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International Starch Institute
Science Park Aarhus, Denmark
ISI 10-2e Determination of Carboxyl Groups in Starch
1. Scope | The method is applicable to oxidised starch | LT 18. Dec. 1964 Rev. LT 15. marts 1998 |
2. Principle | Carboxyl groups are titrated by the Paste Titration Method
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3. Apparatus | 3.1 Analytical balance weighing to the nearest 0.1 mg. 3.2 Shaking boiling water bath. 3.3 Büchner funnel 55 mm |
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4. Reagents | 4.1 Hydrochloric acid 0.1 N 4.2 Sodium hydroxide 0.1 N 4.3 Phenolphthalein: 1 g in 1 litre ethanol 90% 4.4 Silver nitrate, 0.1%
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5. Procedure | Weigh 5 g (w) sample to the nearest 0.1 mg in a 100 ml beaker | |
Conversion |
Add 25 ml hydrochloric acid (4.1) and stir for 1/2 hour. | Use magnetic stirrer |
Washing |
Filter on filter (3.3) or glass crucible. Flush beaker and filter with water until filtrate is free of chloride - test with silver nitrate (4.4) | Increase hydrolysis parameters if flux too low |
Gelatinising |
Slurry filter cake with 300 ml distilled water in beaker. Place beaker in boiling water bath (3.2) for 15 min. | Stir |
Titration |
Titrate with (4.2) and (4.3) while still hot. V = ml (4.2). N = normality of (4.2)
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To pH 8.3 |
6. Calculation | Calculate carboxyl content of sample by averaging results of two samples
with two decimals. COOH % = (100 N V M ) / (1000 w) - c Degree of Substitution (DS) = 0.036 x COOH% |
Molecular weight of COOH = M = 45 c corrects for lipids and P - see notes |
Eventually correct to value on sample dry matter.
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7. Notes | c = approx. 0.1% on dry basis for maize and wheat starch. c = 0 for wheat and maize starch defatted by Soxhlet extraction |
Correction for lipids |
c = 3p for potato starch, where p = phosphorous as P %
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p ~ 0.03 - 0.09% | |
8. Reference | ISO 11214 |
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Keywords: laboratory,method,determination,carboxyl,COOH group,oxidised,starch