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Iron Gall Ink at the Agnes: Analysis of Iron Gall Ink in the Agnes Etherington Art Collection

Emily Cloutier 

The historic European art collection at the Agnes Etherington Art Centre is comprised of important 14^th to 19^th century pen and ink drawings. Given the time period of their creation, the media of a number of these drawings is likely to be iron gall ink which is known for its potential instability. This project surveys a selection of drawings from the collection to ascertain the presence of iron gall ink, characterize the ink recipe, assess the current condition of the drawings and provide long-term conservation recommendations. Studies have shown that copper ions contribute to a greater rate of oxidation than iron (II) ions.  Despite this, most accepted conservation treatments for iron gall ink are targeted for use with ferrous ions. More data on the metallic components of iron gall ink in heritage objects is necessary in order for the conservation community to assess the need for developing alternate treatment methods. Analysis of the ink in the Agnes’ collection involved indicator papers to detect the presence and amount of iron(II) ions. Ultra-violet photography was used to help characterize the extent of degradation and X-ray fluorescence (XRF) was used to identify and establish relative amounts of component metals. Results of the survey indicated that a majority of the ink drawings contained iron gall ink. Iron was the most commonly found metal in the inks, but copper, lead, zinc, arsenic and manganese were also detected. When classified following the condition rating system outlined by the Netherlands Cultural Heritage Agency, the majority of the inks that tested positive for iron content were in good condition.

Borane Tert-Butylamine Complex: Ageing Properties of Residual Materials Left in Treated Paper Objects

Vincent Dion  

Paper-based objects degrade following two major mechanisms: acid-catalyzed hydrolysis and oxidation of the cellulosic structure, with both processes contributing to embrittlement and yellowing. Oxidation has not received the same attention in conservation research resulting in fewer treatment solutions to prevent and remediate it.  Recent studies have pointed to the borane tert-butylamine complex as a promising reagent for the stabilization of cellulose due to its ability to selectively reduce carbonyl groups formed during oxidation back to original hydroxyl groups. A resulting effect of this stabilization is a brightening of the object suggesting it is also a suitable agent for mild and controlled bleaching, a procedure that has fallen out of favour in conservation due to the damaging effects of previous agents used.   While the complex has since informally entered the paper conservator’s toolbox, especially due to its compatibility in rigid gellan gum gel for use on fragile objects, the conservation literature lacks an agreed upon range of working concentrations and a set of directives for carrying out different steps of the treatment.  The project determines the long-term effects and potential toxicity of reaction products and residual reagent remaining in paper samples treated with the borane tert-butylamine complex. Accelerated ageing approximating long-term storage conditions is performed on rinsed and unrinsed samples treated with different concentrations of the reagent and changes are monitored using colorimetry based on the CIE L*a*b* colour space, TAPPI T 509 pH measurements, Fourier transform infrared spectroscopy and zero span tensile strength testing. The authors will report on whether the rinsing step is required after treatment, a procedure many fragile objects are unable to withstand, potentially making the complex a possible treatment for a range of situations where options are limited. This work will provide information needed by conservators to use the reagent with safety for the object and themselves.

Solvent Sensitivity of Water-Mixable Oil Paint

Kelsey Fox

Water-Mixable Oil paints (WMOs) were introduced in the 1990s as a less toxic alternative to traditional oil paints. Generally speaking, these paints are manufactured by introducing  hydrophilic additives to the linseed oil binder so that the paint is water reducible.  As a result, this project operated on the hypothesis that WMOs would be more sensitive to polar solvents than traditional oil paint. Currently, little is known regarding the aging process and behavior of WMOs. This study aims to determine to what extent commonly used solvents might swell and leach components in WMO paint in a typical cleaning scenario. Samples of Winsor & Newton Artisanâ„¢ WMO paints and Wintonâ„¢ linseed oil paints in two colors underwent thermal aging. The samples was immersed in distilled water for 24 hours and in ethanol and acetone for ten minutes. Fourier transform infrared spectroscopy (FTIR) and gas-chromatography (GC-MS) of distilled water, ethanol, and acetone extracts suggested the presence of several fatty acids, including palmitic, stearic, oleic, and azelaic acids. GC-MS of the Artisan paint also found compounds tentatively identified as polyethylene glycols (PEGs), which are known to be used as emulsifying agents. A second set of aged samples were swabbed with the three solvents for approximately one minute. There were significant changes in gloss and color for most of the samples, along with an overall loss of weight. Hardness testing was inconclusive. This study was meant to be an introduction into solvent resistance of WMO paints, and also sought to explore pigment type as potential factors in solvent sensitivity, though due to drying issues, only one pigment was useful in the study. While the ethanol extract removed more components from the Artisan film, analysis of visual changes do not suggest Artisan paint is any more prone to an increase in gloss than Winton films, and may even better resist color change. Further research is needed, but these results may be encouraging to conservators who encounter water-mixable oil paintings in the future.

Stabilization of a Flowing Alkyd and Oil Painting 

Patrick Gauthier

The National Gallery of Canada's collection houses a contemporary alkyd and oil painting with uncommon drying issues. More than six years after its completion, the paint is still viscous and highly sticky. In storage, the still fluid paint has been pulled down by gravity, resulting in disfiguring drips over a large portion of the image. Samples from the paintings were analyzed by the Canadian Conservation Institute (CCI) to better understand the various constituents of the artist's media and discern the causes of the drying problem. Similarities can be observed between the National Gallery’s painting and various published case studies of liquefying and softening artist paint. The aim of this research project was to find a way to harden the paint layers. With both the artist's and the gallery's approval, tests were run on samples from the original painting. Based on CCI’s findings and the experimental treatments tested in the literature, samples were exposure to ultraviolet radiation, driers solutions, and elevated temperature. Under magnification, cross sections of paint were cut to evaluate the physical stabilization of the paint. Photo-documentation recorded the colour and topography changes. Technical analysis, including gas chromatography-mass spectrometry and Fourier transform infrared spectroscopy, were performed by CCI to link the physical impacts of the treatments to the chemical changes of the paint samples. These experiments provide the basis for the development of proper treatment protocols to stabilize other paintings by this artist owned by institutions and private clients. This research expands the literature on liquefying and softening paint media to alkyds based paints by including a new case study.

The Marina Cave Wall Paintings: The Technical Analysis of 12th and 13th Century Byzantine Paintings from Northern Lebanon

Anne-Marie Guérin

The Marina Cave Wall paintings are located near Qalamoun, Northern Lebanon, and consist of five panels dating between the 12th and 13th century C.E. The panels represent religious themes including the life of Saint Marina and the Monk, a local saint from the region. The paintings are situated in a mountain recess overlooking Qalamoun and in the last few decades, have severely degraded due to fire, fluctuating relative humidity and vandalism. In the winter of 2015 a former student of the conservation program at ³ÉÈË´óƬ, Corine Soueid, brought samples from the Marina Cave wall paintings to the program. Students analyzed cross sections from the wall paintings in the context of their microscopy class. The following study is a continuation of the project, with the aim of determining the primary material and structural differences between the panels. This was achieved using Polarized Light Microscopy (PLM), Scanning Electron Microscopy - Energy Dispersive X-ray Spectroscopy (SEM-EDS), and Fourier Transform INfrared Spectroscopy (FTIR). This study contributes to the growing body of literature on Near-Eastern Wall painting materials and techniques of the Middle Ages. 

Scientific Analysis and Treatment of a William Sawyer Photograph Album

Geneva Iklé

The Queen’s University Archives has collection of artifacts that belonged to William Sawyer, a 19^th century painter and artist from Kingston, Ontario. One of those items is a photograph album that Sawyer assembled as a study album, which has been little examined. The album contains a variety of photographs which may represent Sawyer’s experimentations with these processes and photography in general. In addition, there is an accompanying journal of Sawyer’s notes on various photographic processes with which he experimented during the same period in which the photographs in the album were produced. The condition of the photographs and the album as a whole is compromised and an appropriate treatment proposal is necessary to ensure the safety of the album. In order to devise a safe and appropriate treatment plan for the album, the photographic processes that were used to create the photographs needed to be identified. This project used used a variety of analytic techniques, including stereomicroscopy, X-Ray Fluorescence (XRF), and Fourier Transform Infrared spectroscopy (FTIR), to identify the photographic process used to create each photograph and to develop a treatment approach based upon the type and the condition of each photograph. The photographs were identified as follows:  36 were albumen, 13 were salted paper and two were silver gelatin. One photograph of the 52 was unidentifiable, but an analysis of notes from the accompanying journal which Sawyer kept suggested a possible, but unusual, method for the production of this photograph. In addition, the project discussed the comparative utility of each of the analysis methods including, stereomicroscopy, and XRF and FTIR spectroscopy, in the identification of photographic processes.  

Investigation of Nitrile Gloves For the Handling of Silver Objects

Lisa Imamura

Many conservation labs have made the switch to disposable nitrile gloves for handling metals. Nitrile gloves are impermeable to the damaging residues from our skin and provide better grip than cotton. Based on methodology developed in a research project carried out at Queen’s University by William Hoffman in 2009, concerns about the effects of sulfur-containing accelerators on silver were investigated by testing four nitrile gloves. Accelerators are commonly used additives in the manufacture of nitrile gloves, but their use can be avoided if a combination of other additives performs the same cross-linking function. The four gloves included three standard nitrile gloves and one accelerator-free nitrile glove: Ansell TouchNTuff® Disposable Nitrile Gloves, Kimberly-Clark™ Purple Nitrile Powder-Free Exam Gloves, Showa Best™ N-DEX™ Medical nitrile gloves, and Showa Best™ N-DEX™ Free nitrile gloves. Experiments included the silver nitrate test for chlorides, the sodium azide test for reduced sulfur, Fourier Transform infrared spectroscopy of gloves and transferred residues, and Oddy-style accelerated ageing. Of the four nitrile gloves tested, two tested positive for chlorides, three tested positive for reduced sulfur, and three transferred residues that had visible impacts on metal coupons in high heat high relative humidity accelerated ageing conditions. The effects of the residues on silver, sterling silver, and copper are discussed.

Odour Reduction with 2-Hydroxypropyl- ÃŸ-Cyclodextrin and Its Colour Change Effect on Paintings

Spencer Montcalm

This study examines the effectiveness of smoke odour reduction on a painting on canvas using (2-hydroxypropyl)-β-cyclodextrin (HPbCD). Different concentrations of HPbCD were compared to a proprietary, commercially available product with cyclodextrins as the active component in odour reduction, Febreze^® Fabric Refresher: Free. Two methods of application by cotton swab and by spay of treatment solutions were compared. Odour analyses of control paint on canvas samples were compared with treated and not-treated samples by method of seven panelists ranking the odour intensity of the headspace created. Panelist suggested no preferable treatment solution or method of application, but did conclude a reduction of odour with all treatment solutions.  Six sample sets or varying paint material composition and age were created and treated with HPbCD and the proprietary solution. Treated paint samples were compared to controls by colourimetry using a Konica Minolta Spectrophotometer CM-700d under D65 illumination source to obtain colour readings in the CIE L*a*b* 2000 colour space. Readings were taken before and after treatment, and subsequently after artificial aging. Calculated ΔE values were below the threshold of human perceptibility both before and after treatment and when corrected for the effect of artificial aging, with minimal exceptions. This showed that treatment solutions of HPbCD and the proprietary solution do not adversely affect the colour of a variety of fully cured paint films immediately after application or after subsequent artificial aging.

Pacific Silvercloth: Recommendations for Its Use as a Scavenger in Silver Collections 

Gyllian Porteous

Pacific Silvercloth is a common commercial product used in conservation both as a scavenger and barrier to reduce the tarnishing of silver objects. This research builds on the past work of Queen’s Art Conservation graduate, S. Smith, who conducted a series of Oddy tests to determine the effects of ageing on Pacific Silvercloth. Though her results were inconclusive, her observations of silver plating and corrosion on silver, sterling silver, and copper coupons, despite separation of the metals from the Silvercloth by a barrier, raise an important question as to the possible negative effects of employing this commercial product in silver collections.  This study qualified the risks posed by Pacific Silvercloth through a tripartite study. Firstly, an extraction on Pacific Silvercloth was performed revealing the presence of nitrate and phosphate salts. Secondly, an accelerated ageing study was conducted, which placed new Pacific Silvercloth in direct contact with silver, sterling silver, and copper coupons, in a high humidity and high temperature chamber. Extent of corrosion was quantified using a combination of qualitative observations, colorimetry, and scanning electron microscopy (SEM). Results indicated no negative interactions specific to contact between Pacific Silvercloth and pure silver. Pitting, however, was observed on sterling silver coupons aged in contact with Pacific Silvercloth: use of a barrier layer therefore is recommended between Pacific Silvercloth and sterling silver objects. Finally, the two silver impregnated cloths made in house were compared as alternative sulfur-scavengers to Pacific Silvercloth: though the models showed a shorter lifetime than Pacific Silvercloth, a distinct colour change was observable indicating exhaustion of the cloth.

Microfade Tester versus Light Bleaching Unity: A Comparative Experiment 

Christina Prokopchuk

The purpose of this study is to compare the dose-response rate of bleaching (colour change) of historic papers using two different methods of light bleaching, dry/xenon arc lamp microfade tester (4.2 Mlx) versus alkaline water/fluorescent light bleaching unit (19000 lx), in order to determine how well microfade testing can predict the rate of light bleaching by artificial light sources.  Such diagnostic information, better equips the conservator in planning and carrying out an effective artificial light bleaching paper treatment by more accurately considering the unique characteristics of the object, while also adjusting for variables such as: aqueous immersion time, light source heat buildup, and the desired degree of brightening (whitening).  For this experiment, three samples sets were created from two discoloured paper objects of unknown history.  Three samples, one from each sample set, were tested with the microfade tester.  A separate series of samples, from each sample set, were treated by alkaline water/fluorescent light bleaching at varying 30-minute intervals, up to 480 minutes.  Data from the rate and degree of brightening of both the microfade tested samples and alkaline water/fluorescent light bleached samples were graphed and compared.  After experimentation the alkaline water/fluorescent light bleached samples showed a greater degree of bleaching at a lower amount of light dose exposure.  In this particular case, the microfade tester did not have the potential to be used as a pre-diagnostic tool for an artificial light bleaching treatment.