Trial Batch Test Results, Copyright Paul Gobert Nov 2001.

No reproduction without permission.
Constant methanol level(225ml/L WAF), various NaOH levels.
Waste Animal Fat (Frytol)

Titration 2.2ml 0.1% NaOH,indicates optimum 5.7g/L

Agitation, 1Litre of warm oil + methoxide into plastic 2L softdrink bottle.
Shaken vigorously for 10 to 15 seconds.
Temp of reaction 55 deg C.
NaOH used in conc aqueous solution form.
weights represent equivalent ammount of NaOH, ie multiply the weight quoted
by 1.2 to obtain the ammount of NaOH solution I used.

Test methods.
SG. 100ml volumetric flash. weight of contents/100

Viscosity. Time to drain 100ml pipette. Timing from when BD passes graduated
mark to when stream changes to drop. result expressed in seconds.
(Water 25.9 sec, Distillate 30.3 sec,20 grade auto transmission fluid 130
sec.)

pH. 1ml of BD mixed with 1 ml of isopropyl alcohol and treated with
universal indicator liquid.

Acidity. 1ml of BD or WAF mixed with 10ml isopropyl alcohol, phenolphthalein
indicator added,titrated with 0.1% NaOH, result expressed in mls.

RAW BD. 16hrs settling.
g/L........Glycerine............Glycerine.............................BD/gly
cerine Interface
NaOH.Appearance......Composition..............
4.2......Dark,liquid.............uniform........................indistinct,a
lot of meally white material.
4.7......dark,solid...............uniform.......................slight
ammount of meal at interface.
5.2......dark,solid...............uniform.......................small
ammount of meal at interface.
5.7......dark,solid...............uniform.......................good
separation.
6.3......dark,solid..............10% gelatinous
6.8......dark,solid..............25% gelatinous
7.3......dark,solid..............33% gelatinous material+clumps/lumps
7.8......dark,solid,.............50% gelatinous material+clumps/lumps
8.3......dark,solid............100% gelatinous,clumps/lumps.
8.8......dark,solid............. total volume (BD+glycerine)set solid

(Gelatinous deposit in glycerol layer is pale brown in colour with whitish
flecks and increases volume of glycerine layer. See Raw BD yields below).

Raw BD Yields.
BD volume as a % of origional WAF volume.

NaOH Level.................%yield of BD relative to vol WAF used.
4.2g/L...........................>72% Difficulty separating from lower
level.
4.7................................99%
5.2................................98%
5.7(titn)........................95%
6.3................................95%
6.8................................93%
7.3................................85%
7.8................................66%
8.3................................61%

All samples chilled to 9 deg C, held there for 2 days. Allowed to thaw at
room temp (28 deg C). Tallow deposits in all samples.
Vacuum filtration through filter paper (Watman No.1, Buchner funnel + Flask)

NaOH.......Ease of Filtering.....................................Deposit on
filter paper.
4.2g/L........medium...............................................gelatinou
s + whitish deposit.
4.................medium...............................................gelat
inous + crumbly whitish deposit.
5.2..............medium/fast.......................................slight
gelatinous + crumbly whitish deposit.
5.7..............fast......................................................n
o deposit
6.3..............fast......................................................n
o deposit
6.8.............slow.....................................................a
lot of gelatinous material.
7.3............ not recorded
7.8............medium................................................a lot
of gelatinous material.
8.3.............fast.......................................................a
lot of gelatinous material.

Filtered samples stood for 5 days.
NaOH..................................Deposit...............................
..............................................BD
4.2g/L.....25%(of total volume)white sludge + 1/4 cm dark glycerine.........
.....Fairly clear.
4.7..........33% white sludge + 1/2 cm of dark
glycerine....................................Fairly clear.
5.2..........50% white sludge + 1 cm of dark
glycerine.......................................Murky
5.7..........(settled washed and dried prior to standing [impatient],
.................crystal clear stable product
6.3..........gelatinous flock + whitish slurry
6.8..........gelatinous flock + whitish slurry (less than for
6.3).............................Murky
7.3..........gelatinous
flock.......................................................................
...............murky
7.8.........50% flock + some dark liquid on
bottom..............................................fairly clear.
8.3.........33% flock + slight ammount of dark liquid on
bottom.........................fairly clear.


Bubble Washing.
Wash vessel, 2l cylindrical separating "funnel",95mm diameter, wash water
temp 26 deg C (ambient) ww pH 8, BD washed with equal volumes of water.
NaOH
Level
4.2g/L........A lot of persistent foam, 1st wash intermittent, 4 wash/rest
cycles required, pH 9, Addition of water to top for second wash killed
foam.BD sep[arated better after each wash. At finish of wash meally material
released.
4.7..............Persistent foam intermittent bubble washing required.
5.2..............Washed well
5.7(titn)......Washed well,little foam settled and decanted well.
6.3.............Washed well, first wash head of foam equiv to total liquid
volume. Some meally solid at surface of BD.
6.8.............Washed well.
7.3............Washed well,v.small ammount of unstable foam in 1st wash. BD
separated from water well aslarge discrete globules.1st wash very milky pH9.
Second wash water clear, good separation.
7.8............Washed well,v.small ammount of unstable foam in 1st wash. BD
separated from water well               as large discrete globules.1st wash
very milky pH9. Second wash water clear, good separation.
8.3. .........washed well, as for 7.8.

Final wash water drained from sep funnel,washed BD filtered through Watman
No.1 filter paper (filtering much easier/quicker with higher NaOH level
samples).Filtrate was crystal clear except for low level NaOH samples. The
5.7g sample was dried (45 deg C) but the others were not, with the exception
of one which was dried to determine if this would release any water. It did
not.
Heat drying unfiltered BD could liquify any beef tallow present which can
result in cloudy BD upon standing for a short time. This cloudyness will
settle out over time.

Results of tests on final product,settled,washed and filtered.
NaOH......................Visc...........................Acidity
g/L.........SG......sec/100ml pipette...pH.......mls of 0.1% NaOH
4.2.......0.8798.........37.96.............5.5.......0.54
4.7.......0.8774.........36.89.............5.5.......0.54
5.2.......0.8735.........35.68.............5.5.......0.61
5.7.......0.8722.........35.90.............5.5.......0.61
6.3.......0.8708.........34.86.............5.5.......0.31
6.8.......0.8695.........34.73.............5.5.......0.45
7.3.......0.8683.........34.30.............5.5.......0.38
7.8.......0.8711.........34.48.............5.5.......0.45
8.3.......0.8685.........34.11.............5.5.......0.61
8.8 set solid no liquid BD.


I hope this information is of use. Quite a few factors to ballance depending
upon your processing method.
Whilst these results would be reproducable from the same feedstock there
could be some variation with other oils/fats/beef tallow contents.
The above information should be used as a guide and supported by tests on
the oil/fat to be used.

Regards     Paul Gobert.

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