Thursday, November 28, 2019

1. Begin Experiment "Playing With Gold Chemistry"

  1. A solution of chloroauric acid was made some months ago by dissolving 1 gram of pure gold in aqua regia.
    1. Atomic mass of gold = 196.966 grams per mole
    2. 1 gram of gold = 0.0050770 moles of gold
    3. Chloroauric acid = 339.785 grams per mole (anhydrous)
    4. 0.0050770 moles of chloroauric acid = 1.7250 grams anhydrous chloroauric acid
  2. ​​​​​​​Sodium Metabisulfite reduces chloroauric acid or gold(III) chloride to metallic gold powder
    1. ​​​​​​​Molar mass of Na2S2O5 = 190.107 grams per mole
    2. 0.0050770 moles of sodium metabisulfite = 0.965173239‬ grams

Tuesday, November 26, 2019

1. Begin Final Video EK Experimental Run With 1:1 Acetone:Methanol With Fan on Medium Speed - Reshoot

  1. The initial measurement was taken at 11:36. Video File Name = Experimental Initial Measurement
    1. HCHO = 0.992 mg/m3
    2. TVOC = 5.862 mg/m3
    3. PM2.5 = 004 μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 004 μg/m3
    6. Temperature = 14 oC
    7. Relative % Humidity = 62%​​​​​​​
  2. ​​​​​​​The 1 hour measurement was taken at 12:42 Video File Name = 1 Hour Measurement
    1. HCHO = 1.109 mg/m3
    2. TVOC = 5.971 mg/m3
    3. PM2.5 = 002 μg/m3
    4. PM1.0 = 001 μg/m3
    5. PM10 = 002 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 63%​​​​​​​
  3. ​​​​​​​The 2 hour measurement was taken at 13:49 Video File Name = 2 Hour Measurement
    1. HCHO = 0.242 mg/m3
    2. TVOC = 1.105 mg/m3
    3. PM2.5 = 002 μg/m3
    4. PM1.0 = 001 μg/m3
    5. PM10 = 002 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 57%​​​​​​​
  4. ​​​​​​​The 3 hour measurement was taken at 14:45 Video File Name = 3 Hour Measurement
    1. HCHO = 0.108 mg/m3
    2. TVOC = 0.446 mg/m3
    3. PM2.5 = 002 μg/m3
    4. PM1.0 = 001 μg/m3
    5. PM10 = 002 μg/m3
    6. Temperature = 15 oC
    7. Relative % Humidity = 56%​​​​​​​
  5. ​​​​​​​The 4 hour measurement was taken at 15:54. Video File Name = 4  Hour Measurement
    1. HCHO = 0.068 mg/m3
    2. TVOC = 0.284 mg/m3
    3. PM2.5 = 002 μg/m3
    4. PM1.0 = 001 μg/m3
    5. PM10 = 002 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 57%
​​​​​​​Monday, November 25, 2019
  
1. Begin Control VOC Test Re-filming For Final Video Control Experiment Fan on Low - Reshoot
  1. This is an repeat of Experiment #37 except this time temperature control in the shed was initiated so that these experiments would compare better with previous runs. The EK was equilibrated for about an hour and a half and then a heater was placed in the shed and the temperature was set to 18.3 oC (65 oF). As before 10 mL of a 1:1 acetone:methanol mixture was poured into an evaporating dish sitting in very recently boiled water and the doors were shut at 09:10.
  2. The initial measurement was taken at 13:24. Video File Name = Control Initial
    1. HCHO = 0.965 mg/m3
    2. TVOC = 5.606 mg/m3
    3. PM2.5 = 005 μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 005 μg/m3
    6. Temperature = 15 oC
    7. Relative % Humidity = 60%
  3. The 1 hour measurement was taken at 14:33. Video File Name = Control 1 Hour
    1. HCHO = 0.923 mg/m3
    2. TVOC = 4.956 mg/m3
    3. PM2.5 = 004 μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 004 μg/m3
    6. Temperature = 15 oC
    7. Relative % Humidity = 71%​​​​​​​
  4. The 2 hour measurement was taken at 15:38. Video File Name = Control 2 Hour
    1. HCHO = 0.285 mg/m3
    2. TVOC = 1.259 mg/m3
    3. PM2.5 = 003 μg/m3
    4. PM1.0 = 002 μg/m3
    5. PM10 = 003 μg/m3
    6. Temperature = 14 oC
    7. Relative % Humidity = 74%​​​​​​​
  5. The 3 hour measurement was taken at 16:33. Video File Name = Control 3 Hour
    1. HCHO = 0.141 mg/m3
    2. TVOC = 0.596 mg/m3
    3. PM2.5 = 005 μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 005 μg/m3
    6. Temperature = 13 oC
    7. Relative % Humidity = 77%​​​​​​​
  6. The 4 hour measurement was taken at 17:34. Video File Name = Control 4 Hour
    1. HCHO = 0.075 mg/m3
    2. TVOC = 0.321 mg/m3
    3. PM2.5 = 022 μg/m3
    4. PM1.0 = 016 μg/m3
    5. PM10 = 025 μg/m3
    6. Temperature = 12 oC
    7. Relative % Humidity = 87%

Monday, November 18th 2019  

1. Begin Experiment #44: Test Synthesis of Bismuth Tetroxide
  1. A small amount of sodium bismuthate was added to a test tube and a few mLs of water was added. 
  2. About 2 mLs of concentrated nitric acid was added to the test tube and the contents of the tube were heated with a propane torch for several minutes until vigorous boiling had occurred and the color of the solution began to change from a dark to a mid-tone red.
  3. The tube was allowed to cool and was then put into the boiling water bath to continue to react at elevated temperature for about an hour. The tube was swirled every now and again to mix up the solids.
  4. The tube was removed from the boiling water and after the reddish-orange solid was filmed the tube was covered with plastic wrap and left to sit in the lab overnight. 
  5. The next day I came out to the lab to find that the solid had turned a lighter,  more mid-tone orange. 
  6. Post Script 11/21/19: I covered the test tube with plastic wrap and sealed it with a rubber band. I then left the tube undisturbed on one of the tray tables under the canopy except to shake it up once or twice a day. The digestion process has continued with the solid residue losing all of its red color and it is now solidly orange. The solid residue has also decreased in volume exactly as the textbook describes. Although I have not tested the product I am confident that I did indeed produce bismuth tetroxide by this method. 

Sunday, November 17h, 2019
  
1. Begin Experiment #42: Synthesis of Sodium Phosphotungstate
  1. 10 grams of sodium tungstate and 5 grams of dibasic sodium phosphate were dissolved in about 25 mL of water in an evaporating dish over a boiling water bath. 
  2. 11.5 mL of 31.5% HCl was diluted down to 15 mL to prepare 15 mL of 24% HCl. This was added to the evaporating dish once the solution in it had begun to form a skin of crystals. A precipitate appeared that immediately redissolved.
  3. The solution was heated on the boiling water bath until a skin of crystals began to form. At that time it was removed from the heat and allowed to cool and crystallize.
  4. As the solution cooled it seemed as if less crystals were present. So the solution was briefly re-heated. 
  5. When trying to scrape out the crystals with a metal scoopula some of the sodium phosphotungstate turned into tungsten blue. However, it was easily filtered off.
  6. Addition of ascorbic acid produced tungsten blue and showed that some of the tungstate was lost.
  7. The product is very soluble in hot water although not so much in cold water. It is also hygroscopic to the point of deliquescence. Recrystallization should be done in a very minimal amount of water. 
  8. The identity of the product was confirmed by examination of the morphology of the product on a crystal film prepared over 3A MS in a vacuum desiccator using a dissection scope to magnify the crystals ~1600x. 

2. Begin Experiment #43: Synthesis of Sodium Silicomolybdate

  1. 1.6 grams of NaOH was dissolved in 20 mL of water. ~4.35 mL of conc. HNO3 was diluted down to a hair over 6 mL with distilled water.
  2. 5 grams of sodium molybdate was dissolved in 20 mL of hot water. The solution was boiled for a short while. 
  3. While the sodium molybdate solution boiled the 2N NaOH solution was also boiled. A few mLs of the sodium silicate solution were dropped into the boiling 2N NaOH. 
  4. Everything was removed from the heat and allowed to cool to "room temperature" (~50-55 oF). 
  5. The nitric acid was added to the sodium molybdate in portions with swirling. A precipitate formed and then disappeared. It took longer for the precipitate to disappear with each addition but it completely redissolved shortly after the last nitric acid was added.
  6. Then about 0.5 mL of sodium monosilicate solution was added to the solution. It instantly turned a vivid yellow color.
  7. The identity of the sodium silicomolybdate was verified as it precipitated out cesium as cesium silicomolybdate from 3M cesium chloride solution. 
Saturday, November 16th, 2019
  
1. Continue Experiment #41: Synthesis of Chromium(III) Glycinate
  1. All of the filtrates were recombined yesterday and the mixture was allowed to sit overnight. This morning I decanted off the dark purple solution into a 1 liter beaker and obtained about 500 mL of the liquid. The mauve and dark purple solids were discarded. The solution was then boiled to reduce its volume in the hopes that better crystals of the product would be obtained. 
  2. Once the volume of the solution was reduced by about half the beaker was removed from the heat and allowed to sit and cool slowly. 
  3. The only product to crystallize was the same mauve solid. At that point I aborted any further attempts to work with this compound and discarded the product. 
Thursday, November 14th, 2019
  
1. Continue Experiment #41: Synthesis of Chromium(III) Glycinate
  1. The chromium(III) chloride hexahydrate solidified but it did not crystallize. Instead a soft, semi-crystalline mass of chromium(III) chloride hexahydrate was obtained. Since the reaction takes place in aqueous solution the evaporating dish was weighed before any operation was carried out and was found to have a mass of 72.31 grams.
  2. The evaporating dish containing the chromium(III) chloride hexahydrate was put back on the boiling water bath and ~125mL of distilled water was added to the dish. The chromium(III) chloride hexahydrate dissolved into the water to produce an aqueous solution.
  3. Once all of the chromium(III) chloride hexahydrate was dissolved it was transferred to a 1 liter beaker. The evaporating dish was weighed again after it was empty and dried and it was found to have a mass of 56.72 grams. Given this the mass of chromium(III) chloride hexahydrate that went into the reaction is 15.59 grams and the number of moles of chromium(III) chloride hexahydrate that went into the reaction was 0.0585100 moles.
    1. Molar mass of chromium(III) hexahydrate = 266.45 grams per mole.
  4. Three molar equivalents of glycine is 0.17553‬ moles or 13.176 grams of glycine. 13.18 grams of glycine was dissolved in ~50 mL of hot water. 
    1. Molar mass of glycine = 75.067 grams per mole.
    2. Solubility = 24.99 g/100 mL at 25 °C
  5. Three molar equivalents of NaOH is 0.17553‬ moles or 7.020 grams of NaOH. 7.04 grams of NaOH was dissolved in ~20
    1. Molar mass of NaOH = 39.9971 grams per mole.
  6. The glycine solution is added to the chromium trichloride solution in the 1 liter beaker and the solution was placed on the hot plate to boil. 
  7. Once the solution was boiling the solution of sodium hydroxide was added in dropwise. 
  8. The solution failed to turn red but instead turned a vivid purple. The solution was vacuum filtered after several minutes of boiling but only a very small amount of a purple solid was obtained. The fritt was easily cleaned with water and neither product should be overly soluble in water. 
  9. The amounts of NaOH and of glycine were adjusted by adding more of them but to no avail. The solution remained a purple color. 
  10. At this point the volume of the solution had increased to about 300 mL with the extra added washings. The solution was allowed to boil down to reduce its volume and to see if any color change might occur after a long period of boiling. 
  11. This did not produce any effect. So the volume of the solution was increased to ~500 mL and it was heated up to boiling again. The rationale behind this was that the reaction had obviously produced basic chromium glycinate. However the crystals of this were too fine to filter. Some was obtained during the first filtration but most of the compound passed through the fritt. The hope was that increasing the volume of the solution and heating would cause the basic chromium glycinate to redissolve to some extent in the hope that it would produce larger crystals on cooling.
  12. The beaker was removed from the heat and was placed in ice water to cool and to allow the contents of the beaker to settle. 
Wednesday, November 13th, 2019
  
1. Begin Experiment #41: Synthesis of Chromium(III) Glycinate
  1. Chromium(III) chloride was prepared by neutralizing chromium(III) carbonate with conc. HCl diluted in distilled water. The dark green solution produced was filtered through a plug of glass wool and then poured into a 100 mL porcelain evaporating dish in order to obtain crystals of the hydrate. 
  2. The solution of chromium(III) chloride was evaporated down on a boiling water/steam bath until only ~10 mL of liquid was left in the evaporating dish. The dish was removed from the heat source, the bottom of the dish was dried, and the dish was placed in the desiccator with freshly charged 3Å molecular sieves while its contents were still hot. 
  3. The chromium(III) chloride was left in the desiccator overnight to dry out as much as possible. 
Sunday, November 10th, 2019
  
1. Begin Experiment #39: Third Run of the EK with 1:1 Acetone:Methanol at Medium Fan Speed
  1. This is an repeat of Experiment #37 except this time temperature control in the shed was initiated so that these experiments would compare better with previous runs. The EK was equilibrated for about an hour and a half and then a heater was placed in the shed and the temperature was set to 18.3 oC (65 oF). As before 10 mL of a 1:1 acetone:methanol mixture was poured into an evaporating dish sitting in very recently boiled water and the doors were shut at 09:10.
  2. The initial measurement was taken at 09:19. Video File Name = Third Run EK at Mid Speed Initial Measurement 11-10.
    1. HCHO = 0.968 mg/m3
    2. TVOC = 5.527 mg/m3
    3. PM2.5 = 013  μg/m3
    4. PM1.0 = 009 μg/m3
    5. PM10 = 015 μg/m3
    6. Temperature = 11 oC
    7. Relative % Humidity = 79%
  3. A measurement was taken at 10:29. Video File Name = Third Run EK at Mid Speed 1 Hour Measurement 11-10.
    1. HCHO = 0.991 mg/m3
    2. TVOC = 5.702 mg/m3
    3. PM2.5 = 005  μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 005 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 72%
  4. A measurement was taken at 12:40. Video File Name = Third Run EK at Mid Speed 3 Hour Measurement 11-10.
    1. HCHO = 0.102 mg/m3
    2. TVOC = 0.437 mg/m3
    3. PM2.5 = 005  μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 005 μg/m3
    6. Temperature = 17 oC
    7. Relative % Humidity = 59%
  5. A measurement was taken at 13:52. Video File Name = Third Run EK at Mid Speed 4 Hour Measurement 11-10.
    1. HCHO = 0.039 mg/m3
    2. TVOC = 0.163 mg/m3
    3. PM2.5 = 007  μg/m3
    4. PM1.0 = 005 μg/m3
    5. PM10 = 008 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 54%

2. Begin Experiment #40: Control Test Run of 1:1 Acetone:Methanol With Box Fan on Low Setting

  1. This is an exact repeat of control Experiment #38. The 1:1 acetone:methanol was poured and the doors were closed at 14:10. 
  2. The initial measurement was taken at 14:32. Video File Name = Control Run at Low Speed Initial Measurement 11-10.
    1. HCHO = 0.962 mg/m3
    2. TVOC = 5.685 mg/m3
    3. PM2.5 = 010  μg/m3
    4. PM1.0 = 007 μg/m3
    5. PM10 = 011 μg/m3
    6. Temperature = 17 oC
    7. Relative % Humidity = 53%
  3. A measurement was taken at 15:38. Video File Name = Control Run at Low Speed 1 Hour Measurement 11-10.
    1. HCHO = 0.651 mg/m3
    2. TVOC = 3.469 mg/m3
    3. PM2.5 = 010  μg/m3
    4. PM1.0 = 007 μg/m3
    5. PM10 = 011 μg/m3
    6. Temperature = 17 oC
    7. Relative % Humidity = 63%
  4. A measurement was taken at 16:48. Video File Name = Control Run at Low Speed 2 Hour Measurement 11-10.
    1. HCHO = 0.252 mg/m3
    2. TVOC = 1.151 mg/m3
    3. PM2.5 = 016  μg/m3
    4. PM1.0 = 012 μg/m3
    5. PM10 = 018 μg/m3
    6. Temperature = 17 oC
    7. Relative % Humidity = 65%
  5. A measurement was taken at 17:51. Video File Name = Control Run at Low Speed 3 Hour Measurement 11-10.
    1. HCHO = 0.155 mg/m3
    2. TVOC = 0.651 mg/m3
    3. PM2.5 = 038  μg/m3
    4. PM1.0 = 028 μg/m3
    5. PM10 = 044 μg/m3
    6. Temperature = 14 oC
    7. Relative % Humidity = 79%
  6. A measurement was taken at 18:59. Video File Name = Control Run at Low Speed 4 Hour Measurement 11-10.
    1. HCHO = 0.059 mg/m3
    2. TVOC = 0.246 mg/m3
    3. PM2.5 = 020  μg/m3
    4. PM1.0 = 015 μg/m3
    5. PM10 = 023 μg/m3
    6. Temperature = 11 oC
    7. Relative % Humidity = 83%
Saturday, November 9th, 2019
  
1. Begin Experiment #37: Second Run of the EnviroKlenz with 1:1 Acetone:Methanol at Medium Fan Speed
  1. This is a repeat of yesterdays experiment. There was a cold snap last night with temperatures reaching a few degrees below O oC so the testing was delayed a short while until the sun was fully up and the atmosphere in the shed had warmed up significantly. During that time the EnviroKlenz was run on high to equilibrate it in preparation for the tests. This process was begun at 08:19 and continued until the experiment began at 09:47.
  2. The unit was switched to medium speed at 09:48. The meter was turned on after equilibrating outside for several hours and the warm up and calibration were done as normal. As usual 10 mL of a 1:1 acetone:methanol mixture was used and it was dispersed in the shed in the normal way. The EK was allowed to run during this process to disperse the vapors. The process was begun and the doors were shut at 10:18.
    1. I noticed yesterday that I had not changed the time on the air quality meter to reflect the start of Daylight Savings Time. Thus there is a 1 hour discrepancy in the times recorded that the measurements were taken in these notes and on the videos of those measurements being taken. The error has been corrected and the meter now reads the correct time.  
  3. The initial measurement was taken at 10:31. Video File Name = Second Run EK at Mid Speed Initial Measurement 11-9.
    1. HCHO = 0.970 mg/m3
    2. TVOC = 5.538 mg/m3
    3. PM2.5 = 003  μg/m3
    4. PM1.0 = 002 μg/m3
    5. PM10 = 003 μg/m3
    6. Temperature = 12 oC
    7. Relative % Humidity = 47%
  4. A measurement was taken at 11:28. Video File Name = Second Run EK at Mid Speed 1 Hour Measurement 11-9.
    1. HCHO = 0.429 mg/m3
    2. TVOC = 2.037 mg/m3
    3. PM2.5 = 003  μg/m3
    4. PM1.0 = 002 μg/m3
    5. PM10 = 003 μg/m3
    6. Temperature = 10 oC
    7. Relative % Humidity = 56%
  5. A measurement was taken at 12:42. Video File Name = Second Run EK at Mid Speed 2 Hour Measurement 11-9.
    1. HCHO = 0.133 mg/m3
    2. TVOC = 0.558 mg/m3
    3. PM2.5 = 003  μg/m3
    4. PM1.0 = 002 μg/m3
    5. PM10 = 003 μg/m3
    6. Temperature = 11 oC
    7. Relative % Humidity = 52%
  6. Al measurement was taken at 13:50. Video File Name = Second Run EK at Mid Speed 3 Hour Measurement 11-9.
    1. HCHO = 0.046 mg/m3
    2. TVOC = 0.192 mg/m3
    3. PM2.5 = 004 μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 004 μg/m3
    6. Temperature = 10 oC
    7. Relative % Humidity = 55%

2. Begin Experiment #38: Control Test Run of 1:1 Acetone:Methanol With Box Fan on Low Setting

  1. Exactly as above in Experiment #37 except using a box fan running on its lowest setting to approximate the movement of a similar volume of air to the EK. The solvent mixture was poured and the doors were closed at 14:14.
  2. The initial measurement was taken at 14:21. Video File Name = Control Run Box Fan at Low Speed Initial Measurement 11-9.
    1. HCHO = 0.968 mg/m3
    2. TVOC = 5.672 mg/m3
    3. PM2.5 = 004  μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 004 μg/m3
    6. Temperature = 11 oC
    7. Relative % Humidity = 47%
  3. A measurement was taken at 15:30. Video File Name = Control Run Box Fan at Low Speed 1 Hour Measurement 11-9.
    1. HCHO = 0.621 mg/m3
    2. TVOC = 3.090 mg/m3
    3. PM2.5 = 032  μg/m3
    4. PM1.0 = 024 μg/m3
    5. PM10 = 037 μg/m3
    6. Temperature = 10 oC
    7. Relative % Humidity = 57%
  4. A measurement was taken at 17:01. Video File Name = Control Run Box Fan at Low Speed 2 And A Half Hour Measurement 11-9.​​​​​​​
    1. HCHO = 0.242 mg/m3
    2. TVOC = 1.081 mg/m3
    3. PM2.5 = 018  μg/m3
    4. PM1.0 = 013 μg/m3
    5. PM10 = 020 μg/m3
    6. Temperature = 9 oC
    7. Relative % Humidity = 70%​​​​​​​
  5. A measurement was taken at 17:51. Video File Name = Control Run Box Fan at Low Speed 3 And A Half Hour Measurement 11-9.​​​​​​​
    1. HCHO = 0.129 mg/m3
    2. TVOC = 0.528 mg/m3
    3. PM2.5 = 017  μg/m3
    4. PM1.0 = 012 μg/m3
    5. PM10 = 019 μg/m3
    6. Temperature = 8 oC
    7. Relative % Humidity = 76%​​​​​​​

3. Begin Experiment #39: Synthesis of Molybdenum Trioxide From Molybdenum Metal in Fused Potassium Nitrate

  1. 5 grams of molybdenum pellets were weighed out and combined with enough potassium nitrate powder to cover the bottom of the crucible to a depth of about 1 centimeter. 
  2. The crucible was heated with a Meker Burner at low heat to melt the KNO3
Friday, November, 8th, 2019
  
1. Begin Experiment #36: First Run of the EnviroKlenz with 1:1 Acetone:Methanol at Medium Fan Speed
  1. This is an exact repeat of Experiment #28 except in this run the fan speed will be set to medium. The unit was equilibrated for one hour at medium speed before running the test. The unit was not turned off when the test began in order to facilitate homogeneity of the atmosphere in the shed. The dish of acetone:methanol was placed on the surface of the very recently boiled water and the doors were closed at 13:00.
  2. The meter was equilibrated and calibrated as normal. The first measurement was taken at 13:11. This was recorded. Video File Name = First Test Run EK at Mid Speed Initial Measurement 11-8.
    1. HCHO = 0.971 mg/m3
    2. TVOC = 5.641 mg/m3
    3. PM2.5 = 002  μg/m3
    4. PM1.0 = 001 μg/m3
    5. PM10 = 002 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 46%
  3. The meter was re-equilibrated and re-calibrated. A measurement was taken at 14:11. This was recorded. Video File Name = First Test Run EK at Mid Speed 1 Hour Measurement 11-8.​​​​​​​
    1. HCHO = 0.971 mg/m3
    2. TVOC = 5.641 mg/m3
    3. PM2.5 = 002  μg/m3
    4. PM1.0 = 001 μg/m3
    5. PM10 = 002 μg/m3
    6. Temperature = 16 oC
    7. Relative % Humidity = 46%
  4. ​​​​​​​The meter was re-equilibrated and re-calibrated. A measurement was taken at 15:23. This was recorded. Video File Name = ​​​​​​​First Test Run EK at Mid Speed 2 Hour Measurement 11-8.​​​​​​​
    1. HCHO = 0.229 mg/m3
    2. TVOC = 1.327 mg/m3
    3. PM2.5 = 005  μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 005 μg/m3
    6. Temperature = 15 oC
    7. Relative % Humidity = 62%​​​​​​​
  5. The meter was re-equilibrated and re-calibrated. A measurement was taken at 16:12. This was recorded. Video File Name = ​​​​​​​First Test Run EK at Mid Speed 3 Hour Measurement 11-8.​​​​​​​
    1. HCHO = 0.185 mg/m3
    2. TVOC = 0.826 mg/m3
    3. PM2.5 = 006  μg/m3
    4. PM1.0 = 004 μg/m3
    5. PM10 = 006 μg/m3
    6. Temperature = 15 oC
    7. Relative % Humidity = 68%​​​​​​​
  6. The meter was re-equilibrated and re-calibrated. A measurement was taken at 18:07. This was recorded. Video File Name = ​​​​​​​First Test Run EK at Mid Speed 4 Hour Measurement 11-8.​​​​​​​
    1. HCHO = 0.066 mg/m3
    2. TVOC = 0.272 mg/m3
    3. PM2.5 = 005  μg/m3
    4. PM1.0 = 003 μg/m3
    5. PM10 = 005 μg/m3
    6. Temperature = 13 oC
    7. Relative % Humidity = 74%​​​​​​​
Wednesday, November 6th, 2019 - Thursday, November 7th, 2019
  
1. Begin Experiment #35: Synthesis of Rubidium Dichromate (Source: Handbook of Preparative Inorganic Chemistry, Ferdinand Enke Verla, Georg Brauer ed., 2nd Ed., Vol. 2, pages 1388-1389)
  1. (NH4)2Cr2O7 + 2RbCl → Rb2Cr2O7 + 2NH4Cl
    1. Ammonium dichromate = 252.07 grams per mole
      1. 0.09022419596 moles of ammonium dichromate = 22.74 grams
      2. Solubility: 18.2 g/100ml (0 °C), 35.6 g/100ml (20 °C), 40 g/100ml (25 °C), 156 g/100ml (100 °C)
    2. Rubidium chloride = 120.921 grams per mole
      1. 21.82 grams of RbCl = 0.18044839192 moles
      2. Solubility: 77 g/100mL (0 °C), 91 g/100 mL (20 °C), 130 g/100 mL (100 °C)
    3. Rubidium dichromate = 386.92 grams per mole
      1. 0.09022419596 moles of rubidium dichromate = 34.91 grams
      2. Solubility: Moderately soluble in water (5% at 18°C). ~5 g/100mL
        1.  Monoclinic: g/100g H2O: 5.9 (20°C), 10.0 (30°C), 15.2 (40°C), 32.3 (60°C);
        2. Triclinic: g/100g 5.8 (20°C), 9.5 (30°C), 14.8 (40°C), 32.4 (60°C) Data Source
    4. Ammonium chloride = 53.491 grams per mole
      1. 0.206746553 moles of ammonium chloride = 9.65 grams
      2. Solubility: 24.4 g/100mL (−15 °C), 29.4 g/100mL (0 °C), 38.3 g/100mL (25 °C), 45.44 g/100mL (40 °C), 74.08 g/100mL (100 °C)
  1. In one 250 mL beaker 22.74 grams of ammonium dichromate is dissolved in ~75 mL of warm water.
  2. In a second 250 mL beaker 21.82 grams of rubidium chloride is dissolved in ~50 mL of warm water. 
  3. The two solutions are combined and mixed thoroughly.
  4. The solutions are allowed to cool and bright orange crystals of rubidium chromate crystallize out of solution.
    1. Crystals of rubidium dichromate appeared almost immediately on combining the two solutions. Crystal formation began at the surface of the mixed liquids and then rapidly proceeded throughout the entire body of the mixture. 
  5. The crude crystals are filtered out and dried. 
    1. ​​​​​​​I dried the crude crystals out overnight and into the next day over 3Å molecular sieves.
  6. The crude crystals are contaminated with ~5% ammonium dichromate. To remove it the product is calcined at low temperature.
    1. ​​​​​​​On 11/7/19 I calcined 10 grams of the crude product. The calcination was done at 190.5 oC (375 oF) for the first 45 minutes followed by 15 minutes at 204.5 oC (400 oF). This gave a very dark reddish-gray product. This was dissolved in water and filtered through a cotton plug. Then the filtrate was filtered through a 0.2 μm pore filter to exclude any microscopic particles of chromium(III) oxide produced by the thermal decomposition of the ammonium dichromate. 
  7. Recrystallization gives an excellent yield of rubidium dichromate. Trimorphic; forms A and B deposit together from solution above 35°C. Orange-colored monoclinic or red triclinic crystals.
Sunday, November 3, 2019

1. Begin Experiment #34: First Run of the EnviroKlenz with 5 mL of 37% Formaldehyde

  1. This was a modified repeat of Experiment #28 but done with 5 mL of 37% formaldehyde solution instead of 1:1 acetone:methanol. Also the EnviroKlenz was turned on when the formaldehyde was floated on the hot water in the evaporating dish rather than waiting as before. This was done to ensure mixing of the lighter formaldehyde into the atmosphere of the enclosure. The meter, which had been equilibrated and calibrated as normal, was left sitting on top of the EnviroKlenz unit and it's internal recording feature was started. The doors were closed and the atmosphere in the shed was allowed to equilibrate at 11:24.
    1. After 1:20 the meters alarm sounded alerting to the presence of dangerous levels of formaldehyde in the shed. 
  2. After the atmosphere in the shed was thoroughly mixed I opened the doors and went inside just long enough to retrieve the pot of wat4er and to obtain the meter. I did this at 11:29. This was recorded. Video File Name = 1 First Formaldehyde Test Initial Measurement 11-2. 
    1. HCHO = 0.971 mg/m3
    2. TVOC = 5.544 mg/m3
    3. PM2.5 = 002  μg/m3
    4. PM1.0 = Data Not Recorded
    5. PM10 = Data Not Recorded
    6. Temperature = 15 oC
    7. Relative % Humidity = 44%
      1. ​​​​​​​Note recording only lasts for a short time.
      2. Formaldehyde diffuses off the detector faster than acetone or methanol. This was predicted as it is more volatile than both previously used VOCs. ​​​​​​​​​​​​​​
  3. A second reading was taken at 13:10. This was recorded. Video File Name = 2 First Formaldehyde Test Second Measurement 11-2. 
    1. HCHO = 0.254 mg/m3
    2. TVOC = 1.126 mg/m3
    3. PM2.5 = 001  μg/m3
    4. PM1.0 = 000 μg/m3
    5. PM10 = 001 μg/m3
    6. Temperature = 14 oC
    7. Relative % Humidity = 62%
  4. A second reading was taken at 13:10. This was recorded. Video File Name = 2 First Formaldehyde Test Second Measurement 11-2. 
    1. HCHO = 0.254 mg/m3
    2. TVOC = 1.126 mg/m3
    3. PM2.5 = 001  μg/m3
    4. PM1.0 = 000 μg/m3
    5. PM10 = 001 μg/m3
    6. Temperature = 14 oC
    7. Relative % Humidity = 62%​​​​​​​
  5. A third reading was taken at 13:44. This was recorded. Video File Name = 3 First Formaldehyde Test Third Measurement 11-2. 
    1. HCHO = 0.121 mg/m3
    2. TVOC = 0.523 mg/m3
    3. PM2.5 = 001  μg/m3
    4. PM1.0 = 000 μg/m3
    5. PM10 = 001 μg/m3
    6. Temperature = 15 oC
    7. Relative % Humidity = 55%
Saturday, November 2, 2019
  
1. Begin Experiment #33: Indium Monoiodide from Indium(III) Iodide and Indium Metal
  1. Indium(III) iodide was prepared by dissolving indium metal in hydriodic acid prepared on October 29th. The solution obtained from this reaction was filtered and then evaporated in a 100 mL evaporating dish over boiling water. Once solidified the dish was placed in the desiccator with freshly recharged 3Å molecular sieves. The desiccator was placed in the sun covered with a cloth for the indium(III) iodide to fully dry. 
    1. Indium tri-iodide, InI3, is produced when indium is heated with an excess of iodine in an atmosphere of carbon dioxide. It is a hygroscopic, yellow solid, melting at c. 200° to a red liquid which can be slowly distilled in carbon dioxide at high temperatures. The tri-iodide is soluble in water, alcohol, ether, chloroform, and xylene. http://indium.atomistry.com/indium_tri_iodide.html
    2. Indium mono-iodide, InI, is produced when an excess of indium is heated with iodine. Small quantities must be used, unless the reaction is carried out in an atmosphere of carbon dioxide. Indium tri-iodide is reduced to the mono-iodide by repeated distillation in hydrogen. It is a brownish-red solid, which melts at 351° and boils at c. 700°, and maybe distilled in carbon dioxide. Indium mono-iodide is not attacked by hot water, but dissolves in dilute acids with the evolution of hydrogen. It is insoluble in alcohol, ether, and chloroform. The simultaneous action of air and water leads to the production of indium hydroxide and hydriodic acid. This action is slow with cold water, and the hydroxide is obtained in colloidal solution, but with hot water the hydroxide separates in a form easily filtered. http://indium.atomistry.com/indium_mono_iodide.html
  2. The indium(III) iodide was dissolved in xylenes and then indium metal was added to the mixture. No steps were taken to exclude water during this run. The mixture was connected to a vertical condenser and refluxed for an hour.
  3. A white ppt formed as the reflux mixture was cooled. The pieces of indium metal were still intact but were coated with a dark red substance tentatively identified as indium(I) iodide.

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