 12/8: individual discussions of design project reports, especially their theoretical background sections. (Send me an e-mail to set up a 30-60 min meeting!)

 

The final grades have been posted. Class average=76% (B-). (If your records disagree with mine, please contact me asap…) Have a wonderful Holiday Season!

 

lrr3@psu.edu (updated 12/19/2011, 12:15)