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NATIONAL BUREAU OF STANDARDS REPORT

8536

FINAL REPORT

BONDING TO TREATED CONCRETE SURFACES

U.S. DEPARTMENT OF COMMERCE

NATIONAL BUREAU OF STANDARDS
The National Bureau of Standards is a principal focal point in the Federal Government for assuring

maximum application of the physical and engineering sciences to the advancement of technology in industry and commerce. Its responsibilities include development and maintenance of the national stand- ards of measurement, and the provisions of means for making measurements consistent with those standards; determination of physical constants and properties of materials; development of methods

fo'r testing materials, mechanisms, and structures, and making such tests as may be necessary, particularly for government agencies; cooperation in the establishment of standard practices for incorporation in codes and specifications; advisory service to government agencies on scientific and technical problems; invention and development of devices to serve special needs of the Government; assistance

to industry, business, and consumers in the development and acceptance of commercial standards and

simplified trade practice recommendations; administration of. programs in cooperation with United

States business groups and standards organizations for the development of international standards of

practice; and maintenance of a clearinghouse for the collection and dissemination of scientific, technical, and engineering information. The scope of the Bureau’s activities is suggested in the following

listing of its four Institutes and their organizational units. Institute for Basic Standards. Electricity. Metrology. Heat. Radiation Physics. Mechanics. Applied Mathematics. Atomic Physics. Physical Chemistry. Laboratory Astrophysics.* Radio Standards Laboratory: Radio Standards Physics; Radio Standards Engineering.** Office of Standard Ref- erence Data. Institute for Materials Research. Analytical Chemistry. Polymers. Metallurgy. Inorganic Materials. Reactor Radiations. Cryogenics.** Office of Standard Reference Materials. Central Radio Propagation Laboratory.** Ionosphere Research and Propagation. Troposphere

and Space Telecommunications. Radio Systems. Upper Atmosphere and Space Physics.

Institute for Applied Technology. Textiles and Apparel Technology Center. Building Research.

Industrial Equipment. Information Technology. Performance Test Development. Instrumentation.

Transport Systems. Office of Technical Services. Office of Weights and Measures. Office of Engineering Standards. Office of Industrial Services.

* NBS Group, Joint Institute for Laboratory Astrophysics at the University of Colorado. ** Located at Boulder, Colorado.

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NATIONAL BUREAU OF STANDARDS REPORT

NBS PROJECT NBS REPORT

1004-12-10449 1 September 1964 8536

FINAL REPORT

BONDING TO TREATED CONCRETE SURFACES

by

Winthrop C. Wolfe

Organic Building Materials Section

Building Research Division

Institute for Applied Technology

Sponsored by

Office of the Chief of Engineers

Department of the Air Force

Bureau of Yards and Docks

IMPORTANT NOTICE NATIONAL BUREAU OF ST

for use within the Government, and review. For this reason, th whole or in part, is not authoi Bureau of Standards, Washingto

the Report has been specifically

Approved for public release by the

Director of the National Institute of

Standards and Technology (NIST)

on October 9, 2015.

>s accounting documents intended

subjected to additional evaluation

listing of this Report, either in

• Office of the Director, National

iy the Government agency for which

opies tor its own use.

U.S. DEPARTMENT OF COMMERCE

NATIONAL BUREAU OF STANDARDS

FINAL REPORT

BONDING TO TREATED CONCRETE SURFACES

1 . INTRODUCTION

The present study of the adhesion of resilient floor coverings and organic

coatings to concrete surfaces treated with curing, parting, sealing,, hardening, and other agents was initiated during 1962. Occasionally problems are reported with resilient, flooring installations in which the cause is sus- pected to be some treatment applied to the concrete on which the floor is

laid. Some paint failures might also be ascribed to concrete treatments

on floors, walls, and ceilings because membrane curing agents or form oil

have been used on these areas. The first task in this project was to

develop information on concrete treatments and classify them according to

their effect on the adhesion of resilient flooring or paint to concrete

substrates. The second task was to develop methods for determining in

the field whether a particular concrete surface is suitable for the

application of adhesives or organic coatings. A third task was to devise

methods of treating unsatisfactory surfaces to make them suitable for the

application of adhesives or organic coatings.

2 . BACKGROUND

During the course of this project we have cooperated with other Government

agencies and with private associations, such as the Rubber Manufacturers

Association and the Asphalt and Vinyl Asbestos Tile Institute, in collecting

information on commercial curing agents. The private associations mentioned

have made some of this information available to industry in the form of

reports.

Some information on practical tests for adhesion of resilient floor

coverings is available from industry and Government. The only practical

field test which has been published and was available to us appears to

be the procedure mentioned on page 33 of ’“Technical Data 1964-65”,

Armstrong Cork Company, Floor Division, Lancaster, Pennsylvania. In this

test, 3-foot squares of flooring material are installed approximately

50 feet apart in the manner to be used in the final installation. The

panels are examined for secure bonding after two weeks. The material

is considered to be securely bonded if '“unusual force is required to

lift it from the subfloor and If, after doing so, adhesive clings to

both the subfloor and the back of the material.”

We have also investigated the possibility of a field test in which bond

strength could be measured and expressed numerically. Such a quantitative test is written in NAVDOCKS SPECIFICATION 13Yf, December 1960,

CONCRETE CONSTRUCTION, Section 2.13.7, page 12.

3. MATERIALS AND LABORATORY TEST PROCEDURES

3,1 Adhesion of Organic Coatings to Concrete

In testing for adhesion of organic coatings, 108 3- by 5“inch cement mortar

panels, 5/8-inch thick were prepared from approximately 2 parts "high early

strength" portland cement, 6 parts of concrete sand, and 1 part of water,

by weight o The panels were steam cured for 28 days 0 Some of the panels were left untreated and some were coated with various concrete curing

agents. The panels to be treated were first soaked in water for 24 hours,

then curing agents were applied by brush,, After a suitable drying period,

organic coatings were applied to the panels.

Treatments and coatings were applied tp the test panels as indicated in

Table 1. In Table 1, curing agents are identified by capital letters

and organic coatings by Roman numerals. Information on the formulation

of the curing agents and organic coatings is found in Appendix 3 of this

report

.

After the organic coatings had dried for 24 hours, each of the test panels

was divided into four sections from top to bottom as shown in the photographs, These sections were marked off with indelible ink. A section or area 1/4- by 3-inches at the top of each panel was reserved for numbering.

This was followed by three areas, equal in size, each 1-1/2- by 3-inches.

Within each area or section, the top portion was reserved for the

adhesive tape test and the bottom portion, for the thumb nail and knife

blade tests. The bottom area was tested 1 day after applying the organic

coating; the middle or second area was tested after 7 days; and the top area was tested after 30 days.

In the thumb nail test, the thumb nail was scraped across the width of the

panel. In the knife blade test, paint was scraped off the width of the

panel (horizontally in the photograph) with a Bard Parker knife at about

a 30° angle to the panel.

The adhesive tape test was a modification of that described by Henry A.

Gardner and George G. Sward, Paint Testing Manual, 12th edition, March,

1962, p. 165. The procedure is as follows:

Scribe a cross about 1/2- by 1-inch in. the coating. Apply pressure

sensitive tape to the cut and parallel to the long arm of the cross all

the way across the width (horizontal) of the panel (3 inches). Rub to

firm adherence with the fingers. Pull the tape off with a sharp pull

as nearly as possible in the plane of the surface. Observe the removal

of coating visually.
.
Table 1 . ASSIGNMENT OF TREATMENTS TO TEST PANELS

Treatment

Paint A B C D E F G H I Panel Number

I 1 2 3 4 5 6 7 8 9 II 10 11 12 13 14 15 16 17 18

III 19 20 21 22 23 24 25 26 27

IV 28 29 30 31 32 33 34 35 36

V 37 38 39 40 41 42 43 44 45

VI 46 47 48 49 50 51 52 53 54

VII 55 56 57 58 59 60 61 62 63

VIII 64 65 66 67 68 69 70 71 72

IX 73 74 75 76 77 78 79 80 81

X 82 83 84 85 86 87 88 89 90

XI 91 92 93 94 95 96 97 98 99

XII 100 101 102 103 104 105 106 107 108

KEY TO THE CURING AGENTS AND ORGANIC COATINGS

Curing Agents

A. Untreated (water cured). As with the other panels, cured for 28 days

in a steam curing room but no membrane curing agent applied.

B. Commercial curing agent, based on butadiene-styrene copolymer.

C. Commercial curing agent, based on petroleum hydrocarbon resin.

D. Commercial curing agent, a resin type.

E. Commercial curing agent, a wax-resin type.

F. Butadiene-styrene copolymer formulation prepared at the NBS.

G. Petroleum hydrocarbon resin formulation prepared at the NBS.

H. Chlorinated rubber-chlorinated paraffin formulation prepared at the NBS.

I. Wax and oil mixture prepared at the NBS.

Organic Coatings

I. Cement water type concrete paint.

II. Cement, water concrete paint.

III. Chlorinated rubber in solvent.

IV. Butadiene-styrene copolymer in solvent.

V. Butadiene-styrene and acrylic resin emulsion,..

VI. Butadiene- styrene copolymer emulsion.

VII. Polyvinyl acetate emulsion.

VIII. Alkyd modified vinyl, resin eisuision.

IX. Oil-alkyd modified latex paint.

X. Acrylic resin emulsion.

XI. Alkyd enamel.

XII. Alkyd enamel.

- 3

-

The numerical rating system described in the original test was too

cumbersome and,, since there were no replicates, it would be impossible

to determine the precision of the method

„

3o2 Adhesion of Resilient Flooring to Concrete

3.2.1 Qualitative Tests Using Cement Mortar Panels

A number of qualitative adhesion tests were run on cement mortar panels

4-1/2- x 9-inches x 5/8-inch thick. These panels were made from approximately 2 parts "high early strength" port land cement, 6 parts of concrete

sand, and 1 part of water, by weight. In some cases, additional water

was added to make the mix workable. The object of this part of the

program was to evaluate concrete curing agents for adhesion of floor

coverings and to devise a suitable test for such evaluation.

Water-cured panels were steam cured for 28 days and allowed to dry for

several days before applying floor coverings or gauze. Membrane -cured

panels were prepared by applying the curing agents to the "green" or fresh cement mortar surface with a camel's hair brush and storing in a constant temperature-constant humidity room at 73°F., 507. relative

humidity for 28 days. After curing and drying, the panels were coated

with the desired adhesives, using a notched trowel, as in actual practice^ and the selected floor covering was applied. The majority of

tests were made with vinyl asbestos tile, using either an asphalt cutback or an asphalt emulsion adhesive.

Si&ce tests with floor coverings are slow, an attempt was made to

devise a quicker test, using cotton gauze strips in place of floor

coverings. The open structure of the gauze would permit the adhesive

solvent to evaporate more rapidly. The gauze strip test was based on

an earlier method for testing the adhesion of paint films, reported

on page 176 of Henry A. Gardner and George G. Sward, "Physical and

Chemical Examination of Paints, Varnishes, Lacquers, and Colors",

Henry A. Gardner Laboratory, Bethesda, Maryland, 11 edition, 195G.

In this method, strips of silk cloth were pressed on paint films while

still tacky. After the paint had dried, the strips were pulled away

from the substrate with a portable tensile testing instrument. The

instrument used was similar to the "Gardner Tensile Strength and

Elongation Apparatus", Gardner Laboratory, Inc., Bethesda, Maryland,

Catalog No. TG-1500. It was hoped that this portable instrument might

be used to test adhesion of floor coverings, as in NAVDOCKS Specification

13Yf, In the NBS tests, observations with the cotton gauze strips were qualitative and were intended to be exploratory, with quantitative evaluation as the goal. In the qualitative tests, gauze strips one-inch

wide were applied to the cement mortar panels, using asphalt adhesive.

The adhesive was spread with a putty knife, scraping off the excess, so that as thin a film was applied as consistent with efficient wetting of

the gauze and cement mortar surface.

/

3.2.2 Quantitative Straight-pull Adhesion Tests Using Asphalt Tile and

Cement Mortar Cubes

Both the straight-pull and the stripping-pull tests were adapted from

those described by Percy A. Sigler and Robert I. Martens, Building

Materials and Structures Report BMS 59, "Properties of Adhesives for

Floor Coverings", National Bureau of Standards, 19 September 1940.

Specimens for this series of tests were 2-inch cement mortar cubes,

cast in modified "Bowen Expansible Cube Molds", U. S. Patent 2,061,137,

Bowen and Company, Inc., Bethesda, Maryland. The molds were modified

by drilling holes, 17/64-inch in diameter in a position such that the

three completed cubes from each mold would each have a 1 /4-inch diameter

steel pin through the center of two faces adjacent to the top or troweled

surface under test. The pins were inserted through the drilled holes

before casting the cement mortar cubes. The cubes were cast in accordance

with ASTM C-109 except that concrete sand was used in place of graded

Ottawa sand and the mixer accordingly set with greater clearance. Also,

the cement mortar cubes were not leveled immediately, but were placed in

the curing cabinet for about an hour with the mortar heaped up and then

finished with a steel trowel. This was similar to the procedure in

finishing concrete floors. Cubes to be water cured were placed in a moist cabinet overnight; removed from the molds; then placed under water

in the moist cabinet for 6 more days. The cubes were then placed in a constant temperature-humidity room at 73°F. and 507. relative humidity

for 21 days or more. Cubes which were to be membrane cured were coated

with membrane curing agents immediately after troweling, using a camel's

hair brush. The membrane coating was applied only to the top surfaces

of the cubes, which had been troweled. The cubes were then placed

immediately in polyethylene bags, which were tied and placed with the

tied ends inside other polyethylene bags and the outer bags then tied.

The cubes were allowed to cure in the double polyethylene bags at 73°F,

for at least 28 days.

After curing, the test cubes were coated with asphalt cut-back or emulsion adhesive at 73°F. and 507. relative humidity, air dried under these

conditions for approximately 90 minutes, then 2-inch squares of OTAT

applied. OTAT refers to Official Test Asphalt Tile (for 1963) of the

Chemical Specialties Manufacturers Association (CSMA), 50 East 41st

Street, New York, N.Y. 10017. After laying the asphalt tile, pressure

was applied to the top surface of the tile. In some of the tests, the

tile was bonded at a pressure of approximately 0.2 pounds per square

inch (psi) for one hour. A steel plate was placed on 9 specimens at a time, so that the pressure was about 2 psi. This was adapted from
-
- 5

-

Federal Specifications MMM-A-0Q115 and SS-A-128. In other tests, the

tile was bonded by placing the specimen in a Carver hydraulic laboratory

press, such that the pressure was 625 psi and load applied for 30

seconds. After laying the tile and pressing, the specimens were

stored in the constant temperature-humidity room for the desired period

of time for curing or setting of the adhesive.

After the adhesive had cured for the desired time, 2-inch wooden cubes were cemented to the top surfaces of the tile, using commercial epoxy

cement containing a filler. The wooden cubes were also fitted with

steel pins, 1/4-inch in diameter, so that the completed specimen

appeared as in the following sketch."

In order to secure the specimen to a tensile testing instrument, special

yokes were used. On. yoke was clamped in the upper jaw of the instrument

and engaged the steel pin in the wooden cube. The other yoke was clamped in the lower jaw of the instrument and engaged the steel pin in

the cement mortar cube. One of the yokes is illustrated in the following

sketch

:

WOODEN CUBE' -fr* (

s ! M (

CEMENT MORTAR CUBESTEEL PINS

SIDE VIEW OF SPECIMEN (NOT TO SCALE)

SLOT TO ENGAGE

STEEL PIN IN

CUBE

r

DETAIL, SIDE VIEW OF ONE ARM OF .. GKE

TOP VIEW

(WOT TO SCALE)

The instrument used for the test was an Instron Tensile Testing Instrument,

Model TT-B, standard speed, 1,000 lbs. capacity, crosshead. speed 0.02 - 20 inches per minute, Instron Engineering Corporation, 2500 Washington

Street, Canton, Massachusetts. A crosshead speed of 0.05 inches per

minute was used. To determine the variation with different adhesives,

three asphalt cut -back adhesives of three manufacturer's and three

emulsion adhesives of the same manufacturers were used.

3.2.3 Quantitative Stripping-pull Tests Using Flexible Resilient Tile,

Asphalt Adhesives, and. Cement Mortar Prisms

A number of 90° or stripping-pull tests were performed on water cured

cement mortar prisms in order to compare the stress-sfcrain~"or loadelongation relationship with that from the straight-pull tests. For

this purpose, cement mortar prisms, 1.575- by 1.575- by 6.3-inches, were made from modified prism molds as described in Federal Test

Method Standard 158a, Method 2701.1, Section 2.3. Holes, 17/64-inch

in diameter, were drilled in each mold, centers equidistant, from, the

ends of the side plates and 5/8-inch from the bottom. In casting,

stainless steel pins, 1/4- inch in diameter, were inserted through the

holes to serve as handles. Each finished prism had a steel pin 5/8-inch

from the bottom and equidistant from, each end. The pin. was used to hold

the prism in the stripping-pull test. The cement mortar mix and finishing

and curing procedure were similar to those used for the 2 -inch cement

mortar cubes except for the amount of mix. and filling and tamping

procedure outlined in Method 2701.1, Federal Test Method Standard. No.

158a„ The prisms were all water cured in the same manner as the

2 -inch cement mortar cubes.

After curing for 28 days, pieces of flexible tile, 1/8-inch, gauge,

1-5/8 inches wide, and 9 inches long, were cemented to the top or troweled surfaces of the prisms, using asphalt cut~haek or emulsion

adhesive. Brand A. The flexible tile was supplied by the RubberManufacturers Association and was the same as that used in their

laboratory adhesion tests. An, area of tile at the end. of each specimen,

1-5/8 inches wide and 2-1/2 inches long (4 sq. in.), was pressed in a Carver laboratory hydraulic press at 625 psi for .30 seconds. A line was drawn at the end of the pressed area, .2-1/2 inches from the end of

the piece of tile. Following this line, another area of the same size was pressed in the same manner and a second line drawn, 5 inches from

the end of the piece of tile. The second line was, in each case,

positioned in testing such that it was aligned with the bottom ed.ge of

the upper jaw of the tensile testing instrument.
.
In performing stripping-pull tests,, each specimen was secured in a special

stainless steel holder as shown in the sketch. The vertical plate was clamped in the lower jaw of the Instron tensile testing instrument and

the strip of tile was clamped in the upper jaw of the instrument. Pull

tests were run to constant stress or until the strip was free of the

prism.

4. TEST RESULTS

4.1 Adhesion of Organic Coatings to Concrete (See 3.1)

The results of the tests of adhesion of organic coatings to cement mortar

panels are shown, in the following three photographs. The numbers refer

to those given in Table 1. For example,, all specimens in the first

column of each page are controls not treated with curing agents. The rows represent the same paint applied to panels treated with different

curing agents. In examining the photographs it must be remembered that

the bottom section of each panel was used for tests one day, the middle

section seven days, and the top section thirty days after application of

the paint. Also,, the lower half of each section was used for the thumb

nail and knife tests and the upper half for the adhesive tape test.

Aside from the appearance of the panels, which can be seen in the photographs, it is necessary to make the following observations regarding

the thumb nail test. Examination of the photographs will not distinguish

between the thumb nail and knife blade tests.

Coatings on the following panels were easily removed with the thumb nail

one day after application and also after 7 days and 30 days 2

Nos. 2, 3, 4, 5, 6, 7, 8, 13, 14, 15, 16, 17, 18, 54, 63, 72,

81, 90.

Coatings on the following panels were easily removed after 1 day and 7 day

but not after 30 days;

Nos. 66, 75, 84, 99.

Coatings on the following panels were easily removed after 1 day but not

after 7 or 30 days;

Nos. 76, 80, 103, 108.

Coatings on panels 39 and 45 were not completely removed by scraping with

the thumb nail after one day but could be removed completely with the

thumb nail after 7 days or 30 days. The coating on panel No. 48 could be

partially removed after 1 day or 30 days but was completely removed by

thumb nail after 7 days.

SPECIMEN AND HOLDER







- 8 -

4.2 Adhesion of Resilient Flooring to Concrete

4.2.1 Qualitative Tests (See 3.2.1)

Three photographs which follow show the results of qualitative adhesion

tests on 4-1/2- by 9- by 5/8-inch cement mortar panels. One-inch wide

strips of flooring or cotton gauze were removed after various periods of

time of curing or setting of the adhesive. The photographs show the

cement mortar surfaces after removal of the strips. Table 2 is a description and interpretation of the pictures. Panel numbers in the

table correspond to numbers in the panels in the photographs. The order

of removal of the strips was from top to bottom of each panel at time

intervals indicated in order in the table. Panels omitted from the

table were those tested with cotton gauze. Tests with cotton gauze were inconclusive and were therefore not included in the table. Information concerning the curing agents designated by capital letters in

this table and also later in the report is given in Appendix 3.

4.2.2 Quantitative Straight-pull Tests with Asphalt Tile and Cement

Mortar Cubes (See 3.2.2)

The data from the quantitative straight-pull tests are summarized in

Table 3,, which was prepared with the assistance of Dr. David Hogben

of the Statistical Engineering Section^ using an GMNXTAB computer.

Analysis of variance of the test, results showed no significant differences between brands but possibly a significant difference between

asphalt cut-back and emulsion adhesive (Table 3a)

„

From Table 3b it is apparent that increased bonding pressure causes considerable increase in bond strength of asphalt emulsion adhesive,,

but does not affect asphalt cut-back adhesive. Longer curing time up

to 30 days increases the bond strength of asphalt emulsion adhesive

when bonded at 625 psi^, but not when bonded at only 0.2 psi. Asphalt

cut-back adhesive shows very low bond strength after one day curing;

this is increased considerably after 14 days with little change after

30 days.

According to Table 3c j, all membrane curing agents lessen the adhesion

of asphalt emulsion adhesive^, although curing agent N is not significantly different and M. is only barely significant. Curing agents A^,

B,, C^, D, Ej and F definitely lessen adhesion of asphalt emulsion

adhesive to concrete. In the case of asphalt cut-back adhesive.,

curing agent B actually shows better adhesion. There is no significant

change with curing agents C 9 D,, F_, M, and N. This confirms

previous observations that curing agents are generally compatible with

asphalt cut-back adhesive and not with asphalt emulsion adhesive.







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Table 3. Adhesion of Asphalt Tiles Using Asphalt Adhesives

3a. Comparison

Cut -Back

of

and

Three Brands Each

Emulsion Adhesive

Brand ,

of Asphalt

A Brand B Brand C

Asphalt Cut-back Adhesive

Number of Tests 11 1

1

Average maximum load, pounds 26.7 25.0 29.0

Standard Deviation 21 .82 20.44 17.48

Asphalt Emulsion Adhesive

Number of Tests 11 12 11 Average maximum load, pounds 19.5 19.7 20.1

Standard Deviation 8.51 11.60 8.32

Analysis of variance showed no significant difference between brands

„

3b 0 Comparison of Adhesives, Curing Time of Adhesives,

and Pressures Applied to Tiles After Laying

Pressure Curing Time No. of Average Std. on Tile Adhesive of Adhesive Tests Max . Load Dev.

psi asphalt days lbs

.

625 Emulsion 30 12 163.2 64.51

625 Emulsion 14 12 112.3 53.61

625 Emulsion 1 12 71.8 32.05

625 Cut-back 30 12 65.5 38.47

0.2 Cut-back 14 6 63.8 34.48

0.2 Cut-back 30 12 62.2 33.81

625 Cut-back 14 12 57.8 31.37

0.2 Emulsion 30 12 27.6 11.52

0.2 Emulsion 14 6 14.3 10.01

0.2 Emulsion 1 12 11.2 7.65

625 Cut -back 1 12 7.5 9.67

0.2 Cut-back 1 1 1 4.0 6.47

I

I

NOTE ; There are no significant differences between values opposite the same bar. Values outside a bar are significantly different at. 5% level from values inside the bar.

Table 3. (Cont*d) - 2

3c. Effect of Membrane Curing Agents on Adhesion

of Asphalt Tile to Concrete

No. of Average Standard

Adhesive Treatment Tests Max „ Load Deviatii

asphalt lbs

.

Emulsion Control 12 163.2 64.57

Emulsion N 6 158.0 48.91

Emulsion M 6 78.2 53.81

Cut-back B 9 72.8 25.56

Cut-back Control 12 65.5 38.47

Cut-back C 9 44.9 26.15

Cut-back N 6 42.0 30.56

Cut-back M 6 37.2 27.24

Cut -back D 9 30.8 17.30

Cut-back E 9 30.7 13.74

Cut-back A 9 30.7 17.21

Cut-back F 9 27.2 23.73

Emulsion F 9 21.8 19.46

Emulsion D 9 14.3 14.11

Emu 1. s i on C 9 11.4 16.79

Emulsion E 9 10.3 9.25

Emulsion B 9 9.8 6 . 22

Emulsion A 9 7.9 7.5"!

3d„ Comparison of Rough and Smooth Surfaces of Asphalt Tile

Asphalt Gut -back Adhesive Asphalt Emulsion Adhesive

Surface of tile in contact Surface of tile in contact

with adhesive with adhesive

Smoot h Rough Smooth Rough

Number of Tests

Average maximum

6 5 6 6

load,, pounds 119.0 143.2 183.3 176.3

Standard Deviation 15.06 19.52 28.26 20.58

Analysis of variance showed significant difference at 17. level between asphalt

cut-back and emulsion adhesives but no significant difference between rough and

smooth sides of asphalt tile.

- 9

-

In Table 3d are recorded, results of experiments in which all of the

specimens were subjected to 625 psi for 30 seconds 0 In one set of tests

the smooth sides of the tiles were in contact with the asphalt adhesive

and in the other set of tests, the rough sides of the tiles. Statistical

analysis showed a significant difference between asphalt cut-back and

emulsion adhesives but not between the smooth and rough sides of the

asphalt tile.

4.2 o 3 Quantitative Stripping-pull Tests with Flexible Resilient Tile

and Cement Mortar Prisms (See 3.2.2)

In the stripping-pull tests,, ten. replicates were run at a crosshead

speed of 0.5 inch per minute on specimens in which asphalt cut-back

adhesive was used. Another ten replicates were run at the same crosshead speed with asphalt emulsion adhesive. Eight replicates were performed at a crosshead speed of 2.0 inches per minute on asphalt

cut-back and eight on asphalt emulsion adhesive. All specimens showed

good adhesion from qualitative or visual, inspection. Both tile and

concrete surfaces remained coated with adhesive except for portions

where the concrete surface was removed by pulling away the strip.

This was shown by a whitish or grayish deposit on the underside of

the tile, corresponding to bare portions on the concrete surface.

There was very little difference in maximum load on any of the specimens. The load was about 1-2 pounds in each case ; never zero and never

over 2 -pounds.

5. SUMMARY AND COMMENTS

A number of tests have been performed under this program on adhesion

of organic coatings and resilient flooring to test panels and blocks,

which, were made to simulate actual concrete floors as closely as possible. The panels and. blocks were made of a cement mortar mix and were not concrete in the strict sense of the word. The physical

dimensions of the specimens were too small to permit the addition of

aggregate. However, concrete sand was used and the specimens were

hard troweled, so that the top surfaces should be similar to those

of actual concrete floors.

Our tests have established that most concrete curing agents can be used

safely under asphalt or vinyl asbestos tile where asphalt cut-back

adhesive is used. When an asphalt emulsion adhesive is used, on the

other hand, oily or waxy materials may cause trouble unless an asphalt

primer is used. The Rubber Manufacturers Association, as well as prominent flooring manufacturers, are of the opinion that other types

of resilient flooring, such as flexible vinyl and rubber tile, behave

similarly.

- 10 -

Adhesion of cement-water paints was poor to concrete treated with curing

agents, as these paints require a somewhat porous hydrophilic surface,,

Adhesion of other types of paints was excellent to curing agents formulated with butadiene- styrene type copolymer or chlorinated rubberchlorinated. paraffin type of formulation. Other types of curing agents

varied regarding their compatibility with various paints. In general,

emulsion or latex paints did not adhere well to concrete floors treated

with oily or way materials. Organic solvent based paints were generally

satisfactory when applied over oils and waxes. Paints formulated with

butadiene-styrene copolymer or chlorinated rubber in organic solvents

(such as xylene, mineral spirits or petroleum distillate) appeared to

have the best adherence.

The most practical laboratory bond or adhesion test for resilient flooring is qualitative or visual such as the one recommended by the Armstrong

Cork Company, Quantitative bond tests require expensive equipment, are

slow, and require a relatively large number of replicates. Even with

the most careful quantitative tests, it is doubtful whether any more information can be gained than from a qualitative bond test. The

qualitative test for adhesion of floor coverings reported here is to

apply pieces of floor covering to cement mortar panels which have

been water cured or cured with membrane curing agents. The floor

covering material is cut into strips, using a special tip inserted in an electric soldering gun. The test for adhesion consists in pulling

back a strip of material and observing whether the concrete surface

remains coated with adhesive. Strips are removed at various intervals

of time and then the surface tinder the removed strips is photographed.

More reliable results are obtained with large panels in which nine

9- by 9-inch tiles are applied to a cement mortar panel. This type

of test was described in our Second Progress Report, NBS Report No.

8009, 30 June 1963,

We have attempted to develop a field test for adhesion, but such a test does not appear to be feasible. The only practical field test

is to apply the floor covering or paint at various areas on the

surface to be covered and examine visually. Inasmuch as our investigation has shown that asphalt cut-back adhesive can be used

successfully over roost types of concrete treatment the need for a field test is not very important. Further, if the use of an emulsion

adhesive is desired, an asphalt primer can be used as a base over oily or waxy curing agents to provide good adhesion.

Parting agents are oily materials used to separate slabs in lift-slab

and tilt slab construction. These are similar to the oily type of

curing agents, which are commonly advertised for both curing and

parting. Since there is nothing unique about parting agents, they were not studied extensively. The only widely used parting agent

of which we have any knowledge is code K.

So-called concrete sealers and hardeners are generally similar to the

resin type of curing agents and the same product is generally advertised to be a combination curing agent, sealer, and hardener. An

organic coating may be used as a sealer in the sense that an improperly cured concrete surface is characterized by "“laitance" 1 or dust and the organic coating or sealer will cement this laitance to

the surface until the coating is worn off or tile or paint applied.

Some alkaline ““hardeners"” are used, such as sodium silicate, code M,

which is worthless as a curing agent because it is ineffective as a water barrier.

6 . ACKNOWLEDGMENT

The author wishes to acknowledge the assistance of Dr. David Hogben

in the statistical analysis of the data on straight-pull tests,

using the Instron tensile testing instrument.

- 12

APPENDIX 1 o APPLICABLE TEST METHODS

1.1 Tests for Oily and Waxy Curing Agents on Concrete Floors

We have tried to develop several methods of test to detect the presence

of oily and waxy materials on concrete floors simply and rapidly in the

field. None of these methods were entirely satisfactory. The only one which shows any promise is as follows;

Scrape an area about 3“ by 5-inches with a pen knife and brush

the scrapings into a small beaker or test tube. Add three

medicine droppers full of reagent diethyl ether and swirl to

contact the scrapings and ether. Filter through qualitative

(Whatman No, 1) filter paper in a small funnel onto a carefully

cleaned watch glass about 100 mm, in diameter. Repeat this

procedure with the same amount of ether from the same bottle.

Add six medicine droppers of ether from the same bottle to

another clean watch glass. Allow the ether to evaporate over- night in a place as dust free as possible. Examine the watch

glasses for oily or waxy residue.

This procedure was tried on 3“ by 5 -inch cement mortar panels. Both

panels had been treated with paraffin wax in kerosene mixture. One of

the panels had also been given three coats of paste wax. In both

cases,, a waxy residue was visible on the watch glass,, more in the one from the waxed panel. The watch glass in which ether alone had been

evaporated was fairly clean.

Another simple test was tried on two similar panels, both treated with

paraffin wax and kerosene mixture and one also waxed with paste wax. This consisted in placing a piece of qualitative filter paper on each

panel and pressing with a household iron, set at maximum temperature,

to see whether the oil and wax would change the appearance of the

paper. However, there was no detectable change in appearance.

Other tests which have been tried include measuring contact angles or observing the wettability of concrete surfaces, treated and untreated,

and drilling into cement mortar panels with a masonry drill and ex- tracting with solvent. These methods were unsuccessful.

“ 13

1 .2 Water Retention of Concrete Curing Agents

Although this subject is outside the scope of the project, it cannot

be ignored when we are asked to make recommendations concerning con- crete curing agents,, There are three known tests and requirements

for moisture retention of concrete curing agents,, According to ASTM

C-309, a curing agent should restrict the loss of water to not more

than 0.055 g/ cm^ of surface, when tested according to ASTM C-156.

According to U. S 0 Army Engineers CRD-C 300-59, the unit moisture

loss shall not be more than 0.031 g/ cm^ under conditions set forth

in this specification,, The Concrete Manual of the U„ S. Department

of the Interior, Bureau of Reclamation, Denver, Colorado, does not

specify moisture retention required of concrete curing agents.

However, Mr. G„ E. Burnett, Chief Research Scientist of the Bureau

of Reclamation at Denver, has given NBS some information regarding

their work on moisture retention of concrete curing agents and a copy of their "Specifications for Sealing Compound for Curing

Concrete9 ", dated June 1, 1961. Details of the test method and

moisture retention requirement are given in this specification.

The moisture loss specified is 30 grams per 72 sq„ in. or 0.064 g/cm2.

The Bureau of Reclamation has tested about 40 different commercial

concrete curing agents, none of which passed their moisture retention

requirement. However, chlorinated rubber formulations were close to

the requirement.

- 14 -

APPENDIX 2 o REPORT ON CONCRETE DURING AGENTS FROM

THE RUBBER MANUFACTURERS ASSOCIATION

A comprehensive study of concrete curing agents has been made by the

Technical Committee,, Vinyl and Rubber Flooring Division, Rubber

Manufacturers Association, Inc., 444 Madison Avenue, New York, N. Y„

10022 (RMA) o The basis of the study was NAVDOCKS Specification 13Yf,

Section 2.13.7, previously mentioned in this report. The test method

specified in Specification ]3Yf was used in the RMA laboratory investigations. The Portland Cement Association prepared test concrete blocks

in their laboratory in Skokie, Illinois, and forwarded these blocks to

six manufacturers of vinyl and rubber flooring, who conducted tests

in their own laboratories. Some of the blocks were water cured and some membrane cured. The membrane cured blocks were wrapped in

polyethylene bags during the curing period, as the membrane coating

was applied only to the top surface and excessive moisture would otherwise be lost from relatively small specimens.

In addition, the RMA cooperated with other interests in a field study

in which a new building was used as a test site. The test building

is the Cerebral Palsy Treatment Center in Edison, New Jersey. Of

12,000 square feet of concrete flooring in this building, half was water cured and half was cured with commercial curing agent B„ The

floors were finished and cured during the summer of 1961 . Vinyl and

rubber flooring was installed beginning in September, 1951 and com- pleted during the summer of 1962 . Recent inspection, about two years

after all of the flooring had been installed, showed all of the flooring to be in perfect condition. There has never been any loss of adhesion or any other flooring problem, in the entire installation.

- 15

APPENDIX 3. IDENTIFICATION OF COMMERCIAL PRODUCTS

3*1 Curing Agents, Etc* - Information obtained by analysis

or from manufacturers

B 0 CURING AGENT - Xylol solution containing about 1 8% of butadienestyrene copolymer resin* (Resin similar to

"Pliolite S-5" 11 , product of Goodyear Tire and

Rubber Co 8 )

Co CURING AGENT - Xylol solution containing about 28% of a petroleum

hydrocarbon resin* (Resin similar to "Piccopale

100", product of Pennsylvania Industrial Chemical

Corporation*

)

Do CURING AGENT - Composition unknown*

E 0 CURING AGENT - Composition unknown*

(Materials coded F, G, H, and I were prepared at the

Bureau, but are included here for completeness*)

F* Material Parts by Weight

Butadiene-styrene copolymer resin

(Pliolite S-5, Goodyear)

Xylene, reagent grade

18

82

100

G* Material Parts by Weight

Petroleum hydrocarbon resin (Piccopale 100,

Pennsylvania Industrial Chemical Corp*)

Mineral spirits

30

70

100

H„ Material Parts by Weight

Chlorinated rubber (Parion S-10, Hercules) 12*5

Plasticizer (Arochlor 5460, Monsanto) 10*0

Chlorinated paraffin (Chlorafin 40, Hercules) 2*5

Xylene, reagent grade 75*0

100*0

- 16 -

I. Material Parts by Weight

Paraffin, U.S.P., melting point 52-4°C 17

Kerosene, commercial grade 83

100

Jo CURING AGENT - Composition unknown.

K, CURING AND PARTING AGENT - Kerosene solution containing about

137o paraffin wax.

L„ CURING AGENT - Composition unknown.

M. CURING AGENT - Sodium silicate solution.

N„ 40% solution of sodium silicate prepared at the Bureau.

0. PARTING AGENT - Mixture of heavy oils, mineral filler, and

a small amount* of a medium boiling solvent.

P„ EXPERIMENTAL PARTING AGENT - Mainly heavy oils, somewhat similar

to 0, but without mineral filler,

Q» CURING AGENT - Composition unknown

R. CURING AGENT - Composition unknown.

S. EXPERIMENTAL CURING AGENT - Material

Polyvinyl toluene-butadiene copolymer resin

Paraffin wax Aluminum stearate

Naptha

Parts by Weight

15.0

1 .5

1 .5

82.0

100.0

T. CURING AGENT - Composition unknown

17

3.2 Concrete Paints - Information obtained from label

Io CEMENT WATER TYPE

Material By Weight

Hydraulic calcium silicates and aluminates 70.0%

Calcium hydroxide 25.0%

Sodium chloride 5.0%

Tinting pigments not over 5%; T-V-26-R-3

100.0%

CEMENT WATER TYPE

Material By Weight

Silicon oxide 22.0%

Aluminum oxide 4.0%

Calcium oxide 64.0%

Magnesium oxide 2.0%

Calcium stearate 1.0%

Sodium chloride 4.0%

Calcium sulfate 3.0%

Tinting materials less than 1%

CHLORINATED RUBBER IN SOLVENT

100.0%

Pigment (227. by weight)

Titanium dioxide 100.0%

Vehicle (787. by weight)

Chlorinated rubber 23.0%

Plasticizer 10.0%

Esters 18.0%

Aliphatic, aromatic hydrocarbons 49 . 0%

100 . 0%

IVo BURADIENE- STYRENE COPOLYMER IN SOLVENT

Pigment (48% by weight)

Silicates 58.07.

Titanium dioxide 42 . 0%,

100 . 0%

Vehicle (52% by weight)

Non-volatile

Butadiene-styrene resin 28.07.

Volatile

40.0%

32.0%

Aromatic solvents

Mineral spirits

100 . 0%

- 18 -

V. BUTADIENE “STYRENE AND ACRYLIC RESIN EMULSION

Pigment (23.3% by weight)

Titanium dioxide 90.0%,

Aluminum silicates 10.0%

100 . 0%

Vehicle (76.7% by weight) (blend of butadiene-styrene and

acrylic type copolymers)

Non-volatile (synthetic rubber) 24.7%

Volatile (water) 75,3%,

100 . 0%

VI. BUTADIENE -STYRENE COPOLYMER

Titanium dioxide

Barytes

Silica and silicates

Mineral spirits

Synthetic latex solids

Volatile thinner (water)

EMULSION

By Weight

18.0%

5.0%

8 . 0%

7.0%

22 . 0%

4Q 0 Q%

100 . 0%

VII. POLYVINYL ACETATE EMULSION

Titanium dioxide

Silica

Calcium carbonate

*Polyvinyl acetate emulsion

Water

By Weight

14.60%

7 . 36%

15.40%

29.00%

33.64%

100 . 00%

^Non-volatile (Polyvinyl acetate) 42.0%,

Volatile (water) 58.0%,

100 . 0%

Tinting color less than 5%,

- 19 -

VIII. ALKYD MODIFIED VINYL RESIN EMULSION

Pigment (45.17, by weight)

Titanium dioxide 43.9%

Silicates 56.17.

100 . 0%

Vehicle (54,9% by weight) (*Alkyd modified vinyl resin emulsion)

•^Non-volatile - Soya alkyd modified vinyl resin 20,8%

Volatile (water) 79,27,

100 . 0%

IX. OIL-ALKYD MODIFIED LATEX PAINT

Pigment (377, by weight)

Titanium dioxide 50.0%

Magnesium and aluminum silicates 43.07,

Silica 7.07,

100 . 0%

Vehicle (637, by weight)

(Pentaerythritol-Soya Ester- Resin Latex Emulsion)

Non-Volatile resin 9.57,

Non-Volatile synthetic latex 12.57,

Volatile (water) 78.07,

100 . 0%

X. ACRYLIC RESIN EMULSION

Pigment (32.97, by weight)

Titanium dioxide 70.47,

Silica and silicates 29.67,

100 , 0%

Vehicle (67,17, by weight)

Non-volatile (acrylic resin emulsion) 23.57,

Volatile (water) 76.57,

100 , 0%

- 20 -

XI. ALKYD ENAMEL

Pigment (457. by weight)

Titanium calcium 63.07.

Titanium, dioxide 20.07.

Silicates 17.07.

100.07.

Vehicle (557. by weight)

*Varnish 85.07.

Mineral spirits 15.07.

100.07.

^Non-Volatile (Linseed Maleic Alkyd Resin) 58.07.

Volatile (mineral spirits) 42 . 07. 100.07.

XII. ALKYD ENAMEL

Pigment (27.67. by weight)

Titanium dioxide 53.37.

Calcium carbonate 46.57.

Carbon black 0

.

27.

1 00 c 07. Vehicle (72.47. by weight)

Soya alkyd resin,, Tung oil,, Linseed oil.

Ester gum 52.8%

Mineral spirits and driers 47 . 27. 100.07.

USCOMM-NBS-DC


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