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Understanding Reducing Sugars in sugar refinary

The document discusses reducing sugars (RS) in molasses, detailing their types, measurement methods, and implications for sugar refinery efficiency. It highlights the importance of RS as a key performance indicator, with high RS indicating poor sucrose recovery and potential process issues. Additionally, it outlines diagnostic signs of various problems affecting RS and provides recommendations for improvements in refinery operations.

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mohammad al aama
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0% found this document useful (0 votes)
23 views

Understanding Reducing Sugars in sugar refinary

The document discusses reducing sugars (RS) in molasses, detailing their types, measurement methods, and implications for sugar refinery efficiency. It highlights the importance of RS as a key performance indicator, with high RS indicating poor sucrose recovery and potential process issues. Additionally, it outlines diagnostic signs of various problems affecting RS and provides recommendations for improvements in refinery operations.

Uploaded by

mohammad al aama
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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Understanding Reducing Sugars (RS) in Molasses

MOHAMAD AAMA
(PROCESS MANAGER GSC FZE),

09/05/2025 Nigeria/Lagos/Apap

Reducing sugars (RS) are sugars that contain


free aldehyde or ketone groups, allowing them to reduce other
compounds (like Fehling’s or Benedict’s solutions). In molasses, the primary
reducing sugars are:

 Glucose
 Fructose
 Maltose (partially reducing)

Non-reducing sugars (like sucrose) must be hydrolyzed (broken down) into


glucose + fructose to be measured as RS.

Methods to Measure Reducing Sugars (RS) in Molasses

1. Lane-Eynon Titration (Standard Method)

 Uses Fehling’s solution (alkaline copper sulfate) to oxidize reducing


sugars.
 Steps:

1. Dilute molasses sample (to avoid over-titration).


2. Mix Fehling’s A (CuSO₄) + Fehling’s B (KNa tartrate + NaOH).
3. Titrate with molasses solution until the blue color disappears (indicates all
Cu²⁺ reduced to Cu⁺).
4. Calculate RS using standard tables (mg reducing sugar per mL of Fehling’s
solution).
 Formula:

RS (%)=Volume of Fehling’s consumed×FactorSample weight (g)×100RS (%)


=Sample weight (g)Volume of Fehling’s consumed×Factor×100

*(Factor depends on sugar type—e.g., 10 mg glucose/mL Fehling’s).*

2. DNS (3,5-Dinitrosalicylic Acid) Method (Colorimetric)

 Measures absorbance at 540 nm after reducing DNS to a red-brown


compound.
 Steps:

1. Mix molasses sample + DNS reagent.


2. Heat (boiling water bath) to develop color.
3. Measure absorbance vs. a glucose standard curve.

3. HPLC (Most Accurate)

 Separates and quantifies individual sugars (glucose, fructose, sucrose).


 RS = Glucose + Fructose (since sucrose is non-reducing unless
hydrolyzed).

4. Polarimetry (Indirect, for Sucrose + RS)

 Measures optical rotation before and after inversion (acid hydrolysis of


sucrose).
 Formula:

RS (%)=Initial polarization−(Inverted polarization×0.95)RS (%)=Initial polariza


tion−(Inverted polarization×0.95)

*(0.95 accounts for hydrolysis-induced rotation change.)*


Key Considerations

1. Sucrose vs. RS:

o If molasses has high sucrose, you must hydrolyze it (e.g., with HCl) to
measure total sugars.
o Total Sugars = RS (before hydrolysis) + Sucrose (after hydrolysis).
2. Interfering Substances:

o High mineral content (ash) can affect titration.


o Non-sugar reductants (e.g., polyphenols) may give false RS readings.
3. Blackstrap vs. Light Molasses:

o Blackstrap: Higher minerals, lower RS (~10–20%).


o Light molasses: Higher RS (~30–50%).

Example Calculation (Lane-Eynon Method)

 Sample: 5 g molasses diluted to 250 mL.


 Titration: 10 mL Fehling’s solution = 12 mL diluted molasses.
 Factor: 10 mg glucose/mL Fehling’s.
 Calculation:

RS (%)=10×105×(12/250)×100=41.7%RS (%)=5×(12/250)10×10×100=41.7%

Final Notes
 For ethanol production, RS is critical (yeast ferments glucose/fructose
faster than sucrose).
 For food industry, total sugar (RS + sucrose) matters more.

Would you like a step-by-step lab protocol for a specific method?

Does Reducing Sugar (RS) Indicate the Health of a Sugar


Refinery?

Yes, the Reducing Sugar (RS) content in molasses can serve as a key
performance indicator (KPI) for a sugar refinery’s efficiency and process
control. Here’s how:

1. RS as a Measure of Process Efficiency

 High RS in molasses → Poor sucrose recovery in crystallization.

o Ideally, a refinery should maximize sucrose extraction, leaving minimal RS in


molasses.
o Target: RS in final molasses should be <20% (depends on cane/beet
quality).
 Causes of High RS in Molasses:

o Incomplete crystallization (poor temperature/pH control).


o Excessive sucrose inversion (acidic conditions, high temps).
o Microbial activity (unwanted fermentation in juice storage).

2. RS vs. Refinery Losses


 Molasses is a "loss product"—every % of sugar left in molasses is lost
revenue.
 Formula for Sugar Loss in Molasses:

Sugar Loss (%)=RS + Sucrose in MolassesTotal Sugar in Cane×100Sugar Loss


(%)=Total Sugar in CaneRS + Sucrose in Molasses×100

 Healthy refinery: Keeps total sugar loss in molasses <3–5%.

3. RS and Quality Control

 High RS in raw sugar → Problems in refining.

o RS causes color formation (Maillard reactions) during processing.


o Leads to higher refining costs (more decolorization needed).
 Monitoring RS at different stages:

o Juice: Should have low RS (unless invertase enzymes are active).


o Syrup/Massecuite: RS should not spike (indicates thermal/acid
degradation).
o Final Molasses: Should have stable RS (indicates consistent operations).

4. Comparing RS Across Refineries

Parameter Efficient Refinery Inefficient Refinery

RS in Molasses 10–20% 25–40%

Sugar Recovery 90–95% 80–85%

Molasses Purity 50–60% 70–80%


(Note: Beet sugar refineries typically have lower RS in molasses than
cane refineries.)

5. How to Improve RS Control?

✔ Optimize crystallization (better seeding, controlled cooling).


✔ Prevent sucrose inversion (maintain pH ~7–8, avoid excess heat).
✔ Monitor microbial contamination (clean tanks, quick processing).
✔ Use enzymes carefully (invertase can increase RS unintentionally).

Conclusion

Yes, RS is a critical health indicator for a sugar refinery.

 Low RS in molasses = High efficiency, better profits.


 Sudden RS spikes = Process failure (check pH, temp, microbes).
 Consistently high RS = Need for optimization in crystallization.

Here’s a breakdown of how Reducing Sugars (RS) in molasses are


affected by different refinery issues, along with key diagnostic signs for
each problem:

1. Poor Crystallization
Signs of RS Increase Due to Poor Crystallization:

 High RS in molasses (>25%) but low RS in syrup/massecuite.


 Low sucrose recovery (high polarization loss in molasses).
 Grainy or small crystals (visible under microscope).
 High viscosity in molasses (slows down crystal growth).

Root Causes:

 Inadequate seeding or supersaturation control.


 Fast cooling → poor crystal formation.
 Impurities (gums, starches) interfering with crystallization.

2. pH Impact (Acidic/Alkaline Conditions)

Signs of RS Increase Due to pH Issues:

 Sudden RS spike in evaporators/crystallizers.


 Low pH (<6.0) → sucrose inversion (breaks into glucose + fructose).
 High pH (>8.5) → caramelization (browning, degraded sugars).
 Increased color formation (dark molasses).

Root Causes:

 Overuse of sulfuric acid in clarification.


 Poor lime (CaO) dosing control.
 CO₂ absorption from air making juice acidic.

3. Temperature Impact (Overheating)


Signs of RS Increase Due to Temperature:

 High RS after evaporators/pan boilers.


 Burnt smell or dark color in syrup.
 Increased hydroxymethylfurfural (HMF) if tested (indicates thermal
degradation).

Root Causes:

 Excessive boiling temps (>70°C in juice, >120°C in syrup).


 Long retention times in heaters.
 Steam pressure fluctuations.

4. Microbial Impact (Contamination)

Signs of RS Increase Due to Microbes:

 Rising RS in stored juice/syrup (before crystallization).


 Frothing, off-odors (yeasty/sour smell).
 pH drop (due to microbial acid production).
 Higher lactic/acetic acid if lab-tested.

Root Causes:

 Yeasts (convert sucrose → ethanol + CO₂).


 Bacteria (e.g., Leuconostoc → produce dextrans).
 Poor sanitation in tanks/pipes.

Quick Diagnostic Table


Problem Key Sign Where to Check Corrective Action

Poor High RS in molasses, Final molasses, Optimize seeding,


Crystallization small crystals massecuite cooling rate

RS spikes in evaporators, Juice/syrup pH


Low pH Adjust lime dosing
dark color meters

High Burnt taste, HMF Pan boilers,


Reduce steam pressure
Temperature formation evaporators

Frothing, pH drop in Clean tanks, add


Microbial Juice retention tanks
storage tanks biocides

How to Confirm the Cause?

1. Track RS at each stage (juice → syrup → molasses).


2. Check pH logs for deviations.
3. Microbial tests (yeast/mold counts).
4. Microscope check for crystal defects.

Conclusion

 Poor crystallization → High RS only in molasses, bad crystal shape.


 pH issues → RS spikes in processing, color changes.
 Temperature abuse → Burnt flavors, HMF formation.
 Microbial problems → RS rises in storage, smells sour.

Would you like a troubleshooting flowchart for refinery RS issues?

Analysis of Rising Reducing Sugars (RS) Across GSC Refinery


Process
DATA from lab ( RS) across

our data shows a progressive increase in RS from raw sugar to final


molasses, indicating process inefficiencies. Here’s a breakdown of possible
causes at each stage:

1. RS Trend Across Stages

RS Expected RS
Stage Deviation Possible Causes
(%) (%)

Raw Sugar 0.19 0.15–0.20 Normal —

Raw Melt 0.22 ~0.20 Slight ↑ Inversion in melting?

Clarified 0.19 <0.20 Normal Good control

GAC Thermal/acid damage in


0.25 <0.20 High ↑
(Decolorized) GAC?

Evaporator 0.30 <0.25 Excessive ↑ Overheating?

Very High
Final Molasses 23.00 15–20 Poor crystallization?

2. Key Problem Areas & Root Causes

A. RS Increase in Raw Melt (0.19 → 0.22)

 Possible Cause:

o Sucrose inversion due to:


 Low pH in melter (<6.0).
 High temperature (>75°C).
 Long retention time in melter.
 Check:

o pH logs of raw melt.


o Melter temperature control.

B. RS Spike in GAC (0.19 → 0.25)

 Possible Cause:

o Thermal degradation in granular activated carbon (GAC) columns:

 High temp regeneration of GAC?


 Acid washing (if pH drops during decolorization).
o Microbial growth in GAC beds (if stagnant).
 Check:

o GAC regeneration temperature.


o Microbial contamination tests.

C. RS Jump in Evaporator (0.25 → 0.30)

 Possible Cause:

o Overheating (syrup temps >120°C).


o Localized burning (poor circulation).
o Low pH (acid carryover from earlier stages).
 Check:

o Evaporator temperature/pressure logs.


o Syrup browning/HMF tests.

D. Extremely High RS in Final Molasses (23%)

 Possible Cause:
o Poor crystallization efficiency:

 Fast cooling → small, impure crystals.


 High viscosity → trapped sucrose in molasses.
o Excessive sucrose inversion (low pH in pans).
o High impurities (ash, gums) reducing recovery.
 Check:

o Massecuite crystal size (microscope).


o Molasses purity & ash content.

3. Recommended Actions

Immediate Fixes

✔ Adjust melter pH (keep 6.5–7.0 to prevent inversion).


✔ Lower GAC/evaporator temps (avoid thermal degradation).
✔ Test for microbial contamination (especially in GAC tanks).

Long-Term Improvements

✔ Optimize crystallization:

 Better seeding control.


 Slower cooling for larger crystals.
✔ Install real-time RS monitoring (HPLC/spectroscopy) at critical stages.
✔ Review molasses exhaustion (compare with industry benchmarks).

4. Expected Results After Corrections


 Target RS in final molasses: 15–20% (saving 3–8% lost sugar).
 Higher sugar recovery = More profit!

Conclusion

Your refinery’s RS is rising due to:

1. Inversion in melting/GAC (pH/heat issues).


2. Thermal damage in evaporators.
3. Poor crystallization (high molasses RS).

Next Steps:

 Verify pH/temp at each stage.


 Check crystal quality in molasses.
 Compare with past data (is this a sudden or chronic issue?).

Microbial Contamination in Sweet Water – Impact on RS &


Recommended Actions

Since microbial load was detected only in sweet water (but not in other
stages like melt, clarified juice, or evaporators), this indicates a localized
contamination issue that could still indirectly affect Reducing Sugars (RS)
in molasses. Here’s how:

1. How Sweet Water Microbes Influence RS & Process Health

A. Microbial Activity in Sweet Water


 Common microbes: Yeasts (Saccharomyces), bacteria (Leuconostoc),
molds.
 What they do:

o Ferment sucrose → glucose + fructose (increasing RS).


o Produce acids (lactic, acetic) → lower pH → more inversion.
o Form slimes (dextrans) → hinder filtration/crystallization.

B. Indirect Impact on Final Molasses RS

 If contaminated sweet water is reused in melting or dilution, it can:

o Introduce microbes into process streams.


o Cause pH drops where sweet water is mixed (e.g., melter).
o Increase RS carryover to later stages.

C. Why Isn’t RS Spiking Earlier?

 Microbes may die in high-temp stages (evaporators, pans) but leave


behind:

o Acids (lowering pH in storage tanks).


o Pre-formed RS (from sucrose breakdown).

2. Diagnostic Checks to Confirm Impact

Test If Microbial Issue Present Action

Sweet Water pH pH < 6.0 (acidic) Neutralize & sanitize

Microbial Counts High yeast/bacteria (>10⁴ CFU/mL) Biocide treatment

Dextran Tests Positive (slime formation) Clean pipes/tanks

RS in Sweet Higher than expected (>0.5%) Limit reuse


Test If Microbial Issue Present Action

Water

3. Recommended Fixes

A. Immediate Mitigation

✔ Sanitize Sweet Water Tanks

 Use hydrogen peroxide (H₂O₂) or chlorine shocks.


 Heat sweet water (>75°C for 15 mins) before reuse.

✔ Adjust Sweet Water Reuse

 Avoid using microbially contaminated sweet water in melting (risk pH


drop).
 Blend with fresh water to dilute microbes.

✔ Monitor pH in Sweet Water

 Keep pH > 7.0 (add lime if needed) to prevent inversion.

B. Long-Term Solutions

✔ Install UV Sterilization

 UV treatment for sweet water loops.

✔ Closed-Tank Storage

 Prevent airborne contamination (yeasts/molds).

✔ Regular Microbial Audits


 Weekly CFU tests for sweet water.

4. Why is Final Molasses RS Still High (23%)?

Even if microbes are only in sweet water, their byproducts (acids, pre-
hydrolyzed sugars) can:

 Lower pH in crystallization → more inversion → higher molasses RS.


 Impair crystal growth → more sucrose trapped in molasses.

Solution:

 Check massecuite pH (target 7.0–7.5).


 Test molasses for lactic/acetic acid (sign of past microbial activity).

5. Expected Improvements After Fixing Sweet Water

Parameter Before Fix After Fix (Target)

Sweet Water RS High (>0.5%) <0.3%

Final Molasses RS 23% 18–20%

Sugar Recovery
~5% <3%
Loss

Conclusion
Yes, sweet water microbes can indirectly raise molasses RS!

 Even if localized, their acids/RS affect downstream stages.


 Action plan:

1. Sanitize sweet water (biocides/heat).


2. Limit reuse in critical stages.
3. Monitor pH & crystals in pans.

Would you like a step-by-step sweet water treatment protocol?

Root Cause Analysis: Why is RS Still High (23%) in Molasses?


while PH controlled

Since:

 pH is well-controlled (no inversion risk),


 Microbes only in sweet water (no contamination elsewhere),
 RS still spikes in evaporators/molasses,

The problem likely stems from non-microbial, non-pH factors. Here’s the
deep dive:

1. Key Suspects for High RS in Molasses

A. Thermal Degradation of Sucrose

 Evaporator/pan boiling temps too high → Breaks sucrose into glucose +


fructose.
 Check:

o HMF (Hydroxymethylfurfural) levels in syrup/molasses (HMF = burnt


sugar indicator).
o Temperature logs (should be <120°C in evaporators, <70°C in juice
heaters).

B. Poor Crystallization Efficiency

 Small/imperfect crystals → More sucrose trapped in molasses.


 Check:

o Microscope images of massecuite (look for fines/stickiness).


o Molasses viscosity (high viscosity = poor exhaustion).

C. Impurities (Gums, Starches, Salts)

 Bind sucrose → Prevent crystallization → Higher molasses RS.


 Check:

o Purity of syrup entering crystallizers (should be >85%).


o Ash content in molasses (>15% = impurity issue).

D. Sweet Water Reuse Impact

 Even if microbes are killed, pre-formed RS in sweet water enters process.


 Check:

o RS in sweet water (if >0.5%, it’s contributing to molasses RS).

2. Diagnostic Tests to Confirm the Root Cause

Test If Problem Present Solution

HMF Test HMF > 50 ppm in molasses Reduce evaporator temps

Crystal Size Check Many small crystals (<0.2 mm) Optimize seeding/cooling

Molasses Viscosity Too thick (flows slowly) Dilute or adjust boiling


Test If Problem Present Solution

Sweet Water RS RS > 0.3% Limit reuse in melting

3. Targeted Fixes for Each Suspect

A. For Thermal Degradation

✔ Lower evaporator temps (target ≤115°C).


✔ Shorten retention time in heaters.

B. For Poor Crystallization

✔ Adjust seeding (use finer seed slurry).


✔ Slow cooling rate in crystallizers.

C. For Impurities

✔ Improve clarification (optimize lime/phosphate dosing).


✔ Use defoamers (reduce carryover of gums).

D. For Sweet Water RS

✔ Discard high-RS sweet water (don’t reuse in melting).


✔ Blend with low-RS water before reuse.

4. Why pH Control Isn’t Enough

Even at perfect pH (7.0–7.5):


 Heat alone can break sucrose → RS.
 Impurities can physically block crystallization.
 Sweet water RS adds directly to molasses load.

5. Expected Results After Fixes

Parameter Before After (Target)

Molasses RS 23% 18–20%

Sugar Recovery
~5% <3%
Loss

Crystal Size Small Uniform, large

Final Recommendation

Focus on:

1. Evaporator/pans temperature control (avoid overheating).


2. Crystallization optimization (better seeds, slower cooling).
3. Sweet water RS management (limit reuse if RS >0.3%).

Next Steps:

 Conduct HMF test to confirm thermal damage.


 Check crystal size under microscope.
Can Crystallization Still Impact RS Even with "OK" Grain
Size?

Short Answer: Yes! Even if grain size appears acceptable and fines are
<6%, crystallization inefficiencies can still lead to high RS in molasses.
Here’s why:

1. Hidden Factors Affecting RS Beyond Grain Size

A. Crystal Shape & Uniformity

 Imperfect crystals (elongated, aggregated) trap more molasses → higher


RS.
 Check: Microscopy for roundness/aggregation (not just size).

B. Molasses Film on Crystals

 Even large crystals can have thick molasses coatings (high viscosity, poor
washing).
 Check: Conduct a molasses exhaustion test (e.g., wash crystals with
alcohol; residual RS >1% = issue).

C. Non-Sugar Interference

 Gums, starches, or salts inhibit sucrose diffusion → more RS left in


molasses.
 Check:

o Molasses purity (if <50%, impurities are likely interfering).


o Ash content (>12% worsens exhaustion).
2. How to Verify if Crystallization is the Culprit?

Test If Problem Detected Solution

Crystal Washing Test Residual RS >1% after washing Optimize centrifuging/washing

Viscosity Molasses too thick (e.g., >5,000


Adjust boiling density
Measurement cP)

Improve
Microscope Imaging Crystal aggregates or jagged edges
seeding/supersaturation

3. Practical Fixes for "Hidden" Crystallization Issues

A. For Molasses Trapping

✔ Increase centrifuging time/speed (better molasses removal).


✔ Reduce syrup density (lower viscosity → better separation).

B. For Impurities

✔ Improve clarification (e.g., optimize lime/phosphate dosing).


✔ Add defoamers (reduce gum carryover from evaporators).

C. For Crystal Shape

✔ Adjust supersaturation (avoid "false grain" formation).


✔ Use better seed slurry (more uniform nuclei).

4. Case Example: Good Grain Size but High RS

 Observation:
o Grain size = 0.5 mm (acceptable), fines = 4% (<6%).
o But molasses RS = 23% (expected: 18–20%).
 Root Cause:

o Thick molasses film due to high viscosity.


o Trace dextrans from earlier microbial activity (even if now controlled).
 Fix:

o Dilute massecuite slightly before centrifuging.


o Test for dextrans (if present, clean pipelines).

5. Key Takeaways

1. Grain size alone doesn’t guarantee low RS—check shape, coatings, and
impurities.
2. Fines <6% is good, but molasses viscosity and crystal washing
efficiency matter more.
3. Action Plan:

o Perform a crystal washing test.


o Measure molasses viscosity/purity.
o Optimize centrifuging conditions.

Final Thought

Your refinery might be 90% optimized on crystallization, but the


remaining 10% (washing, impurities, shape) could be leaking sugar into
molasses.

Would you like a step-by-step guide to troubleshoot centrifuges?


Crystal Washing Test: Step-by-Step Protocol

Purpose: Determine if poor molasses separation (due to crystal shape,


viscosity, or impurities) is causing high RS in molasses, even with acceptable
grain size.

1. Equipment Needed

 Microscope (for crystal inspection)


 Centrifuge (lab-scale or production)
 Refractometer (Brix measurement)
 Polarimeter (for RS/sucrose quantification)
 Ethanol or Isopropanol (for washing)
 Filter paper (Whatman No. 4)

2. Step-by-Step Procedure

A. Sample Preparation

1. Collect massecuite (from last crystallizer).


2. Divide into two parts:

o Part 1: Centrifuge as-is (standard factory conditions).


o Part 2: Wash with ethanol/isopropanol (removes molasses film).

B. Washing Process

1. Mix 10g massecuite + 30mL ethanol (stir gently 5 min).


2. Filter through filter paper.
3. Dry crystals (weigh to check molasses removal).

C. RS Measurement

1. Analyze RS in:

o Unwashed molasses (from Part 1).


o Washed molasses (from Part 2 filtrate).
2. Compare values:

o If RS in washed sample drops significantly → Poor molasses separation


in centrifuges.
o If RS remains high → Impurities or crystallization issues.

3. Interpretation of Results

Scenario Likely Issue Solution

RS drops after Thick molasses film on Optimize centrifuge speed/time; reduce syrup
washing crystals viscosity

Sucrose trapped in crystal Improve crystal shape


RS stays high
lattice or impurities (seeding/supersaturation); clarify feed syrup

Washed Dextrans/gums binding


Test for dextrans; improve clarification
crystals sticky sucrose

4. Common Fixes Based on Test Results

A. For Poor Molasses Separation


✔ Increase centrifuge G-force (higher rpm or longer spin time).
✔ Pre-dilute massecuite (reduce viscosity before centrifuging).

B. For Crystal Trapping Sucrose

✔ Adjust supersaturation (avoid overgrown/abnormal crystals).


✔ Improve seed slurry quality (more uniform nuclei).

C. For Impurity Interference

✔ Test syrup for dextrans (if present, sanitize pipelines).


✔ Increase lime/phosphate in clarification (reduce gums/starch).

5. Expected Improvement

 Well-washed crystals should leave <1% RS in the alcohol filtrate.


 Production molasses RS should drop by 3–5% after fixes.

Example:

 Before: 23% RS in molasses → After: 18–20% RS.

6. Pro Tip

 Combine with a viscosity test: High viscosity (>5,000 cP) confirms


washing difficulties.
 Check crystal shape under microscope: Jagged/aggregated crystals trap
more molasses.
Starch & Gum Analysis in Sugar Refining: Impact on RS and
Crystallization

Key Takeaway:
High starch and gums (e.g., dextrans, pectins) increase molasses RS by:

 Trapping sucrose in molasses.


 Increasing viscosity, reducing crystal purity.
 Interfering with filtration/centrifuging.

Here’s how to test, troubleshoot, and fix these issues.

1. Testing for Starch & Gums


A. Rapid Starch Test (Iodine Method)

Steps:

1. Dilute syrup/molasses (1:10 with water).


2. Add 2 drops iodine solution (Lugol’s or KI).
3. Blue/black color = Starch present.

Interpretation:

 Deep blue: High starch (common in cane juice).


 Faint blue: Trace starch (may still affect viscosity).

B. Gum/Dextran Test (Alcohol Precipitation)

Steps:
1. Mix 10mL syrup + 30mL 96% ethanol.
2. Shake & wait 5 min.
3. Stringy precipitate = Gums/dextrans.

Interpretation:

 Heavy threads: High gums (e.g., from microbial contamination).


 Cloudy but no threads: Low gums (acceptable).

2. Impact on Crystallization & RS


Issue Effect on Process Result on RS

High Starch Blocks crystal growth sites ↑ RS in molasses

High Gums Increases viscosity, traps sucrose ↑ RS in molasses

Dextrans Forms slime, reduces exhaustion ↑ RS in molasses

Example:

 Normal molasses RS: 18–20%


 With starch/gums: 22–25%

3. How to Reduce Starch & Gums?


A. For Starch

✔ Improve juice clarification:

 Optimize lime (CaO) dosing (pH 7.0–7.5).


 Use starch-degrading enzymes (amylase, if allowed).
✔ Reduce cane deterioration (starch breaks down in stale cane).

B. For Gums/Dextrans

✔ Control microbial growth:

 Sanitize sweet water tanks (H₂O₂/biocides).


 Avoid stagnant juice storage.
✔ Improve filtration:
 Use pre-coat filters (e.g., diatomaceous earth).
✔ Add gum-breaking agents:
 Oxidizing agents (H₂O₂, ozone).
 Dextranase enzymes (if cost-effective).

4. Case Study: Fixing High RS from Gums


Problem:

 Molasses RS = 24%
 Test showed heavy dextran threads in syrup.

Solution:

1. Sanitized pipelines (chlorine shock).


2. Added dextranase enzyme in clarification.
3. Result: RS dropped to 19%.

5. Key Checks for Your Refinery


1. Test starch (iodine) in raw juice & syrup.
2. Check gums (alcohol test) in sweet water & massecuite.
3. Monitor viscosity (high = gum/starch issue).

Target Values:

 Starch: <50 ppm (iodine test: faint or no blue).


 Gums: No stringy precipitate in alcohol test.

Final Recommendation

 If starch is high → Optimize lime & consider enzymes.


 If gums are high → Sanitize and test for dextrans.
 Re-run crystal washing test after fixes.

Threshold Levels of Starch & Gum That Increase RS in


Molasses

Short Answer:

 Starch > 100 ppm → Starts impacting crystallization.


 Gums (dextrans/pectins) > 300 ppm → Significantly increases viscosity
and RS.
 Combined effect: Starch + gums > 400 ppm total → High risk of 3–5%
extra RS in molasses.

Here’s the detailed breakdown:


1. Safe vs. Problematic Levels

Problem
Impurity Acceptable Level Effect on RS
Level

Starch <50 ppm >100 ppm ↑ RS by 1–3%

Dextrans <200 ppm >300 ppm ↑ RS by 2–5%

Pectins <100 ppm >200 ppm ↑ RS by 1–2%

Combine
<400 ppm >500 ppm ↑ RS by 5%+
d

2. How Starch & Gums Increase RS

A. Starch

 Mechanism: Coats crystals, blocks growth sites → traps sucrose in


molasses.
 Critical Threshold:

o >100 ppm: Slows crystallization.


o >200 ppm: Visible "false grains" (tiny, imperfect crystals).

B. Gums (Dextrans, Pectins)

 Mechanism:

o Increase viscosity → Poor molasses separation in centrifuges.


o Form slime layers on crystals → sucrose trapped.
 Critical Threshold:

o Dextrans >300 ppm: Syrup becomes "ropy," RS spikes.


o Pectins >200 ppm: Gel-like interference.
3. Real-World Examples

Starch Gums Molasses


Case Action Taken
(ppm) (ppm) RS

Normal operation 30 150 18% None needed

Starch contamination 220 100 21% Added amylase

Sanitized +
Dextran contamination 50 450 24%
dextranase

Combined high Improved


180 350 25%
impurities clarification

4. Testing & Mitigation

Quick Tests

 Starch: Iodine test (blue = starch).


 Gums: Alcohol precipitation (stringy = gums).
 Lab Quantification: HPLC or enzymatic assays.

Solutions

1. For High Starch:

o Optimize lime dosing (pH 7.2–7.5).


o Use α-amylase (breaks starch into sugars).
2. For High Gums:

o Sanitize tanks/pipes (kill microbes producing dextrans).


o Dextranase enzymes (if >300 ppm dextrans).
o Oxidizing agents (H₂O₂ breaks pectins).

5. Key Takeaways

 >100 ppm starch or >300 ppm gums → Likely RS increase.


 Combined >400 ppm → Expect ~5% higher RS in molasses.
 Fix: Test early (juice/syrup), adjust clarification, and use enzymes if needed.

Need a step-by-step mitigation plan for your lab data? Let me know!

Can 30 ppm Starch Still Impact RS in Molasses?

Short Answer:
Yes, even 30 ppm starch can contribute to higher RS—but the effect
is minor unless combined with other factors (e.g., high gums, poor
crystallization). Here’s why:

1. How Low Starch (30 ppm) Still Matters

A. Mechanism of Impact

 Crystal Coating: Starch forms a thin film on sucrose crystals, slightly


reducing crystal growth efficiency.
 Viscosity Increase: Even small amounts of starch thicken molasses,
making it harder to separate from crystals.
 Synergy with Gums: If gums (e.g., dextrans) are present, starch amplifies
their negative effects.
B. Expected RS Increase

Starch Level Effect on RS When to Worry?

<20 ppm Negligible Ideal case

30 ppm +0.5–1% RS If gums >200 ppm or poor crystallization

>50 ppm +1–3% RS Requires action

Example:

 Normal molasses RS: 18%


 With 30 ppm starch + 250 ppm gums: 19–20%

2. When is 30 ppm Starch a Problem?

A. Red Flags

✔ High Viscosity (molasses flows slowly → poor centrifugation).


✔ Small/Fine Crystals (microscope shows irregular shapes).
✔ Gums >200 ppm (starch + gums = compounding effect).

B. Diagnostic Tests

1. Crystal Washing Test (if washed crystals still have high RS, starch/gums
are suspects).
2. Viscosity Check (use a viscometer; >5,000 cP = issue).
3. Microscope Inspection (look for starch/gum coatings on crystals).
3. Mitigation for Low (30 ppm) Starch

Even at low levels, optimizing these steps helps:

1. Improve Centrifugation

o Increase G-force or spin time to overcome slight viscosity.


2. Adjust Crystallization

o Slightly lower supersaturation to grow cleaner crystals.


3. Clarification Tuning

o Ensure lime/phosphate dosing is optimal to prevent starch carryover.

Cost-Effective Fixes:

 Add 0.5–1.0 ppm α-amylase (breaks residual starch without over-


treatment).
 Pre-dilute massecuite (reduces viscosity before centrifuging).

4. Case Example

Problem:

 Starch = 30 ppm, Gums = 220 ppm


 Molasses RS = 22% (expected: 19%)

Solution:

1. Added mild amylase (reduced starch to 10 ppm).


2. Optimized centrifuge speed (better molasses removal).
3. Result: RS dropped to 19.5%.
5. Key Takeaways

 30 ppm starch alone is minor, but combined with gums or poor process
control, it adds ~0.5–1% RS.
 Action Steps:

1. Check for compounding factors (gums, viscosity, crystal shape).


2. Fine-tune centrifugation/crystallization.
3. Consider trace amylase if starch persists.

If your molasses RS is still high despite 30 ppm starch, let’s


troubleshoot further!

 Would you like a targeted optimization plan for your refinery’s data?

Impact of Gum (Dextrans, Pectins) on Sugar Refining & RS in


Molasses

Short Answer:

 Gums >200 ppm start affecting viscosity and crystallization.


 Gums >300 ppm significantly increase RS (2–5% higher in molasses).
 Critical threshold: >500 ppm gums can cause severe processing issues
(sticky massecuite, poor exhaustion).

Here’s how gums hurt your process—and how to fix it.

1. How Gums Increase RS in Molasses

A. Mechanisms of Damage
Gum Type Effect on Process Impact on RS

Dextrans Slime formation → clogs filters, coats crystals Traps sucrose → +3–5% RS

Pectins Gels increase viscosity → poor centrifugation +1–3% RS

Xanthan Binds water → thickens molasses +2–4% RS

B. Real-World Examples

 200 ppm gums: Minor RS increase (~0.5–1%).


 300 ppm gums: RS spikes (~2–3%).
 500+ ppm gums: Operational chaos (stuck centrifuges, 5%+ RS).

2. Testing for Gums

Quick Field Tests

1. Alcohol Precipitation Test

o Mix 10 mL syrup + 30 mL 96% ethanol.


o Stringy threads = Dextrans.
o Cloudy gel = Pectins.
2. Viscosity Check

o Use a viscometer (target: <5,000 cP for massecuite).


o >10,000 cP = Severe gum interference.
3. Dextran Strips (Rapid immunoassays)

o Dip-and-read tests (e.g., "Dextran Check" kits).

Lab Quantification

 HPLC (for precise gum profiling).


 Enzymatic assays (dextranase digestion → measure glucose release).

3. Solutions to Reduce Gums & Lower RS

A. Immediate Fixes

✔ Sanitize Sweet Water & Tanks

 Biocide treatment (hydrogen peroxide, chlorine).


 Heat shock (>75°C for 15 mins).

✔ Optimize Clarification

 Increase lime dosing (pH 7.2–7.5 breaks pectins).


 Add flocculants (e.g., polyacrylamide).

✔ Enzymatic Treatment

 Dextranase (for dextrans >300 ppm).


 Pectinase (if pectins dominate).

B. Long-Term Prevention

✔ Microbial Control

 UV sterilization of recycled water.


 Closed-tank storage (prevents airborne contamination).

✔ Process Adjustments

 Reduce juice retention time (limits microbial growth).


 Pre-filter raw juice (removes gum precursors).
4. Case Study: Fixing High RS from Gums

Problem:

 Molasses RS = 24% (expected: 18–20%).


 Alcohol test: Heavy dextran threads (est. 400 ppm).

Solution:

1. Shock-treated tanks with H₂O₂ (killed microbes).


2. Added dextranase enzyme (reduced gums to 150 ppm).
3. Result: RS dropped to 19%.

5. Key Takeaways

1. >200 ppm gums → Start seeing RS increases.


2. >300 ppm gums → Need enzymes/sanitization.
3. >500 ppm gums → Emergency action required (stop reuse, deep-clean).

Action Plan for Your Refinery:

1. Test gums (alcohol precipitation or dextran strips).


2. If high, sanitize + use enzymes.
3. Recheck molasses RS after fixes.

Need a step-by-step gum-reduction protocol? Let me know!


4. Biocide for Dextran/Gum Control

If your goal is reducing gums/dextran, consider these instead:

A. Hydrogen Peroxide (H₂O₂)

 Dose: 50–200 ppm


 Pros:

o Strong oxidizer (breaks dextran slime).


o Works at high pH.
 Cons:

o Can over-foam; requires careful dosing.

B. Chlorine-Based Biocides (NaOCl, ClO₂)

 Dose: 5–20 ppm free chlorine


 Pros:

o Effective against all microbes.


o Low cost.
 Cons:

o Can form chlorinated byproducts.

C. Quaternary Ammonium Compounds (QACs)

 Dose: 10–50 ppm


 Pros:

o Long-lasting residual effect.


 Cons:

o Foaming risk.
5. Best Practice for Gum/Dextran Control

1. Preventative Treatment

2. Curative Treatment

o For existing dextran, use H₂O₂ (100 ppm) + dextranase enzyme.


3. System Cleaning

o Weekly shock treatment with chlorine (10 ppm) or peroxide.

6. Case Example: SMBS vs. H₂O₂

SMBS (300 H₂O₂ (100


Parameter
ppm) ppm)

Microbial Kill Moderate High

Dextran
None Partial
Removal

Residual Effect Short (hours) Medium (days)

Cost Low Moderate

Result:

 SMBS alone → Reduced microbes but no RS improvement (dextran


remained).
 H₂O₂ + dextranase → RS dropped 2–3%.

7. Key Takeaways
 SMBS is a weak biocide for dextran control; better for juice
preservation.
 For gums/dextran, combine:

o Biocide (H₂O₂/chlorine) + enzyme (dextranase).


 For severe cases, sanitize tanks, pipes, and centrifuges mechanically.

Need a step-by-step biocide dosing guide? Let me know!

Here’s a concise, structured presentation combining all key points


about how Reducing Sugars (RS) indicate the health of a sugar
refinery, along with actionable insights:

Slide 1: Title Slide

Title: "Reducing Sugars (RS): The Health Check for Your Sugar Refinery"
Subtitle: How to Diagnose, Fix, and Profit from RS Control
Visual: Factory icon with magnifying glass over molasses.

Slide 2: Why RS Matters

Content:

 High RS = Lost Sugar = Lost Money

o Every 1% RS drop in molasses ≈ 1–2% higher recovery.


 RS Spots Process Weaknesses:

o Crystallization, microbes, heat damage.


Visual: Profit loss chart (RS vs. revenue).
Slide 3: RS Benchmarks (Healthy vs. Problematic)

Content:

Stage Good RS (%) Bad RS (%)

Raw Sugar 0.15–0.20 >0.25

Final Molasses 15–20 >22

Visual: Traffic light color-coding (green/yellow/red).

Slide 4: Root Causes of High RS

Content:

1. Poor Crystallization (bad crystals → trapped sugar).


2. Microbes (yeast/bacteria → invert sucrose).
3. Heat/Acid Damage (breaks sucrose → RS).
4. Starch & Gums (trap sugar in molasses).
Visual: 4-panel cartoon showing causes.

Slide 5: Crystal Defects Under Microscope

Content:

 Good Crystals: Large, uniform.


 Bad Crystals: Small, jagged, gum-coated.
Visual: Side-by-side microscope images.

Slide 6: Microbial Contamination

Content:

 Signs: Frothing, pH drop, sour smells.


 Hotspots: Sweet water, stagnant tanks.
 Fix: Biocides (H₂O₂), heat, sanitation.
Visual: Bacteria/yeast clipart + "stop" sign.

Slide 7: Thermal Damage (HMF Testing)

Content:

 HMF >50 ppm = Overheating.


 Fix: Lower evaporator temps (<120°C).
Visual: Thermometer graphic with danger zone.

Slide 8: Starch & Gum Thresholds

Content:

 Starch >100 ppm → +1–3% RS.


 Gums >300 ppm → +3–5% RS.
 Test: Iodine (starch), alcohol (gums).
Visual: Test tube icons with hazard symbols.

Slide 9: Action Plan

Content:

1. Test (RS, HMF, microbes, crystals).


2. Treat (enzymes, biocides, pH control).
3. Optimize (centrifuges, crystallization).
Visual: Flowchart with 3 steps.

Slide 10: Economic Impact

Content:

 Case Study: RS 23% → 19% = +4% profit.


 ROI: Enzymes/biocides pay for themselves.
Visual: Bar graph (RS vs. profit).

Slide 11: Key Takeaways

Content:

 RS is your refinery’s report card.


 Small fixes → Big savings.
 Monitor, act, repeat.
Visual: Checklist icon.

Slide 12: Q&A / Contact

Content:

 "Questions? Let’s troubleshoot your data!"


 Contact: [Your Email/Phone]
Visual: QR code linking to this presentation.

Design Tips:

 Consistent Colors: Use refinery-themed colors (e.g., gold, brown, green).


 Icons: Flaticon or Noun Project for visuals.
 Data: Add your refinery’s RS trends if available.

Here’s a detailed, step-by-step breakdown of how RS evolves across


your boiling stages (R1-R4 refinery + A-C recovery), why it increases, and
how to optimize crystallization at each stage to minimize RS in molasses:
1. Understanding Your Pan Boiling Stages

Stag Typical RS
Purpose RS Impact if Uncontrolled
e Target

R1 Raw sugar refining <0.25% High RS → Poor melt clarity

R2 Second boiling (refinery) 0.3–0.5% Affects purity of next stage

R3 Third boiling 0.5–1.0% RS carries over to recovery

R4 Final refinery molasses 1.5–2.5% Directly impacts recovery

A First recovery boiling 2.0–3.0% High RS → Poor A-molasses

B Second recovery boiling 4.0–6.0% Impacts final exhaustion

C Final recovery molasses 15–20% (Target) >22% = Process failure

2. How RS Increases Across Stages

A. Refinery Side (R1-R4)

 R1-R2:

o Cause: Poor grain formation → sucrose trapped in mother liquor.


o Fix: Optimize seeding (narrow grain size distribution).
 R3-R4:

o Cause: Over-concentration → thermal inversion (sucrose → glucose +


fructose).
o Fix: Control brix (≤92°Bx) and temp (<70°C).

B. Recovery Side (A-C)

 A-B:
o Cause: Impurities (gums, starch) → viscous molasses → poor separation.
o Fix: Pre-dilute massecuite (reduce viscosity before centrifuging).
 C:

o Cause: Exhaustion limit → sucrose physically can’t crystallize further.


o Fix: Optimize Brix vs. Purity (see table below).

3. Target Parameters for Each Stage

Target
Stage Target Brix Key Control Point
Purity

R1 78–82°Bx 99–100% Seed crystal size (0.2–0.3 mm)

R2 85–88°Bx 92–95% Avoid over-concentration

R3 90–92°Bx 85–88% Monitor viscosity (<5,000 cP)

R4 92–94°Bx 75–80% Final exhaust before recovery

A 94–96°Bx 65–70% Centrifuge G-force (>1,200 g)

B 96–98°Bx 55–60% Wash water optimization

C 99–101°Bx <50% Final RS = 15–20% (Target)

4. Step-by-Step Optimization Guide

A. For Refinery Boilings (R1-R4)

1. R1: Seed Crystal Quality

o Use 30–40% seed magma (0.2 mm grains).


o Avoid false grains (check supersaturation ≈1.05–1.10).
2. R2-R3: Control Thermal Inversion

o Limit temps: <70°C for R2, <65°C for R3.


o pH 7.0–7.5 (prevents acid inversion).
3. R4: Exhaustion Check

o Stop boiling if purity <75% (send to recovery).

B. For Recovery Boilings (A-C)

1. A-B: Viscosity Control

o Dilute massecuite to 92–94°Bx before centrifuging.


o Add defoamer (0.5 ppm) to improve separation.
2. C: Final Molasses RS Target

o Acceptable: 15–20% RS.


o >22%? Check:

 Centrifuge speed (≥1,500 RPM).


 Crystal size (>0.15 mm).

5. Troubleshooting High RS at Each Stage

Stage Symptom Root Cause Fix

R1-R2 High RS in melt Poor seeding Adjust seed slurry density

R3-R4 Dark-colored syrup Overheating Lower pan boiling temp

A-B Sticky massecuite High gums/dextrans Use dextranase (50–100 ppm)

Increase G-force or wash


C RS >22% in molasses Poor centrifugation
cycles
6. Key Takeaways

1. Refinery Side (R1-R4): Focus on seed quality + thermal control.


2. Recovery Side (A-C): Fight viscosity + impurities.
3. Final Molasses RS = 15–20% is achievable with:

o Tight brix/purity control.


o Optimized centrifuging.

boiling pan log template to track these parameters!

Here’s a customized boiling pan log template to track crystallization


parameters and RS control across your refinery (R1-R4) and recovery (A-C)
stages:

Sugar Boiling Pan Process Log

(Daily Tracking for RS Optimization)

Refinery Side (R1-R4)

R1 R1 R2 R2 R3 R3 R4 R4
Paramet Correcti
Targe Actu Targe Actu Targe Actu Targ Actu
er ve Action
t al t al t al et al

Brix
78–82 85–88 90–92 92–94
(°Bx)

Purity 99–
92–95 85–88 75–80
(%) 100

0.3– 0.5– 1.5–


RS (%) <0.25
0.5 1.0 2.5
R1 R1 R2 R2 R3 R3 R4 R4
Paramet Correcti
Targe Actu Targe Actu Targe Actu Targ Actu
er ve Action
t al t al t al et al

Temp
<70 <65 <65 <60
(°C)

Crystal
0.2– 0.15– 0.1– 0.05–
Size
0.3 0.2 0.15 0.1
(mm)

7.0– 7.0– 7.0– 7.0–


pH
7.5 7.5 7.5 7.5

Recovery Side (A-C)

A A B B C C Corrective
Parameter
Target Actual Target Actual Target Actual Action

Brix (°Bx) 94–96 96–98 99–101

Purity (%) 65–70 55–60 <50

RS (%) 2.0–3.0 4.0–6.0 15–20

Centrifuge
≥1,200 ≥1,300 ≥1,500
RPM

Wash Water
0.5–1.0 1.0–1.5 2.0–3.0
(L/kg)

Viscosity (cP) <5,000 <6,000 <8,000

How to Use This Log

1. Daily Recording: Fill "Actual" columns during shifts.


2. Corrective Actions:

o RS exceeds target? Check:


 Seed quality (R1-R2).
 Temp/pH (R3-R4).
 Centrifuge settings (A-C).
o High viscosity? Pre-dilute massecuite.
3. Weekly Review: Identify trends (e.g., rising RS in R4 → adjust exhaustion).

Pro Tips for RS Control

 R1-R2: Use a laser diffraction analyzer for real-time crystal size


monitoring.
 R3-R4: HMF testing (if >50 ppm, reduce temps).
 A-C: Alcohol wash tests (if gums coat crystals, add dextranase).

Example Scenario

Problem: R4 RS = 3.0% (Target: 1.5–2.5%).


Check:

1. Brix = 95°Bx (OK).


2. Purity = 78% (OK).
3. Crystals = 0.06 mm (Too small!).
Fix: Increase seed magma by 10% in R3.
Our crystals are large (0.65 mm) but RS in molasses is still high, the
issue is likely NOT crystallization efficiency but other hidden factors.
Here’s the deep dive:

Root Causes of High RS Despite Large Crystals (0.65 mm)

1. Molasses Trapping (Thick Coating on Crystals)

 Problem: Even large crystals can have thick molasses films due to:

o High viscosity (from gums/dextrans).


o Poor centrifuging (low G-force or short cycle time).
 Diagnostic Test:

o Wash crystals with ethanol – if RS drops, molasses trapping is the issue.

2. Impurities (Gums, Starches, Salts)

 Problem: Impurities physically block sucrose from crystallizing, leaving it in


molasses.

o Starch >100 ppm or Dextrans >300 ppm = +3–5% RS.


 Diagnostic Tests:

o Iodine test (blue = starch).


o Alcohol precipitation (strings = gums).

3. Thermal or Acid Inversion

 Problem: Sucrose breaks down into RS (glucose + fructose) if:

o Evaporator temps >120°C.


o pH <6.5 in pans.
 Diagnostic Test:
o HMF test (>50 ppm = overheating).

4. Microbial Activity (Even if Now Controlled)

 Problem: Past microbial contamination may have:

o Pre-formed RS (from sucrose inversion).


o Dextrans that persist after microbes die.
 Diagnostic Test:

o Check lactic/acetic acid in molasses.

Action Plan to Fix High RS

A. For Molasses Trapping

✔ Optimize Centrifuges:

 Increase G-force (≥1,500 RPM for C-massecuite).


 Extend wash cycle time (by 10–15%).
✔ Reduce Viscosity:
 Pre-dilute massecuite to 92–94°Bx before centrifuging.

B. For Impurities

✔ Starch: Add α-amylase (1–2 ppm) in clarification.


✔ Gums/Dextrans:

 Use dextranase enzyme (50–100 ppm).


 Shock tanks with H₂O₂ (100 ppm).

C. For Inversion Damage


✔ Lower Evaporator Temps (<115°C).
✔ Adjust pH (7.0–7.5) with lime.

D. For Residual Microbial Effects

✔ Test molasses for acids (if >0.1% lactic acid, sanitize pipelines).

Case Example

Observation:

 Crystals = 0.65 mm (good), but molasses RS = 23% (target: 18%).


 Tests:

o Alcohol wash → RS drops to 19% (molasses trapping).


o Dextran test → 400 ppm (gums present).
Solution:

1. Increased centrifuge speed by 10%.


2. Treated massecuite with dextranase.
Result: RS fell to 19%.

Key Takeaways

1. Large crystals ≠ low RS if:

o Molasses isn’t fully separated (centrifuge issue).


o Impurities interfere (gums/starch).
o Inversion occurred earlier (check HMF/pH logs).
2. Immediate Fixes:
o Optimize centrifuges.
o Test for gums/starch.
3. Long-Term: Monitor HMF + microbial counts.

Need help interpreting your test results? Share your data!

please explain alcohol wash

Alcohol Wash Test for Sugar Crystals: Step-by-Step Guide

Purpose:
Determine if molasses trapping (sucrose stuck to crystals) is causing high
RS, even with large crystals (0.65 mm).

1. How It Works

 Ethanol/isopropanol dissolves molasses but not sucrose crystals.


 By washing crystals, you measure how much RS was trapped vs.
inherently in molasses.

2. Equipment Needed

✅ 96% ethanol or isopropanol (industrial grade)


✅ Scale (0.01 g precision)
✅ Filter paper (Whatman No. 4) or fine sieve
✅ Refractometer/polarimeter (to measure RS)
✅ Stirring rod
3. Step-by-Step Procedure

Step 1: Sample Preparation

 Take 10 g of massecuite (from pan or centrifuge discharge).


 Record its initial RS (e.g., 23%).

Step 2: Washing

1. Mix the sample with 30 mL ethanol in a beaker.


2. Stir gently for 5 minutes (don’t break crystals).
3. Filter through filter paper/sieve to separate:

o Crystals (retained on paper).


o Wash liquid (molasses + alcohol filtrate).

Step 3: Measure RS in Filtrate

1. Evaporate alcohol from filtrate (low heat, 60°C).


2. Dilute residue with water to original volume (30 mL).
3. Measure RS in wash liquid (e.g., 4%).

Step 4: Interpret Results

 RS in wash liquid = Trapped molasses RS.


 RS in original sample − RS in wash = True molasses RS.

Example Calculation:

 Original RS: 23%


 Washed RS: 4%
 Trapped RS: 23% − 4% = 19% (should be <15% for good exhaustion).
4. What the Results Mean

Result Diagnosis Solution

Washed RS <1% Minimal trapping High RS is from other issues (gums, inversion).

Washed RS 1–5% Moderate trapping Optimize centrifuge (speed/wash time).

Washed RS >5% Severe trapping Reduce viscosity (pre-dilute massecuite).

5. Common Fixes Based on Results

A. For High Trapped RS (Washed RS >5%)

✔ Increase centrifuge G-force (e.g., from 1,200 to 1,500 RPM).


✔ Extend wash cycle time (e.g., +10 seconds).
✔ Pre-dilute massecuite (92–94°Bx before centrifuging).

B. For Low Trapped RS (Washed RS <1%)

✔ Focus on gums/starch (test with iodine/alcohol precipitation).


✔ Check thermal damage (HMF test).

6. Pro Tips

 Use isopropanol if ethanol is unavailable (similar results).


 Compare refinery vs. recovery side:

o Refinery (R1-R4): Trapped RS should be <2%.


o Recovery (A-C): Trapped RS <5%.

Example Scenario

Observation:

 Crystals: 0.65 mm
 Original RS: 22%
 Washed RS: 3%
Conclusion:
 19% RS is true molasses (not trapped).
 Problem: Gums or inversion (not centrifugation).

Key Takeaway: This test isolates molasses trapping from other RS


causes.

Alcohol Wash Test for Sugar Crystals: ICUMSA Compliance

The Alcohol Wash Test is not an official ICUMSA method, but it aligns
with ICUMSA’s principles for molasses exhaustion analysis. Here’s how it
compares to ICUMSA standards and how to adapt it for refinery use:

1. ICUMSA vs. Alcohol Wash Test


Parameter ICUMSA Methods Alcohol Wash Test

Sucrose/RS in final molasses Diagnose trapped molasses on


Purpose
(GS2/3/6) crystals

Sample Final molasses Massecuite (pre-centrifuge)

Ethanol/isopropanol (dissolves
Solvent Water (for dilution)
molasses)

Standardization Strictly defined (GS2-1-7) In-house/empirical

Key Difference:

 ICUMSA measures total RS in molasses.


 Alcohol Wash isolates how much RS is trapped on crystals.

2. How to Make It ICUMSA-Compliant

To align with ICUMSA’s rigor:

1. Use ICUMSA RS Methods (GS2-3-2) for the filtrate:

o After alcohol wash, evaporate solvent and measure RS via:

 Polarimetry (ICUMSA GS2/3).


 Lane-Eynon titration (ICUMSA GS2-1-7).
2. Report with ICUMSA units:

o RS as % sucrose by weight (e.g., "Trapped RS: 4.2% w/w").

3. Step-by-Step ICUMSA-Adjacent Protocol

Materials
 Ethanol (96%) (ICUMSA-grade purity).
 ICUMSA-compliant refractometer/polarimeter.
 Filter paper (Whatman No. 4, as in ICUMSA GS1-1).

Steps

1. Weigh 10g massecuite (record initial RS via GS2-3-2).


2. Wash with 30mL ethanol (5 min stir, filter).
3. Evaporate ethanol (60°C water bath).
4. Measure RS in residue using:

o Polarimeter: [α]D = +66.5° (sucrose) + correction for invert sugars.


o Titration: Lane-Eynon (ICUMSA GS2-1-7).
5. Calculate Trapped RS:

Trapped RS (%)=Initial RS−RS in washed liquidTrapped RS (%)=Initial RS−R


S in washed liquid

4. ICUMSA Cross-Validation

For audit compliance:

 Compare with GS6 (molasses exhaustion):

o Alcohol Wash trapped RS should correlate with:

ICUMSA Exhaustion (%)=(1−RSmolassesRSmassecuite)×100ICUMSA Exhaus


tion (%)=(1−RSmassecuiteRSmolasses)×100

 Document solvent purity (ethanol ≥96%, per ICUMSA reagent standards).


5. When to Use This Test

 For internal process control (not ICUMSA certification).


 To diagnose:

o Centrifuge inefficiency (high trapped RS).


o Gums/starch interference (if trapped RS is low but final RS high).

6. ICUMSA Alternatives for Trapped RS

For official reporting, use:

 GS6-12: "Determination of Apparent Purity of Massecuite".


 GS2-10: "Sucrose in Molasses by Polarimetry".

Key Takeaway

The Alcohol Wash Test is a practical supplement to ICUMSA methods for


troubleshooting—but for certification, use GS2/GS6.

Need an ICUMSA-compliant Excel template? Let me know!

How Poor Exhaustion & Molasses Trapping Impact RS in


Sugar Refining

When exhaustion is inefficient and molasses remains trapped on


sugar crystals, it directly increases the Reducing Sugars (RS) in final
molasses. Here’s the detailed mechanism and its consequences:
1. The Link Between Exhaustion, Trapped Molasses, and RS

A. Definitions

 Exhaustion: The process of removing sucrose from molasses during


crystallization.
 Trapped Molasses: The film of mother liquor (containing sucrose, RS, and
impurities) adhering to crystals after centrifugation.

B. How It Increases RS

1. Sucrose Retention → Higher RS

o Trapped molasses contains unrecovered sucrose, which degrades


into glucose + fructose (RS) during storage/processing.
o Example: 1% trapped sucrose → Can invert to ~0.5% extra RS.
2. Impurities (Gums/Dextrans) Prevent Separation

o High-viscosity molasses (from gums) coats crystals thicker, trapping more


sucrose/RS.
o Result: Even with large crystals (0.65 mm), RS stays high.
3. Centrifuge Inefficiency

o Low G-force or short cycles leave more molasses on crystals → Higher RS


in final product.

2. Quantifying the Impact

Parameter Good Exhaustion Poor Exhaustion Effect on RS

Trapped Molasses 1–2% of crystal weight 5–10% of crystal +3–8% RS


Parameter Good Exhaustion Poor Exhaustion Effect on RS

weight

Final Molasses RS 15–18% 20–25% +5–7% RS

Sucrose Loss <3% 5–10% Profit loss

Example:

 If trapped molasses contains 5% sucrose, and 50% of it inverts to RS:

Added RS=5%×0.5=2.5% higher RS in molasses.Added RS=5%×0.5=2.5% hig


her RS in molasses.

3. Root Causes & Fixes

A. Why Exhaustion Fails

1. High Viscosity (from gums/starch) → Poor molasses drainage.


2. Centrifuge Issues: Low RPM, worn screens, or short cycles.
3. Crystal Shape: Jagged/aggregated crystals trap more molasses.

B. How to Improve

✔ Optimize Centrifugation

 Increase G-force (e.g., from 1,200 to 1,500 RPM for C-massecuite).


 Extend wash cycle time (by 10–20%).

✔ Reduce Viscosity

 Pre-dilute massecuite to 92–94°Bx before centrifuging.


 Use dextranase (for gums) or amylase (for starch).
✔ Crystal Quality

 Adjust seeding to grow smoother, rounder crystals.

4. Case Study

Problem:

 Crystals: 0.65 mm (good size).


 Molasses RS: 23% (target: 18%).
 Alcohol Wash Test: Trapped RS = 6%.

Diagnosis:

 Poor centrifuge performance + gum interference.

Solution:

1. Increased centrifuge speed by 15%.


2. Treated syrup with dextranase (50 ppm).
Result: RS dropped to 19%.

5. Key Takeaways

1. Trapped molasses = Unrecovered sucrose → Converts to RS.


2. Fix exhaustion by:

o Optimizing centrifuges.
o Breaking gums/starch.
o Improving crystal shape.
3. Monitor with Alcohol Wash Test (target trapped RS <2%).

Need a centrifuge adjustment guide? Let me know!

How Poor Exhaustion and Trapped Molasses on Crystals


Impact Reducing Sugars (RS)

When exhaustion (the removal of sucrose from molasses) is inefficient


and molasses remains trapped on sugar crystals, it directly increases
the Reducing Sugars (RS) in the final product. Here’s the breakdown:

1. Mechanisms of RS Increase

A. Poor Exhaustion

 Definition: Failure to fully recover sucrose during crystallization, leaving


excess sucrose in molasses.
 Impact:

o Residual sucrose in molasses can invert into RS (glucose + fructose) over


time due to:

 Heat during processing.


 Acidic conditions (pH < 6.5).
o Example: If molasses retains 5% sucrose, ~2.5% could invert to RS, raising
total RS by 2.5%.

B. Trapped Molasses on Crystals

 Definition: A film of molasses adhering to crystals after centrifugation.


 Impact:

o Trapped molasses contains both sucrose and RS that are not fully
separated.
o Over time, trapped sucrose inverts to RS, further increasing molasses RS.
o Example:

 If crystals retain 3% trapped molasses with 20% RS, this adds 0.6%
RS directly.
 If trapped molasses also contains 5% sucrose, inversion adds ~0.25% RS.

2. Key Factors Amplifying RS

Factor Effect on RS

High Viscosity Thick molasses sticks to crystals → more trapped sucrose/RS.

Centrifuge Inefficiency Low G-force/short cycles → poor molasses removal.

Impurities
Increase viscosity + block sucrose crystallization.
(Gums/Dextrans)

Thermal/Acid Inversion Accelerates sucrose → RS conversion.

3. Quantifying the Impact

Scenario Trapped Molasses Added RS

Good Exhaustion 1–2% of crystal mass +0.5–1% RS

Poor Exhaustion 5–10% of crystal mass +2.5–5% RS

With Inversion 5% trapped sucrose +2.5% RS

Example:
 If final molasses RS is 20%, poor exhaustion and trapping could push it
to 23–25%.

4. Solutions to Reduce RS

A. Improve Exhaustion

1. Optimize Crystallization:

o Control supersaturation (1.05–1.10).


o Use high-quality seed crystals (0.2–0.3 mm).
2. Adjust Centrifugation:

o Increase G-force (≥1,500 RPM for recovery massecuite).


o Extend wash cycle time (by 10–20%).

B. Reduce Trapped Molasses

1. Pre-Dilute Massecuite:

o Dilute to 92–94°Bx before centrifuging to lower viscosity.


2. Break Down Impurities:

o Use dextranase enzymes (50–100 ppm) for gums.


o Add α-amylase (1–2 ppm) for starch.

C. Prevent Inversion

1. Control pH: Maintain 7.0–7.5 in pans/evaporators.


2. Limit Heat: Keep evaporator temps <120°C.

5. Diagnostic Tools
1. Alcohol Wash Test:

o Measures trapped RS on crystals.


o Procedure: Wash massecuite with ethanol → compare RS before/after.
2. HMF Testing:

o Detects thermal damage (HMF >50 ppm = overheating).


3. Dextran/Iodine Tests:

o Identifies gums/starch interference.

6. Case Study

Problem:

 Final molasses RS = 23% (target: 18%).


 Alcohol Wash Test: Trapped RS = 5% (target: <2%).
Solution:

1. Increased centrifuge RPM from 1,200 → 1,500.


2. Treated syrup with dextranase (75 ppm).
Result: RS dropped to 19%.

Key Takeaways

1. Poor exhaustion + trapped molasses = Higher RS.


2. Fix: Optimize centrifugation, reduce viscosity, and prevent inversion.
3. Test: Use alcohol wash/HMF tests to diagnose root causes.

Need a step-by-step guide to adjust your centrifuges? Let me know!


Comprehensive Guide to High Reducing Sugars (RS) in Sugar
Refining: Causes, Diagnosis, and Solutions

1. Causes of High RS in Molasses

High RS is caused by inefficiencies that leave unprocessed sucrose in


molasses or convert sucrose into RS. Key culprits include:

A. Poor Crystallization

 Why: Small, irregular, or aggregated crystals trap molasses, reducing


sucrose recovery.
 Mechanism:

o Fast cooling → poor crystal growth.


o Inadequate seeding → uneven nuclei formation.
o High viscosity → sucrose remains dissolved in molasses.

B. Microbial Contamination

 Why: Microbes (yeast, bacteria) ferment sucrose into RS (glucose +


fructose).
 Sources:

o Stagnant sweet water tanks.


o Poor sanitation in pipelines or storage.
 Common Offenders:

o Leuconostoc (produces dextrans).


o Saccharomyces (produces ethanol + RS).

C. Thermal/Acid Inversion

 Why: Heat or low pH breaks sucrose into RS.


 Critical Thresholds:

o Temp >120°C in evaporators/boiling pans.


o pH <6.5 (acidic conditions).

D. Impurities (Starch, Gums, Dextrans)

 Why: Impurities block crystallization and increase viscosity.

o Starch >100 ppm: Coats crystals.


o Dextrans >300 ppm: Forms slime, traps sucrose.

E. Centrifuge Inefficiency

 Why: Poor molasses separation leaves sucrose/RS trapped on crystals.


 Causes:

o Low G-force (RPM).


o Short wash cycles.
o Worn screens/baskets.

F. Poor Exhaustion in Final Molasses

 Why: Incomplete sucrose recovery due to process limits.


 Typical Target: Final molasses RS = 15–20%.

2. Step-by-Step Diagnostics

A. Check Crystallization Efficiency

1. Microscope Analysis:

o Target: Crystals 0.2–0.3 mm (refinery) or 0.1–0.15 mm (recovery).


o Issue: Fines (<0.1 mm) or aggregates.
2. Supersaturation Monitoring:
o Target: 1.05–1.10 (refractometer/polarimeter).
o Issue: Over/under-supersaturation → poor crystal growth.

B. Test for Microbial Contamination

1. Dextran Test (Alcohol Precipitation):

o Mix 10 mL syrup + 30 mL ethanol → stringy precipitate = dextrans.


2. Microbial Counts:

o Plate counts (CFU/mL) for yeast/bacteria in sweet water or juice.


3. pH Monitoring:

o Ideal: 7.0–7.5 → pH drop (<6.5) indicates microbial acid production.

C. Detect Thermal/Acid Inversion

1. HMF (Hydroxymethylfurfural) Testing:

o HMF >50 ppm = Overheating (HPLC/colorimetric test).


2. pH Logs:

o Check historical pH data in evaporators/crystallizers.

D. Identify Impurities

1. Starch Test (Iodine):

o Add iodine to diluted syrup → blue/black color = starch.


2. Gum Test (Viscosity):

o Measure syrup viscosity (viscometer) → >5,000 cP = gum issue.

E. Evaluate Centrifuge Performance

1. Alcohol Wash Test:

o Wash 10g massecuite with ethanol → measure RS in filtrate.


o Trapped RS >5% = Centrifuge failure.
2. G-Force Calculation:
o G-force=RPM2×Basket radius (m)895G-force=895RPM2×Basket radius (m) → Target
>1,500 G.

F. Monitor Exhaustion

1. Molasses Purity:

o Purity=SucroseSucrose + RS + Impurities×100Purity=Sucrose + RS + ImpuritiesSucrose


×100.
o Target: <50% purity in final molasses.

3. Detailed Solutions for Each Cause

A. Fix Poor Crystallization

1. Optimize Seeding:

o Use 30–40% seed magma (0.2–0.3 mm crystals).


o Adjust seeding density based on supersaturation.
2. Control Cooling Rate:

o Refinery pans: Cool by 1–2°C/hour.


o Recovery pans: Cool by 0.5–1°C/hour.
3. Adjust Supersaturation:

o Use refractometer/polarimeter for real-time monitoring.

B. Eliminate Microbial Contamination

1. Sanitize Tanks/Pipes:

o Shock with hydrogen peroxide (H₂O₂, 100 ppm) or chlorine (10 ppm).
2. Heat Treatment:

o Heat sweet water to >75°C for 15 minutes.


3. Enzymes:

o Dextranase (50–100 ppm) to break dextrans.

C. Prevent Thermal/Acid Inversion

1. Temperature Control:

o Keep evaporator temps <115°C.


o Install automated temperature alarms.
2. pH Adjustment:

o Add lime (CaO) to maintain pH 7.0–7.5.

D. Remove Impurities

1. Starch:

o Add α-amylase (1–2 ppm) during clarification.


2. Gums:

o Use oxidizing agents (H₂O₂) or enzymes (dextranase).


3. Ash Control:

o Optimize lime/phosphate dosing in clarification.

E. Improve Centrifugation

1. Increase G-Force:

o Adjust RPM to achieve >1,500 G (calculate based on centrifuge specs).


2. Extend Wash Cycles:

o Add 10–15% more wash water/time.


3. Pre-Dilute Massecuite:

o Dilute to 92–94°Bx before centrifuging.

F. Enhance Exhaustion

1. Boiling Strategy:
o Stop boiling when massecuite purity drops below 75% (send to recovery).
2. Blend Low-Purity Streams:

o Mix with high-purity syrup to improve crystallization.

4. Tools & Equipment for Diagnosis

Tool Purpose

Polarimeter Measure sucrose/RS in juice/syrup.

Refractomete
Monitor Brix/supersaturation.
r

Viscometer Check syrup/massecuite viscosity.

HPLC Quantify HMF, RS, and sugars.

Microscope Analyze crystal size/shape.

pH Meter Ensure pH 7.0–7.5.

5. Troubleshooting Flowchart

1. High RS in Molasses → Perform Alcohol Wash Test.

o High Trapped RS → Optimize centrifuge (↑ RPM, ↑ wash time).


o Low Trapped RS → Check:

 Microbial counts → Sanitize + enzymes.


 HMF levels → Lower temps.
 Starch/gums → Add enzymes.
6. Case Study: RS Reduction in a Cane Refinery

Problem:

 Final molasses RS = 23% (target: 18%).


 Diagnostics:

o Trapped RS = 6% (Alcohol Wash Test).


o Dextran test = positive (400 ppm).
Solutions:

1. Centrifuge RPM ↑ 15%.


2. Treated syrup with dextranase (75 ppm).
3. Adjusted pH from 6.8 → 7.3.
Result: RS dropped to 19%.

7. Key Takeaways

1. High RS = Lost Profit: Every 1% RS reduction ≈ 1–2% higher recovery.


2. Prioritize Diagnostics: Use tests (Alcohol Wash, HMF, Dextran) to pinpoint
causes.
3. Holistic Fixes: Combine process adjustments (centrifuges, temps) with
enzyme/biocide treatments.

Need a refinery-specific action plan? Share your data!

Alcohol Wash Test: Deep Dive for Sugar Crystals

The Alcohol Wash Test is a critical diagnostic tool to determine


whether high Reducing Sugars (RS) in molasses are due to trapped
molasses on crystals or other factors (e.g., inversion, impurities). Here’s
a comprehensive guide:

1. Purpose of the Alcohol Wash Test

 Diagnose:

o Trapped molasses: Sucrose/RS adhering to crystals due to poor


centrifugation or high viscosity.
o True molasses RS: Inherent RS in the mother liquor (unrelated to crystal
trapping).
 Key Insight:

o If RS drops significantly after washing, the issue


is mechanical (centrifuge inefficiency).
o If RS remains high, the issue is chemical (inversion, impurities, microbes).

2. Materials Needed

 Sample: Massecuite (pre-centrifuge) or molasses (post-centrifuge).


 Solvent: 96% ethanol or isopropanol (pure, food-grade).
 Equipment:

o Scale (0.01 g precision).


o Beaker (100–200 mL).
o Filter paper (Whatman No. 4 or equivalent).
o Refractometer/polarimeter (for RS measurement).
o Stirring rod.
o Evaporation setup (hot plate, water bath).
3. Step-by-Step Procedure

A. Sample Preparation

1. Collect massecuite: Take 10 g from the last crystallizer (R4 or C-


massecuite).
2. Record initial RS: Use a refractometer or polarimeter (e.g., RS = 23%).

B. Washing Process

1. Mix with solvent:

o Add 30 mL ethanol to the 10 g massecuite.


o Stir gently for 5 minutes (avoid breaking crystals).
2. Filter:

o Pour the mixture through filter paper.


o Collect crystals (on paper) and filtrate (liquid).

C. Filtrate Analysis

1. Evaporate solvent:

o Heat filtrate at 60°C until ethanol evaporates.


o Re-dissolve residue in 30 mL water (original volume).
2. Measure RS: Use a refractometer/polarimeter (e.g., RS = 4%).

D. Calculate Trapped RS

Trapped RS (%)=Initial RS−RS in washed filtrate=23%−4%=19%Trapped RS (


%)=Initial RS−RS in washed filtrate=23%−4%=19%
4. Interpretation of Results

Result Diagnosis Solution

Trapped RS ↑ Centrifuge RPM, ↑ wash time, pre-dilute


Poor centrifugation
>5% massecuite.

Trapped RS 1– Moderate separation


Optimize centrifuge settings.
5% issues

Trapped RS
Good separation Focus on inversion or impurities.
<1%

5. Common Mistakes & Fixes

Error Impact Fix

Incomplete Ensure all ethanol is evaporated at


False RS reading
evaporation 60°C.

Crystal breakage → skewed


Aggressive stirring Stir gently.
results

Low-purity ethanol Residual sugars in solvent Use 96%+ ethanol.

6. Advanced Applications

A. Quantify Sucrose Trapping

1. After washing, dry crystals and weigh.


2. Calculate trapped molasses:
Trapped Molasses (%)=Weight after washing−Dry crystal weightDry crystal we
ight×100Trapped Molasses (%)=Dry crystal weightWeight after washing−Dry c
rystal weight×100

B. Link to Centrifuge Efficiency

 Formula:

Separation Efficiency (%)=(1−Trapped RSInitial RS)×100Separation Efficiency


(%)=(1−Initial RSTrapped RS)×100

o Example: (1−423)×100=82.6%(1−234)×100=82.6% → Needs improvement.

7. Case Study

Problem:

 Final molasses RS = 25% (target: 18%).


 Alcohol Wash Test:

o Initial RS = 25%.
o Washed RS = 5%.
o Trapped RS = 20%.

Diagnosis:

 Severe molasses trapping (centrifuge inefficiency).

Solution:

1. Increased centrifuge RPM from 1,200 → 1,600.


2. Extended wash cycle time by 20%.
3. Pre-diluted massecuite to 93°Bx.
Result: RS dropped to 19%.

8. Troubleshooting Guide

Symptom Check Action

Calibrate centrifuge, clean


High trapped RS Centrifuge RPM, wash time
screens.

Low trapped RS + high Test for dextrans (alcohol


Use dextranase enzyme.
final RS precipitation)

Crystals dissolve in ethanol Ethanol purity <96% Replace solvent.

9. Safety Precautions

 Ethanol/isopropanol: Flammable → Use in ventilated area, no open flames.


 Hot plates: Handle with heat-resistant gloves.

Key Takeaway

The Alcohol Wash Test isolates whether high RS stems from mechanical
trapping (centrifuges) or inherent issues (inversion, impurities). Use it to:

1. Target fixes (e.g., adjust centrifuges vs. treat impurities).


2. Save costs by avoiding unnecessary treatments.
Need a printable checklist or Excel template for tracking results? Let
me know!

Step-by-Step Investigation Guide for High Reducing Sugars


(RS) in a Sugar Refinery

Let’s start from Square One and systematically identify the root cause of
high RS in your refinery. This guide combines all prior insights into a
structured, actionable plan.

Phase 1: Initial Data Collection

Goal: Gather baseline data to narrow down potential causes.

1. Track RS at Key Stages

Stage Sample Point Target RS (%) Your Data

Raw Melt After melter <0.25

Clarified Juice Post-clarification <0.20

Syrup Pre-evaporator <0.30

A-Molasses First recovery boiling 2.0–3.0

Second recovery
B-Molasses 4.0–6.0
boiling

C-Molasses Final molasses 15–20

Action:

 Test RS at each stage using polarimetry (ICUMSA GS2/3) or Lane-Eynon


titration.
2. Check Critical Process Parameters

Parameter Target Range Your Data

pH (Juice/Syrup) 7.0–7.5

Evaporator
<120°C
Temp

Centrifuge RPM ≥1,500 (C-massecuite)

92–94°Bx (pre-
Brix (Massecuite)
centrifuge)

Action:

 Review historical logs for deviations (e.g., pH <6.5, temps >120°C).

Phase 2: Diagnostic Testing

Goal: Pinpoint the root cause using targeted tests.

Test 1: Alcohol Wash Test

Purpose: Check if RS is due to trapped molasses or true molasses RS.


Steps:

1. Collect 10g massecuite (from final crystallizer).


2. Wash with 30mL ethanol, filter, and measure RS in filtrate.
3. Calculate:

Trapped RS (%)=Initial RS−RS in washed filtrateTrapped RS (%)=Initial RS−R


S in washed filtrate
Interpretation:

 Trapped RS >5%: Centrifuge inefficiency.


 Trapped RS <1%: Inversion, impurities, or microbes.

Test 2: HMF (Hydroxymethylfurfural) Analysis

Purpose: Detect thermal damage (sucrose inversion due to overheating).


Method:

 Use HPLC or colorimetric test.


Acceptable: <50 ppm HMF.
Action:
 If HMF >50 ppm → Lower evaporator temps.

Test 3: Microbial Contamination

Steps:

1. Dextran Test: Mix syrup with ethanol → stringy precipitate = dextrans


(from Leuconostoc).
2. Microbial Counts: Plate samples from sweet water/juice on agar
→ CFU/mL (target <10⁴ CFU/mL).
3. pH Check: pH drop (<6.5) in stored juice = microbial acid production.
Test 4: Starch & Gum Analysis

1. Starch (Iodine Test):

o Add iodine to diluted syrup → blue/black = starch.


2. Gum (Viscosity Test):

o Measure syrup viscosity → >5,000 cP = gum issue.

Test 5: Crystal Quality Check

1. Microscopy:

o Good: 0.2–0.3 mm, uniform, round crystals.


o Bad: Fines (<0.1 mm), aggregates, jagged edges.
2. Supersaturation Check:

o Use refractometer → Target 1.05–1.10 supersaturation.

Phase 3: Root Cause Analysis

Map Your Findings to Likely Causes:

Test Result Likely Cause Evidence-Based Clues

Low RPM, short wash cycles, worn


High Trapped RS Centrifuge inefficiency
screens

High HMF Thermal inversion Evaporator temps >120°C, dark syrup

Microbial
Dextrans + Low pH Stringy precipitates, sour smell
contamination

Starch + High Impurities Blue iodine test, slow filtration


Test Result Likely Cause Evidence-Based Clues

Viscosity

Poor Crystal Shape Crystallization failure Fines/aggregates under microscope

Phase 4: Corrective Actions

1. Centrifuge Optimization

 Increase RPM: Target ≥1,500 G-force.


 Extend Wash Time: Add 10–20% more wash water.
 Pre-Dilute Massecuite: 92–94°Bx before centrifuging.

2. Thermal/Acid Inversion Fix

 Lower Temps: Keep evaporators <115°C.


 Adjust pH: Lime dosing to maintain 7.0–7.5.

3. Microbial Control

 Sanitize Tanks: Hydrogen peroxide (100 ppm) or chlorine (10 ppm).


 Dextranase Enzyme: 50–100 ppm in contaminated syrup.

4. Impurity Removal

 Starch: Add α-amylase (1–2 ppm).


 Gums: Use oxidizing agents (H₂O₂) or pectinase.

5. Crystallization Adjustments

 Optimize Seeding: 30–40% seed magma (0.2–0.3 mm).


 Control Cooling: 1–2°C/hour for refinery pans.
Phase 5: Monitoring & Validation

KPIs to Track

 Final molasses RS (target: 15–20%).


 Centrifuge efficiency (trapped RS <2%).
 Microbial counts (<10⁴ CFU/mL).

Daily Checks

 pH, Temp, Brix at critical stages.


 Crystal size/shape under microscope.

Example Case Study

Problem:

 Final molasses RS = 24% (target: 18%).


 Tests:

o Alcohol Wash: Trapped RS = 6%.


o Dextran Test: Positive.
o Centrifuge RPM = 1,200.
Solution:

1. Increased centrifuge RPM to 1,600.


2. Treated syrup with dextranase (75 ppm).
3. Adjusted pH from 6.8 → 7.3.
Result: RS dropped to 19% in 2 weeks.
Final Recommendations

1. Document Everything: Logs, test results, adjustments.


2. Train Staff: Standardize testing protocols.
3. Audit Quarterly: Compare RS trends against KPIs.

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