It’s All In the Preparation: Part 1

As earlier posts have mentioned, the first phase of our research aims to establish the lightfastness of the Orasol® and similar Sorasolve metal-complex solvent dyes in isolation‒ that is, in the absence of a binder, and without a chemically active substrate that could potentially influence the behavior of the dyes or interfere with the measurement of color change. To accomplish this we needed a substrate for the dye film that would not be altered physically or chemically by the accelerated aging exposure and would not interfere with our reflectance measurements (reflectance measurements will be discussed further in up-coming posts). The required substrate would need to be:

1.  Optically pure.

Any color or visual irregularities in a substrate would affect our color measurements, and impede an accurate calculation of the dyes’ lightfastness.

2. Durable.

The substrate needs to withstand a degree of handling throughout its use. For example, in one test cycle, the samples are measured for color change 8 times, in addition to before-, during-, and after-treatment photography.

3. Chemically inert.

The substrate must not be altered physically or chemically by the accelerated aging process, to ensure that it does not discolor (impeding accurate measurement of color change in the dye itself) or produce reaction products that could potentially alter the behavior of the dye.

Before making our final choice, we considered and rejected several candidates:

pink dye on wool

BASF dye Pink 478 (CIGN Solvent Red 127) sprayed on wool textile substrate. Although wool readily accepts dye, it was not chosen as the substrate because of its chemical instability during accelerated aging. Note also that the color of the dye is different depending on solvent. Solvent, top to bottom: acetone, ethyl acetate, ethanol, isopropanol, PGME. AMNH/F. Ritchie

Wool textile: inexpensive, readily available, and resilient to handling. It has the great benefit of accepting the dye in a manner very similar to the fur/hair on our taxidermy specimens because it is made from the same material, keratin fiber. However, it is not chemically inert, and is known to bleach or yellow during accelerated aging.

Acid-free paper: durable and inexpensive, but, like wool, is not chemically inert and may undergo color change or influence the stability of the applied dye. In addition, it accepts the dye solutions in a manner quite different from hair/fur, as they are readily absorbed deep into the sheet.

Glass slides or plates: much more chemically stable than wool or paper, though they may still produce reaction products in high temperatures and humidity. Dye applied to glass sits on the surface, similar to keratin fiber. Glass is inexpensive, but could be cleaned and reused if necessary. It is, of course, more fragile than wool or paper.

Ultimately we decided to use thin quartz plates, because they best fulfill our optical, physical, and chemical requirements for a substrate. Quartz plates consist of pure silicon dioxide (SiO2). They are not only optically pure (being transparent and colorless) and have a high damage threshold; they are also non-absorbent and reusable. However, as we came to appreciate, they are typically used in very sensitive research applications, which require high standards of dimensional exactness and chemical/optical purity. As such, they aren’t cheap. Finding affordable quartz plates was very challenging, and eventually took us to a Chinese company that was able to provide us with custom-cut plates that easily met the needs of our project, without the cost that accompanies the exacting standards required by other research applications.

Drawing on the procedure outlined in the ASTM D4303 standard, our testing of each dye solution and set of lighting conditions uses three replicate samples (A, B, and C). Two plates (A and B) are exposed in the aging chamber during the test cycle, and the third (C) is held in dark storage as a control. Throughout each test cycle, color measurements are taken periodically from each replicate. Each plate is measured in three locations, and these results are averaged to produce an overall measurement for that sample at that time index.

Having selected a transparent substrate, it was necessary for us to then identify a material to place behind our samples during our reflectance measurements and accelerated aging cycles. For the former, a standard white backing material was needed — something opaque (to eliminate any influence on the measurement from the tabletop or work surface behind this backing), and either durable or easily replaced. It would also need to be extremely white (i.e. with a uniform high reflectance throughout the visible spectrum) so that it would reflect the light transmitted through the sample back up into our reflectance spectrophotometer without distorting the spectrum of the dye. We chose to use plain white nitrocellulose membrane filters stacked three layers deep to ensure opacity. While a white ceramic tile could also have been used, we felt that the membrane filters would be more easily incorporated into the wooden jig that we are using to standardize our measurement locations.

jig with sample__1

Jig built for the project to hold quartz plate dye samples during color measurements. Note the white nitrocellulose film used to back samples. AMNH/F. Ritchie

For the same reason that a white backing material is helpful in color measurement, it would be problematic in our accelerated aging exposures: a white surface would act as a mirror, reflecting light from the xenon lamp that had already passed through the sample back up toward the plate. This would be exposing the dye films twice, once by direct exposure of the lamps, and a second time by reflected light from below, increasing the light exposure dose by some unknown percentage. This would make our determination of a rough equivalence between accelerated and real time aging periods in our dioramas more difficult. Eliminating the backing altogether would have the same effect: the plates would rest directly on our reflective aluminum sample holders. We needed to identify a material that would absorb the light transmitted through the sample plates but also would withstand the extreme environment within the accelerated aging chamber. We would need to use a black backing inside the chamber.

To realize this light-absorbing backing, we initially lined our aluminum sample holders with black archival matte board. We also added bumpers along the edges of the backing to create a small space for air circulation between the board and the plates, which helps with heat dissipation. Unfortunately, we discovered that the matte board generated a sticky condensate on the underside of the plates during aging. We altered our design to instead use black textile masks and corrugated blue board. These have proven to be free of the condensate problem of the matte board. The masks slowly fade during our exposures that include UV radiation, so we designed our sample mounts in such a way that new masks can be inserted when replacement is needed.

black panel_plate_holder

Clockwise: Quartz plate without dye, sample backing of black textile mask with cardboard bumpers covered in black textile mask, metal sample holder. AMNH/F. Ritchie

sample holders

Top: Dye samples resting on black backing. Bottom: Dye samples assembled in sample holder, ready for testing. AMNH/F. Ritchie

 

 

 

 

 

 

Part Two will describe how we prepare the quartz plate dye samples.

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The Dye Is Cast

The initial sample set undergoing accelerated aging in our Q-SUN chamber is expected to be the largest. It includes all of the Orasol dyes that we have been able to acquire to date from the manufacturer BASF and retail supplier Kremer Pigments, as well as Sorasolve dyes available from Museum Services Corporation (MSC). This post includes a listing of all of our dye samples. For a comprehensive concordance of materials by manufacturer, current and former product names, and Colour Index Generic Names (CIGN), please see the table at the end of the post.

Orasol dyes, manufactured by and available from BASF

BASF does not sell small quantities of its product directly to consumers, but samples may be requested from the company for testing purposes. Materials obtained this way are understood to be of relatively recent production.

  • Orasol® Red 330 (CIGN Solvent Red 130)
  • Orasol® Red 335 (CIGN Solvent Red 122)
  • Orasol® Red 355 (CIGN Solvent Red 119)
  • Orasol® Red 363 (CIGN Solvent Red 125)
  • Orasol® Red 365 (CIGN Solvent Red 160)
  • Orasol® Red 395 (CIGN Solvent Red 122)
  • Orasol® Red 471 (CIGN Solvent Red 118)
  • Orasol® Pink 478 (CIGN Solvent Red 127)
  • Orasol® Orange 245 (CIGN Solvent Orange 56)
  • Orasol® Orange 247 (CIGN Solvent Orange 11)
  • Orasol® Orange 251 (CIGN Solvent Orange 54)
  • Orasol® Orange 272 (CIGN Solvent Orange 99)
  • Orasol® Yellow 081 (CIGN Solvent Yellow 79)
  • Orasol® Yellow 141 (CIGN Solvent Yellow 81)
  • Orasol® Yellow 152 (CIGN Solvent Yellow 88)
  • Orasol® Yellow 157 (CIGN Solvent Yellow 82)
  • Orasol® Yellow 190 (CIGN Solvent Yellow 89)
  • Orasol® Blue 825 (CIGN Solvent Blue 67)
  • Orasol® Blue 855 (CIGN Solvent Blue 70)
  • Orasol® Brown 324 (CIGN Solvent Brown 43)
  • Orasol® Brown 326 (CIGN Solvent Brown 44)
  • Orasol® Black X45 (CIGN Solvent Black 28)
  • Orasol® Black X51 (CIGN Solvent Black 27)
  • Orasol® Black X55 (CIGN Solvent Black 29)

Orasol dyes, manufactured by BASF, and available from Kremer Pigments

Kremer sells small quantities of BASF Orasol dyes retail. To do so, they purchase dyes in bulk from BASF and warehouse the stock until it is sold. As a result, dyes purchased from Kremer have an unknown production and storage history. Orasol products listed in Kremer’s product catalog are identified using both old and newer Orasol naming systems, reflecting the name in use by the manufacturer at the time Kremer made its purchase from BASF.

  • Orasol® Red 395 (CIGN Solvent Red 122)
  • Orasol® Orange 247 (CIGN Solvent Orange 11)
  • Orasol® Yellow 152 (CIGN Solvent Yellow 88)
  • Orasol® Yellow 4GN (CIGN Solvent Yellow 146)
  • Orasol® Yellow 2RLN (CIGN Solvent Yellow 89)
  • Orasol® Blue 825 (CIGN Solvent Blue 67)
  • Orasol® Brown 324 (CIGN Solvent Brown 43)

Sorasolve dyes, manufactured/supplied by First Source Worldwide LLC, and available from Museum Services Corporation (MSC)

Museum Service Corporation’s retail product-catalog lists their metal-complex solvent dyes using the old BASF naming system for the Orasol® brand; however, the dyes are supplied to MSC under the brand name Sorasolve by First Source Worldwide LLC, an American chemical company based in Neenah, Wisconsin. Orasol® and Sorasolve dyes with the same Colour Index Generic Name share an essential colorant with the same chemical constitution.

  • Yellow 2RLN (Sorasolve/CIGN Solvent Yellow 89)
  • Yellow 4GN (Sorasolve/CIGN Solvent Yellow 146)
  • Yellow 2GLN (Sorasolve/CIGN Solvent Yellow 88)
  • Orange G (Sorasolve/CIGN Solvent Orange 11)
  • Red BL (Sorasolve/CIGN Solvent Red 122)
  • Red G (Sorasolve/CIGN Solvent Red 125)
  • Pink 5BLG (Sorasolve/CIGN Solvent Red 127)
  • Blue GN (Sorasolve/CIGN Solvent Blue 67)
  • Brown 2GL (Sorasolve/CIGN Solvent Brown 42)
  • Brown 2RL (Sorasolve/CIGN Solvent Brown 43)
  • Brown 6RL (Sorasolve/CIGN Solvent Brown 44)
  • Black CN (Sorasolve/CIGN Solvent Black 28)
  • Black RLI (Sorasolve/CIGN Solvent Black 29)

We have characterized all of these dyes using fourier transform infrared spectroscopy (FTIR). Our results confirm that samples of old and new Orasol® dyes, as well as the related Sorasolve dyes, have very similar infrared spectra (see image below).

Yellow 89

FTIR spectra for Solvent Yellow 89 samples acquired from BASF (purple line), Kremer (blue line), and MSC (red line). Note the likeness between spectra, indicating that the three dyes sold by three companies under the same CIGN are chemically very similar, if not the same.

All of these dyes are soluble in a wide selection of solvents. As mentioned previously, during dye testing conducted in conjunction with the renovation of the dioramas in the Jill and Lewis Bernard Family Hall of North American Mammals, we observed that solvent choice can have subtle effects on both the color and lightfastness of the dyes. In order to explore these effects more extensively, five different solvents were selected for our present tests. They reflect a range of properties with respect to dye solubility and volatility/evaporation rate. Among them are solvents commonly used in the conservation of art and artifacts, as well as some others used in previous testing by Ciba-Geigy. Unusually toxic solvents or solvents that present other problems precluding their general use in restoration work were excluded.

The solvents we are testing include:

  • Acetone
  • Ethyl acetate
  • Ethanol
  • Isopropanol
  • Propylene glycol monomethyl ether (PGME).
acetone_PGME

Dye sample Red BL (CIGN Solvent Red 122) purchased from Kremer. Note the difference the solvent choice makes in surface texture/coverage between the sample dissolved in acetone (left) and the same sample dissolved in PGME (right). AMNH/F. Ritchie

Dye concordance table

Concordance of dye materials by current and former product names, Colour Index Generic Names (CIGN), chemical composition, and source.