Ichemco Sales MeetingMilano 23-24-25 June 2014

Analytical instruments

and

methods

Main characteristics of an adhesive

� Tack

� Peel

� Shear

TACK

The property of an adhesive that enables it to bond immediately to a surface.

Methods:

PSTC-6 (RBT) ; ASTM D3121 (RBT); ASTM D2979 (PROBE); TLMI (LOOP).

Temperature: 23 ± 2°C

Factors that have an influence on the result:

� Loop Tack LT-1000

� Probe Tack PT-1000

Factors that have an influence on the result:

o Temperature of the test

o Grammage of adhesive

o Speed test

o Type of backing

� Rolling Ball Tack RBT-100

PEEL PA-1000-180

Method: AFERA 5001, ASTM D1000

Speed: 300 mm/min

Angle: 180°

Pressure: 2 kg roll weight for four times

A material's ability to resist forces that

attempt to pull an adhesive apart by

separating flexible surfaces.

Pressure: 2 kg roll weight for four times

Dwell time: within 1 minute

Panel: Steel

Factors that have an influence on the result:

o Temperature of the test

o Grammage of adhesive

o Speed test

o Type of backing

o Dwell time

o Angle

o Pressure

SOLACRIL 758

15.0

20.0

25.0

Peel adhesion

0.0

5.0

10.0

0 5 10 15 20 25 30 35 40 45 50

Peel adhesion

(N/in)

coating weight (g/m2)

peel steel after 24 hrs

peel steel after 20 minutes

peel steel within 1 minute

SOLACRIL 758

20.0

25.0

30.0

Solacril 758

0.0

5.0

10.0

15.0

0 5 10 15 20 25 30 35 40 45 50

coating weight (g/m2)

peel steel after 24 hrs (N/in)

peel HDPE after 24 hrs (N/in)

peel glass after 24 hrs (N/in)

RBT (cm)

SHEARA material's ability to resist forces that

attempt to pull an adhesive apart by

separating flexible surfaces.

Method:

AFERA 5012

Panel: Standard Steel

Test area: 24mm x 24 mm

Weight: 500g or 1000g

Pressure: 2 kg roll weight for four times

� Static shear at 23°C RT-30

• SAFT «Shear Adhesion Failure Temperature»SOSI-8 Integrated SO-8 Oven & HT-8

• Static shear at 70°CFactors that determine the properties:

o Temperature of the test

o Grammage of adhesive

o Weight

o Area

o Pressure

Pressure: 2 kg roll weight for four times

Dwell time: within 1 minute

TECHNICAL SPECIFICATIONS

In our Technical data Sheets and in the Certificate of Analysis, the following

parameters are always shown:

• TOTAL SOLIDS

• VISCOSITY

• pH (for waterborne products)

• MELTING POINT (for solids)

• SOFTENING POINT (for HM)

8

TOTAL SOLIDS

Definition: The total content of suspended and dissolved solids in water/solvent

• Test Method n. 1 Total Solids

• MU: %

• Procedure: A clean tinplate dish is weighed to the nearest mg (W1). 2-3 g of the sample are quickly weighed into the dish and the sample weight recordered to the nearest mg (W2). The content of the dish are spread as evenly as possible over the bottom of the dish by tilting. The dish and its content are then placed in the oven for one hour at 110°C. After the specified time the dish is removed from the oven, allowed to cool in 2-3 minutes, and weighed to the nearest mg (W3). Two determinations shall be carried out and the result reported as the mean of oven, allowed to cool in 2-3 minutes, and weighed to the nearest mg (W3). Two determinations shall be carried out and the result reported as the mean of two, provided the two determinations do not differ more than 2%. Total solids content: (W3-W1)/W2*100 %. If the sample total solids content is less than 5%, 10-15 g must be weighed and the two determinations must not differ more than 0,03%.

• Instruments: Analitic balance with 1mg accurancy. Oven, thermostatically controlled at 110°C. Flat bottomed tinplate dish 75 mm diameter and 10 mm deep.

• Recordings: Report the Total solids content value in % with the sample identifying data.

• References: ASTM D 1644 9

BROOKFIELD VISCOSITY

Definition: It is the measure of fluid friction which can be considered as the

internal friction resulting when a layer of fluid is made to move in relationship to

another layer. Viscosity is a measure of the ratio of shearing stress to rate of shear.

• Test Method n. 3 Brookfield Viscosity 25°C

• MU: mPa.s

• Procedure: Obtain a 500 ml representative specimen of the liquid, bring to a constant temperature

of 23± 2°C. Avoid the collection or formation of foam and skin. Depending on the expected

viscosity range, attach an appropriate spindle to the viscometer. Insert the spindle into the

specimen in the center of the container to the immersion mark and avoid entrapping air. Insert the

thermometer probe into the specimen. Level the viscometer, start the motor, and observe the thermometer probe into the specimen. Level the viscometer, start the motor, and observe the

display. Allow the viscometer to operate for at least 30 s after the display comes to a constant

value. Report viscosity and temperature values. Remove and clean carefully the spindle used.

Instruments: Brookfield Viscometer Mod. RDV-

II+ for medium and high viscosities, or LVDVI+

for low viscosity (<100 cps). Beakers 600 ml.

References: TAPPI T 666, ASTM D 1417, ASTM

D 2196, CEN TC193 N 224

10

pH

Definition: Measure of the acidity or alkalinity level of a solution.

• pH > 7 alkaline solution

• pH < 7 acidic solution

• pH = 7 neutral solution

• Test Method n. 8 pH

• Procedure: From the set of standard buffer solutions, take the one closest to the expected pH value of the test sample, bring it to the closest to the expected pH value of the test sample, bring it to the standard temperature (20-25°C), and set the pH meter to the exact pH value. Wash the glass electrode in the deionized water and dry it with filter paper. Place the electrode in the sample and measure the pH value. Remove the electrode, wash it carefully with deionized water and place it into the preserver solution.

• Instruments: Glass electrode pH meter. Set of standard buffer solutions of known pH. Thermometer, graduated to 0,1°C. Glass beakers.

• References: CEN EN WG1/56, ASTM E70

MELTING POINT

• Definition: The temperature at which a solid becomes a liquid at a fixed

pressure, usually standard pressure.

For polymers, there is not an exact melting temperature, but a

melting range.

Test Method n. 5. Melting Range

• MU: °C

• Procedure: Take the sample used for the determination of residual • Procedure: Take the sample used for the determination of residual

humidity, crush about 1 g of material in a mortar to grain size of about

0,1 mm. Then fill the substance into the capillary tube to about 5-10 mm

by taking up the sample with tube and filling it up to the prescribed level

by knocking (or dropping in a glass tube) the sealed end on a solid base.

Introduce the filled capillary tube into the melting point apparatus and

set the heating up at a rate of 6 °C/min. The change from solid to liquid

state is visually observed and the melting start and end is noted.

• Instruments: Melting point apparatus. Glass capillary tubes. Agate

mortar and glass tube.

SOFTENING POINT

Definition: the temperature or range of temperatures at which a substance

softens without becoming liquid

Test method n. 4. Softening Point, Ring & Ball

• MU: °C

• Procedure: Put the rings on a siliconed paper sheet and pour the melt

product into each ring, trying to avoid air bubbles . Let the product cool

and became solid, levelling the surface with a blade, then let at room

temperature for 30 minutes. Put the rings on the structure and the temperature for 30 minutes. Put the rings on the structure and the

structure into the glycerol bath. The rings must be at 5 cm below the

glycerol level Insert the thermometer in the bath, start stirring (speed

500 rpm) and heating. At 30 °C put the steel spheres in the middle of the

rings and wait for some minutes (spheres conditioning). Then start

heating (temperature gradient = 5 °C/min, check with a cronometer).

Read the temperature when the spheres reach the bottom of the

structure.

• Instruments: Brass rings and structure for R&B measurement, 600cc

becker filled with glycerol, Stirrer, Siliconed paper, blade

• References: ASTM D36