I heated the boiler with 8 litres of 30% ABV wash until vapour temp after dephlagmator crossed 50C. Then I started cooling the condenser and dephlagmator. I left it running for full reflux for 40 mins or so and then then I reduced cooling slowly until some drops started to appear.
I saw the first drops appear at 71.8, then at 77.1 and then at 78.4. The number can be few places off because of maybe a not-so-accurate thermometer. I have highlighted them in the table
I found these numbers in the table at viewtopic.php?t=72149 but could not the understand the labels much even after reading the references.
All I could understand that P(primary) mass % + S(Secondary) mass % = 100. And the ABV I am getting at the most red line is like 70% as in the table.
| Primary | Secondary | Tertiary | Mix BP °C | P BP °C | S BP °C | T BP °C | P mass % | S mass % | T mass % | Notes |
| Acetaldehyde | 21 | 21 | 100 | No water azeotrope | ||||||
| Ethyl formate | Methanol | 51 | 54.1 | 64.7 | 84 | 16 | ||||
| Methyl Acetate | Methanol | 53.8 | 57 | 64.7 | 81.3 | 18.7 | ||||
| Acetone | Methanol | 55.7 | 56.5 | 64.7 | 87.9 | 12.1 | ||||
| Methyl Acetate | Water | 56.1 | 57 | 100 | 95 | 5 | ||||
| Acetone | 56.5 | 56.5 | 100 | No water azeotrope | ||||||
| Methyl Acetate | Ethanol | 56.9 | 57 | 78.44 | 97 | 3 | ||||
| Ethyl Acetate | Methanol | 62.3 | 77.1 | 64.7 | 56 | 44 | ||||
| Methanol | Isopropanol | 64 | 64.7 | 82.5 | 80 | 20 | ||||
| Methanol | 64.7 | 64.7 | 100 | No water azeotrope | ||||||
| Ethyl Acetate | Water | 70.4 | 77.1 | 100 | 91.9 | 8.1 | ||||
| Ethyl Acetate | Ethanol | 71.8 | 77.1 | 78.44 | 69.2 | 30.8 | ||||
| Diacetyl | Ethanol | 73.9 | 88 | 78.44 | 53 | 47 | ||||
| Isopropyl acetate | Isopropanol | Water | 75.5 | 101.6 | 82.5 | 100 | 76 | 13 | 11 | Ternary azeotrope |
| Ethanol | isopropyl acetate | 76.8 | 78.44 | 88.4 | 53 | 47 | ||||
| Ethanol | Methyl butyrate | Water | 77.62 | 78.44 | 102.34 | 100 | 56.63 | 34.88 | 8.49 | Ternary azeotrope |
| Ethanol | Methyl butyrate | 78.13 | 78.44 | 102.34 | 80.78 | 19.22 | ||||
| Ethanol | Water | 78.29 | 78.44 | 100 | 95.68 | 4.32 | ||||
| Diacetyl | Water | 78.5 | 88 | 100 | 89.29 | 10.71 | ||||
| Isopropanol | Water | 80.4 | 82.5 | 100 | 87.7 | 12.3 | ||||
| N-Propyl acetate | Water | Propanol | 82.2 | 101.6 | 100 | 97.3 | 59.5 | 21 | 19.5 | Ternary azeotrope |
| N-Propyl acetate | Water | 82.4 | 101.6 | 100 | 86 | 14 | ||||
| Methyl butyrate | Water | 84.77 | 102.34 | 100 | 82.11 | 17.89 | ||||
| Propanol | Water | 88.24 | 97.3 | 100 | 71.03 | 28.97 | ||||
| Isobutanol | Water | 90 | 108 | 100 | 70 | 30 | ||||
| Isobutyl acetate | Water | 90.26 | 118.04 | 100 | 75.6 | 24.4 | ||||
| N-Butyl acetate | Water | N-Butanol | 90.6 | 125.94 | 100 | 117.8 | 63 | 29 | 8 | Ternary azeotrope |
| N-Butyl acetate | Water | 90.7 | 125.94 | 100 | 72.9 | 27.1 | ||||
| Ethyl butyrate | Water | 91.4 | 120.54 | 100 | 73.24 | 26.76 | ||||
| Butanol | Water | 92.4 | 117.8 | 100 | 55.5 | 44.5 | ||||
| N-Butyl acetate | Water | 92.98 | 125.94 | 100 | 69 | 31 | ||||
| Water | Isoamyl alcohol | Isoamyl acetate | 93.6 | 100 | 130.54 | 142 | 44.8 | 31.2 | 24 | Ternary azeotrope |
| Propyl butyrate | Water | 94.91 | 142.74 | 100 | 61.74 | 38.26 | ||||
| Isoamyl alcohol | Water | 95.31 | 130.54 | 100 | 51.33 | 48.67 | ||||
| Water | Iso-butyric acid | 99.3 | 100 | 154.5 | 79 | 21 | ||||
| Water | Butyric acid | 99.94 | 100 | 163.5 | 81.6 | 18.4 | ||||
| Water | Propionic acid | 99.98 | 100 | 141.1 | 82.3 | 17.7 | ||||
| Formic acid | Water | 107.3 | 100.8 | 100 | 77.5 | 22.5 | Negative azeotrope | |||
| Acetic acid | 118.1 | 118.1 | 100 | No water azeotrope |
The drops were not like drops but filled a litre or so. I was boiling 8 litres of 30% ABV.
At no time my ABV was >80. I use an optical ABV refractometer than has shown me 80 % in my Airstill (Pot still)
I use a 20 litre boiler with a 1400w hot plate.
I use recirculated water
My reflux still is here . viewtopic.php?t=76373
It has a very tightly packed 500mm column (With copper mesh)
Are these three different temps normal?
Which temp I should aim after the dephlagmator?
How do I get a higher ABV? I have tried running it slow as well. The Boiler vapour temp was like 80 C. I used a bimetallic thermometer for this.
Thanks in advance.