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Amine Value

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DETERMINING EPOXIDE EQUIVALENT AND AMINE VALUE OF RESINS

TXDOT DESIGNATION: TEX-815-B

Test Procedure for

DETERMINING EPOXIDE EQUIVALENT AND AMINE VALUE OF RESINS


TxDOT Designation: Tex-815-B
Effective Date: May 2000

Texas Department of Transportation

1.
1.1 1.2 1.3

SCOPE
Use this method to determine the epoxide equivalent for epoxy resins and the amine value for polyamide resins. Reference ASTM D 1652 and D 2074 (modified by D-9-J). The values given in parentheses (if provided) are not standard and may not be exact mathematical conversions. Use each system of units separately. Combining values from the two systems may result in nonconformance with the standard.

2.
2.1 2.2

APPARATUS
Buret, 25 ml (0.85 fl. oz.), for titration. Erlenmeyer flasks, 50 ml (1.7 fl. oz.), with stoppers. two for duplicate titration used in standardization of HBr solution two for duplicate titration used for each sample of epoxy or polyamide resin.

3.
3.1 3.2 3.3 3.4 3.5

MATERIALS
Hydrobromic Acid (HBr), 47-49%, reagent grade. Acetic acid, glacial, reagent grade Potassium acid phthalate (Pht), reagent grade. Methyl violet indicator, 0.1 g in 100 ml (3.4 fl. oz.) glacial acetic acid. Methyl isobutylketone (MIBK), reagent grade. Note 1The presence of water at any time in this procedure will invalidate the results. Cloudiness in the sample or test solutions indicates the presence of water.

CONSTRUCTION DIVISION

13

EFFECTIVE DATE: MAY 2000

DETERMINING EPOXIDE EQUIVALENT AND AMINE VALUE OF RESINS

TXDOT DESIGNATION: TEX-815-B

4.
4.1 4.1.1 4.1.2 4.1.3 4.1.4 4.1.4.1 4.1.4.2 4.2 4.2.1

PROCEDURES
Standardizing Titrant: Prepare the 0.1 N HBr in glacial acetic acid by adding 8 g of hydrobromic acid to 500 ml (16.9 fl. oz.) of acetic acid. Analytically weigh 0.4 0.005 g of potassium acid phthalate into a 50 ml (1.7 fl. oz.) Erlenmeyer flask. Weigh a duplicate. Add 10 ml (0.33 fl. oz.) of glacial acetic acid to each sample and heat gently to dissolve the phthalate. Titrate the sample, using approximately 12.5 ml (0.42 fl. oz.) of the 0.1 N HBr solution, to a green color using two to three drops of methyl violet indicator (See Section 5). Use the same amount of indicator for each sample because of the small amount of solvent. The solution will change from purple to dark, then light blue until obtaining the green color. The final color change is obvious. Determining Epoxy Equivalent or Amine Value: Analytically weigh 1.0 0.001 g of the 75% solids epoxy, 0.4 0.001 g 100% solids epoxy, or 0.4 0.001 g of the 70% solids polyamide sample into a 100 ml (3.4 fl. oz.) beaker (0.75 or 0.35 g for a 100% solids sample). Use a quantity of sample that will yield 0.001 to 0.002 g equivalents of epoxy groups (See Section 5). Also run a duplicate sample. Dissolve the samples in 10 ml (0.35 fl. oz.) of MIBK acid. Just prior to titration, add 10 ml (0.35 fl. oz.) glacial acetic acid to the sample, and titrate with the standardized HBr to the same color as the standards. The endpoint for the amine value is not the same as for the epoxide procedure. The amine value solution turns milky, then green.

4.2.1.1 4.2.1.2 4.2.2

5.
5.1

CALCULATIONS
Calculate the normality of the HBr solution:

Normality of HBr Solution =

Weight of Pht 1000 204.2 mL of HBr

CONSTRUCTION DIVISION

23

EFFECTIVE DATE: MAY 2000

DETERMINING EPOXIDE EQUIVALENT AND AMINE VALUE OF RESINS

TXDOT DESIGNATION: TEX-815-B

5.2

Calculate the epoxy equivalent of epoxy resins:

Epoxy Equivalent = 1000


5.3

Weight of Sample % NVM (fraction) Normality of Hbr mL of Hbr

Calculate the amine value of polyamide resins:

Amine Value =

mL of HBr Normality of HBr 56.1 Weight of Polyamide % NVM (fraction)

6.
6.1

ARCHIVED VERSIONS
Archived versions are available.

CONSTRUCTION DIVISION

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EFFECTIVE DATE: MAY 2000

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