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PAINT FALURE, DIAGNOSIS, CURE, PREVENTION
FAILURE CHECKLIST
  EXTERIOR CLUES
  INTERIOR CLUES
  SITE HISTORY
  FAILURE INDICATORS
COMMON MISTAKES
  BAD SURFACE PREP
  SHORTCUT ERRORS
  PAINT OVER MOISTURE
  INCOMPATIBLE PAINTS
LIST OF FAILURES
PAINT FAILURE INVESTIGATOR/LAB
PAINT LAB SAMPLE PREP
  Flat Surface View of Failing Paint
  Sectional View of Failing Paint
  Simple Chemical Tests
  Contributors & References

PAINT REFERENCES
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Paint Lab Photo:

Paint Sample Preparation and Analysis Pocedures
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This article describes a simple procedure for preparing paint samples for reflected light low to high magnification microscopic examination in the paint failure laboratory. A procedure is described for mounting sectioned paint chips on edge for microscopic examination. This procedure is useful in the determination of paint layers, paint layer thickness measurement, and paint layer interactions. The procedure also permits detection of mold or debris which has been painted over. Two simple chemical tests are described for identification of paint as acrylic or alkyd, useful as a quick, inexpensive alternative to pyrolysis gas chromatography, We include photographs of the procedure for preparing paint chips for cross-section and flat surface analysis. and phots of the results of simple chemical analysis to identify paint samples as acrylic or alkyd paints. This document is a chapter of Diagnosing and Preventing Paint Failure on Building Exteriors. The diagnosis and cure of paint failure on buildings, particularly on wood siding and trim, is quite possible if there is a careful and thorough inspection of the building, its history, its surfaces, and the actual points of paint failure. It is diagnostic to compare the same coating on the same type of surface at different locations on a building and in areas of failed and not-failed paint. © Copyright 2008 Daniel Friedman, All Rights Reserved. Information Accuracy & Bias Pledge is at below-left. Use links at the left of each page to navigate this document or to view other topics at this website. Green links show where you are in our document or website.

Our site offers impartial, unbiased advice without conflicts of interest. We will block advertisements which we discover or readers inform us are associated with bad business practices, false-advertising, or junk science. Our contact info is at inspect-ny.com/appointment.htm.


A Procedure for Preparing Paint Samples for Examination by Reflected Light Microscopy

Flat Surface View of Failing Paint Chips for Paint Failure Diagnosis

Paint chips and samples from a painted surfce can be easily mounted flat for microscopic examination, though care should be taken in selection of mounting media to be sure that the media does not react with or modify the sample. Flat mounting of paint chip samples to examine the exposed and inner surfaces is a basic step in microscopic examination and lab diagnosis of failing coatings.

Examination of the exposed paint surface in flat or planar view may disclose defects such as micro cracking, micro blistering, or contaminants. Examination of the inner, hidden, or release-surface of sample paint chips from a failing coating can provide critical information needed to state the cause of the paint failure with confidence. The inner paint surface may show wood fibers, chalked dust from the painted-on surface, or even separation of paint ingredients or surfactant bleeding which form critical diagnostic data but which cannot be seen with the naked eye. Photographs of these failures are provided in other chapters of this document.


PAINT FALURE, DIAGNOSIS, CURE, PREVENTION
FAILURE CHECKLIST
  EXTERIOR CLUES
  INTERIOR CLUES
  SITE HISTORY
  FAILURE INDICATORS
COMMON MISTAKES
  BAD SURFACE PREP
  SHORTCUT ERRORS
  PAINT OVER MOISTURE
  INCOMPATIBLE PAINTS
LIST OF FAILURES
PAINT FAILURE INVESTIGATOR/LAB
PAINT LAB SAMPLE PREP
  Flat Surface View of Failing Paint
  Sectional View of Failing Paint
  Simple Chemical Tests
  Contributors & References

PAINT REFERENCES
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Sectional View of Failing Paint Chips for Paint Failure Diagnosis

In addition to the examination of the flat surfaces of paint chips under the microscope, the examination of edge-view sectioned paint chips can yield important information. Yet some analysts may be unfamiliar with simple and quick procedures that permit examination of paint in this diagnostic view. It is this more unusual edge view procedure which we want to document here. We make use of a sample lamination procedure introduced by the McCrone Research Institute, Chicago, IL. McCrone offers advanced courses in forensic microscopy useful across various disciplines. (The author has no affiliation with McCrone but is a graduate of a number of McCrone's courses.)

The examination of the edge of a paint chip sample can provide critical information such as:

  • The number of individual paint layers on the surface represented by the paint chip sample.
  • Precise measurements of each individual paint thickness layer, and, by examining along individual samples as well as by examining multiple paint samples, the variation in paint thickness per layer can also be estimated.
  • Identification of micro blisters in paint such as those caused by thermal blistering or solvent blistering in paint
  • The presence of debris or mold between and in paint layers can be viewed and documented

The photographs and text here show how a paint chip can be prepared for a sectioned or edge-view by either low-power stereomicroscope, or by high power forensic microscope. Click any photo to see a larger image.

Paint Lab Photo: equipment needed to section a paint chip 1. Photo of the basic equipment needed to prepare a sectional slice of a paint chip for edge-view microscopic examination.
Paint Lab Photo: 2. Place the selected paint chip on top of a square of clean 6-mil polyethylene sheeting. The square can be oversized to about 1" x 1" or so as it will be trimmed later.
Paint Lab Photo: 3. Place a second square of clean 6-mil poly atop the sample, aligning the edges to make a neat 1" x 1" sandwich of paint chip between the two layers of plastic.
Paint Lab Photo: 4. Place the sample sandwich between two clean glass slides and atop a heating plate such as shown in the photo. You may have to experiment to find the right hot plate temperature to fuse but not over-melt or burn the poly or the paint sample so experiment with non-critical sample material first.

PAINT FALURE, DIAGNOSIS, CURE, PREVENTION
FAILURE CHECKLIST
  EXTERIOR CLUES
  INTERIOR CLUES
  SITE HISTORY
  FAILURE INDICATORS
COMMON MISTAKES
  BAD SURFACE PREP
  SHORTCUT ERRORS
  PAINT OVER MOISTURE
  INCOMPATIBLE PAINTS
LIST OF FAILURES
PAINT FAILURE INVESTIGATOR/LAB
PAINT LAB SAMPLE PREP
  Flat Surface View of Failing Paint
  Sectional View of Failing Paint
  Simple Chemical Tests
  Contributors & References

PAINT REFERENCES
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Paint Lab Photo: 5. This photo shows the poly incompletely fused. More heating was necessary. Our object is to fuse the two layers of poly together so that the paint chip will be firmly secured between them.
Paint Lab Photo: 6. When the poly has become sufficiently hot and is melting together we press it gently to remove air bubbles and to confirm that the two layers of plastic have become fused. There is no problem taking the assembly off of the heater and then returning it to that surface. Be careful of burns.
Paint Lab Photo: 7. Here you can see that the poly is nicely fused but not over-melted or bubbling.
Paint Lab Photo: 8. We cool the sample slides and poly atop a steel spatula used to remove it from the hot plate surface.
Paint Lab Photo: 9. The sample is immediately numbered with our lab control number again to avoid any possible mix-up. However as we normally prepare, examine, and photodocument one sample at a time there is no real chance for a sample labeling or handling error. Keep sample labels identical to those used in the chain of custody form and original sample material labels.
Paint Lab Photo: 10. Trim the sample poly sandwich to approximately 20cm x 20 cm square.

PAINT FALURE, DIAGNOSIS, CURE, PREVENTION
FAILURE CHECKLIST
  EXTERIOR CLUES
  INTERIOR CLUES
  SITE HISTORY
  FAILURE INDICATORS
COMMON MISTAKES
  BAD SURFACE PREP
  SHORTCUT ERRORS
  PAINT OVER MOISTURE
  INCOMPATIBLE PAINTS
LIST OF FAILURES
PAINT FAILURE INVESTIGATOR/LAB
PAINT LAB SAMPLE PREP
  Flat Surface View of Failing Paint
  Sectional View of Failing Paint
  Simple Chemical Tests
  Contributors & References

PAINT REFERENCES
More Information

InspectAPedia TM Home & Site Map
Exteriors
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Paint Lab Photo: 11. A simple razor blade, carefully handled, can produce a sample cross section thin enough for microscopic examination. We will be using reflected, not transmitted light in most instances with these samples. Cut a thin slice of sample sandwich, 1mm or less in thickness, keeping the slice oriented so that you don't lose track of which is the edge view.
Paint Lab Photo: 12. Here is our sliced sample cross-section. The sample side facing up on this slide is not what we want to examine as it shows the sample face, not its cross section.
Paint Lab Photo: 13. So we carefully turn the paint sample sectional slice on its side, exposing its cross section. To keep the sample in the proper orientation, notice that we bent over the plastic ends of the poly sandwich at roughly 90 deg. at each end.
Paint Lab Photo: 14. The sliced, bent paint chip sample section is placed on a clean microscope slide.
Paint Lab Photo: 15. As we wanted to make a permanent slide mount of this sample, and as we didn't want any chemical interaction with the sample, we mounted this cross section of paint chip using clear glass adhesive.
Paint Lab Photo: 16. Here's our paint sample cross sectional slice mounted in glass adhesive and with a 50mm x 22mm coverslip, ready for curing.
Paint Lab Photo: 17. Clear glass adhesive has some nice optical properties, but it needs to be cured by UV light. Rather than place our sample outside in the sun we used this halogen lamp to harden the slide preparation..
Paint Lab Photo: Paint Lab Photo: Paint Lab Photo:
18. Here are some interesting paint chip cross section slices. By calibrating our eyepiece micrometer using a stage micrometer, we can measure paint layer thickness. Other photos here are examples of microscopic blistering which was not visible except at high magnification but quite dramatic when viewed in cross section as shown here. These observations at 120X magnification and top lighting on our forensic microscope were useful in diagnosing the cause of failure of this paint coating.

PAINT FALURE, DIAGNOSIS, CURE, PREVENTION
FAILURE CHECKLIST
  EXTERIOR CLUES
  INTERIOR CLUES
  SITE HISTORY
  FAILURE INDICATORS
COMMON MISTAKES
  BAD SURFACE PREP
  SHORTCUT ERRORS
  PAINT OVER MOISTURE
  INCOMPATIBLE PAINTS
LIST OF FAILURES
PAINT FAILURE INVESTIGATOR/LAB
PAINT LAB SAMPLE PREP
  Flat Surface View of Failing Paint
  Sectional View of Failing Paint
  Simple Chemical Tests
  Contributors & References

PAINT REFERENCES
More Information

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Exteriors
Contact Us

Simple Chemical Tests to Identify Acrylic and Alkyd Paints

The identification of a paint chip sample as acrylic or alkyd-based is important for art conservationists, but also for more prosaic paint failure investigators who examine buildings. With asstance from two experts, one an experienced paint chemist and the other, an expert art conservator, we here document the procedure.

Paint testing laboratories use either chemical methods and/or infra-red spectrometry to identify binders used in paints. Infrared spectroscopy is the most fundamental way to identify almost any organic material.

Pyrolysis GC/MSD is a useful back up method, and has been used in the art conservation field. See Analysis of Modern Paints at References below.

All organic materials have a unique infrared spectrum or 'finger print'. Some paint testing labs (Bodycote) inform us thatthe follwing combination of paint testing methods are the most precise in paint identification and can be used to reverse-engineer a paint from a paint sample.

  • Fourier transform infrared spectroscopy (FTIR) to determine the type of resin in the paint
  • Thermogravimetric analysis (TA) to determine the fillers present in the paint
  • Scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy to determine the elemental composition of the paint chip.

These tests are costly, ranging from $450. to $1000. per test per sample .

A Description of Two Simple Chemical Tests to Examine Paint Chips

Chemical tests to examine paint chips or painted surfaces, while less precise and less informative, are very quick, inexpensive, and can be used in the field as well as in the laboratory. Therefore chemicals are mainly used on site and infra-red is used in the lab.

The most common chemical methods for examining paint in the field or for a "quick lab test" are:

  1. NaOH-solution will make alkyd and oil paint surfaces turn yellow, but will not affect acrylates. (4% NaOH, but KOH can also be used. KOH was used for the tests shown in photographs in this document.)
  2. Ethanol will soften acrylates but will not affect alkyd and oil paints.

Mixed-base paints lead to ambiguous results: This chemical method for paint testing will not always give a definitivee answer. For example if a water-based paint is comprised of both alkyd and acrylate components the chemical test will be ambiguous.

However these tests can be unambiguous: if the surface either turns yellow with NaOH or softens with ethanol, and if the converse test of the same sample using the opposite chemical does not produce the key reaction, then the test is reliable.

We performed the tests shown in this document, followed by sending samples of the same paints to an independent paint testing laboratory for advanced testing. The results of this advanced laboratory analysis will also be reported here as a cross-check on our chemical test for acrylic and alkyd paint.

Ethanol Test on Paint Chips Separate Acrylic from Alkyd

Here are photographs showing the effectiveness of the Ethanol test on two paint chips. One paint chip remained brittle and fragile as it was at the outset, unaffected by the ethanol, indicating that the chip was not an Acrylic. We suspected it was an alkyd paint, confirmed by the KOH test. The second paint chip becomes soft after about 4 minutes in Ethanol, as we demonstrate by curling and rolling the previously fragile brittle chip using our forceps. This confirms that the ethanol-softened paint was an acrylic.

Paint Lab Photo: Paint chip remains flat = alkyd/oil: This paint chip remained flat and brittle, unaffected by submersion in ethanol, suggesting that it is not an acrylic paint. (We suspected that it was an alkyd or "oil" based paint).
Paint Lab Photo: equipment needed to section a paint chip Paint chip softens, curls = acrylic or latex: This paint chip curled when soaked in ethanol for four minutes, and was easily bent and rolled using our fine forceps as shown in the photo. This is an acrylic paint.

NaOH or KOH Test on Paint Chips to Separate Acrylic, Latex, from Alkyd

Here are photographs showing the effectiveness of the KOH test on two paint chip samples. One turned yellow (indicating Alkyd paint) and the other was unchanged (indicating not alkyd paint, in this case suspected Acrylic). [Photos coming]

Summarizing these tests: We use either chemical methods and/or infra-red spectrometry to identify binders. Chemicals are mainly used on site and infra-red is used in the lab. The most common chemical methods are:
1. NaOH-solution will make alkyd and oil paint surfaces turn yellow, but will not affect acrylates.
2. Ethanol will soften acrylates but will not affect alkyd and oil paints.
This chemical method is very crude and will not always give a definite answer (for example if a water-bsed paint comprises of both alkyd and acrylate components), but if the surface either turns yellow with NaOH or softens with ethanol, then you are in business!


PAINT FALURE, DIAGNOSIS, CURE, PREVENTION
FAILURE CHECKLIST
  EXTERIOR CLUES
  INTERIOR CLUES
  SITE HISTORY
  FAILURE INDICATORS
COMMON MISTAKES
  BAD SURFACE PREP
  SHORTCUT ERRORS
  PAINT OVER MOISTURE
  INCOMPATIBLE PAINTS
LIST OF FAILURES
PAINT FAILURE INVESTIGATOR/LAB
PAINT LAB SAMPLE PREP
  Flat Surface View of Failing Paint
  Sectional View of Failing Paint
  Simple Chemical Tests
  Contributors & References

PAINT REFERENCES
More Information

InspectAPedia TM Home & Site Map
Exteriors
Contact Us

Contributors & References

  • Daniel Friedman American Home Service, Poughkeepsie, NY, diagnostic building investigations since 1976, forensic laboratory analysis since 1986
  • Leila Kotama, Product Manager, Tikkurila Paints Oy, Finland. Dr. Kotama has more than 20 years experience as a paint chemist.
  • Ulrik Runeberg, Conservador , Museo de Arte Contemporaneo de Puerto Rico, San Juan Puerto Rico
  • Daniel Friedman, American Home Service, Poughkeepsie, NY, principal author, diagnostic building inspections since 1976, diagnostic lab forensics since 1986
  • Bodycote Materials Testing, Ontario, Canada

  • Paint and Surface Coatings, Theory and Practice, R. Lambourne & T.A. Strivens, Ed., Woodhead Publishing Ltd., William Andrew Publishing, 1999 ISBN 1-85573-348 X & 1-884207-73-1 [This is perhaps the leading reference on modern paints and coatings, but is a difficult text to obtain, and is a bit short on field investigation methods - DF]
  • Analysis of Modern Paints, Thomas J.S. Learner, Research in Conservation, 2004 ISBN 0-89236-779-2 [Chemistry of modern paints, overview of analytical methods, pyrolysis-gas chromatography signatures of basic modern paints and their constituents, Fourier transform infrared spectroscopy for paint analysis, direct temperature-resolved mas spectrometry, and analysis in practice - technical reference useful for forensic paint science, focused on art works -DF]
  • Seeing Through Paintings, Physical Examination in Art Historical Studies, Andrea Kirsh, Rustin S. Levenson, Materials in Fine Arts, 2000 ISBN 99-051835 [ forensic science, technical reference, focused on art works - DF]
  • Paint Handbook: testing, selection, application, troubleshooting, surface preparation, etc., Guy E. Weismantel, Ed., McGraw Hill Book Company, 1981 [Excellent but a bit obsolete paint theory and practice, also a bit light on field investigation methods, out of print, available used-DF]
  • Art, Biology, and Conservation: Biodeterioration in Works of Art, Robert J. Koestler et als. Eds., Metropolitan Museum of Art, 2003, ISBN 1-58839-107-8

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