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Posterior Composites - American Dental Association

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ADA Professional Product Review 1<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Scope<br />

ADA Professional Product Review<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

This protocol for the laboratory testing of posterior composites was developed to provide clinically<br />

relevant laboratory information that will be used as part of a report on posterior composites in the<br />

July 2006 issue of the ADA Professional Product Review. When surveyed, the ADA Clinical<br />

Evaluators (ACE) panel identified wear and shrinkage as important features to be evaluated in the<br />

laboratory. Also, strength, shade/color stability, polishability, and depth of cure were indicated<br />

multiple times as areas of interest. The tests described in this protocol should provide the dental<br />

practitioner with appropriate comparative scientific information to assist in the purchase of<br />

posterior composites.<br />

General Information<br />

All tests were performed with the A3 enamel shade.<br />

Tests in This Protocol<br />

A. Depth of Cure<br />

B. Flexural Strength and Flexural Modulus<br />

C. Water Sorption and Solubility<br />

D. Shade Matching and Color Stability After Water Sorption<br />

E. Radiopacity<br />

F. Polishability<br />

G. Shrinkage<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 2<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Depth of Cure<br />

Identifies the depth of cure achieved according to the manufacturer’s recommended curing time<br />

and offers guidance on the maximum increment-thickness that can be cured under similar<br />

conditions. Darker shades, lower light intensity, and increased distance between the light tip and<br />

the composite will decrease the maximum depth of cure.<br />

Sampling: The test sample shall consist of packages prepared for retail sale from the same<br />

batch and containing enough material to carry out the specified tests, plus an<br />

allowance for repeat tests, if necessary (50 g should be sufficient).<br />

Materials: Stainless steel mold for the preparation of test specimens. Mold should be<br />

6 mm long × 4 mm in diameter, unless the manufacturer claims a depth of cure in<br />

excess of 3 mm; in this event, the mold shall be at least 2 mm longer than twice the<br />

claimed depth of cure.<br />

Two glass slides/plates, each of sufficient area to cover one side of the mold<br />

(standard glass microscope slides may be used)<br />

White filter paper<br />

Film, transparent to the activating radiation, e.g., polyester, 50 ±30 μm thick<br />

External energy source (note that the light intensity should be measured according to<br />

ISO 10650, 3 and the intensity should be above 300 mW/cm 2 ). Include a mylar strip<br />

between the light and the filters while recording the light intensity.<br />

Micrometer accurate to 0.01 mm<br />

Plastic spatula<br />

Procedure: See 7.10 of ANSI/ADA Spec 27 1 or 7.10 of ISO 4049 2<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 3<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Flexural Strength and Flexural Modulus<br />

Represents the composite’s ability to initially withstand occlusal stress and flex under load, but<br />

does not predict resistance to wear or fatigue.<br />

Sampling: The test sample shall consist of packages prepared for retail sale from the same<br />

batch and containing enough material to carry out the specified tests, plus an<br />

allowance for repeat tests, if necessary (50 g should be sufficient).<br />

Materials: Stainless steel mold for the preparation of test specimens. Mold should be<br />

25 ±2 mm × 2 ±0.1 mm × 2 ±0.1 mm (see Figure 7 of ANSI/ADA Spec 271 or ISO<br />

4049 2 ).<br />

One metal plate of sufficient area to cover one side of the mold<br />

Glass microscope slide for use during polymerization<br />

Small clamp<br />

Film, transparent to the activating radiation, e.g. polyester, 50 ±30 μm thick<br />

White filter paper<br />

Water bath capable of being maintained at 37 ±1ºC<br />

External energy source (Note: the light intensity should be measured according to<br />

ISO 10650, 3 and the intensity should be above 300 mW/cm 2 ). Include a mylar strip<br />

between the light and the filters while recording the light intensity.<br />

Micrometer accurate to 0.01 mm<br />

Mechanical test machine appropriately calibrated to provide a constant crosshead<br />

speed of 0.75 ±0.25 mm/min or a rate of loading of 50 ±16 N/min<br />

Flexural strength test apparatus, the apparatus consists essentially of two rods (2 mm<br />

in diameter), mounted parallel with 20 mm between centers, and a third rod (2 mm<br />

in diameter) centered between, and parallel to, the other two, so that the three rods in<br />

combination can be used to give a three-point loading to the specimen.<br />

Procedure: See 7.11 of ANSI/ADA Spec 27 1 or 7.11 of ISO 4049 2<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 4<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Water Sorption and Solubility<br />

Indicates the amount of shrinkage for one hour after polymerization and the rate of stress<br />

development the adhesive would be subjected to during this time. Theoretically, a lower maximum<br />

shrinkage stress and a slower rate of stress development would be advantageous to maintain<br />

marginal integrity, prevent microleakage, and may limit post-operative sensitivity.<br />

Sampling: The test sample shall consist of packages prepared for retail sale from the same<br />

batch and containing enough material to carry out the specified tests, plus an<br />

allowance for repeat tests, if necessary (50 g should be sufficient).<br />

Materials: Mold of internal dimensions 15 ±0.1 mm in diameter and 1.0 ±0.1 mm deep, for the<br />

preparation of specimen discs. A split ring or “washer” mold is suitable. To aid<br />

release of the specimen from the mold, the inner surface of the ring can be lubricated<br />

with a 3% solution of polyvinyl ether wax in hexane.<br />

Film transparent to the activating radiation, e.g., polyester, 50 ±30 μm thick<br />

Two metal plates, each of sufficient area to cover one side of the mold<br />

Two dessicators containing silica gel freshly dried for 5 h at 130ºC. Replace the<br />

silica gel with freshly dried gel after each weighing sequence.<br />

External energy source (note that the light intensity should be measured according to<br />

ISO 10650, 3 and the intensity should be above 300 mW/cm 2 ). Include a mylar strip<br />

between the light and the filters while recording the light intensity.<br />

Oven capable of being maintained at 37 ±1ºC<br />

Analytical balance accurate to 0.05 mg. IMPORTANT: unless specified, weight<br />

measurements should be made at room temperature 23 ±1ºC and humidity 50 ±5%.<br />

Micrometer accurate to 0.01 mm<br />

Plastic tweezers. To avoid contamination of the specimens, they should be handled<br />

at all times with the tweezers.<br />

Hand dust blower or source of oil-free compressed air with micro-jet nozzle<br />

Procedure: See 7.12 of ANSI/ADA Spec 27 1 or 7.12 of ISO 4049 2<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 5<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Shade Matching and Color Stability After Water Sorption<br />

Shade matching verifies the color match between the cured composite and the manufacturer’s<br />

recommended shade guide fore that product. Color stability is a screening test that checks whether<br />

the color of the material initially will remain stable in a moist environment. .<br />

Sampling: The test sample shall consist of packages prepared for retail sale from the same<br />

batch and containing enough material to carry out the specified tests, plus an<br />

allowance for repeat tests, if necessary (50 g should be sufficient).<br />

Materials: Same as for WATER SORPTION AND SOLUBILITY test above.<br />

Procedure: See 7.13 of ANSI/ADA Spec 27 1 or 7.13 of ISO 4049 2<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 6<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Radiopacity<br />

Shows how identifiable the composite will be on a radiograph<br />

Sampling: The test sample shall consist of packages prepared for retail sale from the same<br />

batch and containing enough material to carry out the specified tests, plus an<br />

allowance for repeat tests, if necessary (50 g should be sufficient).<br />

Materials: Same as in the WATER SORPTION AND SOLUBILITY test plus the following:<br />

Single-phase dental x-ray unit with a total filtration of 1.5 mm aluminum and<br />

capable of operation at 65 ±5 kV, with suitable accessories<br />

<strong>Dental</strong> x-ray film of speed group D, developing solution and fixer<br />

Aluminum step wedge, purity at least 98% (mass fraction) with less than 0.1%<br />

(mass fraction) copper and less than 1.0% (mass fraction) iron present, 50 mm long<br />

× 20 mm wide, having a thickness range from 0.5 mm to 5.0 mm in equally spaced<br />

steps of 0.5 ±0.01 mm. The wedge should be free-standing.<br />

Sheet of lead not less than 2 mm thick<br />

Photographic densitometer capable of measuring in the range of 0.5 to 2.5 optical<br />

density<br />

Micrometer accurate to 0.01 mm<br />

Procedure: See 7.14 of ANSI/ADA Spec 27 1 or 7.14 of ISO 4049 2<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 7<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Polishability<br />

Demonstrates the ability to attain maximum surface gloss with a polishing system<br />

Sampling: The test sample shall consist of packages prepared for retail sale from the same<br />

batch and containing enough material to carry out the specified tests, plus an<br />

allowance for repeat tests, if necessary (50 g should be sufficient).<br />

Materials: Stainless steel mold for the preparation of test specimens. Mold should be<br />

25 ±2 mm × 2 ±0.1 mm × 2 ±0.1 mm (see Figure 7 of ANSI/ADA Spec 27 1 or ISO<br />

4049 2 )<br />

One metal plate of sufficient area to cover one side of the mold<br />

Glass microscope slide for use during polymerization<br />

Small clamp<br />

Film, transparent to the activating radiation, e.g. polyester, 50 ±30 μm thick<br />

White filter paper<br />

Water bath capable of being maintained at 37 ±1ºC<br />

External energy source (note that the light intensity should be measured according to<br />

ISO 10650, 3 and the intensity should be above 300 mW/cm 2 ). Include a mylar strip<br />

between the light and the filters while recording the light intensity.<br />

Micrometer accurate to 0.01 mm<br />

Sectioning saw with diamond blade (IsoMet saw, Buehler Ltd.)<br />

Profilometer (Surtronic 3+, Taylor Hobson Ltd.)<br />

Polishing discs (Sof-Lex 3M ESPE), medium, fine, and super fine<br />

Procedure: 1. Cover the metal plate with the filter paper, followed by the polyester film, and<br />

position the mold on it.<br />

2. Prepare the material in accordance with the manufacturer’s instructions and fill<br />

the mold with the material.<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 8<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Polishability, cont’d.<br />

3. Place a second piece of polyester film onto the material in the mold and cover this<br />

with the glass microscope slide.<br />

4. Place the exit window of the external energy source at the center of the specimen<br />

and against the glass plate.<br />

5. Irradiate that section of the specimen for the recommended exposure time.<br />

6. Move the exit window to the section next to the center, overlapping the previous<br />

section by half the diameter of the exit window, and irradiate for the appropriate<br />

time. Then irradiate the section on the other side of the center in the same way.<br />

Continue this procedure until the entire length of the specimen has been irradiated<br />

for the recommended exposure time.<br />

7. Turn the mold over and repeat the irradiation procedure on the other side of the<br />

specimen.<br />

8. Use the sectioning saw with the diamond blade to cut the 25 mm × 2 mm × 2mm<br />

rectangular specimens into thirds, resulting in three 8 mm × 2 mm × 2mm<br />

rectangular specimens. A total of six 8 mm × 2 mm × 2mm rectangular specimens<br />

are required for each product.<br />

9. For each specimen, designate one of the rectangular, 8 mm × 2 mm surfaces to be<br />

the top. Then, using a profilometry system, analyze the top of each specimen and<br />

record its baseline surface roughness (Ra) and the baseline maximum roughness<br />

(Rz).<br />

10. For each specimen, polish the side of the specimen that is analyzed by the<br />

profilometry system (the top side). The polishing procedure shall simulate<br />

clinical conditions by using a series of medium, fine and super fine polishing<br />

discs. Polish each specimen for 30 sec with medium, 30 sec with fine, and<br />

15 sec with super fine polishing discs.<br />

11. Using a profilometry system, analyze the polished surface of each specimen<br />

three times and record the surface roughness (Ra) and the maximum roughness<br />

(Rz) of the polished surface.<br />

12. Repeat for all six specimens.<br />

13. For each product, report the average surface roughness (Ra) and the average<br />

maximum roughness (Rz) of the polished surfaces, along with their standard<br />

deviations.<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>


ADA Professional Product Review 9<br />

<strong>Posterior</strong> <strong>Composites</strong>: Laboratory Testing Methods<br />

Volume 1: Issue 1 Summer 2006 (Online)<br />

www.ada.org/goto/ppr<br />

Shrinkage<br />

(see Shrinkage Testing Method PDF)<br />

References<br />

1. <strong>American</strong> National Standard/<strong>American</strong> <strong>Dental</strong> <strong>Association</strong> Specification No. 27—2005, Resinbased<br />

Filling Materials. Chicago: <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>.<br />

www.ada.org/prof/resources/positions/standards/denmat.asp#ansi<br />

2. International Organization for Standardization. ISO No. 4049:2000, Dentistry—Polymer-Based<br />

Filling, Restorative and Luting Materials. Geneva: ISO. www.iso.org<br />

3. International Organization for Standardization. ISO No. 10650-1:2004, Dentistry—Powered<br />

Polymerization Activators—Part 1: Quartz Tungsten Halogen Lamps. Geneva: ISO.<br />

www.iso.org<br />

4. ASTM International. ASTM E399-90 (1997) Standard Test Method for Plane-Strain Fracture<br />

Toughness of Metallic Materials. West Conshocken, PA: ASTM International. www.astm.org<br />

Document posted 2006<br />

© 2006 <strong>American</strong> <strong>Dental</strong> <strong>Association</strong>

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