125 Pelret Industrial Parkway
Berea, OH 44017
Phone: (440) 973-4909
Fax: (440) 973-4913
 

Deviation Disclosure

 

CRGI was accredited by L-A-B to perform the test methods listed below according to ISO 17025.  For all projects, CRGI will utilize these ASTM or CRGI test methods as described below.  Any deviation from the ASTM method and further information for each method is listed in the table.  NOTE-a client can specifically ask CRGI for a deviation in a test method; this will need to be done on the Sample submission form or request.

 

NOTE: Average ambient temperature of laboratory: 68-73°F/20-60% RH.  More stringent temperature control is available upon request via an environmental test chamber.  Coatings may be applied as indicated in test method or as specified, or over substrate as indicated or as specified. CRGI reserves the right to include only data CRGI deems relevant. 

 

 CRGI ISO Certified Test Methods

Test Method

Methods Used

Deviations/Notes

pH of Aqueous Solutions

 

ASTM E 70

Glass bulb electrodes used.  Commercial NIST traceable buffer standards are used in calibration.  Typically calibrated with pH 7 & 10 buffer solutions (pH 4 available for acidic products).  New plastic cups are used as sample cups for each calibration and are not washed out prior to use.  The sample cups are filled only once per calibration with the buffer.  Paint is measured in original containers.  Standardized daily, when used to ±0.06.  If solution is not within tolerance the instrument is recalibrated.  Samples are measured once.

Cone/Plate Viscosity (ICI)

 

ASTM D 4287

CRGI TM 23

 

 Calibrated with 2 oils, Instrument is checked by running highest viscosity oil until stabilized (30 sec).  Paint evaluated at 25°C ± 0.2 Poise. Typically, one measurement made for each sample.  CRGI uses one to two drops for sample amount.  Instrument calibrated every three months. 

Stormer Viscosity

 

ASTM D 562

Method B

Digital KU Viscometer with a range of 54-140 KU. Calibrated with 2 oils every three months.  Oils are typically ~20KU units apart.  Typically measured in pint or quart container at; half-pint cans can be used for oven stability or freeze-thaw.  Do not use “hold” button.  Measurements taken at 77º (±1°F) unless otherwise noted in test report.  Report KU units only.

Volatile and Non-Volatile by Weight

ASTM D 2369

CRGI TM 41

Test evaluated in, forced air oven at 110±5°C for 60 minutes.  Sample size typically between 0.4-0.9 grams. Pans are not preconditioned in an oven or stored in a desiccator. Paint applied directly to aluminum pan using a pipette in place of a syringe.  Pan not placed in desiccators to cool after taking out of oven.  CRGI spreads the paint thinly with a paperclip or tip of pipette.  Duplicate samples are done. Oven calibrated annually.

VOC

 

ASTM D 3960

EPA Method 24

 

Calculation of VOC using section 10.2: % Water- (ASTM D 4017),% NVW (ASTM D 2369) and density (ASTM D 1475). Note: method is not precise for waterborne coatings under 50 g/l.  Due to the known errors in EPA Method 24 it is possible to calculate negative VOC values.  No product should be assumed to be zero VOC or have a negative VOC regardless of test data results.

Density

 

ASTM D 1475

Metal weight-per-gallon cup (for liquids). Calibrated with DI water.  Cups are made in such a way that the measurement is done by back-weighing a sample and using a correction factor (divide by 10).  Measurement done at room temperature. Calibrated annually with DI water.   Only one determination done.  Chemist is not required to use an analytical scale, however the scale should read to two decimal places.

Application by Brush

 

ASTM D 4958

CRGI TM 64

Rate foam, and hide. (other properties will be rated as requested) 5=excellent, 1=Poor.  Typically applied at room temp over S-W calendar paper or drywall.  Brush may be less than 2” and application time is usually longer than 30 sec. The same chemist will evaluate all paints in a series the same way to minimize subjectivity.  Ratings 1 to 10 (10=excellent, 1=poor)

Percent Water in Paints Materials by Karl

Fischer Method

 

ASTM D 4017

 

Mettler DL-38 Karl Fischer (Composite 5 titrant and (40%) Chloroform/ (60%) Methanol

solvent) with 5 mL burette. Latex products evaluated using solvent

extraction (methanol, diethylene glycol mono-n-butyl ether, or other

suitable solvent). CRGI uses stirring of solvent/paint blend with a spatula

(not a sonic bath). Solvent/paint blend evaluated according to section 8 in

TM (also see Appendix X1). Calibrate instrument when used with DI water to ±1%. 1% commercial water standard traceable to NIST is used to qualify new reagents or as a secondary calibration source.  Karl Fisher apparatus is rinsed with Methanol.  A pipette may be used in place of a syringe to introduce sample into test chamber. For paints with water above 1%, the sample size typically is 0.0050 g- 0.0600 g (about 1 drop). For materials with less than 1% water, sample size Is typically above 0.1 g.

Blocking Resistance of Paints

ASTM D 4946
CRGI TM 81

 

Use 4-mil Bird bar. Panel cured at ambient conditions.  Panels may be tested after any amount of dry time, but are typically tested after 24 hr. dry and/or 7-day dry. Panels can be placed on a glass plate, aluminum tray or wood board.  After removal from oven, cooled at ambient a minimum of 5 minutes before pulling apart.  A maximum of 3 samples can be placed under one stopper/weight.  Samples evaluated in duplicate or triplicate.  Instead of placing panels in an oven they may also be tested at room temperature, where the weight is left on panel overnight.

Water Vapor Transmission (perms)

 

ASTM D 1653

Method A-Dry Cup

CRGI TM 66

 

Free films tested via permeability cups. Films are applied over Leneta Release paper and dried for 7-days at ambient temperature prior to testing.  Films are not removed from substrate to allow previously unexposed surface to dry additional 7 days.  All films are inspected for pinholes prior to testing and measured with a micrometer. Anhydrous calcium chloride desiccant is used. It is not dried at 400°F before use, but is discarded at completion of test.  For a sealant, CRGI uses high-vacuum grease and polypropylene gaskets. Cups are weighed every 24 hours until weight change stabilizes (usually one week).  Use the stabilized weight loss for calculations. A minimum of 2 cups are used per sample, but typically

CRGI uses 3 cups. CRGI does not graph results but takes an average of results when the weight change is consistent.  Results [Perms] are reported in grains per ft2 per hr per inch of Hg. Only ASTM D 1653 Method A is included on the scope.  Tested at  50% ± 5% RH and 73°F±3.4° (22.2-23.3º C±2°C).

Sag Resistance of Paints

 

ASTM D 4400

 

Leneta Anti-Sag Medium bar used (4-24 mil). Tested at ambient

Temperature using a pipette or spatula to place paint on Leneta sag chart. A

white chart may be used for tinted paint samples. Paint mixed prior to application (stirred with spatula or on shaker-no syringe used). No straightedge is used; CRGI uses an automatic film applicator. Report whole number of stripe that does not sag more than half into the next stripe, not fractions.  

Pencil Hardness

 

ASTM D 3363

CRGI TM 60

Films cured for 1 week or specified time at ambient conditions. Films also tested at ambient conditions.  Typically, paint applied with 4 mil Dow bar over glass plate; aluminum Q-Panel also can be used.  CRGI uses Prismacolor Turquoise Mechanical Pencils unless otherwise specified.  Chemist must use same type of pencils for all testing in one project.  Tested using chemist hand (not holder). The same chemist will evaluate all paints in a series to minimize subjectivity.  Due to the soft nature of latex films, CRGI starts with the softest pencil.   The number reported is the hardest pencil that won’t scratch through the film.

 

Tape Test Adhesion

 

ASTM D 3359

Method B

Dry films ~2 mils have 1 mm parallel cuts; 2-5 mils have 2 mm parallel

Cuts. Cut with cutting tool and cutting guide.  Intertape 51596 or equivalent tape is used (pulled directly from roll) and pressed into place with an eraser, knife handle or finger. Rate using ASTM 0B to 5B scale or by % coating removed. CRGI performs method on all types of substrates including metal, plastics, woods and cements.  Typically tested after 7-day air dry. The same chemist will evaluate all paints in a series on the same substrate to minimize subjectivity.

Practical Washability

 

ASTM D 4828

CRGI TM 79

Panels usually applied using 7 mil Dow bar.  Panels cured for 1 week at ambient temperature. Tap water is used. Rated only for stain removal: 10=stain removed, 0=unchanged. Stains applied to panel by hand, using cotton swab, pipette or drawdown cube. Pencil/crayon/lipstick applied by same applicator by hand using same pressure for all panels.  Before placing onto washability machine panel is rinsed lightly with water to remove excess stain. Use section 8.7-mechanical method (ASTM D 4828) and rate after the completion of 100 cycles unless otherwise noted.  Formula 409 or simple green is used as the cleaner.  The amount of cleaner used is determined by multiplying the number of stains by 2mL; this amount is poured over the stained area. Any scrub machine in service is considered equivalent and may be used.  Machine number will not be recorded unless requested.

Chemical & Household Stain Resistance

 

ASTM D 1308  

(Section 7.2-Spot Test

Covered)

CRGI TM 58

Panels cured for 1 week or specified time at ambient conditions. Substrate can be black plastic chart, glass plate, metal panels or cement blocks. Rate for severity (5=no effect, 1=severe effect) and type of defect (ex: blistering, discoloration, softening, wrinkling, removal of film and yellowing). Place 2-3 drops of the selected chemical on panel and cover with watch glass.  Apply non-liquid stains with a cotton swab and cover. Typically evaluated after 1 hour of exposure and after overnight recovery. Choice of chemical determined by ultimate coating use or as specified.

Scrub Resistance

 

ASTM D 2486

Method A

 

Panels cured for 1 week at ambient conditions.  Use abrasive scrub

medium which can be made by CRGI using the formula in ASTM D 2486. or purchased from Leneta.  Gasket frame and rubber mat is typically not used.  Use 7cc of scrub medium/5 cc of water every 500 cycles. (Note 7cc scrub medium is equivalent to the 10 g scrub medium specified in test method) CRGI typically uses duplicate plastic shims on the same panel.  One test panel is run unless otherwise requested.  Brushes are conditioned when new for 400 cycles.  Any scrub machine in service is considered equivalent and may be used.  Machine number will not be recorded unless requested.

Fineness of Dispersion

 

ASTM D 1210

 

Tapered Gage. Typically measured on Hegman scale (0-8).  The Hegman reading is defined as the point where particles begin to appear on the wet film.  Ensure paint/grind paste is mixed prior to testing.  One reading evaluated.  The lighting used to read the gage is overhead fluorescent lighting in the lab.  Gage is cleaned with water for water-based paints or acetone for solvent-based paints.

Impact Resistance

 

ASTM D 6905

CRGI TM 77

 

Panels cured for 1 week at ambient conditions.  One panel is typically used for testing each coating. Coatings typically applied to steel Q-Panels. Indent the face of panel (impact) and/or back side of panel (elongation).  Test 2 spots on 1 panel.

Drying, Curing or Film Formation of Coatings at

Room Temperature

ASTM D 1640

(Sections 7.2, 7.6 and

7.7)

Substrate used will be a sealed chart and application method will be a 4 mil wet drawdown unless otherwise specified. Temperature/humidity is at ambient. Film thickness may not be measured.

Drying, Curing or Film Formation of Coatings using a dry time recorder

ASTM D 5895

Coatings will be drawn down using a 4 mil bird bar or otherwise specified and coating film thickness will not be measured.  Drawdown will be automatic unless otherwise specified.  Coatings are dried at ambient temperature and humidity unless otherwise specified.  The temperature and humidity will be recorded on the original data.  Finished panels will be evaluated under laboratory lighting or as specified.  Tests will be run in duplicate unless a different number of trials is requested.  The cycle used will be the shortest one that gives the requested results unless otherwise specified.  If the requested dry time stage is reached the test may be stopped prematurely.  The cycle used will be recorded.

Test Method A-straight line recorder: The coating is drawn down over a 10 inch sealed chart (larger charts may be cut to 10 inches.  The time of the application is not recorded.  A marker will be used to mark the beginning of the test.  The dry time cycle used will be the shortest to give the results requested or as specified.  The cycle time used will be recorded. 

Test Method B-cyclic recorder:  A white sealed chart or other specified substrate will be used with a minimum area of 6x6.  Time of application is not recorded.  A marker may be used to mark the beginning of test, but it is not required

Mandrel Bend

 

ASTM D 522a

Method B

 

Test specimens applied over aluminum Q-panels.  CRGI’s apparatus measures ½”, ¼”, 1/8”.

Measured pass/fail.  One sample may be used.

Low Temperature Coalescence

CRGI TM 50

CRGI runs 40°F/40% RH-any other temperature will be noted. Panels applied using 4 mil Bird bar.

Leveling of a Coating-Leneta Bar

 

ASTM D 4062

 

Evaluated and applied at ambient conditions. Paint applied to panel using a pipette or spatula, not a syringe   Paints applied without a straightedge. Rated using Leneta Leveling Standards under ambient lighting conditions in the lab at 90° and 30º.  The same chemist will evaluate all paints in a series to minimize subjectivity.

CRGI Odor Test

 

CRGI TM 78

 

Higher VOC paints above 100 g/l would typically have an odor of 0-6 (0=severe odor, 6=some odor).   At least 3 individuals need to participate in a test in order for it to be valid.   A control paint may or may not be used.

Burnish Resistance

 

ASTM D 6736

 

Panels are cured at ambient conditions. CRGI does not use a gasket on the scrub machine, panels are clamped down. We typically measure either in center or on one side of panel.  Any scrub machine in service is considered equivalent and may be used.  Machine number will not be recorded unless requested.

Application and Evaluation of Brush and Roller

Applied Paint Films

 

ASTM D 7073

 

Applied at ambient conditions over primed drywall (min 1’ x 2’) or gray single striped paper at a natural spread rate unless specific spread rate is specified. Use 9” roller for application unless otherwise specified; brush is typically 1½”-2”. Two coats may be applied (depending on the test requirements).  The final coat can be touched up by roller or brush.  The same chemist will evaluate all paints in a series to minimize subjectivity. Primer can be tinted gray or black to test hide of the topcoat.  Rate 10=excellent, 1=poor

Color

 

ASTM D 2244

E 805

CRGI TM 51

CIE Lab D65/10°, specular included. Calibrated daily/when used.  At least 2 spots are checked, and X-Y-Z data or L*a*b* data is obtained. Location where readings made is not recorded. 

Specular Gloss

(20°, 60°, 85°)

ASTM D 523

 

Instrument standardized prior to use. Note, the precision of this method can be affected by the smoothness of the substrate. CRGI typically evaluates a drawdown using a 4 mil bird bar dried overnight.

Contrast Ratio (Hiding Power)

ASTM D 2805 (sect 3.2.1.1)

CRGI TM 27

2.5/4 wet mil bird bar applied to black and white sealed chart using pipette or spatula. Applied/cured at ambient conditions.  One chart used for each coating tested unless a specific comparison study requires side by side drawdowns.   

 

Package Stability of Paints

 

ASTM D 1849

CRGI TM 24

 

Chemist uses their own spatula that has not been weighed or measured. Record viscosity, pH and prepare a draw down.   Unless otherwise noted, 4 weeks at 120±5 °F. Rate for syneresis, settling, viscosity, color and pH compared to initial observations. Typically material is evaluated by pouring into ½ pint containers, not in duplicate and without a room temperature control.  Weight loss is not calculated for coating being tested, paint is not stirred a certain number of times (stirred until a uniform consistency is reached).  Paint is only applied if there is settling or grit formation suspected, paint is applied using a 4 mil Bird bar.  Comments on skinning, grit and coagulation are given instead of rating those properties.  Syneresis, ICI, KU and pH can be measured after paint has been in the oven.

UV Exposure

 

ASTM D 4587

 

Condensation and/or UV cycles. Panels cured for 1 week ambient prior to

Exposure unless otherwise specified.  Evaluate panels for tint and gloss

retention and film defects (e.g. blistering). Typically, QUV (UV-A bulbs)

set for 4 hours UV at 340 nm/60°C and 4 hours condensation/50°C [Cycle 2]. However, CRGI can change to UV-B bulbs or change upon request. CRGI evaluates single samples per QUV side unless duplicates are requested.  Specimen holders are rotated every 200 hours, specimens are not rotated.  Film thickness is not always measured.  Unexposed panels are not retained unless requested.

Water Resistance using Water Fog

 

ASTM D 1735

 

Panels cured for 1 week at ambient prior to testing. Use DI water.  Chamber cleaned of salt prior to use.   Typically tested at 35±2°C (1-3 mL/hr). Panels rotated weekly.  No continuous monitoring recorder available.  Temperature can be adjusted based on test method.  Air is filtered.  Panels may or may not be tested in duplicate.

Yellowness Index

 

ASTM E313

 

Based on the Cx/Cz values for C, 1964 Obs.  Calculated automatically by Datacolor or BYK software.

Salt Fog

ASTM B 117

 

 

Tested in Q-Fog SSP600 (calibrated annually). Q-Panel Cold-rolled Steel panels. Typically, panels are scribed.  Back of panels coated with anti-corrosive spray paint or clear tape.  Panel edge is taped with electrical tape. Use 5% by weight NaCl solution. All water is DI.  After testing, panels cleaned with DI water. Panels rotated weekly. Collections and solution data is taken daily while in use.

Cyclic Prohesion

 

ASTM D 5894

 

Panels cured for 1 week at ambient temperature prior to testing QUV (UV-

A bulbs) set for 4 hours UV at 340 nm/60°C and 4 hours

condensation/50°C.  After 1 week sample is placed in Q-Fog (1 hour fog/1 hr dry at 35°C) using a 0.05% sodium chloride/0.35% ammonium sulfate solution. Use Cargill Hi-Grade Salt and chemical grade ammonium sulfate. Paints applied at specified film build, back of panels coated with anti-corrosive spray paint or covered with packing tape.  Panel edge is taped with electrical tape.  A control is not always run with panels and panels are usually run in duplicate or singularly. Temperature of cabinet is controlled through the Q-Fog instrument and also measured by an external thermometer.

Evaluation of Blistering

ASTM D 714

Visual ratings of coatings defect. Rated by same individual in a series to

lessen variation. 10=no defects, 1=severe defects.  The condition of the wood board is taken into account when rating checking and/or cracking.  If entire board shows a crack down the middle, chemist will not rate panels as poor cracking.  Rust type will not be noted  unless requested.

 

Evaluation of Chalking

 

ASTM D 4214

Method A

Evaluation of Checking

ASTM D 660

Evaluation of Cracking

ASTM D 661

Evaluation of Rusting

ASTM D 610

Evaluation of Flaking

ASTM D 772

Evaluation of fungal/algal growth or soil/dirt

ASTM D 3274

Mildew rated on 1-10 scale using pictures of actual mildew and not drawings (10=excellent, 1=poor) and not rated using designations spot growth, non-uniform spread, and complete coverage (S,P,G).  Dirt rated using pictorial standards developed by CRGI.

Falling Sand

CRGI TM 84

Use ASTM 20-30 Sand (US Silica).  Run in duplicate, typically over aluminum panels.  Film thickness tested is upon request, if none specified, CRGI will use 2 wet mils.  Control can be used in this test.  Sand is used for 10 passes and then discarded.  In cases where duplicate panels fail at the same time the weight lost is calculated to determine a rank order.  Value reported is amount of sand used if less than 80kg.  If more than 80kg then +80kg is reported.

Lid Skinning

CRGI TM 86

A deviation for this method would be to place into a refrigerator after the oven to simulate rapid cooling (note-some members believe rapid cooling can induce lid skinning).

Penetration

CRGI TM 85

Filter paper is Whatman #1 unless specified otherwise in report.  Report average of 3 areas around ring.

Sandability

CRGI TM 83

Use 150 grit sandpaper unless otherwise noted.  All samples in a series will be rated by the same chemist with same type of sandpaper to minimize deviation.

Enamel Holdout

ASTM D 7786

CRGI TM 82

 

High gloss topcoat typically used because difference in gloss is being measured.  Primer is dried 24 hours.  Topcoat is applied and evaluated after 24 hours.

Paint and primer systems will be evaluated by top coating over itself.

 

 

Exterior Exposure Testing

 

ASTM D 1006-01

 

Berea, OH exposure site. Open backed metal racks on asphalt slab.  Open backed panels will be used unless otherwise specified.   Panels typically exposed at 45° South.

 

Additional asphalt area available for horizontal panel exposure (deck stains).  If necessary horizontal coatings can be exposed on pallets.  Panels will be evaluated typically at 6 months, 1 year, and 2 years unless otherwise specified.  A report will detail substrate type and a client can contact CRGI for any further details on the substrate used.  CRGI washes panels using dish soap and water. 

 

CRGI subcontracts panels to Q-Panel for exposure (Homestead ,Florida, and Buckeye, Arizona) if needed.

 

Berea weather information yearly averages is presented below.  Humidity is not available. This information is directly from the NOAA website www.noaa.gov .  It is from the weather station at Cleveland Hopkins airport which is about five miles away from Coatings Research Group Exposure Site.

 

 

Normal Total Precipitation(in)

Normal Mean High Temperature (F)

Normal Mean Low Temperature (F)

Normal Mean Avg Temperature (F)

Normal Snowfall(in)

January

2.72

34.4

21.7

28.1

18.7

February

2.34

37.5

23.6

30.5

14.9

March

2.93

46.6

30.2

38.4

12.6

April

3.49

59.1

40.4

49.8

3.3

May

3.66

69.5

50.1

59.8

 

June

3.43

78.6

59.8

69.2

 

July

3.46

82.6

64.3

73.5

 

August

3.51

80.8

63.1

72

 

September

3.81

73.9

56

65

 

October

3.07

62.3

45.4

53.8

0.2

November

3.62

50.8

36.9

43.9

4.3

December

3.1

38.3

26.4

32.4

14.1

Revision History

Date

Revision

Revised By:

Changes

5-15-14

6

CRGI Lab Staff

Changed temperature range testing conducted at typically, clarified some test method deviations.

6-26-15

7

CRGI Lab Staff

Changed the type of bar used for most test methods, added coatings can be drawndown as specified

7-20-15

8

CRGI Lab Staff

Added ASTM D 5895 Changed permeability to 50 +/- 5% humidity.  Updated burnish, washability and scrub to include recording machine used.  Added dry time with a recorder test method.

2-2-16

9

CRGI Lab Staff

Revised VOC, application, adhesion, washability and salt fog deviations.  Added updated weather data to the exposure test method deviation.

12-22-16

10

CRGI Lab Staff

Revised deviations for: Blocking, Perms, Sag resistance, Film Forming, Gloss, Package Stability, Falling Sand and Enamel Holdout. Added ASTM Methods in addition to CRGI Methods where appropriate.

CRGI is certified as an ISO 17025 accredited testing laboratory by ANAB. Through a system of international agreements, this accreditation is recognized worldwide.
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