Professional Documents
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Measurement
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a r t i c l e i n f o a b s t r a c t
Article history: The manuscript studied here dates to 19th century, and consists of paper pages and leather
Received 14 June 2010 bookbinding. This study aims to use analytical techniques in order to identify the compo-
Received in revised form 10 May 2011 nents of the manuscript and to explain its deterioration process. Visual assessment, isola-
Accepted 21 June 2011
tion and identification of fungi, pH measurements, and investigation of the surface
Available online 29 June 2011
morphology by a scanning electron microscope (SEM) were used to explain paper and
leather deterioration. X-ray diffraction with EDAX, Fourier Transform Infrared Spectros-
Keywords:
copy (FTIR), and chemical analysis were used to identify pigments, binder of pigments,
Paper
Leather
ash, lignin, and the a-cellulose content of papers. The shrinkage temperature measurement
Microscopes was used to explain the deterioration process of leather. SEM was used to identify the type
XRD of animal skin used for the bookbinding and high performance liquid chromatography
EDAX (HPLC) was used to identify the vegetable tanning material used with the bookbinding.
Microorganisms The results revealed that the ink used was a mixture of carbon with iron gall. The pig-
Chemical analysis ments used on the paper were gold leaf or gold shell, cobalt oxide, and mercuric sulfide
HPLC for the gold, blue and red colors respectively. Sodium chloride was the main salt crystal-
lized on the surface of paper. Calcium carbonate was the filler used in the paper making
process. Cotton fibers may have been used as a raw material in the creation of paper.
The values of the shrinkage temperature and pH were lower than in normal conditions,
indicating that the leather bookbinding suffers from deterioration. Aspergillus sp., and
Penicillium sp. were the most dominant fungi found on the manuscript. Goat skin was
identified as the animal skin of the bookbinding, and Acacia Arabica was identified the
tanning material used with the bookbinding. The condition of the manuscript studied with
its components play an important role in its deterioration.
Ó 2011 Elsevier Ltd. All rights reserved.
0263-2241/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.measurement.2011.06.017
G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617 1607
bookbinding are caused by poor handling, poor storage and surrounding environmental damages, especially from
methods, inappropriate display methods, wear and tear salts, such as sodium chloride.
from repeated use, chemical changes in the materials mak-
ing up the leather objects, chemical changes caused by 3. Material and methods
atmospheric pollutants and chemicals in contact with the
leather objects, and a combination of any or all of these For the determination of materials used with the man-
(http://archive.amol.org.au) [8]. uscript and to explain the deterioration processes, all the
Chemical deterioration of leather occurs through two analytical techniques used in this study (pH, SEM, EDAX,
competitive and interactive chemical mechanisms, X-ray diffraction, FTIR, measurement of the shrinkage
oxidation and acidic hydrolysis [9]. Oxidation is generally temperature, HPLC and chemical analysis of paper) were
caused by free radicals generated by heating, UV light, considered micro-destructive techniques because a few
and SO2 and NOx pollution. The side chains of some amino micrograms are needed and can be collected from the loose
acids are initially involved, but oxidation can also occur in and separated fibers from the manuscript. The micro-
the backbone of collagen through the rupture of N–C cova- destructive techniques used were selected to obtain a sig-
lent bonds [10]. Hydrolysis is catalyzed by both hydroxyl nificant identification and to obtain the optimum amount
and hydrogen ions, especially when atmospheric pollu- of information concerning the materials used. The analyti-
tants such as SO2 and NOx act in conjunction with air cal techniques used were more effective in explaining the
humidity, and cleavage of peptide bonds disrupts the deterioration processes of the manuscript.
hierarchical structure of collagen [10]. Gelatinization, in
further denaturation and aggregation, leads to the irrevers- 3.1. Visual assessment
ible formation of a heavily hydrated gel matrix. Partially
degraded collagen is especially susceptible to gelatiniza- Visual assessment, by the critical eye of the author, was
tion in warm, damp environments, since H-bonds are applied to determine the aspects of deterioration found on
exposed to the action of water [10]. the manuscript’s paper and leather. This method is very
The development of specific analytical techniques effective because the causes and mechanism of deteriora-
improves the procedures to authenticate patrimonial ob- tion may be easily identifiable. The critical eye of conserva-
jects made from collagen and cellulose-based materials tor can also determine the most effectiveness techniques of
as well as the methods to study the impact of the environ- analysis, which should be applied for identifying the condi-
mental factors. During the last few decades, many methods tion of the manuscript studied.
of the analysis of paper and leather have been used for the
identification of the material compounds and for the esti- 3.2. Isolation and identification of fungi
mation of the deterioration processes. For paper, Ververis
et al. [11] used chemical analysis for the determination Sterile swabs were used to wipe the surface of the paper
of hemicelluloses, lignin, and ash content in paper. Strlič and the leather to isolate the fungi, especially in the
et al. [12] mentioned that the measurement of the pH of contaminated area. Isolation was made directly in the
historical paper plays an important role to explain the laboratory after wiping process. The fungi were isolated by
mechanism of deterioration. Many authors used different wiping the swabs on culture medium of potato-dextrose-
analytical techniques for the identification of pigment used agar (PDA) then incubated at 28 °C for 1–2 weeks. Czapek
on paper manuscripts [1,13,14]. FTIR was used for the yeast extract agar (CYA) composed of K2HPO4 1 g, Czapek
identification of ink binder [15,16]. For the leather book- concentrate 10 mL, yeast extract (Difco) 5 g, agar 15 g, dis-
binding, the measurement of the shrinkage temperature tilled water 1 L [25]. The source of carbon (sucrose) was
is vital and is considered one of the most important tools not used and the paper and leather samples were the source
used for the determination of leather deterioration [16– of carbon. Seven-day cultures on Malt Extract Agar (MEA),
21]. The measurement of leather pH reveals the state of which consists of maltose 12.75 g, dextrin 2.75 g, glycerol
leather inside a museum or in storage [7,22]. Microbiolog- 2.36 g, peptone 0.78, agar 15 g and distilled water 1 L, was
ical studies and investigation of the surface morphology used for identification of isolated fungi [25]. Fungi colonies
are also very important for the estimation of the deteriora- were identified according to Raper and Fennell [26], Barnett
tion process for paper and leather [22–24]. and Hunter [27], and Watanabe [28]. The balance used to
This study aims to identify the materials used in the man- weight the components of media used for the isolation
uscript studied, apply the most effectiveness techniques of and identification of fungi was calibrated using standard
analyses for the determination of paper and bookbinding weights traceable to SI (International Measurement Sys-
degradation, and explain the mechanism of deterioration. tem). All glass wares used here were calibrated and have
traceability to SI. Isolation and identification of fungi were
carried out at microbiological laboratories, the Department
2. Historical background of Microbiology, Krakow University of Agriculture, Poland.
The manuscript was found in the library of Ahmed Al- 3.3. pH measurement
Bajam Mosque, located in Mehalit Marhoum Village, Tanta
City, Egypt. It was discovered during the destruction of the 3.3.1. Determination of leather bookbinding pH
mosque. It dates back to 19th century, and contains part of The pH value of leather was determined by Abdel-Mak-
the 28th chapter of the Holy Qur’an. It suffers from ground soud [22] in accordance with Wouters et al. [29] and the
1608 G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617
National Library of the Netherlands [30] but with some instrument throughout the routine maintenance to achieve
modifications. Samples (0.025 g) of leather bookbinding best performance. For EDAX analysis, link ISIS Oxford was
is enough for the measurement and was taken mechani- used. The quantitative method used was ZAF. The results ob-
cally, in the form of loose fibers, from as near as possible tained from EDAX were automatically normalized to 100%.
to the damaged area on the surface (grain) of the leather. EDAX was calibrated by the standard nickel rod purchased
The sample was cut into very small pieces. The pH was along with the instrument. The Calibration was conducted
measured approximately 6 h after the suspension had been by count calibration mode in the software. EDAX were also
prepared to allow the ions to migrate into the solution. The performed at the Scanning Electron Microscope Laboratory,
measurement of pH value of the bookbinding was done The central Laboratory unit, Assiut University, Egypt.
using a 315i InhaltsverzeTechnische Werkstatten GMBH
& Co. UG provided with a combination electrode and cali- 3.5. X-ray diffraction and EDAX analysis of ink and pigments
brated to between 2 and 7, at 21–22 °C. The calibration used
of pH meter was done by immersion of the pH electrode
firstly in distilled water and secondly into buffer solutions The ink samples of red, blue, and gold colors were
(2 and 7). The model numbers of the technical buffers used analyzed by X-ray diffraction using Compact X-ray Diffrac-
was 108,708 for the first buffer (pH 2) and 108,706 for the tometer System PW 1840 – Analytical Equipment – Philips
second buffer (pH 7). After each measurement of the buf- – Eindhoven – the Netherlands (CU Ka radiation with
fers used, the pH electrode was rinsed in distilled water Ni-filter). Calibration of X-ray diffraction was done by
followed by immersion in the buffer solutions. The calibra- using a silicon standard sample. The tube of copper was
tion of pH meter was ok when the reading of pH meter was used for the measurement. The mA and kV were adjusted.
stable and closed to the selected buffer value. The mea- The mA control was adjusted until the meter indicates at
surement was performed in the Central Laboratory, Faculty 50 mA. The kV was increased to 40. Two reflection angles
of Archaeology and Anthropology, Yarmouk University, for the silicon standard should appear. One should appear
Jordon. at 28.44 h and the other appears at 56.12 h. By this opera-
tion, the instrument was ready for the measurement. The
3.3.2. Determination of paper pH measurement was performed at the Laboratory of X-ray
The measurement of the pH of the paper was in accor- diffraction analysis, Conservation Department, Faculty of
dance with Strlic et al. [31] with little modification. A drop Archaeology, Cairo University, Egypt. Link ISIS Oxford
of distilled water was placed on the paper of the manu- was used for EDAX analysis. The results obtained from
script, the flat-surface combined pH electrode pressed EDAX were automatically normalized to 100%. It should
against it, and the pH value read after being constant for be mentioned that all the decimal points obtained from
30 s. The results are an average of five determinations. EDAX were effective. EDAX were performed at the Scan-
The pH-meter Metrohm 691 (Metrohm, Herisau, Switzer- ning Electron Microscope Laboratory, The central Labora-
land) was used with flat combined electrode (Metrohm tory unit, Assiut University, Egypt.
6,0253.100). Before the measurement of pH, the sensor
was calibrated using the provided buffer solutions accord- 3.6. Identification of pigment binder by FTIR
ing to the instructions placed nearby the pH meter, pH
measurement was calibrated using three two standard In order to identify the binder of the ink and pigments
buffers (Metrohm buffers) of 4 and 7. The electrode with used on paper of the manuscript, a few milligrams of the
immersed assembly in the first buffer and the temperature ink and pigments taken from the manuscript was ground
measured was 25 °C when the reading was stable and into a powder and then mixed with KBr and placed in a
closed to the selected buffer (pH 4), the measurement of DRIFT cell. The measurement range is between 4000 and
the first buffer was finished. The electrode was rinsed 400 cm1. The examination was done by using an infrared
again in distilled water. The pH electrode was rinsed into instrument (Bruker) to identify the binder used with black
the second buffer solution. When the reading of pH was ink and pigments. Before measurement, the standard sam-
closed to the second buffer (pH 7), this means that the ple provided by the company of instrument is polystyrene
pH meter was ready to measure the pH value of the histor- film. According to the instruction of the manufacturer, the
ical paper samples. The measurement was performed at ideal measurement of this sheet must be placed in the
the Organic Chemistry Laboratory, Department of Chemis- same position and intensity as the standard spectrum
try, Krakow University of Agriculture, Poland. saved at the library of the instrument. Before measurement
process, the background measurement was performed in
3.4. Investigation of the surface morphology by SEM and EDAX order to reduce the effect of the atmospheric carbon diox-
analysis ide and water vapor. FTIR was performed at the Laboratory
of FTIR, Microanalysis Laboratory, Faculty of Science, Cairo
A scanning electron microscope, JEOL-JSM-5400LV, was University, Egypt.
used for the investigation of the surface morphology of the
paper and the leather. The fine gold coating (JEOL-JFC- 3.7. Measurement of hydrothermal stability of leather
1100E) was used. All samples were photographed by SEM bookbinding
at the Scanning Electron Microscope Laboratory, The central
Laboratory unit, Assiut University, Egypt. This laboratory This measurement was in accordance with Larsen [7]
achieves the traceability via the manufacturer of the but with little modification. A sample of about 0.3 mg fiber
G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617 1609
from the corium part of the leather was wet with distilled before chromatography, an aliquot of the water/acetone
water for at least 10 min on a microscope slide. Then the extract was diluted fivefold with methyl alcohol. Extract
samples were transferred to another slide with acetone analyses were performed immediately. The results pre-
for at least 30 min and again transferred to distilled water sented here are those recorded for the bookbinding and
and glycerin. The fibers are separated, air bubbles were Acacia Arabica powder because of their similarity. The
removed with a needle, and the fibers were well dispersed samples were analyzed using a Varian Pro Star, 3 lm,
on the slide and secured. The microscope slide was placed 100 6.4 mm column; pump (Varian Pro Star 230); 990+
on the hot table. The gradient heat controller was cali- photodiode-array detector (Varian Pro Star 335); data
brated at 22 °C, as well as 80 °C to achieve the traceability handling using Star chromatography WS (work station)
to ITS 90 (International Temperature Scale). The timer was version 6; 20 lL sample loop; flow rate: 1.2 mL/min; ana-
calibrated using a calibrated stope watch traceable to lytical wavelength 280 nm (other postrun selections possi-
NIST–USA (National Institute for Standard and Technol- ble between 200 and 800 nm); flow scheme (A = methanol,
ogy). The measurement of hydrothermal stability was B = water, C = 50 g/L phosphoric acid in water): 10A/80B/
performed at the Analysis Laboratory, Animal Physiology 10C for 2 min, linear gradient to 90A/10C over 17 min,
Department, Jagiellonian University, Poland. 90A/10C for 3 min; temperature 21 °C. The identification
of tanning was performed at the Analytical chemistry
3.8. Identification of animal skin used for the bookbinding Laboratory, the Department of Chemistry, Yarmouk
University, Jordan.
The surface examination by a scanning electron micro-
scope, JEOL-JSM-5400LV, was used to identify the type of 3.10. Chemical analysis of paper
animal skin used for the leather bookbinding. A specimen
of about 2 mm 4 mm was aligned on a stub, with the hair 3.10.1. Ash content
follicles opening towards the stub as viewed under the The ash was estimated by igniting in a muffle furnace a
microscope. The specimen was mounted on stub and weighed sample in a porcelain crucible for 30 min at
coated with fine gold. The nominal thickness of the sample 400 °C, then continuously for 45 min at 850 °C and then
was 20 nm. The study of Haines [32] was taken as a refer- gravimetrically estimated (Tappi standard 211-om 85)
ence in order to be compared with the identified skin from [35]. The percentage of ash was calculated from:
the bookbinding studied. SEM was performed at the Scan-
ning Electron Microscope Laboratory, The central Labora- Weight of ashðafter ignitionÞ
Ash % ¼
tory unit, Assiut University, Egypt. Weight of dry paper sampleðbefore ignitionÞ
100
3.9. Identification of tanning material by High Performance
Liquid Chromatograpy (HPLC) Muffle furnace was calibrated at 400 °C, 850 °C and
1000 °C using calibrated thermocouple that has traceabil-
The samples and analytical procedure for High Perfor- ity ITS 90 (International Temperature Scale). Ash content
mance Liquid Chromatograpy (HPLC) were in accordance was determined at the Cellulose Laboratory, Department
with Wouters [33], and Abdel-Maksoud [34]. HPLC system of Cellulose and Paper, National Research Center (NRC),
was calibrated for the flow rate using calibrated stopwatch Egypt.
(traceable to standard cesium clock that has direct trace-
ability to SI measurement system at NIST–USA) and volu- 3.10.2. Lignin
metric flask traceable to Si Measurement system. The An exact weight of 1 g of the air-dried sample was
flow rate uncertainty was found 0.02%. Regarding the par- treated with 15 mL of 72% sulfuric acid for 2 h at room
ticle sizes, the system was calibrated using the standard temperature. The material was then transferred into a 1 L
polystyrene dispersed particulates in aqueous system of flask, diluted with 560 mL of distilled water, and boiled un-
sizes 2 and 3 lm. Photometric scales was calibrated using der reflux for 4 h. The lignin was filtered on a previously
standard [0.1 N] potassium dichromate solution and the weighed dry ashless filter paper, and then washed with
total expanded uncertainty was found ±0.20% with cover- hot distilled water till neutrality. The filter paper and lignin
age factor of two to give confidence level of 95%. were transferred to a weighted porcelain crucible and
Samples were prepared from the bookbinding and from dried in an oven at 105 °C (The drying oven was calibrated
Acacia Arabica, supplied by the Commercial Tannery, Cairo, at 105 using calibrated glass thermometer traceable to ITS
Egypt, and mimosa and quebracho powders, supplied by 90) till constant weight.
Abd El-Rahman M. Harraz. Agricultural Seeds, Spices and For ash correction, the contents of the crucible were
Medicinal Plants Company, Cairo, Egypt. A sample of dry ignited at 400 °C for 30 min and then at 850 °C for further
vegetable-tanned bookbinding weighing 50 mg was col- 45 min. The weight of the ash was subtracted to give the
lected from loose fibers around the bookbinding. 100 mg weight of the pure lignin. Lignin percent is calculated from:
of each of the new tanning powders was weighed and
weight of lignin Weight of its ash
soaked in a solution of water/acetone (1/1, v/v) in closed Lignin % ¼ 100
Weight of moisture free pulp
vessels at room temperature for 24 h. The volume of the
extract liquid was 20 mL for 20 mg of acclimatized vegeta- Determination of lignin was performed at the Cellulose
ble tanned bookbinding and tanning powder, weighed Laboratory, Department of Cellulose and Paper, National
after conditioning for at least 48 h at 65%RH and 20 °C. Just Research Center (NRC), Egypt.
1610 G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617
Fig. 1. Aspects of deterioration found on Qur’an manuscript: (1A and 1C) aspects of deterioration of a bookbinding, (1B and 1D) aspects of deterioration of
papers.
process, and external factors such as environmental These elements are responsible for the combustion,
conditions. fermentation, hydrolysis, and the oxidation of books and
In the paper making process, especially in the late 19th documents. The atmosphere, especially of industrialized
century, paper deterioration was further hastened by the zones, also contains a series of impurities, the results of
introduction of mechanically produced ground wood pulp. pollution or contamination, such as carbon dioxide, nitro-
These products, frequently not chemically purified, re- gen dioxide, and sulfur dioxide. By-products of industrial
sulted in weaker paper and the additional formation of combustion which, catalyzed by metals, react with water
acids and peroxides that promote the aging process. The to form acids. The most important of these is sulfuric acid,
paper made of ground wood pulp contained lignin, which which leads to total weakness in the paper [42].
degrades to form acids and peroxides that further promote
the aging process. It can be added that the using of alum- 4.4. Investigation of the surface morphology by SEM and EDAX
rosin sizing, especially in the mid 19th century onward, analysis
causes the paper to eat itself from the inside out. In reac-
tion with the natural residual moisture in paper, alum Investigation of the paper by a SEM showed that fibers
gradually breaks down to sulfuric acid, which attacks the of the original paper (Fig. 2A) seem to be from cotton.
long chains of cellulose, breaking them into shorter and Small amounts of filler materials appeared between the fi-
shorter fragments. The paper steadily weakens until it fi- ber structures. Some contaminations (Fig. 2B) from stains
nally becomes so brittle that it is unusable [41,42]. and dusts were noticed on the surface of the original paper.
The external factors contain a series of chemical ele- Damages caused by insects (Fig. 2C) appeared in the form
ments such as oxygen, nitrogen, ozone, and carbon dioxide. of bores, and the tearing of paper fibers and deformation
1612 G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617
Fig. 2. Investigation of deteriorated of paper by SEM: (A) original paper manuscript; (B) original paper with some stains and dusts; (C) original paper with
damaged caused by insects; (D) restoration paper; (E) exterior lining paper; (F) interior lining paper.
of the paper appearance was also noted. The restoration the surface of leather. Calcium was found in the high per-
paper (Fig. 2D) displayed advanced deterioration. Many centage of 27.77%. Magnesium, aluminum potassium, and
forms of deterioration such as dust, stains, and the random silicon were also found, and this may indicate that the
distribution and destruction of the fibers were recorded. ground consisted of lime with traces of clay minerals and
For the exterior lining paper (Fig. 2E) dust and stains cov- sand. Sulfur may act as a contaminant from the surround-
ered the surface of paper and the fiber structures is unrec- ing environment or from the manufacturing process of
ognizable. The amount of filler materials seems to be leather bookbinding. Sodium also was found and may have
greater than in the original paper. For the interior lining derived from the burial environment of the manuscript.
paper (Fig. 2F) accumulated dust and large amounts of fil- The sodium was further identified as sodium chloride
ler materials were noted. and it was found on all of the paper pages of the manu-
Investigation of leather bookbinding (Fig. 3) showed the script. This type of salt led to the erosion of the surface
destruction and random distribution of the fiber struc- of both the papers and leather. The source of sodium chlo-
tures, erosion of the fibers, and many bores. There was to- ride in the case study may be from saline in the soil and
tal deformation of the surface morphology. groundwater, air pollution, and human contaminants. Salt
The results obtained by EDAX analysis of stains found damage takes place when evaporation takes place, leaving
on leather bookbinding supported the fact that the manu- the salt to grow as crystals within the pores of the leather
script was found under the ground of the destroyed mos- or paper. The growth pressure of developing crystals is
que, and this was reflected by the elements present on very high and sufficient to cause erosion on the leather
Fig. 3. Investigation of the surface morphology of leather bookbinding by SEM and analysis of stain found on the leather surface by EDAX.
G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617 1613
or paper sheets. The final result is total deformation of the lightproof. It needed a binder like gum Arabic [43]. Sodium
surface. chloride was also identified, and was found with paper
support of the manuscript.
4.5. X-ray diffraction and EDAX analysis of ink and pigments
used 4.5.4. Black ink
Iron gall ink is the most important ink used in old
4.5.1. Gold color manuscripts. Many recipes exist for manufacturing black
It was clear from X-ray diffraction (Fig. 4A) and EDAX ink (Fig. 4D), and usually contained a mixture of carbon
(Table 1) that the gold color was from gold leaf or gold and iron gall. Therefore a wide range of different compo-
shell. Gold leaf was applied before any painting was done nents and impurities exist for historical inks. The results
because it would stick to the medium used to suspend from the analysis of black ink showed the use of iron and
the paints. Shell gold was also used to illuminate manu- sulfur (iron sulfate), as seen in Table 1. In this study the
scripts, it is made of powdered gold suspended with ink used may be a mixture of carbon and iron gall ink.
gum. It was cheaper than gold leaf and could be applied The significant amount of calcium, potassium, and magne-
with a pen or brush. Shell gold allowed for finer detail sium in the black ink samples demonstrates the possible
and could be applied after the paint. use of gum Arabic as a binding media [13].
Fig. 4. X-ray diffraction pattern of ink and pigments used on the paper of the manuscript.
1614 G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617
Table 1
EDAX analysis of ink and colorants used on paper manuscript.
Fig. 6. Microscopic pictures of vegetable tanned leather bookbinding: (A) shrinkage temperature of the sample at room temperature at 22 °C, before
shrinkage; (B) shrinkage activity of individual fibers at 48 °C; (C) shrinkage activity in more than one fiber at 55 °C; (D) shrinkage activity in some fibers at
59 °C; (E) the final shrinkage activity at 64 °C; (F) shrinkage temperature measurement of different sample of the leather bookbinding.
4.9. Identification of tanning material by High Performance these peaks were 235.20 nm, 257.53 nm, 292.15 nm,
Liquid Chromatography (HPLC) 369.85 nm and 456.20 nm, respectively. The retention
times (min) of the effective peaks of the extracted tannin
The identification of the tannin type used with the book- from the leather bookbinding (Fig. 8B) were 1.727, 2.270,
binding was determined by the comparison of the retention 2.670, 3.804 and 4.330 min, respectively, and the UV spec-
times and UV spectra between Acacia Arabica powder and tra of these peaks were 230.10 nm, 260.45 nm, 296.65 nm,
tannin material extracted from leather bookbinding. It 365.28 nm and 450.20 nm, respectively. It should be noted
was clear from the data obtained (Fig. 8A and B) that there that most of the intensity of the tanning material extracted
was a close similarity in the retention times for the effective from Acacia Arabica powder was higher than tanning mate-
peaks of tanning extracted from the bookbinding studied rial extracted from vegetable-tanned leather bookbinding.
and the tanning extracted from Acacia Arabica powder. The clarity and high intensity of peaks of the spectra for Aca-
The close similarity in the retention times ranged from be- cia Arabica powder compared to those for the vegetable-
tween 1.727 and 4.454 min. The results proved that there tanned leather bookbinding may have been due to the
was a similarity in the spectral characterization of individ- mechanism of deterioration, oxidation or hydrolysis pro-
ual tanning peaks. The retention times (min) of the effective cesses, of the vegetable-tanned leather bookbinding. This
peaks of Acacia Arabica powder (Fig. 8A) were 1.918, 2.268, comparison clearly shows that the tanning material used
2.623, 3.820 and 4.454, respectively, and the UV spectra of on the bookbinding has some similarity to Acacia Arabica.
Fig. 7. Identification of animal skin: (A) goat skin (after Haines, 1981), (B) goat skin from the historical bookbinding.
1616 G. Abdel-Maksoud / Measurement 44 (2011) 1606–1617
Fig. 8. HPLC elution profile: (A) New tanning material extracted from Acacia Arabica. (B) Tanning material extracted from vegetable-tanned bookbinding.
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