Synthesis and Analysis of Copper Hydroxy Double Salts.
`
`Laura M. Brigandi, Phyllis A. Leber, and Claude H. Yoder
`Department of Chemistry
`Franklin & Marshall College
`Lancaster, PA 17604
`
`Supplemental Material for Online Publication
`
`Lab Documentation
`
`Student Material
`
`I. Experimental Procedure
`
`Due to the possible hazards involved in working with acid and hydroxide
`
`solutions, safety glasses should be worn at all times. Gloves are also recommended.
`
`Synthesis of the Copper Hydroxy Double Salts
`
`Malachite – Cu2(OH)2CO3 (1)
`
`Weigh approximately 4 g of CuSO4•5H2O to the nearest 0.01 g and dissolve it in
`
`approximately 20 mL distilled water. Next, weigh approximately 2 g of Na2CO3 to the
`
`nearest 0.01 g, and dissolve in approximately 20 mL distilled water. Add the Na2CO3
`
`solution to the CuSO4 solution and stir. Heat the solution, covered with a watch glass, on
`
`a hot plate for 30 minutes on low heat, then let the solution cool for 1 hour. Filter the
`
`solution using suction with a Buchner funnel and fine filter paper. Let the precipitate air
`
`dry for 1 hour, then dry in a 120ºC oven for 1 hour in a crystallizing dish.
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`Liquidia's Exhibit 1030
`IPR2020-00770
`Page 1
`
`
`
`Laura M. Brigandi, Phyllis A. Leber, and Claude H. Yoder
`Department of Chemistry
`Franklin & Marshall College
`Lancaster, PA 17604
`
`Supplemental Material for Online Publication
`
`Lab Documentation
`
`Student Material
`
`I. Experimental Procedure
`
`Due to the possible hazards involved in working with acid and hydroxide
`
`solutions, safety glasses should be worn at all times. Gloves are also recommended.
`
`Synthesis of the Copper Hydroxy Double Salts
`
`Malachite – Cu2(OH)2CO3 (1)
`
`Weigh approximately 4 g of CuSO4•5H2O to the nearest 0.01 g and dissolve it in
`
`approximately 20 mL distilled water. Next, weigh approximately 2 g of Na2CO3 to the
`
`nearest 0.01 g, and dissolve in approximately 20 mL distilled water. Add the Na2CO3
`
`solution to the CuSO4 solution and stir. Heat the solution, covered with a watch glass, on
`
`a hot plate for 30 minutes on low heat, then let the solution cool for 1 hour. Filter the
`
`solution using suction with a Buchner funnel and fine filter paper. Let the precipitate air
`
`dry for 1 hour, then dry in a 120ºC oven for 1 hour in a crystallizing dish.
`
`Liquidia's Exhibit 1030
`IPR2020-00770
`Page 1
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`Brochantite – Cu4(OH)6SO4
`
`Weigh, to the nearest 0.01 g, approximately 2 grams solid NaOH, to make 50 mL
`
`of 1.0 M NaOH solution. Prepare the solution by dissolving the solid in distilled water
`
`and diluting to 50 mL in a graduated cylinder. Next, prepare 50 mL of a 1.0 M solution of
`
`CuSO4•5H2O by weighing out 12.5 g of solid and dissolving in distilled water, then
`
`diluting to 50 mL in a graduated cylinder. Pour the CuSO4 solution into a 250 mL beaker.
`
`Add the NaOH solution by buret, allowing the NaOH to drip quickly into the 250 mL
`
`beaker while the CuSO4 solution is being stirred on a magnetic stir plate. Let the solution
`
`stir on the stir plate for at least 30 minutes after all the NaOH has been added. Filter the
`
`solution using suction with a Buchner funnel and fine filter paper. Let the precipitate air
`
`dry for 1 hour, then dry in a 120ºC oven for 1 hour in a crystallizing dish.
`
`Paratacamite – Cu4(OH)6Cl2 (2)
`
`Prepare 50 mL of a 0.5 M solution of CuCl2•2H2O by weighing out 4.3 g and
`
`dissolving in distilled water, then diluting to 50 mL in a graduated cylinder. Pour the
`
`CuCl2 solution into a 250 mL beaker. Next, weigh out, to the nearest 0.01 g,
`
`approximately 2 g of NaOH and dissolve in distilled water to make 100 mL of 0.5 M
`
`solution. Add the NaOH solution in 5- or 10-mL aliquots, stirring with a stirring rod after
`
`each addition. Also, after each addition, test the solution’s pH using pH paper. Add
`
`enough NaOH to bring the solution to a pH of 9. As the pH approaches 9, reduce the
`
`aliquot size to 1 mL so as not to pass the required pH.
`
`Heat the solution, covered with a watch glass, on a hot plate for 30 minutes on
`
`low heat, then let the solution cool for 1 hour. Filter the solution using suction with a
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`IPR2020-00770
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`Buchner funnel and fine filter paper. Let the precipitate air dry for 1 hour, then dry in a
`
`120ºC oven for 1 hour in a crystallizing dish.
`
`Cu4(OH)6Br2
`
`Weigh, to the nearest 0.01 g, approximately 2 grams solid NaOH, to make 50 mL
`
`of 1.0 M NaOH solution. Prepare the solution by dissolving the solid in distilled water
`
`and diluting to 50 mL in a graduated cylinder. Next, prepare 50 mL of a 1.0 M solution of
`
`CuBr2 by weighing 11.2 g of solid and dissolving in distilled water, then diluting to 50
`
`mL in a graduated cylinder. Pour the CuBr2 solution into a 250 mL beaker. Add the
`
`NaOH solution by buret, allowing the NaOH to drip quickly into the 250 mL beaker
`
`while the CuBr2 solution is being stirred on a magnetic stir plate. Let the solution stir on
`
`the stir plate for at least 30 minutes after all the NaOH has been added. Filter the solution
`
`using suction with a Buchner funnel and fine filter paper. Let the precipitate air dry for 1
`
`hour, then dry in a 120ºC oven for 1 hour in a crystallizing dish.
`
`Analysis of the Copper Hydroxy Double Salts
`
`Qualitative Tests
`
`In order to ensure that a compound has been made with the expected ions,
`
`qualitative tests may be performed on a small scale in a test tube or small beaker.
`
`Copper, found in all four compounds, can be identified by the complex ion it
`
`forms with ammonia, Cu(NH3)4
`
`2+, as shown in the equation below.
`
`Cu2+ + 4NH3 ! Cu(NH3)4
`
`2+
`
`(1)
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`IPR2020-00770
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`Addition of 6 M ammonia to a small sample of the solid compound will dissolve the
`
`product and produce a dark blue solution if copper is present.
`
`The hydroxide ion, also found in all four compounds, can be identified by infrared
`
`spectroscopy. The IR spectrum obtained from a dry mineral oil mull should contain a
`
`broad OH peak at 3100 - 3300 cm-1 if the compound contains the ion.
`
`The carbonate ion in malachite is determined by reaction with acid. The addition
`
`of 6 M HCl to a small sample of the solid compound will liberate CO2 gas, indicated by
`
`the fizzing of the sample. The reaction of carbonate is shown in the following reaction.
`
`CO3
`
`2- + 2H+ ! H2O + CO2(g)
`
`(2)
`
`The chloride in paratacamite and the bromide in Cu4(OH)6Br2 can be observed by
`
`precipitation of AgCl or AgBr with AgNO3.
`
`Ag+ + Cl- ! AgCl(s)
`
`(3)
`
`Additionally, the sulfate ion in brochantite can be identified by precipitation of BaSO4
`
`with BaCl2.
`
`Ba2+ + SO4
`
`2- ! BaSO4(s)
`
`(4)
`
`In all three reactions, a small sample of the compound is dissolved in nitric acid, and the
`
`BaCl2 or AgNO3 solution is added and mixed well. The observation of a white precipitate
`
`is indicative of the desired ions.
`
`% Copper by Colorimetry (3)
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`IPR2020-00770
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`Before analyzing the double salts, a graph of standard solutions must be prepared
`
`against which the double salt values will be compared. Begin by preparing at least 5
`
`standard solutions by measuring out approximately 0.7 g CuSO4•5H2O (weighed to 1 mg)
`
`and dissolving it in 20 mL of distilled water. Add 6 M NH3 until the solution is dark blue
`
`and clear. Dilute the solution with distilled water to 100 mL in a volumetric flask.
`
`Carefully measure out 60 mL of this solution in a graduated cylinder and dilute again
`
`with distilled water to 100 mL in a volumetric flask, adding 6 M NH3 if the solution
`
`appears cloudy. Continue this process of dilution to make 5 solutions.
`
`Place a sample of each solution in a colorimeter to determine the absorbance at a
`
`wavelength of 650 nm. Once all 5 absorbances are obtained, prepare a graph of
`
`absorbance v. concentration of copper. This graph will be used to calculate the
`
`concentration of copper of the double salt solutions.
`
`Next, dissolve a 0.1 g sample of the double salt (measured to 1 mg) in 6 M NH3.
`
`Dilute to 100 mL with distilled water in a volumetric flask. Place a sample of the solution
`
`in the same colorimeter and determine the absorbance at a wavelength of 650 nm.
`
`Calculate the percent copper in the sample using the equation from the graph and the
`
`mass of double salt used.
`
`% Carbonate by Formation of CO2 (4)
`
`Weigh approximately 0.1 g of malachite to the nearest 1 mg. Place the sample in a
`
`side-arm test tube with a 12-inch length of tubing attached to the sidearm. Next, pour 2
`
`mL of 6 M HCl into a small test tube and slide the test tube inside the side-arm, being
`
`careful not to spill any HCl. Stopper the side-arm test tube. Then fill a large crystallizing
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`IPR2020-00770
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`dish with water. Fill a 25-mL graduated cylinder to the brim with water and place
`
`parafilm over the top. Try to get as little air in the graduated cylinder as possible. Turn
`
`the graduated cylinder upside down, place it in the crystallizing dish, and carefully
`
`remove the parafilm. Insert the other end of the tygon tubing (from the side arm test tube)
`
`into the graduated cylinder.
`
`Begin the reaction by turning the test tube upside down so that the HCl spills out
`
`of the small test tube and reacts with the solid on the bottom. The CO2 that forms will
`
`bubble into the graduated cylinder. If necessary, repeatedly flip the side-arm test tube
`
`until the entire compound has reacted with the HCl and a green liquid remains in the test
`
`tube. When finished, record the volume of CO2 in the graduated cylinder, the temperature
`
`of the water, and the atmospheric pressure, and calculate the percent carbonate using the
`
`ideal gas law and the mass of malachite used. The vapor pressure of water should be
`
`taken into account in the calculation.
`
`% Sulfate by Gravimetric Precipitation
`
`Weigh approximately 0.1 g of brochantite (to the nearest 0.1 mg) into a beaker
`
`and dissolve in 40 mL of H2O with 6 mL of 1 M HNO3. Add 4 mL 0.2 M BaCl2. Heat the
`
`solution on a hot plate for 1 hour, then let the solution sit overnight to allow the
`
`precipitate to digest. Test the solution for complete precipitation by adding a drop of 0.2
`
`M BaCl2. If more precipitate forms, add more BaCl2 and heat again. Continue this until
`
`no additional precipitate forms when BaCl2 is added. Once the solution is completely
`
`precipitated, filter using a glass gravity funnel and fine ashless filter paper. Let the
`
`precipitate air dry, then place the filter paper in a previously dried and weighed crucible.
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`Liquidia's Exhibit 1030
`IPR2020-00770
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`Next, heat the crucible using a Bunsen burner for 4 hours with the lid on. The lid
`
`may need to be heated by itself to remove any excess carbon. When finished, all the filter
`
`paper should be burned off and only the white precipitate should remain. When the
`
`crucible is cool, weigh again to determine the mass of precipitate. Use this and the mass
`
`of brochantite to calculate the percent sulfate.
`
`% Chloride and Bromide by Gravimetric Precipitation
`
`Weigh approximately 0.1 g (to 1 mg) of paratacamite or Cu4(OH)6Br2 into a
`
`beaker and dissolve it in 20 mL of 6 M HNO3. Add 6 mL of 0.1 M AgNO3 and cover the
`
`solution with a watch glass. Heat on a hot plate for 30 minutes on low heat. Let the
`
`solution sit for 60 minutes in a closed locker. Due to the reduction of silver ions to silver
`
`metal in the presence of light, the solution should not be exposed to light more than
`
`necessary. Test the solution for complete precipitation by adding a drop of 0.1 M AgNO3.
`
`If more precipitate forms, add more AgNO3 and heat again. Repeat until no additional
`
`precipitate forms. When precipitation is complete, filter the solution using suction with a
`
`previously oven-dried and weighed filter crucible. Dry the precipitate in the crucible in
`
`120°C oven for 2 hours. Weigh the crucible when cool to obtain the mass of precipitate.
`
`Use this and the mass of double salt used to calculate the percent anion.
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`IPR2020-00770
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`II. Background Information
`
`Each of the compounds in this project forms under slightly different conditions in
`
`nature. These differences can tell us about the environments in which the minerals are
`
`found, and are reflected in the laboratory procedures for synthesis.
`
`For example, malachite is the only mineral in this project for which the simple
`
`salt, CuCO3, is not used as a starting material. Indeed, the simple salt of CuCO3 does not
`
`form in the reaction of carbonate with Cu2+ in aqueous solution. Because the carbonate
`
`ion is the conjugate base of a weak acid, the solution containing Cu2+ and CO3
`
`2- is basic
`
`(contains OH- ions) and forms the double salt CuCO3•Cu(OH)2. For this reason, the
`
`addition of NaOH is not necessary in this procedure.
`
`One might also note that while brochantite and Cu4(OH)6 Br2 are formed by drop
`
`wise addition of NaOH, the procedure for paratacamite requires larger aliquots of NaOH
`
`added to pH of 9. Experimentation indicated that drop wise addition of NaOH caused the
`
`formation of extremely small particles of paratacamite, making the precipitate difficult to
`
`filter. The use of larger aliquots and stabilization of pH at 9 yielded larger, more easily
`
`filtered particles. This same difficulty has been noted in the preparation of malachite (1).
`
`The particle size of brochantite and Cu4(OH)6Br2 appeared to be unaffected by either pH
`
`or method of NaOH addition.
`
`The distinguishing feature of Cu4(OH)6Br2 is its inability to withstand extended
`
`heating. The only compound in this project that does not exist naturally as a mineral, it
`
`decomposes to copper oxide if left in the oven for more than 1 hour. The other three
`
`minerals are much more stable and may be heated for several hours without
`
`decomposition, although it has been found that when malachite is prepared using equal
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`IPR2020-00770
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`molar amounts of copper and carbonate ions, the product tends to partially decompose to
`
`copper oxide (1).
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`IPR2020-00770
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`Instructor’s Notes
`
`I. Background Information
`
`See Background information (Section II) in Student Material.
`
`II. Lab Preparation and Equipment (per student)
`
`Synthesis of Malachite (Cu2(OH)2CO3)
`
`1. 4 g CuSO4•5H2O, CAS # 7758-99-8
`
`2. 2 g Na2CO3, CAS # 497-19-8
`
`3. 1 beaker, 250 mL
`
`4. 1 watch glass, 100 mm
`
`5. 1 hot plate
`
`6. 1 Buchner funnel, 5.5 cm
`
`7. Qualitative P2 filter paper, porosity: fine, flow rate: slow, 5.5 cm
`
`8. 1 filter flask, 500 mL
`
`9. crystallizing dish, 90x50 mm
`
`Synthesis of Brochantite (Cu4(OH)6SO4)
`
`1. 2 g NaOH pellets, CAS # 1310-73-2
`
`2. 12.5 g CuSO4•5H2O, CAS # 7758-99-8
`
`3. 1 volumetric flask, 50 mL
`
`4. 1 beaker, 250 mL
`
`5. 1 buret, 50 mL, Teflon stopcock
`
`6. 1 magnetic stir plate
`
`7. 1 magnetic stir bar
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`IPR2020-00770
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`8. 1 Buchner funnel, 5.5 cm
`
`9. Qualitative P2 filter paper, porosity: fine, flow rate: slow, 5.5 cm
`
`10. 1 filter flask, 500 mL
`
`11. 1 crystallizing dish, 90x50 mm
`
`Synthesis of Paratcamite (Cu4(OH)6Cl2)
`
`1. 4.3 g CuCl2•2H2O, CAS # 10125-13-0
`
`2. 2 g NaOH pellets, CAS # 1310-73-2
`
`3. 1 volumetric flask, 50 mL
`
`4. 1 volumetric flask, 100 mL
`
`5. 1 beaker, 250 mL
`
`6. 1 glass stirring rod
`
`7. pH paper, range 1-12
`
`8. 1 watch glass. 100 mm
`
`9. 1 hot plate
`
`10. 1 Buchner funnel, 5.5 cm
`
`11. Qualitative P2 filter paper, porosity: fine, flow rate: slow, 5.5 cm
`
`12. 1 filter flask, 500 mL
`
`13. 1 crystallizing dish, 90x50 mm
`
`Synthesis of Cu4(OH)6Br2
`
`1. 11.2 g CuBr2, CAS # 7787-70-4
`
`2. 2 g NaOH pellets, CAS # 1310-73-2
`
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`IPR2020-00770
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`3. 1 volumetric flask, 50 mL
`
`4. 1 beaker, 250 mL
`
`5. 1 buret, 50 mL, Teflon stopcock
`
`6. 1 magnetic stir plate
`
`7. 1 magnetic stir bar
`
`8. 1 Buchner funnel, 5.5 cm
`
`9. Qualitative P2 filter paper, porosity: fine, flow rate: slow, 5.5 cm
`
`10. 1 filter flask, 500 mL
`
`11. 1 crystallizing dish, 90x50 mm
`
`Qualitative Tests
`
`1. 0.1 g of each double salt (prepared during lab)
`
`2. 20 mL 6 M NH3, CAS # 7664-41-7
`
`3. 5 mL 6 M HCl, CAS # 7647-01-0
`
`4. 10 mL 0.1 M AgNO3, CAS # 7761-88-8
`
`5. 5 mL 0.2 M BaCl2, CAS # 10361-37-2
`
`6. 15 mL 3 M HNO3, CAS # 7697-37-2
`
`7. 8 test tubes, 10x75 mm
`
`8. 1 infrared spectrometer
`
`% Copper by Colorimetry
`
`1. 0.7 g CuSO4•5H2O, CAS # 7758-99-8
`
`2. 70 mL 6 M NH3, CAS # 7664-41-7
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`3. 0.1 g each double salt (prepared during lab)
`
`4. 1 volumetric flask, 100 mL
`
`5. 1 graduated cylinder, 100 mL
`
`6. 1 colorimeter
`
`7. 5 colorimeter cuvettes
`
`% Carbonate by Formation of CO2
`
`1. 0.1 g Cu4(OH)6CO3 (prepared during lab)
`
`2. 2 mL 6 M HCl, CAS # 7647-01-0
`
`3. 1 side-arm test tube
`
`4. 1 test tube, 10x75 mm
`
`5. 1 rubber stopper, size 0
`
`6. 1 length of tygon tubing, 12 in
`
`7. 1 crystallizing dish, 90x50 mm
`
`8. 1 graduated cylinder, 25 mL
`
`9. laboratory parafilm
`
`% Sulfate by Gravimetric Precipitation
`
`1. 0.1 g Cu4(OH)6SO4 (prepared during lab)
`
`2. 6 mL 1 M HNO3, CAS # 7697-37-2
`
`3. 5 mL 0.2 M BaCl2, CAS # 10361-37-2
`
`4. 1 beaker, 250 mL
`
`5. 1 magnetic heat/stir plate
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`6. 1 magnetic stir bar
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`7. 1 glass funnel, 65 mm
`
`8. fine ashless filter paper, 110 mm
`
`9. 1 glass stirring rod with rubber policeman
`
`10. 1 porcelain crucible, size 0, with lid
`
`11. 1 Bunsen burner
`
`12. 1 piece of rubber tubing
`
`% Chloride by Gravimetric Precipitation
`
`1. 0.1 g Cu4(OH)6Cl2 (prepared during lab)
`
`2. 20 mL 6 M HNO3, CAS # 7697-37-2
`
`3. 7 mL 0.1 M AgNO3, CAS # 7761-88-8
`
`4. 1 beaker, 250 mL
`
`5. 1 watch glass, 100 mm
`
`6. 1 hot plate
`
`7. 1 filter crucible, 30 mL, porosity M
`
`8. 1 Walter crucible holder
`
`9. 1 filter flask, 500 mL
`
`10. 1 glass stirring rod with rubber policeman
`
`% Bromide by Gravimetric Precipitation
`
`1. 0.1 g Cu4(OH)6Br2 (prepared during lab)
`
`2. 20 mL 6 M HNO3, CAS # 7697-37-2
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`3. 7 mL 0.1 M AgNO3, CAS # 7761-88-8
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`4. 1 beaker, 250 mL
`
`5. 1 watch glass, 100 mm
`
`6. 1 hot plate
`
`7. 1 filter crucible, 30 mL, porosity M
`
`8. 1 Walter crucible holder
`
`9. 1 filter flask, 500 mL
`
`10. 1 glass stirring rod with rubber policeman
`
`III. Tips
`
`1. The instructions indicate that the sodium hydroxide solution used in preparation of the
`
`double salts should be made from solid NaOH pellets. However, the solutions may also
`
`be prepared by diluting concentrated NaOH solutions instead.
`
`2. As indicated in the background information, copper hydroxy bromide has a tendency
`
`to decompose to copper oxide if heated too long. Students should not dry samples in the
`
`oven more than 1 hour. All other compounds may be heated for several hours without
`
`decomposition.
`
`3. If time is an issue, the qualitative section may be skipped, as most of the tests are
`
`similar to the quantitative procedures of analysis.
`
`4. XRD results indicated, with a figure of merit of 10.8, that the compound Cu4(OH)6Cl2
`
`was paratacamite, and not atacamite.
`
`5. In the quantitative analysis of sulfate, the amount of time required to burn off the
`
`paper my be reduced by use of a Meker burner.
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`6. If the instructor feels that the use of graduated cylinder should be avoided in
`
`dilutions, the solution volumes can be adjusted so that pipetting aliquots into
`
`volumetric flask can be used.
`
`7. If additional reading on copper minerals is desired
`
`Literature Cited
`
`1. Sheeran, D. J. Chem. Educ. 1998, 75, 453-5.
`
`2. Sharkey, J.B.; Lewin, S.Z. American Mineralogist. 1971, 56, 179-91.
`
`3. Yoder, C. H.; Smith, W. D.; Katolick, V. L.; Hess, K. R.; Thomsen, M. W.; Yoder, C.
`
`S.; Bullock, E. R. J. Chem. Educ. 1995, 72, 267-9.
`
`4. Stone, C. H. J. Chem. Educ. 1944, 21, 350.
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