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Amine Aqueous Solution Total Amine Concentration Potentiometry

This document describes a potentiometric method for determining the total amine concentration in aqueous amine solutions, such as those used for acid gas scrubbing. The method involves titrating a sample of the amine solution with sulfuric acid and monitoring the pH. For regenerated solutions, two inflection points are observed corresponding to the free and total amine concentrations. For new solutions, a single inflection point indicates the total amine concentration. The amine concentration is calculated based on the titration volume and molecular weight of the amine. The method can measure amine concentrations typically ranging from 3 to 4 mol/L with a repeatability precision of 0.05 × [Amine (g/L)].

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Nguyen Nguyen
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369 views

Amine Aqueous Solution Total Amine Concentration Potentiometry

This document describes a potentiometric method for determining the total amine concentration in aqueous amine solutions, such as those used for acid gas scrubbing. The method involves titrating a sample of the amine solution with sulfuric acid and monitoring the pH. For regenerated solutions, two inflection points are observed corresponding to the free and total amine concentrations. For new solutions, a single inflection point indicates the total amine concentration. The amine concentration is calculated based on the titration volume and molecular weight of the amine. The method can measure amine concentrations typically ranging from 3 to 4 mol/L with a repeatability precision of 0.05 × [Amine (g/L)].

Uploaded by

Nguyen Nguyen
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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INSTITUT FRANÇAIS DU PÉTROLE

Physics and Analysis Division Analytical Methods

IFP 0507

AMINE AQUEOUS SOLUTION


TOTAL AMINE CONCENTRATION
POTENTIOMETRY

1 05/06/05 M. DIGNE N. SCHILDKNECHT P. BECCAT modifié le


RÉV. DATE RÉDIGÉ VÉRIFIÉ APPROUVÉ REMARQUES

Institut français du pétrole


IFP-Lyon ■ BP 3 ■ 69390 Vernaison ■ France

529872645.doc
INSTITUT FRANÇAIS DU PÉTROLE ANALYTICAL METHODS
N° laboratory N° method Rev. Page
Physics and Analysis Division
AM SP13 0507 1 2/4

1. SCOPE
1.1 This method applies to the determination of amine concentration in amine aqueous
solution, either regenerated (lean amine) or not (new amine). The amine concentration could usually
be in the range of 3 to 4 mol/l.
1.2 This standard may involve hazardous materials, operations, and equipment. This standard
does not purport to address all of the safety problems associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use.

2. REFERENCED DOCUMENTS
2.1 Total Analysis Method N° 181 "Determination of the concentration of monoethanolamine
(MEA), diethanolamine (DEA) or methyldiethanolamine (MDEA)".

3. TERMINOLOGY
3.1 Lean amine means amine aqueous solution after regeneration, exhibiting low residual
concentration in CO2 (lower than 100 g/L) and H2S (lower than 50 g/l).
3.2 New amine means fresh amine solution before contact with acid gas.
3.3 Amine must be monoethanolamine (MEA), diethanolamine (DEA) or
methyldiethanolamine (MDEA).

4. SUMMARY OF THE METHOD


4.1 The amine concentration is measured by titration with a normal solution of sulphuric acid,
using a pH-meter. For regenerated sample, the titration is characterized by two inflection points: the
first one corresponds to the free amine, and the second one to the total amine. The difference
between total and free amine is called the residue. For new sample, a single inflection point is found
corresponding to the total amine.

5. APPARATUS
5.1 Buret or automatic titrator.

Institut français du pétrole


IFP-Lyon ■ BP 3 ■ 69390 Vernaison ■ France

529872645.doc
INSTITUT FRANÇAIS DU PÉTROLE ANALYTICAL METHODS
N° laboratory N° method Rev. Page
Physics and Analysis Division
AM SP13 0507 1 3/4

5.2 Laboratory pH-meter with combined glass-calomel electrode.


5.3 Standard laboratory glassware (class A).

6. REAGENTS AND MATERIALS


6.1 Standard solution of sulphuric acid (N = normality of H2SO4, ideally 1 mol/L).
6.2 Distilled water.

7. PREPARATION OF APPARATUS
7.1 Calibrate the pH-meter, according to the standard procedures.

8. PROCEDURE
8.1 Pipet with precision 5 ml of amine into the titration cup and add about 150 ml of water.
8.2 Titrate with the solution of sulphuric acid.
8.3 Record the volume(s) required to reach the inflection point(s).
8.4 The duration of analysis is roughly 15 minutes.

9. CALCULATION
9.1 New amine
Calculate the concentration of total amine, as follows:
M×V×N
[Total amine (g/l) ] =
5
where:
N = normality of H2SO4 solution (mol/l),
V = volume of H2SO4 required to reach the equivalence point (ml),
M = molecular weight of amine (g/mol) (see 9.3).

9.2 Lean amine


Calculate the concentration of free and total amine, as follows:
M × V1 × N
[Free amine (g/l)] =
5
M × V2 × N
[Total amine (g/l)] =
5

Institut français du pétrole


IFP-Lyon ■ BP 3 ■ 69390 Vernaison ■ France

529872645.doc
INSTITUT FRANÇAIS DU PÉTROLE ANALYTICAL METHODS
N° laboratory N° method Rev. Page
Physics and Analysis Division
AM SP13 0507 1 4/4

where:
N = normality of H2SO4 solution (mol/l),
V1 = volume of H2SO4 required to reach the first inflection point (ml),
V2 = volume of H2SO4 required to reach the second inflection point (ml),
M = molecular weight of amine (g/mol) (see 9.3).

9.3 Molecular weight for standard amines


M (MEA) = 61 g/mol,
M (DEA) = 105 g/mol,
M (MDEA) = 119 g/mol.

10. PRECISION
10.1 Estimation of repeatability (r) from the IFP laboratory data - The difference between two
tests results, obtained by the same operator with the same apparatus under constant operating
conditions on identical test material, would in the long run, in the normal and correct operation of the
method, exceed the following value only in one case in twenty:
r (g/l) = 0.05  [Amine (g/l)]

Institut français du pétrole


IFP-Lyon ■ BP 3 ■ 69390 Vernaison ■ France

529872645.doc

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