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Five white solids

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How a first-year heat lab moved from hot metal to five white solids in a plain beaker.

AluminiumBrassIronCopperIceAcid-base titrationHeat capacity of a metalSize of the temperature changeThermometer precisionHeat leakWaterEthanolSilicone oilAluminium9%Brass14%Iron25%Copper46%050%Gap from the literature heat capacityAcid, molHeatNeutralisation, then titrate to check12345See the solid dissolveFeel the glass warm or coolHeat crosses the glassAbout 4 g of solid40.0 mL of waterStartLowest or highestHeat of dissolution, kJ per gWarms the waterCools the waterAcid up, base down, per gramKOHNaClUreaToo close to callCitric acidAscorbic acidAcidsBaseAscorbic acidCitric acidTitrant, same molar concentration0-1.00.3Heat of dissolution, kJ per gPotassium hydroxideSodium chlorideCitric acidAscorbic acidUreaLiteratureClass mean, sdCitric acid, g per mol185230Anhydrous 192Monohydrate 210+ one water, 18Class mean 217KOHNaClCitricAscorbicUreaJournal of Chemical Education, 2020ThermometerCold metalLiquidsNeutralisationPublishedThermometerCold metalLiquidsNeutralisationPublishedPublished designRationale1 / 20
  1. Rationale

    1For years our first-year chemistry lab taught two set pieces in separate weeks: an acid-base titration, and a hot metal dropped into water to watch the heat move.From ICCH224 syllabi, 2018-19 · Paper, pp. 2356-2357 · Equipment sketches, p. 1

  2. 2Three things set how well heat can be measured: how big the temperature change is, how precise the thermometer is, and how much heat the calorimeter lets through.From Paper, p. 2357 (Background) · Equipment sketches, p. 3

  3. Prototype 1: Thermometer

    3In the trials, my first change was the thermometer: a digital probe in place of the glass one made the readings more precise.From Equipment sketches, p. 1

  4. Prototype 2: Cold metal

    4In the next trial I turned the experiment around: the metal was chilled in an ice bath, then dropped into room-temperature water.From Week 5 methods, pp. 1-2 · Equipment sketches, p. 2

  5. Prototype 3: Liquids

    5I also tried other liquids in the calorimeter, ethanol and silicone oil, and water worked best.From Week 5 methods, pp. 1-2 · Equipment sketches, p. 1

  6. Prototypes: The gap

    6Even so, the metal values stayed too far from the literature: in our hot-metal trials the mean absolute error ran from about 9% for aluminium to 46% for copper, too far to check the Dulong-Petit law.From Heat capacity workbook, aggregate · Paper, p. 2357

  7. Prototype 4: Neutralisation

    7So I tried neutralisation instead: an acid and a base react fast with a large temperature change, which is likely to produce better results, and a titration can check the answer.From Paper, p. 2357 · Calorimetry trial 3 sketch, p. 1

  8. Final: Design

    8The design we published uses five white solids, each with its own heat of dissolution, and a titration for the two that heat alone cannot tell apart.From Paper, abstract and p. 2358 · Paper, graphical abstract and Figure 1

  9. 9The plain beaker is a choice: heat moves in and out through the glass, and in return students see the solid dissolve and feel the beaker warm or cool.From Paper, pp. 2358-2359

  10. 10A plain 50 mL beaker took the place of an insulated calorimeter: about 4 g of solid into 40.0 mL of water, reading the starting temperature and the lowest or highest one.From SI instruction sheet, p. 2 · Paper, p. 2358, Figure 1

  11. Final: Findings

    11Each solid becomes a point on one axis: its literature heat of dissolution per gram, warming the water to the left and cooling it to the right.From Paper, Figure 2 and Table 1

  12. 12Heat alone names three: potassium hydroxide warms the water most, urea cools it most, and table salt barely moves it.From Paper, p. 2359 and Table 1

  13. 13The two acids are too close for heat to separate: citric acid 0.100 against ascorbic acid 0.118 to 0.124 kJ per gram.From Paper, Table 1 and p. 2358

  14. 14So students titrate each acid with the potassium hydroxide solution to a phenolphthalein end point: at the same molar concentration, citric acid needs about 3-fold the titrant of ascorbic acid.From Paper, p. 2358 · Paper, Figure 2 and p. 2359

  15. 15On the map that becomes a second axis, acid or base equivalents per gram: citric acid rises well above ascorbic acid, and the only base drops below zero.From Paper, Figure 2 and p. 2358

  16. 16With help from the instructor, ranking the five on this map is enough to match them, with no calculation at all.From Paper, p. 2359

  17. 17In class, 18 results per compound gave means of ascorbic acid 0.109, citric acid 0.113, potassium hydroxide -0.505, table salt 0.048 and urea 0.211 kJ per gram.From Paper, Table 1 · SI class results, aggregate

  18. 18The titration also weighed the hidden water: the class put citric acid at 217 g per mol, above 192 for the anhydrous form, and most students answered monohydrate.From Paper, Table 1 and p. 2358

  19. Final: Impact

    19Every student matched the five compounds.From Paper, p. 2358 (Results)

  20. 20The two set pieces I started with, calorimetry and titration, became one problem: matching five unknowns. We published it in the Journal of Chemical Education in 2020.From Paper, pp. 2356-2359

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