BP Chapter 1 - Fiber Identi cation

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1. Fiber Identi cation

Date: 1994 Compiler: Debora Mayer TABLE OF CONTENTS: 1.1. Purpose 1.2. Factors to Consider 1.3 Materials and Equipment 1.4 Treatment Variations 1.5 Bibliography (see also AIC/BPG/PCC 4. Support Problems 4.4.1) Fiber identi cation generally involves taking samples from the artifact and viewing them at 100 times or greater magni cation to study the ber morphology. Stains are often employed to accentuate features and to determine pulping processes. Fiber identi cation, especially in the case of samples from paper, is not necessarily straightforward. Consultation and study using reference material and known ber samples is essential.

1.1 Purpose
Identi cation of the ber content of the artifact may aid in dating the artifact determining the provenance of the artifact understanding the artist's technique, and, nally, in the selection of conservation treatment procedures and techniques. e introduction and usage of some bers and manufacturing process are known. erefore, it is possible, at times, to date (post) the manufacture of the artifact. Speci c bers and types of paper are sometimes more commonly utilized in certain countries or regions assisting in establishing the provenance of the artifact. Sensitivity to an artist's work and understanding visual qualities of the work can often be enhanced by knowledge of the ber content and manufacturing process. Dierent bers have dierent chemical and physical properties, including, but not limited to: lignin content, color, absorbency and dimension. Knowledge of the properties may help in predicting how a paper will react to speci c treatments (for example: wetting, bleaching, deacidi cation).

1.2 Factors to Consider

1.2.1 History of Fiber Usage 1.2.2 Fiber Qualities 1.2.3 Sampling Guidelines
(see AIC/BPG/PCC Spot Tests 10.2)

1.2.4 Representative Sampling

1.2.5 Fiber Classi cations

see Cote 1980 for Fiber Nomenclature) A. Plant Fibers 1. Wood Fibers a. Gymnosperm (non owering) conifers most important group, they are generally evergreen and called softwood by tradespeople [examples: pine, spruce, hemlock] cell types: longitudinal tracheids ( bers), parenchyma architecture: bordered pits and ray cross eld pitting on tracheids b. Angiosperm ( owering) both monocotyledon and dicotyledon trees can be evergreen or deciduous, called hardwood by tradespeople [examples: oak, maple, poplar, red and black gum] cell types: tracheids, vessels, parenchyma, vasi-centric tracheids architecture: simple and scaliform perforation plates, spiral thickening and pitting patterns on vessels 2. Fruit Fibers cotton: seed hair from cotton boll, lint (long), linters, (short) coir: hairs from husk of coconut palm kapok: hairs from pod of kapok tree cell types: bers architecture: cotton: collapsed lumen, convolutions 3. Bast Fibers comes from inner bark - phloem trees and shrubs: kozo, mitsumata, gampi herbaceous dicotyledons: ax, hemp, ramie, sunn, jute, kenaf cell types: bers, sometimes shive, parenchyma at times; associated cells generally not found when primary source is from textile architecture: type and frequency of nodes and crossmarking on bers, lumen and ber width, ber contour 4. Monocot Leaf Fibers vascular bundles from xylem [examples: abaca or manila hemp, sisal, pineapple, New Zealand ax] cell types: bers, sometimes vessel segments, epidermal and parenchyma cells architecture: lumen and ber width, ber contour, sometimes ne crossmarkings on ber, sometimes lumen contains granular material 5. Grass/Stem Fibers monocots plant pulped for ber or used whole for ethnographic artifacts [examples: cereal straws (wheat, rice, oat, rye, barley) sugar cane bagasse, cornstalk, bamboo, esparto, rush] cell types: bers, vascular bundles, sclerenchyma bundles, serrated epidermal cells, parenchyma, vessels, stomate (trichomes in esparto) architecture: dimension of bers, vessels and associated cells; pitting on vessels, annular thickening on vessels; shape of trichomes B. Animal Fibers Animal bers are not pulped to form paper, however animal bers can be found as inclusions in paper. Colored bers may be from wool. Usually these bers are intentional additions to the pulp, often from textile sources.

1. Hair protein [examples:wool, mohair, cashmere] cell type: ber architecture: shape of medulla, cross sectional shape, scale pattern, all can vary from root to tip within same animal 2. Secretions protein [examples: silk, Bombyx Mori (cultivated), Tussah silk (wild)] cell type: ber architecture: smooth or slightly striated bers, no skin or outer covering, triangular or wedge- shaped cross-sectional shape C. Man Made Fibers ese bers are not generally found in paper except in small percentages on modern specialty papers. Synthetic bers however, are used extensively in conservation treatment and storage materials. 1. Cellulose-based [examples: viscose rayon, acetates] 2. Synthetic ber [examples: nylon, polyester, acrylic] architecture: long bers, smooth pro le without scales or convolutions, may have striations, generally identi ed by stains, interference colors and cross sectional shape D. Mineral Fibers Rarely found in paper. Strathmore made a watercolor paper in the 1970s with a small percentage of berglass. [examples: asbestos, glass]

1.2.6 Optic Properties of Fibers 1.2.7 Wood Fiber Pulping Processes

A. Mechanical B. Semi Chemical And Semi Mechanical C. Soda D. Sul te E. Sulfate (Kraft)

1.3 Materials and Equipment

1.3.1 Materials
A. Microscope Slides and Coverslips; Microscope Slide Boxes B. Teasing Tools C. Water D. Stains E. Mounting Media F. Marking Pens G. Reference Samples

1.3.2 Equipment

A. Microscopes 1. Stereo binocular microscope or other magni cation 310x 2. Bright- eld light microscope and accessories B. Sectioning Equipment

1.4 Treatment Variations

1.4.1 Sample Preparation
(see AIC/BPG/PCC Spot Tests 10.4.1 and 10.4.2, 1990) A. Dispersed Fiber Sample (Directly from Object) Basic steps: (done with the aid of magni cation, usually 525x) e artifact is thoroughly examined. Initial observations about ber content are made. (Example: paper appears homogeneous or heterogeneous, colored bers present or not, ber clumps or shive present). A sample location on the artifact is selected after careful consideration of possible sites. Generally samples are taken from the verso and near the edge of the artifact. ere are numerous considerations which determine the most appropriate sample locations. e sample site is often dampened (if previous testing has shown staining will not occur) with deionized or distilled water applied with a small brush. A ne stainless steel tweezers or needle can be used to pull individual bers out of the paper. e bers are carefully transferred to a microscope slide prepared with a drop of water. Tools must be clean and inert. e sample site is placed under blotter and weight as necessary to minimize injury caused by sampling. e ber sample, now on the microscope slide, is teased apart with needles or probes in order to separate the sample into individual bers to the extent possible. Placing the microscope slide on top of a dark background can help visualize the degree of separation. Let the drop of water on the microscope slide evaporate prior to the application of stain, reagent or mounting media. Low heat, warming tray or room temperature all work well. Protect sample from contamination during drying process. B. Fiber Staining A standard ber staining technique is to apply a few drops of the stain solution to the dispersed ber sample on a glass microscope slide. Place a coverslip over the sample, lowering it at an angle to avoid creating air bubbles. Allow the slide to stand 12 minutes then drain o excess liquid, preferably by tilting the long edge of the slide into contact with a blotter or paper towel. C. Slide Labelling D. Permanent Mounts E. Reference Collection F. Disintegration of Dicult Fiber Samples G. Cross Sectioning Cross sectioning can provide useful information for the identi cation of many bers. Often it is not a conclusive test but cross sectional shape can provide con rmatory evidence. ese techniques are primarily designed for textile and ethnographic materials. 1. Plate Method is is the quickest and least expensive way to section a sample. Materials: 1) a plate 1" x 3" (25 x 75mm) the same size as a microscope slide but .010.020" thick (about 0.5mm) with holes drilled in it. e holes are .0350.40" in diameter (about 0.75 mm) made with a No. 65 or No. 60 drill respectively.

2) needle threader or thread 3) new single edge razor blades Note: the plate can be made of smooth shim brass or plastic. inner plates have diculty in holding the ber plug and thicker plates interfere with the transmission of light. With regard to hole size, small holes are dicult to thread and large holes tend to lose the ber slice. Procedure: Pull a tuft of bers through the hole in the plate with either a loop of thread (of known identity such as wire laments, sewing thread, polyester thread, etc.) or with a needle threader. e tuft of bers must be tightly jammed in the hole to insure that it remains after the top and bottom have been sliced o. If the tuft can be easily pulled through the hole than the nished slice will fall out easily. If the plug is too large the thread or needle threader will break. e tufts on each side of the plate are cut as ush as possible with a new single edge razor blade. It works well to cut the side with the needle threader rst. Contrast of the ber cross sectional shape can be enhanced by use of uids between the sample and the coverslip. e background of light, bright bers can be darkened by using a drop of liquid with a low refractive index such as n-decane (1.41) or dibutylphtalate (1.49). Dark, dull bers will appear black against a light background if a liquid of high refractive index, such as bromonaphthalene (1.66) is used. 2. in Cross Sections is method requires the use of a mechanical microtome - either rocking, rotary or sliding type. Basically, the microtome cuts sections 1 micron or greater in thickness. e individual sections are the transferred to a microscope slide for viewing.

3. Other methods include hardy microtome, and grinding embedded samples.

1.4.2 Selected Stains Reagents

A. Safranin-O 0.1% Safranin-O in water Various formulations, some use 50% ethanol is is a non-speci c plant stain used to enhance ber morphology. All plant parts stain red to pink. It can be used to make permanent slide mounts. B.Toludine B 0.1% aqueous solution is is general stain for woody tissue. Primary cell walls stain purple and secondary walls blue to blue-green. It can be used to make permanent slide mounts. C. Gra-C-Stain Integrated Paper Services, 101 West Edison Avenue, Suite 250 P.O. Box 446, Appleton, WI 549120446 One of the most common all purpose stains used by paper ber microscopists. A dispersed ber sample is stained and the color reaction is observed with transmitted light. Yellow indicates high lignin content. is typically includes mechanical or semi-mechanical wood pulp and jute bers. Raw grass, leaf or shive bers can also stain yellow. Partly puri ed wood, straw, grass or jute bers stain less yellow and show greenish, orangeish, or brownish colors. A color shifty from yellow to green to blue to red is an indication of the degree of

processing and reduction in the lignin content of the ber of the pulp. Blue indicates well puri ed pulp. is can include wood, grass and leaf bers.

Red indicates absence of lignin. is inherently includes cotton and the bast bers (except jute): ax, hemp, ramie, kozo and also includes: high alpha celluloses and highly bleached leaf bers (manila hemp or abaca). e stain cannot be used to make permanent slide mounts.

(see AIC/BPG/PCC 10. Spot tests p. 1416) D. Herzberg Stain (see AIC/BPG/PCC 10. p. 1617) E. Azo Stain (Yorsten and Green Stain) Institute of Science and Technology, 500 10th Street., NW tlanta, 30318-5794

Speci c stain to con rm unbleached sul te bers. Unbleached sul te bers stain red or pink while all other bers stain clear or colorless. F. 17.5% NaOH Used to distinguish between mitsumata and gampi bers. (see AIC/BPG/PCC 10. p. 17) G. Dupont Fiber Stain #4 Pylam Products Co., Inc., 1001 Stewart Avenue, Garden City, NY 11530 is stain is speci cally intended to be used for the identi cation of synthetic bers. It is most useful for the identi cation of nylon, rayon and cellulose acetate. Boil large sample in a beaker or in a test tube on a hot plate for a few minutes. Withdraw sample and rinse with water. Observe color reaction with re ected light. is procedure is designed for large sample size but the technique can be adjusted, with experience, to use on a micro scale. Place sample on microscope slide. Drop stain onto a sample forming a puddle around the ber. A ratio of twenty parts stain to ber is recommended. Heat the slide (and sample) on a hot plate. Rinse sample with water using a pipette to clear stain. Although the stain is intended to be observed with re ected light, the stain can sometimes be observed with transmitted light. e stain has a long shelf life. Shake stain prior to use to thoroughly re-mix settled out portion. Color reactions: nylonred rayonblue cellulose acetateorange polyesterpale yellow/yellow tan/beige acrylicbeige ole nlight tan wood/cottongreen glassdoesn't stain H. Shirlastains A,C,D and E

Crosrol, Inc., P.O. Box 6488, Tower Drive, Greenville, SC 29606 Designed to be used directly on textile threads. Color reaction is viewed in normal re ected light without the aid of a microscope. May be able to adjust technique to use on micro sample. Shirlastain A - for the identi cation of non-thermoplastic bers, i.e. cotton, wool and other natural bers; viscose rayon and other regenerated bers. Shirlastain C - for better distinction between natural cellulosic bers such as cotton, ax, hemp and jute. Shirlastain D - for distinction between cotton and spun viscose rayon. Shirlastain E - for the identi cation of thermoplastic bers (nylon, cellulose acetate, etc.)

1.4.3 Analysis of Fiber Mixtures

A. Counts B. Weight Factors

1.4.4 Other Tests

A. Drying/Twist Test for Bast Fibers e direction bers twist upon drying is sometimes used in the identi cation of bers, particularly to dierentiate between ax and hemp in the textile industry. Materials: water, hot plate, tweezers Procedure: Ultimate bers or thin ber bundles 58 cm in length are immersed in warm water for a few minutes. A ber is withdrawn and one end held in place on a hot plate (low) and the other free end is directed towards the observer. Direction of twist upon drying is observed. A dark background is helpful. Results: Flax and ramie twist clockwise. Hemp and jute twist counterclockwise. B. Scale Casts With Clear Nail Polish Often it is dicult to see the scale pattern on animal hair bers, especially those that are dyed dark, densely pigmented, or those that have a wide medulla. Materials: clear nail polish (Hard as Nails, Strong Nails, etc.) Procedure: A thin layer of the clear nail polish is brushed evenly over a microscope slide. Let the slide dry slightly. Place the ber on the coated side and allow to dry thoroughly. If possible, weight down the ber(s) as they are drying. When the slide has been allowed to dry the ber(s) can be removed an the slide examined under the microscope with transmitted light. Other methods include 3% gelatin solution in water and cellulose acetate photographic lm base softened with acetone. procedure is most easily performed with a ber length of 1 inch or greater and it is primarily designed for textile or ethnographic artifacts. e

1.5 Bibliography
1.5.1 Paper History 1.5.2 Fiber Microscopy
Appleyard, H. M. Guide to the Identi cation of Animal Fibers. Wira, Leeds, UK, 1960, 1978. Catling, Dorothy and John Grayson. Identi cation of Vegetable Fibres. London: Chapman and Hall, 1982. Collings, omas and Derek Milner. e Identi cation of Oriental Paper Making Fibres, e Paper Conservator, Journal of

the Institute of Paper Conservation 3 (1978): 5179. Collings, omas and Derek Milner. e Identi cation of Non-Wood Paper-Making Fibres: Part 2, e Paper Conservator, Journal of the Institute of Paper Conservation 4 (1979): 1019. Collings, omas and Derek Milner.. e Identi cation of Non-Wood Paper-Making Fibres, e Paper Conservator, Journal of the Institute of Paper Conservation 7 (1982/3): 2427. Collings, omas and Derek Milner.. e Nature and Identi cation of Cotton Paper-Making Fibers in Paper, e Paper Conservator, Journal of the Institute of Paper Conservation 8 (1984): 5971. Cote, W. A. et al. Papermaking Fibers, A Photomicrographic Atlas. Syracuse University Press, State University College of Forestry at Syracuse University, 1980. Florian, Kronkright and Norton. e Conservation of Artifacts Made from Plant Material. Getty Trust, 1990. Goodway, Martha. Fiber Identi cation in Practice, Journal of the American Institute for Conservation 26, no. 1 (1987): 2737. Gra, J. H. Color Atlas for Fiber Identi cation. Appleton, WI: Institute of Paper Chemistry, 1940. Isenberg, I. H. Pulp and Paper Microscopy. Appleton, WI: Institute of Paper Chemistry, 1967. Mauersberger, Herbert R. ed. Matthew's Textile Fibers - eir Physical, Microscopical, and Chemical Properties. 5th ed., New York: John Wiley & Sons, 1947. Menzi and Bigler. Identi cation of Bast Fibers, Ciba Review no. 123, 3335. Parham, R. A. and R. L. Gray. e Practical Identi cation of Woody Pulp Fibers. TAPPI Press, 1962. Parham, R. A. and H. M. Kaustinen. Papermaking Materials. An Atlas of Electron Micrographs. Appleton, WI: Institute of Paper Chemistry, 1974. Schaer, E. Fiber Identi cation in Ethnological Textile Artifacts, Studies in Conservation 23, no. 3 (1981): 571585. Strelis, I. and R. W. Kennedy. Identi cation of North American Commercial Pulpwoods and Pulp Fibers. Toronto: University of Toronto Press, 1967. Technical Association of the Pulp and Paper Industry, Atlanta, GA. T401: Fiber Analysis of Paper and Paperboard. Textile Institute, Manchester. Identi cation of Textile Materials. 7th ed., Manchester, 1985. Tullis Russel & Co. Papermaking Fibres. Scotland: Markinch Fife, 1950.

1.5.3 General Microscopy

Delly, John Gustav. Photography through the Microscope. Rochester, 1980, 1988. McCrone, Walter; McCrone, Lucy and John Gustav Delly. Polarized Light Microscopy. Ann Arbor, 1978.

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