Water-Based Aerosol for Book Deacidification: Experimental Apparatus and Theoretical Interpretation of Results
Abstract
:1. Introduction
- The “Sablè” method is a French variation of the Wei T’o system invented by Richard D. Smith and developed by the National Archive in Canada. It was adopted between 1987 and 1989. The system consists of the insertion of open volumes, kept in a vertical position inside metal baskets, into an autoclave. The volumes are first dried at 45 °C and then impregnated for 10 min with a mixture consisting of ethoxy-magnesium carbonate and ethanol [21,22];
- The Bookkeeper® method, devised in 1985, is based on the use of magnesium oxide microparticles dispersed in perfluoroheptane and the addition of a surfactant. The volumes are placed on vertical supports and opened at an angle of 90° and then placed inside four reactors that operate sequentially and can treat 32 volumes in 2 h. The deacidifying product is inserted, after establishing vacuum conditions. This is one of the most popular methods for its speed of execution and relatively low costs. The Bookkeeper® method provides a considerable reduction of paper degradation and does not affect inks and book ligatures. However, it is reported in the literature that this method appears less efficient for the treatment of large-sized books due to the fact that the alkaline reserve is low and the deacidification is not very uniform. The solvent seems to have a low penetration capacity into the paper fibers, and some white patina appears on the surface [2,21,23,24];
- The “ZFB:2” method, devised in 2011, uses calcium carbonate and magnesium oxide dispersed in heptane. The volumes are not opened, and the process takes about four weeks [26];
- The “Papersave” method from Battelle Ingenieurtechnik GmbH and the “Papersave Swiss” method use magnesium and titanium ethyloxides dissolved in hexa-dimethyl siloxane and provide good penetration and an alkaline reserve, reducing the degradation of cellulose with aging. However, the treatment cannot be applied to leather covers, pergamene covers, patinated papers and newspapers. Inconvenient decreases in paper mechanical strength, discoloration, white deposits and ink bleeding have been observed [27].
2. Materials and Methods
2.1. Aerosol System
- The book “Studi di Enologia” del cav. Angelo Mona (Brescia—Pio Istituto Pavoni—1875), the title page of which is shown in Figure 4, after being weighed, was supported on the holder, as indicated in Figure 2b, and inserted into the flask. At the actual development stage of our homemade apparatus, only a limited number of pages could be homogeneously treated with the alkaline droplets. For this reason, only 12 (from 1 to 6 and from 91 to 96 pages) of the almost 200 pages of the book were kept wide open to facilitate a uniform deposition of the aerosol through a single nozzle. The other pages were kept firmly closed in order to exclude them from the deacidification process;
- The book, placed into the flask, was exposed to a dry air flux at the temperature of 45 °C for 15 min. Then, it was extracted from the chamber and weighed. The weight variation was 3.45%;
- The book was replaced in the chamber. A cloud of nebulized solution was fluxed above the open pages through the nozzle placed on the top hemisphere. The aerosol inlet was left to flow for 3 min, while the valve on the bottom of the flask was kept open to ensure a constant pressure in the flask;
- The book was removed from the flask and weighed in order to measure the amount of the absorbed basic solution and inserted back into the treatment chamber;
- Dry air at the temperature of 45 °C was let gently fluxed into the flask for 3 min, entering with the help of a small pressure gradient (around 0.05 atm) and exiting through the bottom open valve. The rehydration of the air gradually removed the absorbed humidity from the book. After the above dehydration cycle, the book was weighed. This step was repeated 5 times in order to bring the book to a constant weight;
- The pH on every treated page was measured in six different points, as described in Section 2.4, and the average value was recorded;
- The procedure described above, as defined in Steps 3 to 6, was repeated 8 times in order to reach a satisfactory pH value.
2.2. X-ray Fluorescence (XRF)
2.3. FTIR Spectroscopy
2.4. Powder X-ray Diffraction (PXRD)
2.5. Contact pH Meter
2.6. Artificial Aging
2.7. Colorimetry and Optical Microscopy
2.8. Determination of the Degree of Polymerization (DP)
2.9. Alkaline Reserve Determination
3. Results and Discussion
3.1. FTIR Results
3.2. PXRD Results
3.3. X-ray Fluorescence Results
3.4. pH Results
- A 40 μL volume of water droplets is dispersed on the paper to measure the pH, and droplets diffuse on the surface corresponding to the measure electrode surface (0.78 cm2);
- The total surface of the opened pages, hypothesized to be the only absorbers of the nebulized solution, is equal to 1560 cm2;
- The concentration of the Ca2+ ion in the nebulized solution is equal to 8.73 × 10−3. Simple calculations made on the assumption that the added calcium hydroxide dissolves completely in the water droplet dispersed under the pH measure electrode would lead to a theoretical value of the β factor equal to about 10−4; that is to say, a value one order of degree bigger with respect to that furnished by the fit of the titration curve. This apparent discrepancy can be explained, in our opinion, considering that a greater part of the added calcium hydroxide can react with the atmospheric CO2, during the drying stage of the paper, becoming calcium carbonate, which remains in the system as an alkaline reserve. On the basis of this hypothesis, the values of β could justify a contribution to the alkaline reserve of the order of about 0.15% of calcium carbonate with respect to the weight of the paper.
3.5. Colorimetric and Optical Microscopic Analysis Results
3.6. Cellulose Degree of Polymerization
3.7. Alkaline Reserve Results
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Wavenumber (cm−1) | Functional Chemical Groups | Chemical Compound |
---|---|---|
3680–3000 | OH stretching | Cellulose |
2900 | CH stretching | Cellulose |
2740–2700 | CH stretching | Cellulose |
2540–2510 | CO stretching | CaCO3 |
2230–2130 | CO stretching | CaCO3 |
1735 | C=O stretching | Cellulose |
1650–1635 | OH bending/adsorbed water | Cellulose and others |
1430 | CO stretching | CaCO3 |
1372 | CH bending | Cellulose |
1340 | CH bending | Cellulose |
1320 | CH bending | Cellulose |
1280 | CH2 twisting | Cellulose |
1174 | C-C stretching | Cellulose (and others) |
1130 | SO stretching asym | Ca(SO4)·2H2O |
1090 | CO stretching asym | CaCO3 |
1050–1015 | SO stretching | Ca(SO4)·2H2O |
870–880 | CO stretching asym | CaCO3 |
715 | CO stretching asym | CaCO3 |
670 | Ca-OH bending | Ca(SO4)·2H2O |
640–610 | Ca-OH bending | CaCO3 |
460–430 | Ca-OH stretching | CaCO3 |
PXRD Identified Compound | Common Name | 2θ (°) | N.° Ref. |
---|---|---|---|
KAl(SO4)2·12H2O | K-alum | 12.6; 17.9; 20.4; 31.2; 32.3; 34.7; 44.7 | R040134 |
KAl3(SO4)2(OH)6 | Alunite | 17.9; 25.7; 29.6; 39.4; 47.8 | R060430 |
FeO(OH) | Goethite | 21.0; 33.6; 34.7; 36.8 | R050142 |
Ca4Al6O12(SO4) | Ye’elimite | 23.5; 33.6; 36.3; 50.5; 56.6; 58.4; 60.5; 62.4 | COD 9009938 |
TiO2 | Anatase | 25.1; 37.7; 47.8 | R060277 |
CaCO3 | Calcite | 29.6; 39.4; 48.5 | R040070 |
NiO | Bunsenite | 37.7; 43.5; 63.5; 75.5 | R080121 |
Colorimetric | Pages Average | SD Pages | Ink Average | SD Ink | |
---|---|---|---|---|---|
Coordinate | Value | Value | |||
(a) Untreated | L* | 70.4 | 0.5 | 51.0 | 1.0 |
a* | −14.2 | 0.2 | 3.6 | 1.0 | |
b* | 16.2 | 0.2 | 16.0 | 0.5 | |
W | 71.8 | 0.7 | 45.3 | 1.2 | |
(b) Deacidified | L* | 69.8 | 0.7 | 50.7 | 0.8 |
a* | −15.4 | 0.3 | 3.0 | 0.4 | |
b* | 16.6 | 0.3 | 16.6 | 0.6 | |
W | 71.5 | 1.1 | 45.1 | 1.1 | |
Variation between b and a (deacidified − untreated) | ΔL* | −0.6 | 1.2 | −0.3 | 1.8 |
Δa* | −1.2 | 0.6 | −0.6 | 1.4 | |
Δb* | 0.4 | 0.5 | 0.6 | 1.1 | |
ΔW | −0.3 | 1.8 | −0.2 | 2.3 | |
ΔE* | 1.4 | 0.9 | 0.9 | 2.2 | |
(c) Untreated and aged | L* | 62.5 | 0.2 | 61.7 | 0.7 |
a* | −21.3 | 0.3 | −18.4 | 1.5 | |
b* | 20.8 | 0.1 | 18.5 | 0.8 | |
W | 64.2 | 0.5 | 61.4 | 1.7 | |
Variation between c and a (Untreated and aged − untreated) | ΔL* | −7.9 | 0.7 | 9.8 | 1.8 |
Δa* | −7.1 | 0.5 | −21.9 | 2.5 | |
Δb* | 4.5 | 0.2 | 2.5 | 1.4 | |
ΔW | −7.3 | 1.2 | 16.1 | 2.9 | |
ΔE* | 11.5 | 1.0 | 24.1 | 2.6 | |
(d) Deacidified and aged | L* | 67.8 | 0.2 | 52.9 | 0.5 |
a* | −18.3 | 0.4 | 2.7 | 0.2 | |
b* | 17.5 | 0.3 | 18.1 | 0.5 | |
W | 70.1 | 0.6 | 47.7 | 0.7 | |
Variation between d and a (deacidified and aged − untreated) | ΔL* | −2.6 | 0.7 | 1.9 | 1.5 |
Δa* | −2.9 | 0.7 | −0.9 | 1.2 | |
Δb* | 1.3 | 0.5 | 2.1 | 1.1 | |
ΔW | −1.7 | 1.2 | 2.4 | 1.9 | |
ΔE* | 4.1 | 1.0 | 2.6 | 2.0 |
Sample | DP |
---|---|
(a) Untreated | 825 ± 31 |
(b) Untreated and aged | 369 ± 26 |
ΔDP = A − B | 456 ± 57 |
Depolymerization (%) | 55 |
(c) Deacidified | 700 ± 37 |
ΔDP = A − C | 125 ± 68 |
Depolymerization (%) | 15 |
(d) Deacidified and aged | 568 ± 20 |
ΔDP = A − D | 257 ± 51 |
Depolymerization (%) | 31 |
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Chidichimo, G.; Crispini, A.; Tursi, A.; Basile, M.R.; Lania, I.; De Filpo, G.; Rossi, C.O.; Scarpelli, F. Water-Based Aerosol for Book Deacidification: Experimental Apparatus and Theoretical Interpretation of Results. Molecules 2021, 26, 4249. https://doi.org/10.3390/molecules26144249
Chidichimo G, Crispini A, Tursi A, Basile MR, Lania I, De Filpo G, Rossi CO, Scarpelli F. Water-Based Aerosol for Book Deacidification: Experimental Apparatus and Theoretical Interpretation of Results. Molecules. 2021; 26(14):4249. https://doi.org/10.3390/molecules26144249
Chicago/Turabian StyleChidichimo, Giuseppe, Alessandra Crispini, Antonio Tursi, Maria Rita Basile, Ilaria Lania, Giovanni De Filpo, Cesare Oliviero Rossi, and Francesca Scarpelli. 2021. "Water-Based Aerosol for Book Deacidification: Experimental Apparatus and Theoretical Interpretation of Results" Molecules 26, no. 14: 4249. https://doi.org/10.3390/molecules26144249
APA StyleChidichimo, G., Crispini, A., Tursi, A., Basile, M. R., Lania, I., De Filpo, G., Rossi, C. O., & Scarpelli, F. (2021). Water-Based Aerosol for Book Deacidification: Experimental Apparatus and Theoretical Interpretation of Results. Molecules, 26(14), 4249. https://doi.org/10.3390/molecules26144249