Lee R.

Madsen II, Research Associate†/Doctoral Student‡

†
LSU AgCenter, ‡ LSU Dept. of Chemistry

Funded in part by: the Louisiana Board of Regents,

the American Sugarcane League and Cargill, N.A.
Things Were not looking good…

Left, syrup
A, without
dilutedIron;
to 32%bx
B, with Iron
Right, decolorized syrup diluted to 32%bx
Amino Acids React with Phenolics in the Presence of Iron

77g/mL
Left, Caffeic acid with varying amounts of iron added
Right, Caffeic acid and glutamine with varying
amounts of iron
 Eureka!
Why was this leading to an increase in color?
The complexes formed are highly colored and
polymerization via Fe is relatively slow.
Result? Highly colored molecules that are too
small to ppt.
Maybe the free NH2 groups on the protein in the
raw juice might react with Fe complexed
phenolics, causing the adducts to precipitate
(ppt).
When tested on Raw juice, we saw rapid ppt.
with a concomitant removal of color.
The Goods:

Left, Mixed Juice clarified

normally

Right, DC juice, treated

with 400 mg/kg ds Fe3+ and
then hot-limed normally
 How we are doing this:
The raw juice is treated with Fe at ambient
temperature (20-30°C). Cationic flocculant
increases the settling rate significantly, but is
not required if this is run hotter*.

The first stage is settled and decanted then is

subject to hot-liming with anionic flocculant
(5 ppm max.)

*Greater density gradient, but is limited by iron dosage, discussed later.

Iron in Juice:
There is a threshold on
iron concentration where
flocculation/
decolorization is most
efficient.
Fe g/g: 0, 50, 100, 150, 200, 250, 300, 350, 400, 450, 500, 1000
Raw juice, settling, top.

Raw juice, decanted,

bottom.
 The Fine Print
The method works well and can eliminate in
excess of 70% of the colored materials
expressed from cane.
Higher temperatures lead to run-away color
formation. The upper temp. is dictated by
the amount of iron applied.
It appears to be reliable only with good
juice. Juice that is badly deteriorated
(microbially) is made worse. Why?
 How Does This Work?
The hypothesis: The phenolic materials are
oxidized by iron/O2 and couple to free NH2
groups on the protein. These protein:phenolic
adducts can precipitate.

In order to help verify this, the system was

“reverse-engineered” from raw sugar “melts”.
 How Does This Work?
Using BSA and Fe it
was found that CFA can be
made to precipitate
quantitatively from water.

In solutions of raw sugar, the

behavior is not straight-forward.
It was found that acetate,
applied as AcONa/AcOH(1M)
is required for flocculation
 ~7000 mg/kg
monocarboxylic
acids in juice*

5000-6000
mg/kg protein
in juice*

Total Acidic
Phenolics ave.
250 mg/kg in
juice*

*Van der Poel, P.W., Schiweck, H. and Schwartz, T. Sugar Technology: Beet and Cane Sugar
Manufacture. (1998). ISBN 3-87040-065-X. pp. 151-157.
 Take Home Messages:
For color ppt. to occur there must be a
certain amount of 1) protein, 2) phenolic
material, 3) iron and 4) organic acid.
Fortunately, the optimized values are close
to what is normally found in juice—
Unless… the juice is bad; this leads to a
drop in pH and along with it, the ppt of
protein. Eliminating this component likely
explains why the method failed with
deteriorated juice.
Thank you For Playing!

Funded in part by: the Louisiana Board of Regents,

the American Sugarcane League and Cargill, N.A.