Imaging and Assessment of the Microstructure of Conserved Archaeological Pine
Abstract
:1. Introduction
2. Materials and Methods
2.1. Samples
- 1.
- Reference
- 2.
- Alkohol-ether resin
- 3.
- Melamine formaldehyde (Kauramin 800®, BASF, Ludwigshafen, Germany)
- 4.
- Lactitol-trehalose
- 5.
- Polyethylene glycol (PEG 2000) one-step and freeze-drying
- 6.
- Polyethylene glycol (PEG 400 and 4000) two-step and freeze-drying
- 7.
- Polyethylene glycol (PEG 400, 1500 and 4000) three-step and freeze-drying
- 8.
- Saccharose
- 9.
- Silicone oil
2.2. Methods
2.2.1. Optical Microscope
2.2.2. Computed Tomography
2.2.3. Scanning Electron Microscope
3. Results
3.1. Air-Dried Reference Sample
3.2. Alcohol-Ether-Resin
3.3. Melamine Formaldehyde (Kauramin 800)
3.4. Lactitol/Trehalose
3.5. PEG 2000 and Freeze-Drying
3.6. PEG 400, PEG 4000 and Freeze-Drying
3.7. PEG 400, PEG 1500, PEG 4000 and Freeze-Drying
3.8. Saccharose
3.9. Silicone Oil
4. Discussion
4.1. Distribution of the Conservation Agent
4.2. Relationship between Microscopic and Macroscopic Level
5. Conclusions
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
Appendix A
Conservation Method | Institutions and Short Descriptions of the Methods | |
---|---|---|
Air dried reference | Institution: | Leibniz-Zentrum für Archäologie, Mainz, Germany |
Treatment: | none, air-drying | |
Impregnation solution: | none | |
Alcohol-ether-resin | Institution: | Schweizerisches Nationalmuseum, Zürich, Switzerland. |
Treatment: | Exchange of water with ethanol. Exchange of ethanol with diethyl ether. Soaking of wood with diethyl ether in resin-diethyl solution. Drying by evaporation of the diethyl ether in the vacuum vessel. Application of surface protection 3% Paraloid B72 solution in acetone. | |
Impregnation solution: | 70.7% diethyl ether, 16.1% dammar resin, 6.4% rosin, 3.2% dienol D102, 3.2% rhizinus oil, 0.4% PEG 400 | |
Kauramin 800 | Institution: | Leibniz-Zentrum für Archäologie, Mainz, Germany |
Treatment: | Soaking in demineralized water. Bath impregnation at room temperature. Replacement of the solution when early polymerisation occurs. Curing of the impregnated wood in the heating cabinet at 60 °C. Afterwards slow, controlled air-drying. Dip in linseed oil varnish. | |
Impregnation solution: | 25% Kauramin 800 solution (72 L resin + 210 L deionised water, 3.6 L urea, 7.2 L triethylene glycol) | |
Lactitol-trehalose | Institution: | Brandenburgisches Landesamt für Denkmalpflege, Zossen, Germany |
Treatment: | Starting with 30% concentration. Increasing monthly in 10% steps up to 70%. Bath temperature 55 °C. After removal from the bath, the surfaces were dusted with crystalline lactitol monohydrate and dried in a heating oven over a period of one week. After drying, the surface was cleaned by dabbing with damp cloths. | |
Impregnation solution: | lactitol-trehalose solution (9:1) 30%–70%. Addition of biocide if necessary (0,1% Bioban 404) | |
Polyethylene glycol (PEG 2000) one-step and freeze-drying | Institution: | Nationalmuseet, Copenhagen, Denmark |
Treatment: | Starting with 10% PEG 2000 solution. Increasing the concentration up to 40% at room temperature. Freeze-drying in cooled chamber (approx. −30 °C). Removal of excess PEG from the surface with a soft brush and ethanol. Subsequent surface stabilisation with 25% PEG 2000 solution in ethanol. | |
Impregnation solution: | PEG 2000, 10–40% solution with tap water | |
Polyethylene glycol (PEG 400 and 4000) two-step and freeze-drying | Institution: | Brandenburgisches Landesamt für Denkmalpflege, Zossen, Germany |
Treatment: | Soaking in demineralised water. Starting with 5% PEG 400 solution. Raising the concentration in 5% steps every 4 weeks. At its calculated final concentration, it was kept constant. Then the increase of PEG 4000 solution was continued in 5% steps up to its final concentration where it was kept for 10 weeks. Precooling of the wood to 5 °C then deep-freezing to −25 to −35 °C, freeze-drying in cooled chamber (approx. −30 °C). | |
Impregnation solution: | PEG-solution in demineralised water (PEG 400 and PEG 4000) was adapted according to the condition of the wood (PEGcon): 35% PEG solution (of which 10% PEG 400 and 25% PEG 4000) in demineralized water, impregnation at room temperature | |
Polyethylene glycol (PEG 400, 1500 and 4000) three-step and freeze-drying | Institution: | Archäologische Staatssammlung, Munich, Germany |
Treatment: | Soaking in demineralised water. Starting with 11% increasing to 15% PEG 400 solution at room temperature. 16% increasing to 20.5% PEG 1500 solution at 40 °C. 20.5% increasing to 27.5% PEG 4000 solution at 40 °C. Washing of the wood and wrapping in cellulose tissues. Intermediate storage in freezer (−25 to −35 °C) until freeze-drying. Subsequent freeze-drying in a cooled chamber (approx. −30 °C). Excess of PEG was removed with a brush and ethanol. | |
Impregnation solution: | PEG-solution in demineralised water: 15% PEG 400, 20.5% PEG 1500, 27.5% PEG 4000 | |
Saccharose | Institution: | Sächsisches Landesamt für Archäologie, Dresden, Germany |
Treatment: | Concentrated the solution in 10% steps, from 10% up to 60% sugar solution at room temperature. Slow, controlled air-drying in microperforated bags. Removal of crystallised sugar residues from the surface with damp sponge. | |
Impregnation solution: | Aqueous saccharose solution 10%–60%. If necessary biocide addition composed of 0.6%, sodium benzoate (E211), 0.5% Parmetol K40, 0.5% Quartasept Plus and 0.02% Tallofin OT | |
Silicone oil | Institution: | Texas University, Texas, USA |
Treatment: | Exchange of water with ethanol. Exchange of ethanol with acetone. Placing the still dripping wet acetone-impregnated samples in impregnation solution under normal atmospheric conditions. Triggering the polymerisation of the impregnation solution by gaseous catalyst: DBTDA (dibutyl diacetate). | |
Impregnation solution: | 80% silicone oil (SFD1 (66%) + SFD5 (34%)—silanol functional polydimethylsiloxanes “PDMS”) and 20% crosslinker MTMS (methyltrimethoxysilane) |
Sample | Database [33] | Conservation | Condition | Analysis | ||
---|---|---|---|---|---|---|
CT | SEM | LM | ||||
Pi-Air-ld | V03-01 | None, air-drying | Low degraded | x | x | |
Pi-Air-hd | heavily degraded | x | x | x | ||
Pi-AlEt-ld | V03-17 | Alcohol-ether-resin | Low degraded | x | ||
Pi-AlEt-hd | heavily degraded | x | x | x | ||
Pi-K800-ld | V03-41 | Melamine formaldehyde | Low degraded | x | x | |
Pi-K800-hd | heavily degraded | x | x | x | ||
Pi-LaTr-ld | V03-28 | Lactitol-trehalose | Low degraded | x | x | |
Pi-LaTr-hd | heavily degraded | x | x | x | ||
Pi-PEG1-ld | V03-35 | PEG 2000 | Low degraded | x | x | |
Pi-PEG1-hd | heavily degraded | x | x | x | ||
Pi-PEG2-ld | V03-32 | PEG 400 and 4000 | Low degraded | x | x | |
Pi-PEG2-hd | heavily degraded | x | x | x | ||
Pi-PEG3-ld | V03-20 | PEG 400, 1500 and 4000 | Low degraded | x | x | |
Pi-PEG3-hd | heavily degraded | x | x | x | ||
Pi-Sac-ld | V03-45 | Saccharose | Low degraded | x | x | |
Pi-Sac-hd | heavily degraded | x | x | x | ||
Pi-Sil-ld | V03-42 | Silicone oil | Low degraded | x | x | |
Pi-Sil-hd | heavily degraded | x | x | x |
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Contemporary Pine Sample | Archaeological Pine Sample | |
---|---|---|
Basic density (BD) (kg/m³) | 420 | 251 |
Cellulose (%) | 49 | 27 |
Lignin (%) | 28 | 53 |
Hemicellulose (%) | 23 | 20 |
Maximum water content MWC (%) | 26–180 1 | 332 |
Residual basic density (%) | - | 60 |
Holocellulose, lignin ratio (H/L) | 2.6 | 0.7 |
Sample No. | Sample No. | Volume Shrinkage (%) | Anti-Shrink Efficiency (%) |
---|---|---|---|
Pi1-Air | V03-01 | 23.07 | 0 |
Pi1-AlEt | V03-17 | 5.65 | 76 |
Pi1-K800 | V03-41 | 3.06 | 87 |
Pi1-LaTr | V03-28 | 2.63 | 89 |
Pi1-PEG1 | V03-35 | 2.03 | 91 |
Pi1-PEG2 | V03-32 | 3.05 | 87 |
Pi1-PEG3 | V03-20 | 3.37 | 85 |
Pi1-Sac | V03-45 | 2.38 | 90 |
Pi1-Sil | V03-42 | 5.67 | 75 |
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Stelzner, I.; Stelzner, J.; Gwerder, D.; Martinez-Garcia, J.; Schuetz, P. Imaging and Assessment of the Microstructure of Conserved Archaeological Pine. Forests 2023, 14, 211. https://doi.org/10.3390/f14020211
Stelzner I, Stelzner J, Gwerder D, Martinez-Garcia J, Schuetz P. Imaging and Assessment of the Microstructure of Conserved Archaeological Pine. Forests. 2023; 14(2):211. https://doi.org/10.3390/f14020211
Chicago/Turabian StyleStelzner, Ingrid, Jörg Stelzner, Damian Gwerder, Jorge Martinez-Garcia, and Philipp Schuetz. 2023. "Imaging and Assessment of the Microstructure of Conserved Archaeological Pine" Forests 14, no. 2: 211. https://doi.org/10.3390/f14020211