Historical Silk Flags Studied by Scanning Electron ... - ACS Publications

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Historical Silk Flags Studied by Scanning Electron Microscopy-Energy Dispersive X-ray Spectrometry M. Ballard , R. J. Koestler, C. Blair, and N. Indictor 1

2

Department of Objects Conservation, Metropolitan Museum of A r t , New York, N Y 10028

Samples of colored silk taken from brittle flags in the National Museum of American History (Washington, DC) have been subjected to light microscopy and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDS). The presence of mordants, weighting materials, and colorants is discussed with reference to the embrittlement of the silk. The ash content of the samples is reported. Micrographs of individual fibers are examined. The correlation between fiber deterioration and elemental composition (as a reflection of possible manufacturing processes) is discussed.

S I L K F A B R I C S H A V E B E E N H E L D I N H I G H E S T E E M for centuries. T h i s c o n sideration outweighs some of the p r o b l e m s i n h e r e n t to the silk fibers, such as s u s c e p t i b i l i t y to damage f r o m l i g h t a n d e m b r i t t l e m e n t w i t h age. T h i s esteem has encouraged m u s e u m s to e x h i b i t s u p e r b examples of the t e c h nological a n d aesthetic achievements associated w i t h the silk w e a v i n g of past centuries. E v e n w h e n treated p o o r l y , some examples of silk art have s u r v i v e d quite w e l l . A m o n g 19th-century silks, C h i n e s e robes a n d silk e m b r o i d e r i e s are p o p u l a r collectors' i t e m s . F a r E a s t e r n silks have often s u r v i v e d export, r e v c u r r e n t address: Conservation Analytical L a b , Smithsonian Institution, Washington, D C 20560 C u r r e n t address: Chemistry Department, Brooklyn College, City University of New York, Brooklyn, N Y 11210 2

0065-2393/89/0220-0419$06.00/0 © 1989 A m e r i c a n C h e m i c a l S o c i e t y

Allen; Archaeological Chemistry IV Advances in Chemistry; American Chemical Society: Washington, DC, 1989.

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ARCHAEOLOGICAL CHEMISTRY

o l u t i o n , a n d the vagaries of use q u i t e w e l l . E u r o p e a n a n d A m e r i c a n silks of the same p e r i o d have not. I n contrast to the h e a l t h of F a r E a s t e r n silks, m a n y examples of E u r o p e a n a n d A m e r i c a n silk fabrics are s h r e d d e d , split, a n d i n u n e x h i b i t a b l e c o n d i t i o n . F i g u r e 1 is an example of a deteriorated 19th-century silk. S u c h degradation has b e e n ascribed to the t i n w e i g h t i n g ( I , 2), w h i c h was especially p o p u l a r i n the last half of the 19th c e n t u r y . Because the standard m e t h o d of a n a l y z i n g w e i g h t i n g processes requires gram quantities of silk, curators a n d conservators have b e e n reluctant to sacrifice samples. R e c e n t l y , w e d e m o n s t r a t e d the possibility of d e s c r i b i n g w e i g h t e d silks b y u s i n g scanning electron m i c r o s c o p y - e n e r g y dispersive X - r a y spectrometry ( S E M - E D S ) o n p r e p a r e d m o d e r n samples (3, 4). Several k i n d s of silk fibers, w e i g h t e d i n a v a r i e t y of ways, w e r e successfully analyzed i n a set of b l i n d experiments. T h e w e i g h t i n g procedures w e r e based o n recipes taken f r o m standard processes d e s c r i b e d i n the l i t e r a t u r e . T i n a n d i r o n c o m p o u n d s , along w i t h other inorganic substances, w e r e used i n the w e i g h t i n g treatments. It was generally possible to d i s t i n g u i s h b e t w e e n the w e i g h t i n g treatments e n t i r e l y o n the basis of E D S results. T h e methods u s e d are s i m i l a r to those used o n m o r d a n t e d (5-8) a n d m e t a l - w r a p p e d textiles (9, 10). Because of the success w i t h S E M - E D S , the D i v i s i o n of A r m e d F o r c e s H i s t o r y at the N a t i o n a l M u s e u m of A m e r i c a n H i s t o r y s u p p l i e d some actual, d e t e r i o r a t e d , accessioned m u s e u m m a t e r i a l for examination b y l i g h t m i -

Figure 1. A deteriorated 19th-century silk.



24.

421

Historical Silk Flags

B A L L A R D ET AL.

croscopy a n d S E M - E D S . A part of each s p e c i m e n was also analyzed for ash content. Some samples w e r e tested for dye class. T h e samples w e r e taken f r o m the vast group of m i l i t a r y flags transferred from the Q u a r t e r m a s t e r M u s e u m C o l l e c t i o n i n P h i l a d e l p h i a to the S m i t h sonian I n s t i t u t i o n b y the W a r D e p a r t m e n t i n 1919. T h i s donation of m i l i t a r y m a t e r i a l was so large that it was s h i p p e d b y railroad boxcar. A l l the flags s a m p l e d predate the year 1919. U n l i k e most silk fabrics, they can be d a t e d q u i t e accurately. T h e flags are also n o t e w o r t h y for t h e i r deteriorated state. M a n y a r r i v e d at the S m i t h s o n i a n I n s t i t u t i o n w r a p p e d i n b r o w n paper, l a b e l e d " p o o r c o n d i t i o n " . T h e i r fragmentary c o n d i t i o n , together w i t h t h e i r late 19th-century o r i g i n , has l e d the curatorial a n d conservation c o m m u n i t y to assume that the damage was the result of w e i g h t i n g d u r i n g the fabric manufacture. T a b l e I gives catalog n u m b e r s a n d descriptions of the flags f r o m w h i c h specimens w e r e o b t a i n e d at the N a t i o n a l M u s e u m of A m e r i c a n H i s t o r y , Washington, D C .

Experimental Details Samples (about 1-2 mm ) were taken from the specimens and arranged on spectroscopically pure carbon stubs in a manner that would permit viewing (either with optical microscopy or scanning electron microscopy). 2

S E M - E D S Analyses. After observation at about 40 X magnification through a light microscope (Wild M8), the samples were carbon coated and subjected to S E M - E D S analysis (AMRay 1600T equivalent with attached Kevex E D S ) . Generally, the operating conditions for the collection of E D S data were as follows: 15 kV, 200-s collection time, 2.56 Χ ΙΟ μπι (—0.25 mm ) excitation areas. For some sam ples, up to 10 replicate scans were performed at different spots. Sample preparation and data treatment have been described (4-9, J I). Photomicrographs and printouts of E D S scans were retained for files. 5

2

2

Ash Content. Samples were removed from the specimens and submitted for ash analysis (Schwartzkopf Microanalytical Laboratory, Woodside, NY). Samples were burned in oxygen at 900-1000 °C for about 0.5 h. Color Analysis. Samples were removed from the specimens and analyzed for the colorants according to methods described in references 12 and 13.

Results and Discussion Table I I lists the qualitative E D S results of the 14 specimens. O n l y elements of atomic n u m b e r > 1 1 w e r e detected. T h e results w e r e o b t a i n e d as n o r m a l i z e d percentages according to the software p r o g r a m ( A S A P ) usually e m p l o y e d i n analyses from this laboratory.



— —

—. —

69143

_

81745W07 81759W59

Unknown

RWW81759W52

81745W00 81711W11

Unknown

W8 W9

W10

Wll

W12 W13

W14

"Repp is warp-faced plain weave fabric.

64127

81711W10 81745W06 81745W07

W5 W6 W7

—

—

64127

— —

81711W14 Unknown 81711W10

W2 W3 W4

— Silk repp", from U . S . flag, (38 stars, 13 stripes, "Corps of Cadets" on 7th stripe) Silk repp, as in W l Silk repp, C i v i l War Silk repp, 3rd Regiment Q . M . National Color, 36-star flag Silk repp, as in W 4 Silk repp, H . Q . of U . S . A Silk repp, Regimental Colors, 45-s tar flag, U . S . Reg. of Inf. Silk repp, as i n W 7 Silk repp, U . S . flag (stars and stripes) Silk repp, Flag embroid. " H o n - aux Américains," red and white stripes, Storage Unit No. 1449 Silk repp, U . S . National Standard, post 1912 Silk repp, painted flag Silk repp, Sheridan, Commander of the army flag Silk repp

Description

Table I. Description of Flags Sampled Inventory No.

81711W14

Catalog No.

Wl

Sample No.

1875-1900 Nov. 1, 1883Aug. 3, 1888 unknown

Blue Blue Cream

July 4, 1912-1920

July 4, 1863July 3, 1865 WW I

ca. 1884 July 4, 1896July 3, 1908

July, 1865

unknown July 1863-

—

Date July 4, 1877July 4, 1890

Red

Cream

Cream Cream

Cream Blue Red

Cream Cream Red

Cream

Color


24.

B A L L A R D ET AL.

423

Historical Silk Flags Table II. Qualitative E D S Results


Sample No. Wl W2 W3 W4 W5 W6 W7 W8 W9a W9b W10 Wll W12a W12b W13a W13b W14

Na

Mg

Al

Si

Ρ

—

—

+

—

-

+

+ + + + + + + + + + + + + + + + +

-

+ +

+ +

fl

—

(+)

-_ (+)

4-

-

+ +

(+ ) (+ )

(+)

—

(+ ) (+ ) + + +

&

_

+

(+) + (+)

-_ -—

s + + + + + + + + + +

+ + + + + + + + + +

(+) + + + + + + -h + + + + +

Cl

κ

Ca

Fe

Sn

—

(+) (+)

+ (+ ) + + + + +

+ (+ )

+ +

(+) (+)

+ -+

(+) +

-

+ (+)

(+)

-

(+) + (+)

-

+

(+)

-

+ +

-

(+)

-

-

(+ ) + + (+ ) (+ ) +

+ +

-

-

(+) + (+) — (+) — + (+) SYMBOLS: + +, present in significant amounts (>30% of elements of atomic no. >11); +, present; - , Absent (not detected); and ( + ), possibly present (ca. 5% of elements of atomic no. >11). "Cream specimen: a is the darker (stained?) area; b is the lighter (unstained?) area. Blue specimen: a is the lighter (impainted) side; b is the darker (painted) side. Blue specimen: a is the lighter (more faded?) side; b is the darker (less faded?) side. (Under a light microscope, at ca. 40 X magnification both sides look alike.) c

—

(+)

-

fc

c

T h e w i d e v a r i e t y a n d variability of elements detected for i d e n t i c a l l y c o l o r e d silks i m m e d i a t e l y suggested that the methods o f c o l o r i n g these h i s torical flags w e r e not at a l l standardized. O f the three b l u e specimens, two contained i r o n , one d i d not. O f the three r e d samples, one contained i r o n , one c o n t a i n e d b o t h i r o n a n d t i n , a n d one contained n e i t h e r i r o n n o r t i n . T h e c r e a m samples showed four w i t h i r o n , one w i t h t i n , a n d three w i t h neither iron nor tin. F o r three o f the specimens E D S data w e r e collected i n two different areas: • S p e c i m e n 9 (cream colored) s h o w e d greater discoloration i n one area (9a) than i n area (9b). T h e E D S data s h o w e d a larger variety o f elements i n the d i s c o l o r e d p o r t i o n , possibly because o f the presence of s o l u b l e salts (Na). • S p e c i m e n 12 (painted blue) appeared to b e p a i n t e d d a r k e r b l u e o n one side (12b), a n d l i g h t e r b l u e o n the other (12a). T h e E D S data i n d i c a t e d no difference i n the e l e m e n t a l d i s t r i b u t i o n s o n e i t h e r side.


424


• S p e c i m e n 13 (blue) appeared similar o n b o t h sides u n d e r the light microscope at about 40 X magnification. B o t h sides s h o w e d traces of i r o n , s i m i l a r to the p r e c e d i n g result.


T a b l e I I I shows raw data for s p e c i m e n 12b (painted blue) from scans p e r f o r m e d o n the p a i n t e d side. Variations i n the n u m e r i c a l values illustrate the extent o f n o n u n i f o r m i t y i n the sample a n d the general l e v e l of r e p r o d u c i b i l i t y achievable i n p e r f o r m i n g such analyses. T w o of the specimens, W 1 0 (cream) a n d W l l (red), showed substantial amounts of t i n . T h e t i n i n W l l is p r o b a b l y m o r d a n t , b u t i n W 1 0 i t appears to b e present as a w e i g h t i n g m a t e r i a l , as suggested b y the results p r e s e n t e d i n T a b l e IV. Table I V shows the results of ashing the textile samples i n oxygen at 9 0 0 - 1 0 0 0 °C for about 0.5 h . T h i s table shows that, of the 14 specimens tested, o n l y W 1 0 was f r o m a w e i g h t e d silk. T h e ash content was consistent w i t h w h a t m i g h t b e expected from m o r d a n t i n g a n d accretions gathered d u r i n g the l i f e t i m e of the silks. N o attempt was m a d e w i t h these samples of to r e m o v e d i r t or accretions that m a y have h a d a small effect o n the E D S a n d ashing results. A c o m p a r i s o n o f sample W 1 0 w i t h sample W 8 u s i n g S E M ( F i g u r e 2) confirms that no i d e n t i f y i n g surface characteristics distinguish w e i g h t e d from u n w e i g h t e d silk. T h e p r o m i n e n c e of sulfur, the major e l e m e n t i n a l l scans, reflects 1. its presence i n the backbone chains of the fibroin (14) ( m e t h i o n i n e , etc.) 2. possible residue of b l e a c h i n g or other processing left from the original manufacture 3. that it was a possible c o m p o n e n t of the d y i n g or m o r d a n t i n g process Table ΙΠ. E D S Data for Sample 12b Sample No.

Al

Si

S

Cl

Κ

Ca

Fe

W12b W12bA W12bB W12bC W12bD W12bE W12bF W12bG W12bH

4.41 5.39 4.74 6.21 4.95 6.71 3.28 4.89 4.26

16.74 16.47 15.35 18.15 15.52 18.13 16.01 17.98 16.90

60.56 51.05 52.38 50.87 54.89 46.99 56.79 52.39 50.19

1.24 1.86 2.59

1.60 3.78 3.31 1.42 1.30 4.08 5.30 3.18 2.23

10.84 10.55 17.89 12.90 17.85 14.01 11.25 14.40 15.05

4.62 10.90 3.74 10.46 3.1 7.23 3.80 3.68 6.59

—

2.34 2.86 3.58 3.48 4.78

NOTE: All values are percents. All elements are of atomic number >11; data were obtained from ASAP routine, normalized; normalization factors varied from 0.86-0.91. Na, Mg, P, and Sn were not present in any sample. All samples are from the painted blue specimen, darker (painted) side.


24.

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425


4. that it was a possible c o m p o n e n t of the w e i g h t i n g process 5. that it was a possible c o m p o n e n t of soil, d i r t ,

atmospheric

p o l l u t i o n , etc. that accumulated at the fabric surface.


I n previous reports (4-8), w e discussed the p r o b l e m s of d i s t i n g u i s h i n g the presence of mordant i n historical textiles, the confounding effects of Table IV. Ash Content of Flag Samples Sample No. Wl W2 W3 W4 W5 W6 W7 W8 W9 W10 Wll W12 W13 W14

Sample Color Cream Cream [Cream] Red Cream Blue Red Cream Cream Cream Red Blue Blue [Cream]

fc

fc

% Ash

a

Ash Color

0.61 0.50

Black Rust

2.79 1.13 0.42 1.32 1.77 1.81 46.49 4.32 0.89 0.37

Rust Rust Rust White Black Rust White Rust Rust Rust

—

—

—

—

"Samples burned under oxygen at 900-1000 °C, ca. 0.5 h. No sample taken. &

Figure 2. Scanning electron microscopic image of sample W10.



426


accretions, a n d the possible use of sulfur as an i n t e r n a l standard (present as part o f the fiber chains i n a l l silk a n d w o o l samples). A l t h o u g h the p e r c e n t sulfur i n p u r e , u n t r e a t e d silk is far less t h a n i n w o o l , it always represents a v e r y substantial percentage of the E D S analyzable elements present. I n silk samples, it is i n v a r i a b l y o b s e r v e d a n d falls w e l l w i t h i n the range of detectability. H o w e v e r , because sulfur may b e p a r t of the b l e a c h i n g a n d d y e i n g processes (15-18), a n d p r e s e n t as part of the historical accretion, the ass u m p t i o n of sulfur as an i n t e r n a l standard m u s t b e made w i t h great c a u t i o n . I n this set o f E D S data, w i d e variations i n sulfur w e r e o b s e r v e d a n d , except for one sample (W10), sulfur h a d the highest p e r c e n t c o m p o s i t i o n o f all elements of atomic n u m b e r > 1 1 . I n that sample (W10) i n w h i c h sulfur was o b s e r v e d i n trace amounts (about 5%), the w e i g h t i n g agent was so abundant that the amount of sulfur detected r e p r e s e n t e d o n l y a small a m o u n t of the total d e t e c t e d material. T h e percentage of t i n o b s e r v e d i n the w e i g h t e d s p e c i m e n was w i t h i n the range o b s e r v e d a m o n g t i n - w e i g h t e d standards that h a d b e e n p r e v i o u s l y analyzed (cf. Table V , reference 4). S o m e o f the colorants w e r e analyzed w i t h techniques d e v e l o p e d b y S c h w e p p e (12, 13), a n d i n c o n j u n c t i o n w i t h descriptive i n f o r m a t i o n d e l i n eated i n the Color Index (20). T h e tests are essentially spot tests that are done b o t h separately a n d sequentially. T h e spot tests indicate the presence of sulfonic a c i d groups i n the dyestuffs. T h e colorants r e p r e s e n t e d about 1 - 5 % of the total w e i g h t of the sample.

Table V. D y e Analyses Sample

Color

W4

Red

Testing H 0 : si. sol.; C H O H : insol.; cone. C H C O O H . si. s o l ; cone. N H : soin, yellow, fiber colorless; + C H O H : pale red; cone. H S 0 : soin, red-violet, fiber dark red; + H 0 : soin. si. yellow, fiber bright red. Indicative of Ponceau R R (C. I. Acid Red 26) H 0 : soin. si. yellow, fiber insol. ; C H O H : soin, pink, fiber, n.r.; cone. CH3COOH; n.r.; cone. N H : soin, red; cone. H S 0 : soin, red, fiber dark red; + H 0 : soin, yellow, fiber red. Indicative of: Ponceau R R (C. I. Acid Red 26) H 0 : n.r.; C H O H : soin, pink, fiber, n.r.; cone. CH3COOH: n.r.; cone. N H : sol. pink, fiber colorless; + cone. Sol. colorless, fiber colorless Indicative of Fast Red AV (C. I. Acid Red 88) H 0 : i n s o l ; C H O H : n.r.; cone. C H 3 C O O H : n.r.; cone. N H : soin, and fiber nearly colorless; + cone. CH3COOH: sol. blue; cone. H S 0 : soin, and fiber brown-red; + H O : sol. blue. Indicative of Water Blue I N (C. I. Acid Blue 93) 2

2

5

3

3

2

2

5

4

2

W7

Red

2

2

5

3

2

Wll

Red

2

4

2

2

5

3

CH3COOH:

W6

Blue

2

2

5

3

2

4

z


24.

BALLARD ET AL.


427

E n g l i s h , F r e n c h , a n d G e r m a n 19th-century dye texts (16-19) suggest a p e n c h a n t for the use of sulfuric a c i d , not o n l y i n the d y e i n g process to m a i n t a i n an acidic p H , b u t m o r e i m p o r t a n t l y , as a final " s o u r " or c l e a r i n g rinse.


Summary 1. N o standard process for the use of colorants o n flags was d i s covered: • R e d (three examples): O n e had i r o n (traces); one h a d i r o n (traces) a n d t i n ; one h a d n e i t h e r i r o n nor t i n . • R l u e (three examples): T w o h a d i r o n (no tin); one h a d n e i t h e r iron nor tin. • C r e a m (eight examples): F o u r h a d i r o n ( t r a c e - s m a l l amounts) a n d no t i n ; one h a d t i n (large amount) a n d no i r o n ; three h a d n e i t h e r i r o n n o r t i n . 2. O n l y one silk s p e c i m e n from this group (W10) a p p e a r e d to be w e i g h t e d . T h e w e i g h t i n g agent was t i n i n some f o r m . I n this sample, the most abundant e l e m e n t (of those elements of atomic n u m b e r >11) was t i n . I n a l l other specimens, the most abundant e l e m e n t (of those elements o f atomic n u m b e r >11) was sulfur. 3. L i g h t a n d S E M images of the w e i g h t e d silk s p e c i m e n w e r e c o m p a r e d to other specimens that w e r e not w e i g h t e d . N o obvious distinctions w e r e r e v e a l e d , despite the presence o f about 5 0 % ash i n the case o f the w e i g h t e d silk a n d o n l y about 1% ash i n other cases.

I n some cases, the deteriorated c o n d i t i o n of historic silk flags m a y be the result of w e i g h t i n g , b u t other factors m u s t be i m p o r t a n t because e v e n these l i m i t e d data show that m a n y silk flags contain silks that are not w e i g h t e d . E x a m p l e s of factors other than w e i g h t i n g that may account for the d e t e r i o r a t e d c o n d i t i o n of the banners are original m a n u f a c t u r i n g p r o c esses ( d e g u m m i n g , b l e a c h i n g , etc.); storage (indoor air p o l l u t i o n , t e m p e r a t u r e - r e l a t i v e h u m i d i t y c y c l i n g , etc.); a n d conservation practices of the past. T h e w i d e l y h e l d o p i n i o n that w e i g h t i n g is the cause of silk d e t e r i o r a t i o n may give way, w i t h further study, to an u n d e r s t a n d i n g of deterioration as a result of acid treatments or other m a n u f a c t u r i n g processes u s e d i n E u r o p e a n a n d A m e r i c a n workshops d u r i n g the late 19th century.


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References 1. Howitt, F. O. Bibliography of Silk; Hutchinson's Scientific and Technical Pub lications: London, 1946; Chapter 8. 2. Ross, J . E.; Johnson, R. L.; Edgar, R. Text. Res. J. 1936, 6, 207-216. 3. Ballard, M.; Koestler, R. J.; Indictor, N . Preprints of Papers, 13th Annual Meeting; American Institute for Conservation of Historical and Artistic Works: Washington, DC, 1985; p 155. 4. Ballard, M.; Koestler, R. J.; Indictor, N . Scanning Electron Microsc. 1986, 2, 499-506. 5. Koestler, R. J.; Sheryll, R.; Indictor N . Stud. Conserv. 1985, 30, 58-62. 6. Indictor, N.; Koestler, R. J.; Sheryll, R. J. Am. Inst. Conserv. 1985, 24, 104-109. 7. Koestler, R. J.; Indictor, N.; Sheryll, R. J. Am. Inst. Conserv. 1985, 24, 110-115. 8. Williams, E . T.; Indictor, N . Scanning Electron Microsc. 1986, 2, 847-850. 9. Indictor, N.; Koestler, R. J . Scanning Electron Microsc. 1986, 2, 491-497. 10. Indictor, N.; Koestler, R. J.; Blair, C.; Wardwell, A . Textile History 1988, 19(1), 323 11. Goldstein, J.; Newbury, D . E.; Echlin, P.; Joy, D . C.; Fiori, C.; Lifshin, E . Scanning Electron Microscopy and X-Ray Microanalysis; Plenum: New York, 1984. 12. Schweppe, H . Identification of Dyes on Textile Materials; Course, Conservation Analytical Laboratory, Smithsonian Institution, 1985, 1986. 13. Schweppe, H. In The Analytical Chemistry of Synthetic Dyes; Venketararian, K., Ed.; Wiley: New York, 1977; Chapter 2. 14. Carboni, P. Silks: Biology, Chemistry, Technology; Walter, Κ., translator; Chap man and Hall: London, 1952. 15. Ganswindt, A . Dyeing Silk, Mixed Silk Fabrics and Artificial Silks; Salter, C., translator; Scott, Greenwood and Son: London, 1921. 16. Hummel, J . J . Colouring Matters for Dyeing Textiles, revised ed.; Hasluck, P. N., Ed.; Cassell: London, 1906. 17. H u m m e l , J . J . Mordants, Methods, and Machinery Used in Dyeing, revised ed.; Hasluck, P. N., Ed.; Cassell: London, 1906. 18. Hurst, G . H. Silk Dyeing, Printing, and Finishing; George Bell and Sons: L o n don, 1892. 19. Knecht, E.; Rawson, C.; Loewenthal, R. A Manual of Dyeing, 2nd ed.; Charles Griffin: London, 1910. 20. Color Index, 3rd ed.; Society of Dyers and Colourists: Bradford, England, and American Association of Textile Chemists and Colorists: Research Triangle Park, N C , 1971. RECEIVED for review June 11, 1987. ACCEPTED revised manuscript February 25, 1988.


Historical Silk Flags Studied by Scanning Electron ... - ACS Publications

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