Article

Stabilising local areas of loss in iron gall ink copy documents from the Savigny estate

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Abstract

A local method for the stabilization of weakened iron gall ink areas in iron gall ink copy documents is presented. The special quality of iron gall ink copy process documents, made of thin, ink-permeable paper, is discussed, as well as the special quality of iron gall copying inks because these were modified by hygroscopic additives. These inks remain extremely water sensitive due to the additive and may suffer from ink corrosion. Selected analysis including iron(II) testing and micro pH extraction are reported. To prevent bleeding and to inhibit the progress of ink corrosion, the mechanical stabilization of weakened areas had to employ only minimal amounts of water. This involved coating Berlin Tissue (kozo-mitsumata fibre content) with gelatin, producing a prefabricated repair paper that is a variation of the well-known remoistenable tissue. The tissue is prepared in a separate step preceding its application on the object, and it is adhered with the aid of the suction table. The application of the remoistenable tissue is expedient, can be carried out with great precision, and minimises risks associated with the treatment and preservation of iron gall ink-corroded areas.

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... In this context, and because of the fact that in many cases local damage has to be treated, the development and the increased use of coated stabilizing papers (remoistenable and heat-set tissues) represents an interesting methodical approach. They allow for easier processing of the very thin Japanese tissue papers, a standardization of the adhesive quantity, and the minimization of the influence of moisture or better humidity control during the paper stabilization phase [7,8]. For this purpose, fabrication and processing technologies are helpful [7][8][9]. ...
... They allow for easier processing of the very thin Japanese tissue papers, a standardization of the adhesive quantity, and the minimization of the influence of moisture or better humidity control during the paper stabilization phase [7,8]. For this purpose, fabrication and processing technologies are helpful [7][8][9]. ...
... Two application methods were tested: application by brush, a traditional method in paper conservation, and using a film applicator, based on the positive results obtained with adhesive processing during the preparation of remoistenable tissues [7]. The suspensions were always applied with vacuum in order to quickly reduce the high water content. ...
Article
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Historical papers are often locally damaged by exogenous influences and/or have endogenously degraded paper areas. The stabilization of such papers is very important because further use of the object can cause additional damage. Different types of nanocellulose are interesting as a novel stabilizing materials for paper due to their close structural relation to the paper matrix. Therefore, the present study investigated whether the treatment of historical papers with nanocellulose suspensions is a novel method for paper stabilization. Two different types of nanocelluloses, bacterial cellulose and a mechanically nanofibrillated cellulose based on wood pulp, were tested with regard to their performance in stabilizing fragile papers. Concerning material handling and application in conservation steps, different ways to modify the suspensions were tested. The resulting suspensions were applied to historical papers from several centuries with different extents of damage. The paper-nanocellulose composites were characterized with regard to their optical and microscopic integrity and by physical and chemical analyses. The treatment of mechanical damage and the consolidation of weakened paper areas could be realized by the application of a nanocellulose suspension without an additional adhesive. The results of the treatment depend on the type of nanocellulose, on the paper material, on processing and application techniques. The paper discusses the applicability and stability of the differently prepared nanocellulose suspensions, also with regard to their mode of application and long-term performance. Advantages and limitations are addressed in detail.
... • Deacidification with various compounds • Boiling in water (Tse et al. 2005) • Paper splitting (Brückle and Dambrogio 2000) (see below) • Electrolysis • Radical scavengers • Ammonium caseinate treatment • Oxidation inhibitors • No treatment or consolidation only (Low 1994;Titus et al. 2009) There are several concerns in applying aqueous treatments to iron gall corroded paper, including ink solubilization and spreading, iron diffusion to noninked areas, loss of fragments of corroded paper, and of course long term effects, especially the issue of ''waking up'' the ink (Huhsmann and Hähner 2008;Neevel and Reissland 1997;Van Gulik and Kersten-Pampiglione 1994). Many colleagues advised against aqueous treatments, while others suggested that with caution and when the ink appears stable, aqueous deacidification is a possibility that may improve the condition of the artefact (Van Gulik and Kersten-Pampiglione 1994). ...
... A new alternative method for the evaluation of the effects of treatments of iron gall corroded documents is proposed by Kolar and Strlic (2004). Kolbe (2004) recommends the use of gelatine for resizing iron gall ink manuscripts, since according to his research it slows down ink corrosion, an opinion shared by Titus et al. (2009). This claim was not verified by later research (Potthast et al. 2008). ...
Article
The main paper conservation methods are presented, classified in the following categories: preparation of the intervention, disinfestation and disinfection/sterilization, surface/dry cleaning, wet cleaning, chemical stabilization, paper repairs, consolidation and strengthening. Treatment documentation is also discussed. The targets, the historical aspects, the general principles, the materials and equipment, the acceptance and criticism pertaining to each method are briefly reviewed, and the most important research for their evaluation is presented. Several paper stabilization strategies, such as deacidification and iron gall ink stabilization, applicable to paper are elucidated. Specific consolidation and strengthening methods for paper, such as lamination and paper splitting are also discussed. The review mainly focuses on the established methods, but experimental, abandoned or insufficiently documented methods are also included. Shortcomings and limitations of several methods were found in the literature, concerning health issues, limited effectiveness, adverse side-effects on the treated artefacts and restricted applicability.
... In treatments of strongly degraded verdigris it can be necessary to stabilize a tear from the recto side. Due to the water sensitivity of the pigments it was decided to use pre-coated Japanese tissue papers based on research and experience in the treatments of iron gall ink on paper (Titus et al. 2009). The adhesive layer of these papers can be activated with a minimum amount of moisture, by solvents or by heat (Pataki 2009, Anderson and Reidell 2009, Jacobi et al. 2011, Völkel 2012. ...
... The mixture of wheat starch paste and methylcellulose has been recommended for remoistenable tissues (Brückle 1996, Wagner 1996. Gelatine (Titus et al. 2009, Kolbe 2004) and the hydroxypropylcellulose ether Klucel® G (Anderson andReidell 2009, Pataki 2009) have been used to reinforce tears on papers with iron gall ink and verdigris as shown in the answers to the survey. Kolbe, Nguyen and Curtis discuss the properties of different types of gelatine and their use in conservation (Kolbe 2001, Nguyen 2005, Curtis and Uchida 2011. ...
Article
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Verdigris (copper acetate) has been frequently used in manuscripts, early printed books and on maps. Dyes and pigments from plants have been added to modify the colour. Depending on the mode of application, paper quality, size and environmental factors like light and humidity the green colour of verdigris can discolour to brown tones and chemically damage the paper carrier. Treatment options include the application of solutions to stabilize cellulose chemically and mechanical reinforcement of the brittle or broken papers with Japanese paper and adhesives. Samples of copper acetate in gum arabic on rag paper were pre-aged to induce moderate degradation of cellulose. Deacidification, antioxidant and complexing solutions were applied by airbrush or by brush. Japanese tissue papers were coated with different aqueous or non-aqueous adhesives and applied by activation with water, ethanol or heat. The effect of the coated tissue papers was visually and mechanically evaluated before and after ageing. This contribution gives an overview of the project and focuses on mechanical stabilization and the implications of results for conservation.
... This observation corresponds to an alteration of the size by iron gall ink, which is not yet completely understood. In addition, gelatin is currently used in paper conservation workshops for mending or for re-sizing fragile papers (or papers that have undergone washing) [27]. Moreover, it has been shown that a certain type of gelatin, used as resizing agent, induced a decrease of iron gall ink corrosion at the macroscopic and macromolecular scale [28,29], thus highlighting interactions occurring between gelatin and the paper/iron gall ink system. ...
Article
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Iron gall Inks corrosion causes paper degradation (browning, embrittlement) and treatments were developed to tackle this issue. They often include resizing with gelatin to reinforce the paper and its cellulosic fibers (of diameter approx. 10 µm). This work aimed at measuring the distribution of ink components at the scale of individual paper fibers so as to give a better understanding of the impact of gelatin (re-)sizing on iron gall ink corrosion. For this purpose, scanning transmission X-ray microscopy (STXM) was used at the Canadian light source synchrotron (CLS, Saskatoon). This technique combines nano-scale mapping (resolution of 30 nm) and near edge X-ray absorption fine structure (NEXAFS) analysis. Fe L-edge measurements enabled to map iron distribution and to locate iron(II) and iron(III) rich areas. N K-edge measurement made it possible to map gelatin distribution. C K-edge measurements allowed mapping and discrimination of cellulose, gallic acid, iron gall ink precipitate and gelatin. Three fibers were studied: an inked fiber with no size, a sized fiber that was afterwards inked and an inked fiber sprayed with gelatin. Analysis of gelatin and ink ingredients distribution indicated a lower amount of iron inside the treated cellulosic fiber, which may explain the beneficial effect of gelatin on iron gall ink corrosion.
... This observation corresponds to an alteration of the size by iron gall ink [14], which is not yet completely understood. In addition, gelatin is currently used in paper conservation workshops for mending or for resizing fragile papers (or papers that have undergone washing) [15]. Moreover, it has been shown that a certain type of gelatin, used as resizing agent, induced a decrease of iron gall ink corrosion at the macroscopic and macromolecular scale [16,17], thus highlighting interactions occurring between gelatin and the paper / iron gall ink system. ...
Preprint
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Iron gall Inks are known to promote paper degradation, thus jeopardizing the conservation of written Heritage. This phenomenon, also called iron gall ink corrosion, is not only governed by chemical reactions occurring between ink constituents and cellulose (the main constituent of paper) but also by the penetration of ink components inside the paper. This penetration depends on the ability of water and ink soluble components to migrate inside the sheet. This latter is composed of hydrophilic cellulosic fibers (of diameter approx. 10 µm) embedded in a size that lowers water affinity and thus makes it suitable for writing. This work aims to better understand the impact of gelatin size on iron gall ink corrosion by investigating the distribution of gelatin and ink components at the scale of individual paper fibers. STXM, a nano-scale mapping technique (resolution of 30 nm) that also allows NEXAFS analysis was used for this purpose. Fe L-edge measurements enabled to map iron distribution and to locate iron(II) and iron(III) rich areas. N K-edge measurement made it possible to map gelatin distribution. C K-edge measurements allowed mapping and discrimination of cellulose, gallic acid, iron gall ink precipitate and gelatin. Three fibers were studied: an inked fiber with no size, a sized fiber that was afterwards inked and an inked fiber sprayed with gelatin (to model the impact of conservation treatments that use gelatin as a re-sizing agent). Analysis of gelatin and ink ingredients distribution inside and outside the cellulosic fiber gave some clues to account for the limiting impact of gelatin on iron gall ink corrosion.
... Research indicates that type-B gelatin with a high or medium Bloom degree has a considerable capacity to protect paper by preventing migration of free ironII ions (Kolbe 2004). The gelatin-coated tissue (0.4% Type-B gelatin, 275 Bloom) was reactivated in situ, using a 3:1 ethanol-water solution (Pataki 2009;Titus et al. 2009). Figure 3 shows the difference between repairs done in 1987 and recent repairs. ...
... Pre-coated Japanese tissue papers (Pataki, 2009;Titus et al., 2009) proved to stabilize rag paper mechanically without inducing further damage after light and thermal ageing (Hofmann et al., 2015). When applied on the recto of coloured areas, thin papers, 2-3.7 g m −2 , with a matte adhesive coating, only compromise the visual appearance moderately. ...
Article
The results of a research project on verdigris on paper have been applied in the conservation of a celestial atlas and a series of printed books with images of cities in Renaissance time. Paper degraded by verdigris was chemically stabilized by applying a solution of benzotriazole, a copper complexing agent, in ethanol by brush from the verso. Tears and brittle areas were mechanically stabilized with pre-coated Japanese tissue papers. The copper ion content and the effect of complexation were monitored with self-prepared copper ion indicator papers. Paper samples with different concentrations of benzotriazole were light-aged to evaluate the effect of yellowing.
... The mechanical properties are only slightly improved by the aqueous treatment and the object will often have to be mechanically reinforced in a separate step. There are several descriptions of possible treatments of iron gall ink degraded papers based on the application of the Berlin Tissue (Martin et al. 2011;Titus et al. 2009). Investigations by Rouchon et al. (2012) and Desroches et al. (2012) present possible solutions for treating heavily degraded iron gall ink corroded documents favouring a float washing approach and also give a descriptive handling guidance how to wash and line affected documents. ...
Article
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Paper documents with severe iron gall ink corrosion are difficult to handle. While a defined treatment for the chemical stabilisation exists already, methods to improve the mechanical stabilisation have yet to be developed. The degradation of the selected objects was so advanced that the documents needed special attention concerning handling and mechanical re-enforcement. After a calciumphytate-calciumhydrogen treatment, documents were lined with light weight Japanese paper and gelatine. A workflow for treating severely degraded iron gall ink documents was developed. Since the removal of objects from the silk screen frames after the wet treatment proved to be too difficult, a PE-board was introduced as an alternative washing support. Most synthetic fleeces such as Hollytex or Paraprint adhere to its granulated surface by mechanical means. This makes PE-board a practical support during any wet treatment of paper-based objects.
... Since aqueous treatment is not appropriate for the treatment of copying books, no treatment has been shown to safely chemically stabilize the rampant iron gall ink corrosion in them. Currently, the most effective treatment for copying books is mechanical stabilization by mending or lining with a solvent-set or heat-set method (Ubbink and Partridge 2003; Antoine 2009; Titus 2009). In the last decade, a few projects have been undertaken to develop a treatment for water-sensitive objects that contain iron gall ink. ...
Article
This study investigates the conservation treatment options to preserve the treasured Smithsonian collection of letterpress copying books handwritten by Spencer Fullerton Baird (1823–1887), the second Secretary of the Smithsonian Institution. This study employs analytical techniques to investigate the complex nature of the materials, explores and evaluates treatment options with experimental procedures using artificially aged samples, and investigates best practices for the digitization of the materials. Technical analysis showed that iron II ion migration is a particularly severe problem in copying books and confirms a correlation between iron migration and the severity of ink corrosion. Several conservation treatments were conducted including anti-oxidant treatments, sizing, de-acidification, and paper splitting. One of the most promising treatments conducted is a non-aqueous anti-oxidant treatment using Tetrabutyl Ammonium Bromide [TBAB] in ethanol followed by non-aqueous de-acidification with magnesium oxide using the Bookkeeper spray and sizing with Klucel G in ethanol. Several imaging techniques were explored, and a simple and inexpensive set-up and procedure was found to give excellent results.
... However, when the mechanical properties of cellulose-based artifacts are lost upon aging, a reinforcement is needed, in addition to a deacidification process. For instance, a relining can be carried out on canvases [25], while the mending using Japanese paper and adhesives is usually selected for paper [26]. ...
Article
Hypothesis: Strongly degraded cellulosic artworks usually need deacidification and consolidation. Alkaline nanoparticles are known to be effective in neutralizing the acidity, while cellulose nanocrystals have the potential to be used as compatible and effective strengthening agents. Experiments: We have grafted cellulose nanocrystals with oleic acid using a CDI-mediated procedure, to increase their dispersibility in organic solvents, and synthesized Ca(OH)2 or CaCO3 nanoparticles via a solvothermal process. Grafted nanocellulose and alkaline nanoparticles were used to prepare ethanol-based “hybrids”. Prior to the application, the physico-chemical properties of nanocellulose dispersions and “hybrids” were studied by rheology and small-angle X-ray scattering. Findings: Cellulose nanocrystals were effectively grafted and stably dispersed in ethanol. It was shown that the use of ethanol as a dispersing media, and the addition of alkaline nanoparticles act in a synergistic way, increasing interactions between grafted cellulose nanocrystals, leading to the formation of clusters. These dispersions are thixotropic, a behavior particularly appealing to conservation purposes, since they can be applied in the liquid state, or, when a more confined application is required, they can be applied in a gel-like state. As a result of the application, an improvement in the mechanical properties of paper and an increase of pH were obtained.
... In most of the cases, reinforcement is also needed, which is usually devoted to stabilisation of the mechanical properties so as to allow manipulation and handling of the artefact. Depending on the original material, different approaches can be used, such as relining for canvases [16] or mending using Japanese paper and adhesives for paper [17]. ...
Article
Full-text available
The conservation of textiles is a challenge due to the often fast degradation that results from the acidity combined with a complex structure that requires remediation actions to be conducted at several length scales. Nanomaterials have lately been used for various purposes in the conservation of cultural heritage. The advantage with these materials is their high efficiency combined with a great control. Here, we provide an overview of the latest developments in terms of nanomaterials-based alternatives, namely inorganic nanoparticles and nanocellulose, to conventional methods for the strengthening and deacidification of cellulose-based materials. Then, using the case of iron-tannate dyed cotton, we show that conservation can only be addressed if the mechanical strengthening is preceded by a deacidification step. We used CaCO3 nanoparticles to neutralize the acidity, while the stabilisation was addressed by a combination of nanocellulose, and silica nanoparticles, to truly tackle the complexity of the hierarchical nature of cotton textiles. Silica nanoparticles enabled strengthening at the fibre scale by covering the fibre surface, while the nanocellulose acted at bigger length scales. The evaluation of the applied treatments, before and after an accelerated ageing, was assessed by tensile testing, the fibre structure by SEM and the apparent colour changes by colourimetric measurements.
... Ink corrosion is often accompanied by severe mechanical damage (cracks, fractures) which makes additional physical stabilization necessary (12,13). Hence, local support of damaged paper areas with Japanese papers, adhesives or remoisturizable tissues is usually applied depending on the degree of damage (14)(15)(16)(17). ...
Preprint
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Because of its acidic and oxidative nature, iron gall ink promotes the endogenous degradation of paper manuscripts. Mechanical damage in areas of concentrated ink application or along mechanically stressed edges or folds results in problems during storage and handling. So far, such strongly degraded areas have usually been locally stabilized with thin Japanese paper and adhesives. A new and innovative material – nanocellulose – is being evaluated as a stabiliser for manuscripts that have been degraded by iron gall ink. The aim of this study is to integrate the nanocellulose application into a multi-stage calcium phytate/calcium hydrogencarbonate treatment to combine deacidification and stabilization, thus avoiding an additional stabilization and drying step. Two differently fibrillated nanocelluloses were applied on manuscripts damaged by iron gall inks in different treatment steps. The newly formed, interlinked network of nanocellulose and paper was characterised before and after accelerated ageing in closed vials. The effects on the paper cellulose were analysed by size exclusion chromatography and light scattering with carbonyl group profiling to follow cellulose hydrolysis and oxidation pathways. In addition, the migration behaviour of iron ions was examined by laser ablation coupled with metal analysis. This paper discusses the applicability and stability of nanocellulose on paper damaged by iron gall ink with regard to its long-term performance. Advantages and limitations are covered in detail.
... Klucel ® G in ethanol). > Preparing a 'Remoistenable Tissue' to transfer a minimal amount of solvent (Brückle 1996;Wagner 1996;Titus et al 2009: 33-38, Pataki 2009van Velzen and Jacobi 2011: 36). ...
Article
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Local mending of ink-corroded areas with a water-based adhesive bears one serious risk: too much moisture transports invisible, detrimental compounds like iron(II)ions and acids out of the ink lines into surrounding paper areas, spreading ink corrosion. Several common mending techniques are compared, the least detrimental was further developed to an effective, safe and applicable conservation method for ink corroded papers. A novel way to control any aqueous mending technique for iron gall inks was developed and is available on the market.
... Ink corrosion is often accompanied by severe mechanical damage (cracks, fractures) which makes additional physical stabilization necessary [23,24]. Hence, local support of damaged paper areas with Japanese papers, adhesives or remoistening tissues is usually applied, depending on the degree of damage [25][26][27][28]. In the case of severely impaired manuscripts, several authors suggested lining the documents with Japanese paper directly after aqueous or chemical treatment [18,23,24,29]. ...
Article
Full-text available
Abstract Because of its acidic and oxidative nature, iron gall ink promotes the endogenous degradation of paper manuscripts. Mechanical damage in areas of concentrated ink application or along mechanically stressed edges or folds results in problems during storage and handling. So far, such strongly degraded areas have usually been stabilized locally with thin Japanese paper and adhesives. A new and innovative material—nanocellulose—is being evaluated as a stabilizer for manuscripts that have been degraded by iron gall ink. The aim of this study is to integrate the nanocellulose application into a multi-stage calcium phytate/calcium hydrogencarbonate treatment to combine deacidification and stabilization, thus avoiding an additional stabilization and drying step. Two different types of fibrillated nanocelluloses were applied on manuscripts damaged by iron gall inks in different treatment steps. The newly formed, interlinked network of nanocellulose and paper was characterised before and after accelerated degradation in closed vials. The effects on the paper cellulose were studied by size exclusion chromatography and light scattering with carbonyl group profiling to follow cellulose hydrolysis and oxidation pathways. In addition, the migration behavior of iron ions was examined by laser ablation coupled with metal analysis (ICP-MS). This paper discusses the applicability and stability of nanocellulose on paper damaged by iron gall ink with regard to its long-term performance. Advantages and limitations are covered in detail.
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Paper is still the most important carrier of information and knowledge in the form of books, journals, documents of historical value located in libraries and archives. Being a material of biomass origin it is subject to chemical, physical and biological degradation. For many decades it has been accepted that the main factor contributing to the paper degradation is acid hydrolysis and several modes of deacidification have been elaborated and successfully applied to paper aimed at slowing down its degradation and preserving its quality. A less attention has been devoted to oxidative modes of paper degradation. This minireview is focused just on these modes. In particular, oxidation involving reactive oxygen species and reactions catalyzed by transition metals species are dealt with. Oxidation of paper induced by iron-gall inks in documents of historical value is discussed in more detail due to importance of such documents as part of cultural heritage of mankind.
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For the aqueous treatment of iron gall ink corrosion using calcium phytate and calcium hydrogen carbonate, a standardized work procedure is presented suitable for single page treatment. This standardized procedure was developed specifically for the stabilization of autograph manuscripts from the Savigny estate, that is, for German handwritten documents, letters and manuscripts from the 18th and 19th centuries. The work process involves eleven steps, of which three concern the preliminary examination and eight the actual treatment itself. The requisite materials for the implementation of this procedure, as well as for its step-by-step execution, are compiled in a systematic description for the conservation practice. The eleven steps consist of: the visual characterization of the ink (1), the testing for the iron ions (2), the test of the wettability of the object in question (3); if it is decided to pursue treatment: humidification (4), wetting (5), washing (6), the binding of free iron ions with a calcium phytate solution (7), the introduction of an alkaline buffer by means of calcium hydrogen carbonate (8), the strengthening and mechanical stabilization via a treatment using a dilute gelatin solution (9), transfer to a drying stack (10) and finally the drying of the objects under light weight (11). Individual parameters, such as the time interval between humidification and wetting, as well as the creation of a slight suction during double-screen washing can be adapted to the material properties and the condition of the objects without compromising the effectiveness of the treatment. The application of this treatment takes into account the specific material properties of for ink-corroded documents. For this reason, there is always a preliminary decision to be made, in cooperation with those responsible for the collection, either for or against an aqueous treatment. The risk that remains after such deliberation in case of an aqueous treatment is to be assessed and clearly demonstrated prior to treatment via a standardized preliminary evaluation.
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Copies of documents have been made on copy presses since 1780. For the process, documents were written with special copying ink and pressed whilst moist onto very thin and usually smooth, unsized paper that would accept the ink. Due to their composition the inks are sensitive to water and sometimes exhibit damage within the ink lines. The history and manufacture of copies is especially significant with regard to conservation and storage of these documents. Conservation interventions can have severe consequences if the documents have not been clearly identified as copy press copies in advance of treatment. In order to assist the conservator the identification characteristics of historical copies are represented in this paper.