Dye Analysis of a Group of Late Intermediate Period Textiles from Ica

21 Dye Analysis of a Group of Late Intermediate

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Period Textiles from Ica, Peru M. E. GEISS-MOONEY and H . L. NEEDLES 1

Division of Textiles and Clothing, University of California, Davis, CA 95616 This chapter reports the analysis and identification of the natural dyestuffs used on a group of Late Intermediate Period, epoch 3B textiles from one grave lot (Site Z, grave 4, Hacienda Galagarza) in Ica, Peru. With no written records from the Peruvians themselves, dye analysis can provide information on the technology and ethnobotany of the culture that created the textiles. This information also can be used in conjunction with other research to prolong the life of the textiles. Thin layer chromatography and UV/vis spectroscopy were used since these analytic techniques can utilize the small samples necessary when sampling from historic textiles. Comparisons were made between the archaelogical samples and standards dyed with known dyestuffs. In general, the textiles from this grave site have reds that match the date for cochineal (carminic acid) and blues and greens that match indigo (indigotin). Whites, yellows, and browns were found to be the natural colors of the cotton and camelid fibers. "ip\ye analysis, especially in conjunction with other research, can provide -"-^ much information for those entrusted with historic textiles. Information regarding the effects of pesticides, conservation procedures, storage environments, and exhibition conditions on fibers and dyes will allow curators and conservators to make decisions in the best interest of the preservation of the textiles. In the past, dye analysis of historic textiles has not always been successful, attributable to a great extent to the small sample sizes afforded. Refinements in the field of thin layer chromatography, especially in adsorbants, has made dye analysis much more 1

Current address: P.O. Box 11002, Santa Rosa, C A 95406.

©

0065-2393/81/0193-0291$05.00/0 1981 American Chemical Society

In Preservation of Paper and Textiles of Historic and Artistic Value II; Williams, J.; Advances in Chemistry; American Chemical Society: Washington, DC, 1981.

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successful with sample sizes of a half-inch of fiber. This research analyzed a group of textiles excavated by Max Uhle at Galagarza, Site Z, grave 4, Peru at the turn of the century (1897-1905). The collection is dated at Late Intermediate Period, epoch 3B (A.D. 1050-1170) ( J ) and is housed at the R. H . Lowie Museum of Anthropology, University of California, Berkeley campus. Experimental Procedures First, the textiles were photographed, using 35-mm photoflood slide film and a seven-inch Kodak color separation ruler. This gives an idea of scale and color trueness in the photography. Samples of one-half to one inch were removed with scissors and tweezers, from protected areas if possible. Because of the deterioration of construction, none of the textiles were taken apart in any way. Sampling was done from different constructions and different colors as discernable to the unaided eye under fluorescent lighting. This may have led to some duplication of samples. Munsell notation was then assigned, using natural southern exposure lighting (Tables I and II) (2). Fiber analysis was conducted using a binocular microscope and η-heptane as the mounting fluid for the longitudinal view. The plate method of cross sectioning with dull cellulose acetate as the packing fiber also was done. Casts were not successful as the fibers proved to be too brittle. Scanning electron microscopy was performed on a few samples with a Cambridge Stereoscan Mark IIA scope after sputtering a 200-Â layer of gold over the sample mounted on an aluminum stub. Polaroid film was used to record the images. All samples (all colors cotton and camelid) first were washed in warm distilled water for 30 min and blotted on filter paper. When dry, the sample (except for blue- and green-colored samples) was then placed in a 25-mL round-bottom flask with four drops of 10% hydrochloric acid and heated in a warm water bath (90°C) for 20 min. Seven to ten milliliters of spectroscopic grade methanol was added and the flask then was hooked up to a micro Soxhlet apparatus. The flask was heated in a water bath for 30-45 min, the methanol collecting in the Soxhlet chamber and concentrating the solution in the flask. The sample was removed to filter paper and the two solutions to separate flasks. The extraction solution was spotted onto precoated 5 X 10 cm 10% acetylated cellulose plates (J. T. Baker), allowed to dry, and developed in Table I.

Munsell Notation for Yellow and Brown Camelid Fibers 7.5 Y R 6/8 5 Y R 2/2

10 Y R 6/8 5 Y R 5/8 Table II.

Munsell Notation for Yellow and Brown Cotton Fibers 10 Y R 8/4 5 Y R 4/6

2.5 Y 8/4

7.5 Y R 6/6 2.5 YR4/6


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Table III.

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Textile Dye Anaylsis

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Munsell Notation for Red Camelid Fibers

Before Extraction

After Extraction

7.5 R 3/6 5 R 4/10

7.5 Y R 6/8 7.5 Y R 6/8


Table IV. Munsell Notation for Blue and Green Camelid Fibers Before Extraction

After Extraction

5 Β 3/2 10 B G 2/2 2.5 B G 3/2 10 G 3/2 10 G Y 4/2

7.5 7.5 7.5 7.5 7.5

YR YR YR YR YR

5/6 5/6 5/6 5/6 5/6

a saturated chamber with an eluent mixture of ethyl acetate-tetrahydrofuran-water (6:35:47). The elution took about 30-40 min to complete. The solvent front was marked and the plate examined under fluorescent lighting and short-wave (350 nm) U V light, marking any spots and noting colors. The plate was then sprayed with a 1% solution of 2-aminoethyldiphenyl-borate (Naturstoff reagent, Tridom Chemical) in methanol and re-examined under the previously mentioned lighting con ditions. Spot colors were again noted. R values were calculated. The rest of the extraction solution was then placed in a semimicro cuvet (10-mm path length) and run on a Beckman D B - G grating spec trometer between 200 cm and 800 cm" , the visible and U V range. The other methanol solution was used in the reference cuvet. The spectrum curve was recorded on a chart paper recorder. Infrared spectroscopy also was tried, dropping the extraction solution onto potassium bromide powder and drying in a hot vacuum oven before pressing into a pellet using handpress equipment (Perkin-Elmer). But the results were not definitive nor conclusive. Munsell notation was assigned to the dried extracted samples, using the same lighting conditions as before (Table III). The blue- and green-colored samples were not affected by the methanol extraction and so were analyzed differently. After washing, the sample was placed in a small test tube with 1 mL of a solution containing 50 g of sodium hydrosulfite and 50 g of sodium hydroxide per liter of water. The test tube was warmed in water for a few minutes and then one drop of spectroscopic grade ethyl acetate was added. The test tube was shaken. If the ethyl acetate layer turns clear bright blue, indigo is present (3). The ethyl acetate layer was spotted onto 10% acetylated cellulose plates and developed in an eluent mixture of ethyl acetateethanol-water (2:1:1). Spot color was noted and R calculated. The ethyl acetate layer also was run through UV/vis spectroscopy with a reference of spectroscopic grade ethyl acetate. If the ethyl acetate layer stayed clear, the sample was run as a normal one. Munsell notation was assigned to the dried extracted samples, using the same lighting condi tions as before (Table I V ) . f

1

f



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Known dyeings of natural dyes on sheep wool and synthetic equivalents of the dye constituents also were characterized by the same analytical scheme. These included cochineal, carminic acid, ( H . Kohnstamm & Company), madder, alizarin (Aldrich Chemical), purpurin (J. T. Baker), Relbunium hypocarpium, pseudopurpurin (K&K-ICN Labs), brazilwood, and brazilin (J. T. Baker) for reds; indigo, indigotin (J. T. Baker), logwood, and Genipa americana for blues; Bixa orellana for oranges; Schinus molle, Baccharis genistolloides, Bidens andicola, Dicliptera hookeriana, Berberis species, curcumin (J. T. Baker), lawsone (Aldrich Chemical), and crocetin (J. T. Baker) for yellows (4,5,6). Results and Conclusions In regards to fiber analysis, it was not possible to differentiate between archaeological alpaca, llama, and possibly vicuna and so the woolen fibers were called camelid (Figure 1). The cottons had the appearance in cross section of cotton today that is unmercerized. One cotton sample proved to be very interesting as an earth pigment was used for the bright orange color (Figure 2). X-ray fluorescence analysis confirmed that the earth pigment used was cinnabar (mercury sulfide) (Figure 3). None of the other cotton samples were dyed except for one blue sample, which was dyed with indigo and used as a decorative warp stripe (Figure 4) along one selvedge of the textile 4-4873B. The camelid samples were the naturally occurring fiber colors except for the reds, blues, and greens (Figure 5). The reds were obtained from a source of carminic acid,

Figure 1. Scanning electron microscopy: textile 4-4868, camelid fiber (504X)



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Figure 2.

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Scanning electron microscopy: textile 4-4842, cotton fiber with cinnabar pigment (186 X)

probably the native Dactylopius confusus (cochineal) species (7) (Table V and Figure 6). The blues and greens were obtained from a source containing indigotin, probably the native species of Indigofera suffruticosa (8) (Table VI and Figure 7). Much dye analysis work remains to be done on historic textiles of all kinds. Recently, there has been some research including thin layer chromatography using micropolyamide plates with much success (9,10). Future work could use both types of plates to increase the accuracy of identification. Thin layer chromatography is proving to be an inexpensive and simple method for the identification of dyestuffs used on historic textiles. As well as providing information used in conjunction with other research that could increase the longevity of the textiles, information on the culture and technology that created the textiles is also a welcome result. Acknowledgments We thank the staff of the R. H . Lowie Museum of Anthropology for their assistance in providing well-provenanced textiles. Thanks to Dr. Wilfred Ward, USDA Regional Lab, Albany, California, for the confirmatory camelid fiber analysis. Also, many thanks for the help for so long



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Figure 3. X-rayfluorescenceanalysis: textile 4-4842, cottonfiberwith cinnabar pigment; 10-min scan, Cu and Ar peaks are artifacts of the instrument.

Figure 4.

Textile 4-4873B, only dyed cottonfiberin grave lot



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Figure 5.

AND NEEDLES


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Textile 4-4866, example of full range of natural and dyed camelid fibers


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PRESERVATION OF PAPER AND TEXTILES II


Table V. Thin Layer Chromatography of Red Knowns and Unknown 4-4866 in Methanol on 10% Acetylated Cellulose Plates

R Unknown 4-4866

f

Spot Color (Fluorescent) Unsprayed/ Spray ed a

Spot Color (350 cm' ) Unsprayed/ Sprayed* 1

Cochineal, Sn Mordant, Sheep Wool

0.86 pale pink/bright pink/pink pink 0.86 orange/dark rose bright pink/dark pink pink

Carminic Acid Dye Powder

0.86 orange/dark rose bright pink/dark pink pink

a

1% solution of 2-aminoethyldiphenylborate in methanol.

XT

Figure 6. UV/vis spectroscopy: ( ) known cochineal on sheep wool; ( ) unknown 4-4866 in methanol


GEISS-MOONEY

Textile Dye Anayhis

AND NEEDLES

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Table VI. Thin Layer Chromatography of Blue Knowns, Unknowns 4-3 873 A (Cotton) and 4-4866 (Camelid) in Ethyl Acetate on 10% Acetylated Cellulose Plates R

e

0.82 0.82 0.82 0.82

Unknown 4-4873A (Cotton) Unknown 4-4866 (Camelid) Indigo, Sheep Wool Indigotin Dye Powder β

f

Spot Color (Fluorescent) pale blue pale blue pale blue pale blue

After positive result of initial test for indigo.

%T

—I

1

1

1

1

1

1 — ι — ι — t — ι — —

Figure 7. UV/vis spectroscopy: ( ) known indigo on sheep wool; ( } unknown 4-4866 (blue) in ethyl acetate after positive initial test for indigo.


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by K. Alger, Textiles & Clothing, University of California, Davis. And thanks to G . Caniveau, Research Laboratory, Metropolitan Museum of Art, New York City for the confirmatory x-rayfluorescenceanalysis.


Literature Cited 1. Menzel, D. "The Archaeology of Ancient Peru and the Work of Max Uhle"; University of California Printing Department: Berkeley, 1977; pp. 58, 131. 2. Munsell Color Company "Munsell Book of Color"; Munsell Color Company: Baltimore, MD, 1954. 3. Hofenk-deGraaf, J. Stud. Conserv. 1974, 19, 54. 4. Autunez de Mayolo, Kay K. M.S. thesis, California Polytechnic Univ., San Luis Obispo, 1977. 5. Yacovleff, E.; Herrera, F. L. "El Mundo Vegetal de los Antiguos Peruanos," Rev. Mus. Nac. (Lima) 1934, 3(3), 243. 6. Towle, M. A. "The Ethnobotany of Pre-Columbian Peru"; Aldine Publishing: New York, 1961. 7. Brunello, F. "The Art of Dyeing in the History of Mankind"; Phoenix Dye Works: Cleveland, OH, 1973; 344. 8. MacBride, J. Francis, ed. "Flora of Peru," Field Museum of Natural History Botanical Series; Field Museum Press: Chicago, 1943; Vol. 13, Part 3, No. 1. 9. Schweppe, H. "Nachweis von Farbstoffen auf alten Textilien," Z. Anal. Chem. 1975, 276, 291. 10. Schweppe, H. "Identification of Dyes on Old Textiles," J. Am. Inst. Conserv. 1980, 19(1), 14. RECEIVED November 27,

1979.


Dye Analysis of a Group of Late Intermediate Period Textiles from Ica

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