BENFIELD LIQUOR:Determination of Diethanolamine Using an Auto Titrator 1 SCOPE AND FIELD OF APPLICATION This method is suitable for the determination of diethanolamine in Benfield Liquor. 2 PRINCIPLE Diethanolamine is converted quantitatively into ammonia by boiling in the presence of sulfuric acid and copper sulfate. The ammonia is distilled from an alkaline medium and absorbed into boric acid. The solution is titrated with standard acid.

1. GBH Enterprises, Ltd.
Plant Analytical Techniques
BENFIELD LIQUOR: Determination of Diethanolamine - using
an auto titrator
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2. BENFIELD LIQUOR:
1
Determination of Diethanolamine –
using an auto titrator
SCOPE AND FIELD OF APPLICATION
This method is suitable for the determination of diethanolamine in Benfield
Liquor.
2
PRINCIPLE
Diethanolamine is converted quantitatively into ammonia by boiling in the
presence of sulfuric acid and copper sulfate. The ammonia is distilled
from an alkaline medium and absorbed into boric acid. The solution is
titrated with standard acid.
3
Reagents
During the analysis use only reagents of analytical reagent grade, unless
otherwise specified, and water which has been deionized and then
distilled from an all glass apparatus, or water of equivalent purity.
3.1 Digestion mixture. dissolve 12 g of copper (11) sulfate crystals in 400
mL of water then carefully add 1600 mL of concentrated sulfuric acid
(S.G.= 1.84)
SULFURIC ACID - REACTS VIGOROUSLY WITH WATER WITH
EVOLUTION OF HEAT – CAUSES SEVEREBURNS - DIGESTION
MIXTURE IS CORROSIVE.
3.2
Hydrochloric acid. c(HC1) = 0.1 M
HYDROCHLORIC ACID - CAUSES BURNS AND HAS A
HARMFUL VAPOR
3.3
Boric acid, 1% with bromocresol green / methyl red indicator
solution. Dissolve 100 g of boric acid in 10 L of water. Add 100 ml
bromocresol green solution (100 mg in 100 ml methanol). Add 70
ml methyl red solution (alcohol soluble grade) (100 mg in 100 ml
methanol). Mix thoroughly.
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3. Transfer 25 ml of the boric acid solution to a receiver flask and add
100 ml of water. If the solution in the flask is still red, titrate with 0.1
M sodium hydroxide solution until a neutral grey color is obtained.
Calculate the amount of sodium hydroxide solution necessary to
adjust the boric acid solution in the
10 L flask with the formula:
ml 1.0 M alkali = ml titre x 40
Add the calculated amount of 1.0 M alkali solution to the boric acid
solution. Mix. Check the adjustment result by distilling a new blank
sample.
METHANOL - TOXIC BY INGESTION - DAMAGING IF SPLASHED IN
EYES. HIGH CONCENTRATIONS OF VAPOR MAY CAUSE
DIZZINESS, STUPOR, CRAMPS AND DIGESTIVE DISTURBANCE.
LOWER LEVELS MAY CAUSE HEADACHE AND NAUSEA.
BROMOCRESOL GREEN AND METHYL RED - HARMFUL AVOID
CONTACT WITH EYES AND SKIN. SODIUM HYDROXIDE IRRITATING TO EYES AND SKIN.
3.4
Sodium hydroxide solution, 35-40%.
SODIUM HYDROXIDE - CAUSES BURNS AVOID CONTACT WITH
EYES AND SKIN.
4
APPARATUS
4 .1
Standard volumetric glassware. Class A.
4.2
Digestion system, a Tecator Digestion system 6 1007 Digester
is suitable.
4.3
Auto-titrator, a Tecator Kjeltec AUTO 1030 analyzer is suitable.
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4. 5
5.1
Procedure
Blank determination
Perform a blank determination using 50 ml of water, following the
procedure described in sub-section 5.2 from "Connect the distillation
tube".
5.2
Calibration
Dry ammonium sulfate at 105 deg C for 1 hour. Weigh exactly 0.1000 g.
Transfer to the distillation tube of the auto-titrator (4.3), add approximately
50 ml water. Connect the distillation tube to the splash head. Start the run
in accordance with the manufacturer's instructions. (see Annex 1 for
Parameters and Operational procedure for the Tecator Kjeltec AUTO 1030
analyzer).
5.3
Preparation of the solution.
5.3.1 Weigh 10 g to the nearest 0.001 g of sample and transfer
quantitatively into a digestion tube. Add carefully and slowly
(dropwise initially) 20 ml of digestion mixture (3.1). Set up the
digestion system (4.2) according to the manufacturer's instructions.
Place the digestion tube in the digestion system (4.2). Heat the
mixture in the digestion system to boiling and continue to digest for
1 hour (following manufacturer's instructions).
5.3.2 Cool the mixture, and then carefully add approximately 40 ml of
water. Mix thoroughly.
5.4
Determination
Set up the auto-titrator according to the manufacturer's instructions.
Transfer the sample as prepared in sub-section 5.3 into the distillation
tube of the auto-titrator (4.3). Add approximately 40 mL of water. Continue
as described in sub-section 5.2 from "Connect the distillation tube.......".
6
Expression of Results
6.1
Express the results of analysis as a percentage of diethanolamine
in the Benfield Liquor as % m/m.
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5. ANNEX 1 – Parameters
Ensure the Tecator Kjeltec AUTO 1030 analyzer is set up as below:
A B and C are the front panel settings
Where
A = Delay time
B = Factor for converting mL of 0.1 M HCl to
diethanolamine % m/m.
[( § is given by the expression 1.05 x 1 )]
M
10
where
M = mass of sample
C = Blank value
(* is the current blank value as obtained in sub-section 5.1 e.g. for 0.2 mL
the blank value is 0.2 x 10 i.e. 20)
Operational
After the appropriate parameters have been set up as shown above proceed as
follows:
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6. Close the safety door after completion CYCLE OVER light will come on
permanently.
Open safety door and wait until CYCLE OVER light comes on
permanently.
Remove digestion tube (DANGER - HOT SURFACE) and carefully wash six
times with water, then wash with dilute sulfuric acid finally wash with
water.
Result is displayed directly on left of front panel as % m/m.
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