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An Evaluation of selected applied polymers for the treatment of parchment Gomaa Abdel-Maksoud Cairo University, Faculty of Archaeology, Conservation Department Contact

Abstract

Representative samples of the new parchment were prepared to be in an advanced state of degradation by application of artificial heat aging. The degraded aged samples are submitted to experiments concerning applied consolidation materials (polymers) on parchment. The purpose of this study is to establish if an increase in the properties of parchment can be attained with none or as less as possible interference with the appearance of the object. A comparison is made between six polymers by impregnation method. Investigation of some mechanical properties, change of color and the humidity sorption were used to evaluate the studied polymers. The results revealed that the polymers, which dissolved in organic solvents, were better than that dissolved in water.

Introduction

There are numerous parchment manuscripts in museums, storage, libraries and excavation areas in many countries, and especially in Egypt. In Egypt parchment was first used during the Middle Kingdom. Observation of the parchment manuscripts has shown that most of these items in many places in Egypt are in dry conditions and thus create risk of damage caused by climatic conditions especially physical factors (such as relative humidity, temperature, light, etc). Depending upon natural and environmental conditions, these factors affect the properties of the parchment. Natural aging usually causes parchment to become usually wrinkled, dry, brittle, hard and sometimes deformed due to water loss. From last conditions, parchment manuscripts need to be treated with consolidation materials from time to time. So,this study aims to Focus on the consolidation materials used for the treatment of parchment in order to evaluate their suitability for the conservation of historical parchment.

Materials and methods

Used samples: New parchment
Goatskin prepared by Abdel-Maksoud (Abdel-Maksoud 1999).

Used consolidation materials
Six consolidates accordance with many authors (Peacock, 1986, Puissant, 1996, Marttein, 1996, Bansa, 1996, 1996, Dignard et al, 1997) were examined to test their effectiveness in preventing deterioration (see table 1). The samples were impregnated in the polymers solutions until fully saturated. The samples after consolidation process were allowed to air dry naturally.

Commercial name	Supplier	Chemical type	Solvent	Concentrations
Klucel G	Hercules powder Co.	Hydroxypropyl-cellulose	Distilled water	1%, 2 %, 3 %
Paraloid B. 67	Rohm and Haas	Acrylic polymer	Acetone	2 %, 4 %, 6 %
Plexisol P. 550	Rohm and Haas	Acrylic polymer	Xylene	2 %, 4 %, 6 %
Polyvinyl alcohol	Hoechst	Acrylic polymer	Distilled water	2 %, 4 %, 6 %
Primal AC. 33	Rohm and Haas	Aqueous acrylic polymer	Distilled water	2 %, 4 %, 6 %
Primal E. 330	Rohm and Haas	Aqueous acrylic polymer	Distilled water	2 %, 4 %, 6 %
Table 1: Used consolidation materials

Accelerated aging
Heat treatment according to Abdel-Maksoud and Marcinkowska (1999) at 100 ^oC for two weeks was used to prepare aged parchment before the conservation treatments. Heat treatment at 100 ^oC for one week was used after the conservation treatments (consolidation materials). The accelerated aging was by convective, thermal drying, absolute humidity in the ageing chamber was 4.2 ÷ 6.7 g H₂O / kg dry air, time of aging was 2 weeks before treatment and 1 week after conservation treatment,volume of the chamber is about 50 dcm³, The samples were put on three plates in the aging chamber. Each plate has holes (113 holes). The distance between the plates was 10 cm and The thickness of the samples were 0.33 mm ± 0.02mm.

Change of colour
The effects of heat were measured using CIE*Lab system, commonly used to compare the colors of two samples. The L scale measures lightness, and varies from zero for black to one hundred for perfect white. The (a) scale measures redness-green (+a) is red; (-a) is green. The (b) scale measures yellowness-blueness (+b) is yellow; (-b) is blue. The E scale measures the total color. The measurement was made using Shimadzu Double Beam UV-2101 PC Spectrophotometer Egvipped with ISR 48 Integrating Sphere (Billmeyer and Saltzman 1981).

Humidity sorption
Determination of moisture based on the weight loss of a sample dried by the action of infrared heating rays directly on the sample (heating from within) using a Mettler LP 16 Infrared Dryer. The instrument is mounted on a precision balance, which is connected up to a computer and printer in order to produce complete records of the drying profiles and the final results. The temperature during this process is 105 ^oC. The water molecules show a pronounced desorption at these wavelengths; they heat up and evaporate. The samples dried by this procedure were placed in the top of the disiccator, the bottom of which was filled with di-sodium hydrogen orthophosphate (Na₂ HPO_4*12 H₂O) in order to create a relative humidity of 95%. The temperature was 20^o C.

Mechanical properties
Mechanical properties were measured according to ISO 3376. Samples were taken from adjacent zones of a skin. Their length was 90 mm, the free length between jaws of the testing machine was 50 mm, the width of the free length was 10 mm. The average of the new samples thickness was 0.33 mm ± 2 mm. Six samples were taken, three perpendicular to and three parallel to the backbone and the three results averaged from each side. The speed of testing machine during measuring was 100 ± 20 mm/min. A Universal Testing Machine (Model 1435, producer: Zwick, Germany) was used for measuring. The samples were measured after conditioning for 48 hours at 20 ^o C and 65 RH according to ISO 554. The tensile strength is found by dividing the breaking force (N) by the product of width and thickness of the samples (mm). The results are N per mm². The elongation at break is given in %.

Results and discussion

Change of color
Color by definition has three dimensions: the first dimension of color is known as reflectance also defined as value of lightness. The second dimension of color is known as hue. Hue is the attribute of color that distinguishes green from red and blue from yellow. The third dimension of color is saturation of chrome.

The color we see ranges from violet (400 to 430 nm), blue (430-458 nm), green (485 to 570 nm), yellow (570 to 585), orange (585 to 610 nm), to red above 610 nm. This range comprises what is known as the visible spectrum of color. Qualitatively, the nature of the color can be understood by examining the visible reflectance spectrum before and after the samples have been treated with polymers and exposed to artificial heat aging.

From color measurement data (table 2) it becomes clear that the L value (brightness) is 95.51 in the control sample but after aging, this value reduced. This reduction was 12% after two weeks and 22% after three weeks (aged untreated sample). It was noticed by the comparison of the treated and aged treated samples with aged sample (after two weeks) that the L value decreased as the concentration of polymers increased. The reduction of the L value after the treatment at the first concentration was: both Plexisol P.550 and Paraloid B.67: 1%, Polyvinyl alcohol: 2%, Primal E.330: 7%, Primal AC.33: 41%, Klucel G: 43%. The reduction at the second concentration was: Paraloid B.67: 2%, Plexisol P.550: 3%, Polyvinyl alcohol: 7%, Klucel G: 43%, Primal AC.33: 50%, Primal E.330: 51%. The reduction at the third concentration was: Plexisol P.550: 6%, both Paraloid B.67and Polyvinyl alcohol: 9%, Klucel G: 45%, Primal AC.33: 59%, Primal E.330: 62%. The reduction of aged treated samples increased after aging. The reduction of aged treated samples at the first concentration was: Paraloid B.67: 2%, Polyvinyl alcohol: 3%, Plexisol P.550: 4%, Primal E.330: 43%, Primal AC.33 45% and Klucel G: 48%. The reduction at the second concentration was: Paraloid B.67: 1%, Plexisol P.550: 4%, Polyvinyl alcohol: 9%, Klucel G: 48%, Primal AC.33: 58% and Primal E.330: 61%. At the third concentration the reduction was as follow: Plexisol P.550: 10%, Polyvinyl alcohol: 13%, Paraloid B.67: 19%, Klucel G: 50%, Primal E.330: 63% and Primal Ac.33: 66%.

It was noticed that the a value of aged samples increased by comparison with the control sample. The increasing of aged sample after 2 weeks was 70% and the aged sample after 3 weeks was 77%. By comparison of treated samples with aged sample after 2 weeks, there are some variations between polymers. A value with some polymers decreased and others increased than the aged sample. At the first concentration the results obtained were as follow: the increasing was in: Plexisol P.550: 2%, Primal E.330: 3%, Polyvinyl alcohol: 4%, Paraloid B. 67: 7%. The decreasing was in: Primal AC.33: 11% and Klucel G: 38%. At the second concentration the increasing was in: Plexisol P.550: 6%, Paraloid B. 67: 7% and Polyvinyl alcohol: 18%. The decreasing was in: Klucel G: 3%, Primal AC.33: 22% and Primal E.330: 31%. At the third concentration, the decreasing was in: Klucel G: 5%, Primal AC.33: 20%, and Primal E.330: 47%. The increasing was in: Paraloid B.67: 5%, Plexisol P.550: 9% and Polyvinyl alcohol: 20%. After aging the treated samples, the results obtained comparison with aged sample (2 weeks) were as follow: at the first concentration, the decreasing was in: Primal E.330: 3%, Primal AC.33: 14% and Klucel G: 18%. The increasing was in: Plexisol P.550 and Paraloid B.67: 13% and Polyvinyl alcohol: 15%. At the second concentration, the decreasing was in: Primal AC.33: 22% and Primal E.330: 31%. The increasing was in: Klucel G: 0.11%, Plexisol P.550: 9%, Paraloid B.67: 14% and Polyvinyl alcohol: 21%. At the third concentration, the decreasing was in: Primal AC.33: 69% and Primal E.330: 93%. The increasing was in: Klucel G: 4%, Plexisol P.550: 13%, Paraloid B.67: 21% and Polyvinyl alcohol: 22%.

For the b value, there are some variations in the treated samples before and after aging. Since this value increased with some polymers and decreased with others by comparison with aged sample after 2 weeks. The following results were obtained from treated samples before aging: at the first concentration, the increasing was in: Primal AC.33: 41%, Primal E. 330: 59% and Klucel G: 68%. The decreasing was in: Polyvinyl alcohol: 6%, Paraloid B.67: 10 and Plexisol P.550: 16%. At the second concentration, the increasing was in: Plexisol P.550: 0.3%, Polyvinyl alcohol: 15%, Klucel G: 58%, Primal E.330: 62% and Primal AC.33: 68%. The decreasing was only with Paraloid B.67: 10%. At the third concentration, the increasing was in: Plexisol P.550: 6%, Polyvinyl alcohol: 17%%, Primal E.330: 57%, Klucel G: 63% and Primal AC.70%. For the aged treated samples at the first concentration the increasing was with all polymers as follow: Polyvinyl alcohol: 1%, Plexisol P.550: 2%, Paraloid B.67: 19%, Primal AC.33: 40%, Primal E.330: 58% and Klucel G: 69%. At the second concentration the increasing was in: Plexisol P.550: 12%, Polyvinyl alcohol: 20%, Primal AC.33: 62%, Primal E.330: 62% and Klucel G: 63%. The decreasing was only with Paraloid B.67: 6%. At the third concentration the increasing was with all polymers as follow: Plexisol P.550: 16%, Polyvinyl alcohol: 37%, Paraloid B.67: 44%, Primal E.330: 61%, Klucel G: 64% and Primal AC.33: 71%.

The E value (total color), there are some variations between treated and aged treated samples. Since with some polymers increased and with others decreased. From the treated samples the obtained results were as follow: at the first concentration the increasing was in: Plexisol P.550: 0.3%, Polyvinyl alcohol: 0.5%, Paraloid B.67: 2% and Primal E.330: 3%. The decreasing was in: Primal AC.33: 22% and Klucel G: 55%. At the second concentration the increasing was in: Plexisol P.550: 1%, Paraloid B.67: 2%, Polyvinyl alcohol: 6%. The decreasing was in: Klucel G: 15%, Primal AC.33: 19% and Primal E.330: 29%. At the third concentration, the increasing was in: Paraloid B.67: 1%, Plexisol P.550: 2% and Polyvinyl alcohol: 8%. The decreasing was in: Klucel G: 14%, Primal AC.33: 31% and Primal E.330: 54%. For the aged treated samples at the first concentration the increasing was in: Plexisol P.550: 5%, Paraloid B.67: 6% and Polyvinyl alcohol: 7%. The decreasing was in: Primal E.330: 15%, Klucel G: 17% and Primal AC.33: 25%. At the second concentration, the increasing was in: Plexisol P.550: 3%, Paraloid B.67: 7% and Polyvinyl alcohol: 9%. The decreasing was in: Klucel G: 12%, Primal AC.33: 29% and Primal E.330: 32%. At the third concentration, the increasing was in: Plexisol P.550: 2%, Paraloid B.67: 7% and Polyvinyl alcohol: 10%. The decreasing was in: Klucel G: 10%, Primal AC.33: 39% and Primal E.330: 53%.

Table 2: Change of color parameters of consolidated parchment before and after accelerated aging at 100o C
Samples	First concentration				Second concentration				Third concentration
	L	a	b	E	L	a	b	E	L	a	b	E
Control sample	95.51	23.47	2.05	98.37	95.51	23.47	2.05	98.37	95.51	23.47	2.05	98.37
Aged sample	84.28	78.83	17.94	116.78	84.28	78.83	17.94	116.78	84.28	78.83	17.94	116.78
Aged untreated sample	74.64	103.73	26.19	130.77	74.64	103.73	26.19	130.77	74.64	103.73	26.19	130.77
Klucel G
Treated sample	48.32	49.154	56.74	89.27	47.63	76.41	42.44	99.54	46.01	75.00	48.31	100.37
Aged treated sample	43.92	64.44	57.29	96.77	43.45	78.92	48.53	102.33	42.23	82.20	49.52	104.84
Paraloid B.67
Treated sample	83.04	84.58	16.14	119.62	83.00	84.58	16.14	119.59	76.79	83.11	21.13	115.11
Aged treated sample	82.23	90.47	18.28	123.62	83.04	92.06	16.89	125.12	68.02	101.02	32.17	125.96
Plexisol P.550
Treated sample	83.67	80.56	15.03	117.12	81.48	83.66	17.99	118.15	79.52	86.58	19.04	119.09
Aged treated sample	81.23	90.47	18.28	122.95	80.77	86.35	20.51	120.00	75.74	90.16	21.42	119.68
Polyvinyl alcohol
Treated sample	82.33	81.87	16.93	117.33	78.34	95.82	20.99	125.54	76.87	98.75	21.69	127.00
Aged treated sample	81.71	93.03	18.21	125.15	76.98	99.55	22.48	127.83	72.97	102.92	28.37	129.31
Primal Ac.33
Treated sample	49.60	70.30	30.55	91.29	42.27	64.71	55.28	95.02	34.54	41.675	59.01	80.07
Aged treated sample	46.45	67.41	29.83	87.12	35.48	58.46	46.79	82.85	28.20	24.71	61.10	71.68
Primal E.330
Treated sample	78.19	81.04	43.75	120.81	41.04	54.13	47.36	82.80	31.69	10.13	41.71	53.35
Aged treated sample	47.63	76.41	42.44	99.54	33.29	54.13	47.36	79.25	31.08	5.14	45.63	55.44
Table 2: Change of color parameters of consolidated parchment before and after accelerated aging at 100o C

Humidity sorption
The humidity sorption in control sample was 50.33%, but the humidity sorption of aged sample reduced comparison with the control sample. This reduction was 52 % after 2 weeks and 58 after 3 weeks. It was clear from data (table 3) that the humidity sorption of the treated and aged treated samples with all polymers decreased comparison with aged sample after 2 weeks. The reduction of the humidity sorption of the treated samples was as follow: at the first concentration, Polyvinyl alcohol: 21%, Primal AC.33: 17%, Paraloid B.67: 16%, Plexisol P.550: 14%, Primal E.330: 13% and Klucel G: 12%. At the second concentration, the results obtained were as follow: Paraloid B.67: 38%, Plexisol P.550: 34%, Polyvinyl alcohol: 30%, Primal AC.33: 22%, Primal E.330: 19% and Klucel G: 17%. At the third concentration the results were as follow: Paraloid B.67 58%, Plexisol P.550: 54%, Polyvinyl alcohol: 41%, Primal AC.33: 32%, Primal E.330: 29% and Klucel G: 23%. For the aged treated samples, the results at the first concentration were as follow: Polyvinyl alcohol: 14%, Paraloid B.67%: 14%, Primal AC.33: 11%, Plexisol P.550: 10%, Primal E.330: 5% and Klucel G: 4%. At the second concentration, the results were as follow: Paraloid B.67 33%, Plexisol P.550: 27%, Polyvinyl alcohol: 22%, Primal AC.33: 15%, Primal E.330: 10% and Klucel G: 10%. At the third concentration, the results were as follow: Paraloid B.67 52%, Plexisol P.550: 47%, Polyvinyl alcohol: 33%, Primal AC.33: 21%, Klucel G: 16%, Primal E.330: 14%.

Table 3: Humidity sorption of consolidated parchment before and after artificial heat aging
Samples	First concentration		Second concentration		Third concentration
	Humidity sorption	Standard deviation	Humidity sorption	Standard deviation	Humidity sorption	Standard deviation
Control sample	50.33	0.44	50.33	0.44	50.33	0.44
Aged sample	24.36	0.95	24.36	0.95	24.36	0.95
Aged untreated sample	21.15	0.65	21.15	0.65	21.15	0.65
Klucel G
Treated sample	21.40	0.66	20.22	0.82	18.86	0.55
Aged treated sample	23.37	0.55	22.03	0.82	20.46	0.15
Paraloid B.67
Treated sample	20.40	0.62	15.10	071	10.27	0.87
Aged treated sample	21.00	0.21	16.23	0.56	11.63	0.32
Plexisol P.550
Treated sample	21.06	0.21	16.13	0.32	11.27	0.66
Aged treated sample	22.00	0.46	17.78	0.30	12.90	0.46
Polyvinyl alcohol
Treated sample	19.30	0.20	17.13	0.31	14.33	1.04
Aged treated sample	20.80	0.23	18.93	0.40	16.22	0.86
Primal AC.33
Treated sample	20.20	0.30	18.90	0.71	16.60	0.55
Aged treated sample	21.80	0.26	20.73	0.15	19.33	0.73
Primal E.330
Treated sample	21.20	0.10	19.70	0.38	17.33	0.38
Aged treated sample	23.13	0.25	21.93	0.15	21.00	1.00
Table 3: Humidity sorption of consolidated parchment before and after artificial heat aging

Mechanical Properties
It was clear from data (table 4, 5) that the mechanical properties (tensile strength and elongation) in the perpendicular direction of control sample was 25.60 in the tensile strength and 21.12 % in elongation and in the parallel direction 42. 17 in the tensile strength and 20.40 % in the elongation. After aging, it was noticed a reduction in this properties. This reduction was 26% in tensile strength and 35 in elongation after 2 weeks and 43% in tensile strength and 51% in elongation after 3 weeks in the perpendicular direction. In the parallel direction, the reduction was as follow: tensile strength: 33% and elongation: 23% after 2 weeks. After 3 weeks aging, tensile strength: 52% and elongation 59%.

After the treatment in the perpendicular and parallel directions, it was clear that there is an increasing in the properties tested with increasing the concentration of polymers by comparison with aged sample after 2 weeks. For aged treated samples, there is also an increasing but better than aged samples (without primal AC.33 and Primal E.330 at the first concentration in the perpendicular direction) and lower that the treated samples before aging. It was clear also that the arrangement of polymers at all concentrations from the high to the lower increasing in the perpendicular and parallel directions after both the treatment and aging were as follow: Plexisol P.550, Paraloid B.67, Klucel G, Polyvinyl alcohol, Primal AC.33 and the lowest increasing was with Primal E.330.

Table 4: Mechanical properties of treated parchment with polymers (perpendicular direction)
Samples	First concentration		Second concentration		Third concentration
	Tensile strength N/mm2	Elongation %	Tensile strength N/mm2	Elongation %	Tensile strength N/mm2	Elongation %
Control	25.60	21.12	25.60	21.12	25.60	21.12
Aged sample	18.90	13.66	18.90	13.66	18.90	13.66
Aged untreated sample	14.60	10.41	14.60	10.41	14.60	10.41
Klucel G
Treated sample	20.77	15.20	22.00	16.20	23.13	17.43
Aged treated sample	19.90	14.33	21.50	15.43	22.23	16.73
Paraloid B.67
Treated sample	21.40	15.63	22.86	17.00	23.93	17.50
Aged treated sample	20.60	15.13	22.10	16.17	22.70	16.62
Plexisol P.550
Treated sample	21.54	15.90	23.10	17.20	24.23	17.83
Aged treated sample	20.83	15.30	22.37	16.40	23.00	17.20
Polyvinyl alcohol
Treated sample	20.33	14.90	21.93	15.87	22.83	16.80
Aged treated sample	19.53	14.23	21.27	14.97	22.00	15.97
Primal AC.33
Treated sample	19.88	14.30	20.73	15.53	22.50	16.43
Aged treated sample	18.83	13.80	19.90	14.53	20.77	15.40
Primal E.330
Treated sample	19.72	14.10	20.53	15.33	22.37	16.37
Aged treated sample	18.70	13.77	19.73	14.27	20.50	15.27
Table 4: Mechanical properties of treated parchment with polymers (perpendicular direction)

Table 5: Mechanical properties of treated parchment with polymers (parallel direction)
Samples	First concentration		Second concentration		Third concentration
	Tensile strength N/mm2	Elongation %	Tensile strength N/mm2	Elongation %	Tensile strength N/mm2	Elongation %
Control	42.71	20.40	42.71	20.40	42.71	20.40
Aged sample	28.67	15.68	28.67	15.68	28.67	15.68
Aged Untreated	20.49	8.33	20.49	8.33	20.49	8.33
Klucel G
Treated sample	30.36	17.23	32.70	18.50	34.7	19.57
Aged treated sample	29.4	16.40	31.50	17.33	32.50	18.60
Paraloid B.67
Treated sample	31.00	17.50	33.50	19.10	35.33	20.50
Aged treated sample	30.20	16.92	32.30	18.17	33.70	19.60
Plexisol P.550
Treated sample	32.03	18.03	34.67	19.83	36.13	21.00
Aged treated sample	31.00	17.10	33.20	18.75	34.77	19.83
Polyvinyl alcohol
Treated sample	29.90	16.70	31.50	17.40	33.50	18.40
Aged treated sample	29.30	16.10	30.53	16.70	32.17	17.50
Primal AC.33
Treated sample	29.30	16.40	31.00	17.30	32.33	18.27
Aged treated sample	28.80	15.93	30.13	16.57	31.10	17.10
Primal E.330
Treated sample	29.03	16.30	30.8	17.23	32.20	18.23
Aged treated sample	28.73	15.73	29.86	16.37	30.87	16.83
Table 5: Mechanical properties of treated parchment with polymers (parallel direction)

Conclusions

1. For the lightness color (L value), it can be said that the treated and aged treated samples with Paraloid B.67, Plexisol P.550 and Polyvinyl alcohol were good colors at all concentrations and were approximately near from aged sample after 2 weeks, but the first and the second concentrations were better than the third concentration, which was little dark especially after aging with Paraloid B.67. The treated and aged treated samples with Primal AC.33, Primal E.330 and Klucel G gave poor lightness at all concentrations, since all the results obtained tend to dark color without Primal E.330 after the treatment (it gave a good result).
2. For the red color (a value), the best results were obtained from the treated samples with Klucel G at the second and the third concentrations and Primal E.330 at the first concentration after both the treatment and aging. The results obtained from the treatment and aged treated samples with Plexisol P.550, Paraloid B.67 and Polyvinyl alcohol were quite good after both the treatment and aging. The poor result were obtained from Klucel G at the first concentration, Primal E.330 at the second and the third concentration and Primal AC.33 at all concentrations.
3. For the yellow color (b value), the treated and aged treated samples with Paraloid B.67, Plexisol P.550 and Polyvinyl alcohol were good and more better than Klucel G, Primal AC.33 and Primal E.330.
4. For the total color (E value), it can be said that the changes in total color with treated and aged treated samples with Plexisol P.550, Paraloid B.67 and Polyvinyl alcohol were little better than with Klucel G, Primal E.330 and Primal AC.33.
5. The results confirmed that the treated samples with paraloid B.67, Plexisol P.550 and polyvinyl alcohol were good after both the treatment and aging. Since they have given high reduction in the humidity sorption especially at the second and third concentrations. This gave indication that these polymers tolerated the heat aging. The reduction of the humidity sorption of treated and aged treated samples with Primal AC.33, Primal E.330 and Klucel G gave poor reduction (without Primal AC.33 at the first concentration) compared with the last three polymers.
6. All the polymers studied gave an increasing in the tensile strength and elongation in both perpendicular and parallel directions (compared with aged samples after 2 weeks).

References

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