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Tests and specifications

In general, national standards for emulsion only include tests on the emulsion itself, but some application tests are recommended as well. Even if the tests on the emulsion are satisfactory, there is no guarantee that the application will work. The specifications are sometimes very wide, for example the viscosity in ASTM. A narrower internal specification is, therefore, recommended. The tests described here are taken from ASTM and DIN as well as from recommendations worked out by Asphalt Applications. They are only described briefly and a thorough study of the test method is, therefore, recommended before doing the test. The type of test is given in brackets.

Brief description of the test methods

Viscosity (Saybolt Furol, ASTM D244-89) Viscosity is defined as a fluid's resistance to flow. 100 ml of emulsion is poured into a cup with a hole at the bottom. A measuring glass is placed under the cup. The emulsion is let out and the timer is started. The time it takes for a certain amount of emulsion is noted as the viscosity. Storage stability (ASTM D244-89) Due to differences in density between water and bitumen, the bitumen droplets will either move down or up. 500 ml of emulsion is poured into a glass cylinder. Then it is left for 24 hours at room temperature. 50 ml is taken from the top and 50 ml from the bottom. The bitumen content of both samples is measured using the residue by evaporation. The storage stability value is calculated by subtracting the top residue from the bottom residue. Breaking index (FAS 345-89, Swedish standard) This test shows the breaking rate of the emulsion. It is only used on CRS emulsions. 100 grams of emulsion is poured into a steel container. Special filler is then added to the emulsion at a rate of 18 grams per minute. A rod or a knife is used to agitate while adding the filler. When the emulsion breaks and forms a ball, the amount of filler added is noted as the breaking index. Coating ability (ASTM D244-89) This is a test to see the coating ability between the bitumen and the aggregate. The emulsion is mixed with the aggregate that is to be used in the project. The mix is mixed for 5 minutes and then the coverage of the aggregate is evaluated. Part of the mix is then rinsed with water. The coverage is then noted again. This test can be done with both dry and wet aggregate.

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Sieve test (ASTM D244-89) This test shows whether there is a problem with the stability of the emulsion, flocculation or coalescence. 100 grams of emulsion is poured through an 850-micron sieve. The sieve is rinsed with water, placed on a steel pan and left at 105C for 2 hours. The weight of the sieve after it has been dried minus the weight before is the sieve residue. Cement mixing (ASTM D44-89) This test determines the breaking rate for slow-setting emulsions. The emulsion is diluted to a residue of 55%. The emulsion is mixed with a certain amount of cement for one minute. The water is added and the mixing is continued for 3 minutes. The mix is poured through a sieve. The sieve is dried. The amount of mix left on the sieve is noted. Residue Using Metal still (ASTM D244-89) This is the only test that determines the content of both bitumen and solvent in an emulsion. 200 grams of emulsion is poured into a metal cylinder. Using a gas burner, the cylinder is heated to 215C high up on the cylinder and then the burner is lowered to the bottom. The cylinder is heated to 260C and this temperature is kept for 15 minutes. The water and the solvent in the emulsion evaporate and are cooled down and end up in a graded beaker. The content of water and solvent can then be read in the glass cylinder.

Using Hot plate (Asphalt Applications) This is a quick method to determine the percentage of bitumen in the emulsion. If solvent is added to the emulsion, this method is not reliable. In that case, use the water content or the metal still test.

A small sample, 8-12 grams, is poured into a steel cup with a stirring rod. The cup is then put on a hot plate to boil away the water in the emulsion. The cup is taken off the hot plate when the boiling stops. The percentage is calculated by dividing the weight of the emulsion by the weight of the residue.

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By evaporation (ASTM D244-89) This test determines the bitumen content in an emulsion. If solvent is added to the emulsion, the water content test or the metal still test is recommended. 50 grams of emulsion is poured into a 1-litre steel container. It is left at 165C for three hours. The bitumen percentage is calculated by dividing the weight of the emulsion by the residue. Water content (ASTM D244-89) This test determines the water content in the emulsion. This method is more accurate than hot plate and easier than metal still.

Cooling water out

Cooling water in

Toluene

50 grams of emulsion is poured into a roundbottomed beaker together with 200 grams of toluene and a couple of boiling stones. The beaker is placed in a heater and a water trap and a cooler are placed on top. The emulsion is then boiled until no more water evaporates. When the boiling has stopped, the water content is read in the water trap. The water content is then divided by the emulsion content.

Water

Emulsion and toluene

Penetration of the bitumen (ASTM D5-86) This test determines the hardness of the bitumen. 50 grams of bitumen is poured into a steel beaker and tempered to 25C. A needle is pushed with a load of 50 grams for 5 seconds. The distance the needle sinks into the bitumen is multiplied by ten to give the penetration value.

pH in emulsion (Asphalt Applications) The pH is measured in the emulsion by a pH-meter. The pH value is generally not higher than 3.4-4.0.

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Particle size distribution (Asphalt Applications) The particle size distribution can be measured in different ways. Normally a laser is shot into the diluted sample and the angle of the light scattered from the particles is measured. Three different parameters are noted: <90%, <10% and median. The particle size distribution is affected by emulsifier type and content, colloid mill being used, type of bitumen and temperatures during production. A normal emulsion has the following values: <90% <10% Median 10-20 microns 1-2 microns 3-8 microns

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Recommended tests

The table shows the recommended tests and the values as specified in the corresponding standard, for example AST One of the sieve tests is a test developed by Asphalt Applications and no specification is available, but the recomme 0.1%. The emulsions are not called the CRS, CMS or CSS in the DIN standards. These standards have a corresponding em taken from them.
Type Grade Spec. Viscosity, SF, 25C, Viscosity, SF, 50C, Storage stability Breaking index
1

Rapid setting CRS-1 min max CRS-2 min max min

Medium setting CMS-2 max CMS-2h min max

Sec. Sec. % w/w g

ASTM ASTM ASTM FAS ASTM good fair fair fair good fair fair fair 0.1 0.1 20 100 1 90 100 400 1 90 50 450 1 140 140 50 450

Coating ability Coating dry aggregate Coating after spraying Coating wet aggregate Coating after spraying Sieve test, 0.850 mm Sieve test , 0.125 mm Cement mixing
2 2

% w/w % w/w % w/w

ASTM AA ASTM ASTM ASTM ASTM 60 100

0.1 0.1

0.1 0.1

Solvents, by volume of emulsion Residue Penetration % w/w mm/10

3 65 250 100

3 65 250 100

12 65 250 40

1 2

This method is used in Europe instead of the demulsibility test. This test is developed by Asphalt Applications to ensure early observation of when the emulsion sta

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Recommended tests
This chart shows the recommended tests.
Specification Viscosity, SF, 25C, Viscosity, SF, 50C, Storage stability Breaking index Coating ability Coating dry aggregate Coating after spraying Coating wet aggregate Coating after spraying Sieve test, 0.850 mm Sieve test, 0.125 mm
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Note This spec can be calculated to Standard Tar value by dividing the result by 6.204

Sec. Sec. % w/w g

ASTM ASTM ASTM FAS ASTM

European test method instead of demulsibility test

% w/w % w/w

ASTM AA Test method developed by Asphalt Applications. Recommended spec. <0.1%

Cement mixing

% w/w

ASTM ASTM ASTM ASTM Hot plate and water content without solvent; metal still if solvent is added

Solvents, % by volume of emulsion Residue Penetration % w/w mm/10

ASTM American Society for Testing Materials FAS Swedish standard AA Asphalt Application test method

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