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The Effect of an Alkaline Rinse on the Aging of Cellulosic Textiles

The Effect of an Alkaline Rinse on the Aging of Cellulosic Textiles

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Ira Block

ABSTRACT—In Part I of a four-part series, the author reviews the literature on the aging of cellulose, notes the reasons why an alkaline rinse should be effective in retarding the aging of cellulosic textiles, and presents preliminary results which indicate that treating new cotton and rayon cloth with a dilute calcium hydroxide solution can increase their resistance to accelerated aging.In Part II the results of a more detailed study of the effect of a calcium hydroxide rinse on the strength retention and color change of new cellulosic fabrics are reported. It is shown that the treatment is successful in retarding strength loss, but that it has no effect upon color change.


1.1 INTRODUCTION DURING A SABBATICAL YEAR tenure at the Conservation Analytical Laboratory of the-Smithsonian Institution, the author studied the efficacy of the deacidification of cellulosic textile materials as a conservation treatment. In this series of papers the some-what unexpected results of this investigation are reported. In Part I, the reasons for believing that deacidification would be effective are discussed, and preliminary results on new rayon and cotton cloth are presented. Part II reports a detailed examination of the kinetics of strength loss and color change. Part III will report the effect of a calcium hydroxide rinse on artifically aged cellulosics, which turns out to be less effective than on new cloth. This leads to the prediction that an alkaline rinse will not be more effective than soaking in deionized water when treating old cellulosic fabrics. Part IV shows that the conclusions reached in Part III are valid and explains why. It is shown that provision of an alkaline reserve is effective in retarding the degradation of new fabrics, but is useful for old fabrics only in protecting against the absorption of acidic species from the environment. In a recent review article, Daniels1 pointed out that as early as 1898 it was known that the acidic impurities in paper could greatly increase its rate of deterioration. Shaw and O'Leary2 noted in their investigations on the stability of book papers that ―calcium carbonate pigments had a protective or inhibiting effect in the aging test,‖ and

and the usual procedure for the care of textiles. other work leads to this conclusion. 7 and organometallic compounds.17 In addition to the literature on paper conservation. pure water can improve its color.‖ . et al19.‖ They note that the degradation of cotton is greater in air than in nitrogen and is enhanced by moisture. However. and can be used without shortening the life of the paper. Peters and Still18 point out that it ―is difficult to differentiate the thermal degradation at low temperatures from the normal aging of cellulose.10–15 as was once the case for the treatment of paper. These materials are often washed as part of their conservation treatment. This procedure appears to have been originally recommended by Pahir in a 1925 patent and rediscovered by Wilkie in 1929. since cellulosic fibers such as cotton.Barrow's3 investigation of the causes of deterioration of books showed that treatment with an alkaline solution could increase the life of books by neutralizing the acids present in the paper and by providing an alkaline reservoir which would shield against further acidification. Although it is well known that washing or rinsing old paper in clean. 9 The above work is of some significance to the conservation of textile products. conservators would be provided with an important new tool for treating many fabrics. Arney. it has been only recently that the alkaline treatment of nearly neutral papers has been investigated. Tang and Jones4 noted that ―Distilled or deionized water passed through a column of calcium carbonate chips becomes acceptable for paper washing. The literature indicates that it should be possible to stabilize cellulosic textiles.8. and other workers have investigated the protection afforded paper when rinsed with amines6. jute and rayon comprise an appreciable fraction of textile artifacts. for which washing is indicated as part of the conservation treatment.16 has been to use water of as high a quality as possible. linen. a mildly alkaline rinse could enhance the resistance of cellulosic textile fibers to degradation at ambient temperatures. and that both types of processes are affected by deacidification treatments. and suggest that the formation of carboxyl (− COOH) and carbonyl (>C = 0) groups is important in the degradation of cellulose. They further state that their results suggest that ―the influence of acidity on the rate of natural paper degradation would be the same regardless of which degradation process predominates at room temperature. by a mild alkaline rinse which would neutralize the internal acids.‖ Wilson. et al5 have discussed the efficacy of magnesium bicarbonate treatment of old papers. strength and folding endurance. 20 argue that the degradation of cellulose in paper is due to both oxygen-dependent and oxygen-independent processes. if when washing is indicated.

respectively. The problem is to determine how high a temperature can be considered ―low‖. the author has endeavored to apply a test method which would not introduce extraneous . Unfortunately. In this work it was found that dry baking at 100°C for one week caused essentially no change in fabric properties. Davidson and Standing22 hypothesized that ―hydrolysis of the glycosidic linkages is catalysed by hydrogen ions derived from the ionization of the free (unneutralized) carboxyl groups in the oxycellulose molecule. It should be noted that at this writing the only accepted standards for aging of textile materials are those promulgated by the American Association of Textile Chemists and Colorists (AATCC). yet proceed rapidly enough to allow results to be obtained in a reasonable time period. AATCC 26-1978 and 111A.D-1978. Davidson and Nevelle21 studied the degradation of acidic oxycelluloses. decided to conduct the aging at 150°C at low humidity. in agreement with the data of Kerr.40 However.25–38 Since artificially degraded fabrics do not duplicate naturally aged materials in all respects (cf reference 39). therefore. are specifically devised for determining the resistance of textiles to sulfur dyes and weather resistance. a review of the literature25– 38 indicates that temperatures below 180°C do not introduce chemical reactions which are not present at room temperature. cellulosic textiles do not age rapidly enough at 100°C to permit a reasonable time frame for the experiment. These tests.‖ It was shown that oxycelluloses containing the free acid were unstable even when stored at room temperature and low relative humidities. supported these conclusions. has been intensively studied. Thus. They were able to show that a major cause of the degradation of cellulose is the formation of carboxyl groups on the C6 carbon of the anhydroglucose unit.H. It was. and that conversion of the carboxyl groups from the free acid to the sodium salt form greatly stabilized the cellulose. and are not applicable to comparisons of the relative effectiveness of methods for reducing the rate of degradation of fabrics.C.2 EXPERIMENTAL THE ACCELERATED AGING of fibrous materials by oxidation in both dry and humid ovens at various temperatures.23 More recent studies by Shenai and Shah24 among others. 1. As noted earlier. with and without light.18 low temperature thermal degradation is almost identical to normal aging. et al.B. it is necessary to choose a test protocol in which the chemical processes do not differ substantially from those occurring at room temperature.In a series of investigations. Wilson and Parks25 noted that artificial aging at 100°C ―with some moisture‖ gave results that were closer to naturally aged paper than did artificial aging at 90°C and 50% R.

266) supplied by Testfabrics Inc. it was decided to limit this study of the effect of elevated temperature and low humidity.2 Reagents The reagents used were calcium hydroxide [Ca(OH)2] and sodium carbonate [Na2CO3] supplied by Fisher Scientific Co.01% (w/v) solution. shaking and allowing the solids to settle overnight. The cloths were washed and dried twice as per AATCC Test Method No. 124-1978. 400) and a plain weave. . Calcium hydroxide solution was prepared by adding at least three grams of solid to one liter of water. while still taking into account the important role played by moisture.2.4 ml were made up to one liter to give an approximately 0. 1. Fifty milliliters of the saturated solution were made up to one liter to provide an approximately 0. 1.. Solution pH was maintained by dropwise addition of the saturated solution [(Ca(OH)2 or Na2CO3 as appropriate] to the rinse bath. A saturated solution of sodium carbonate was prepared in a similar manner.5.2. Although it is recognized that other environmental factors such as light.2. and deionized water of about 1 megohm resistance. different treatments can be compared with a minimum of extraneous factors.1 Fabric The fabrics in this study were a plain weave. 80 × 80 cotton print cloth weighing 103 g/sq m (no. 1. Nine of the specimens were added to a one-liter bath of solution maintained at 30°C by circulation of the solution through a coil of polyethylene tubing immersed in a temperaturecontrolled bath. In this way. and 1.3 Application The test fabrics were cut to the proper dimensions with an NAEF die.chemical reactions and which would permit comparisons between treatments.01% (w/v) solution with a pH of 9–9. 80 × 80 spun rayon cloth weighing 132 g/sq m (no. relative humidity and atmospheric gases will affect the results of both natural and accelerated aging.

samples were stored in a closed container over silica gel until cool. Since the oven was open to the atmosphere in the laboratory (approx.39 shows. After cooling samples were stored in sealed plastic bags until testing. 1.2.27 Upon removal from the oven after baking.0 and 9.19 drained and dried overnight on glass fiber screens.For treatment A.5 Tear Testing Prior to testing. tear testing is more rapidly performed than tensile testing. removed from the bath. and soaked an additional hour in the Na2CO3 solution at 30°C to precipitate CaCO3. given a fast rinse in deionized water to remove surface solution. as the work of Berry. The degradation of the samples was measured by the loss in tear strength. This parameter was chosen since. Each of the specimens in a sample was supported on a glass fiber screen while being baked in a Fisher Isotemp forced draft oven at 150 ± 2°C. For treatment B.5. et al. The Ca(OH)2 converts to CaCO3 by reaction with the carbon dioxide in the atmosphere. in keeping with the recommendation of Wilson and Parks25 and the work of Williams. drained and dried overnight on glass fiber screens. 1. at 21% and 65% RH. the bags containing the samples were opened and the samples were stored at standard conditions of 21°C and 65% RH for at least twelve hours. both tear strength and tensile strength follow essentially the same kinetics. removed from the bath. 1. the specimens were soaked for 2 hr in Ca(OH)2 solution maintained at a pH between 9.2. specimens were soaked for 3 hr in Ca(OH)2. Tear testing was performed on an Elmendorf Apparatus as per ASTM D 1424–63. and tearing more closely approximates the stresses put on a fabric when handled than does tensile testing. et al. 21°C and 55% RH) the relative humidity in the oven varied.3 RESULTS AND DISCUSSION . but remained low.4 Aging Each sample was made up of three specimens of fabric chosen at random from the treated or untreated materials as applicable.

however.‖ . The logarithm of the percent strength retained is plotted versus the logarithm of the baking time. It was found that the untreated fabric samples had a pH of 5. and the way in which deacidification treatments may alter the various deterioration processes is.5 after drying overnight. The major results of this portion of the study are shown in Fig. For as Arney. Subjective evaluation of the hand indicated that the treatments did not cause harshening or brittleness. as yet. 1.0. and would. so that the results should not be interpreted as a quantitative description of the chemistry of the system.19 have noted ―the influence of acidity on the thermally induced deterioration of [cellulosics] appears to be more complex than has previously been assumed. It should be noted. that the pH of samples immediately after soaking was between 8. Thus. The surface pH of the samples was measured with an lonalyzer fitted with a flat-bottomed electrode. about 2% calcium carbonate on weight of fabric (owf). relate directly to the reaction rates. This corresponds to an equation of the form Fig. not thoroughly understood.0 and 8.0 and 7. the 2hr or the 3-hr soak provided the maximum uptake of calcium.5 to 6. Tear strength and color of the treated samples was measured and found to be essentially the same as the control fabric. that tear strength is a complex function of fabric and yarn structure as well as fiber strength. et al.5. if tear strength were related directly to the chemistry of the system. . and that the pH fell to between 7.IN A SERIES OF preliminary experiments it was found that soaking in Ca(OH)2 solution for 2 hours gave the same weight gain as soaking for five hours.

and (3) the point at which Y becomes sensitive to T. conclude that . the chemistry of the rayon system may be different from that of the cotton. we may conclude that identical processes are at work in the cotton samples irrespective of treatment. and that the rayon samples are subject to the same processes irrespective of treatment. 1. (2) a later period in which Y decreases linearly with T. Thus we may. At some point. (T). is insensitive to the log(Baking Time). The slopes of the lines are: Regression analysis indicates that there is no significant difference between the slopes of the three lines for each of the respective fibers. The curves of Fig. (Y). However. again. Since the early data for both treated and untreated fabrics fall on a single line with zero slope. Logarithm of Percent Strength Retained vs Logarithm of Baking Time. 1 reveal three important features: (1) an initial period in which log(Strength Retained).Fig. Y begins to decrease linearly with T.

01% calcium hydroxide bath at 30°C and allowing it to air dry can increase its lifetime by about a factor of 2. This equivalence indicates that the treatment is effective irrespective of the source of the cellulose. It is interesting to note that in both cases the ratio of Tc for Treatment A to Tc for the control is about 1. (Tc). 1. and that at some point the calcium ions are no longer effective. The treated samples degraded faster than the controls. It was found that the logarithm of the percent strength retained (Y) could be related to the logarithm of . We may postulate. it appears that soaking new cotton or rayon cloth for about 3 hours in a 0.16 To test this hypothesis a set of samples was subjected to Treatment A.4 CONCLUSIONS FROM THE RESULTS to date. Treatment A is not as effective as Treatment B. It is at this point that the slope of Y vs T abruptly changes. respectively. then. probably because rinsing did not remove all of the sodium ions.1 INTRODUCTION IN PART I.5 without affecting color or hand. 2 PART II: STRENGTH RETENTION AND COLOR CHANGE 2. and may mean that the chemistry of the degradation process is independent of the source of the cellulose. Clapp has pointed out the deleterious effects of sodium on the aging of paper. The time at which the alkaline treatment begins to lose its efficacy.5. that the effect of the calcium carbonate is to inhibit the deterioration processes. 12 hr and 19 hr. and that the same holds true for the rayon cloth. these events occur at about 8 hr. about 7 hr for the samples subjected to Treatment A and about 10 hr for the samples which were given Treatment B.5 hr for the untreated cotton.identical processes are operating in the cotton samples irrespective of treatment. it was reported that a treatment in dilute calcium hydroxide solution could increase the resistance of cellulosic textiles to degradation by heating at 150°C. is found to be about 4.5 and the ratio of Tc for Treatment B to Tc for the control is about 2. an accelerated aging test that should predict the results of natural aging. For the rayon samples. but given only a fast rinse in deionized water.

If first-order kinetics apply. aging and tear testing were provided in Part I. In both cases.2.3 RESULTS 2. the rate of decrease in strength retention should be proportional to the strength retained.1 Strength Retention The results of this study of the strength retention of artificially aged cotton and spun rayon fabric are shown in Figs. 2 and 3.the baking time (T) by an equation of the form: Y = A + n·T. respectively. 2. 2. This part presents the results of a more detailed study of the effect of a Ca(OH)2 rinse on the strength retention and color change of new cellulosic fabrics subjected to accelerated aging. and it was concluded that the treatment is effective irrespective of the source of the cellulose.1 Color Measurement The color change of the test samples was monitored by measuring the color of fabric samples with a Hunterlab Model D25D2 Color/Difference Meter.2 EXPERIMENTAL 2. and a plot of the log(strength retained) vs time would be linear.3. it is seen that such an assumption is valid for less than forty hours baking time at 150°C . A glossy black support was used to insure that the background color for all measurements was the same. The details of reagent application. The slopes of the lines for specimens which remained untreated or were subject to treatment for each of the respective fibers were essentially the same. it appeared that the chemistry of the degradation process was independent of the source of the cellulose. In addition.

Fig. 2. Baking Time at 150°C for Cotton Cloth. Strength Retained vs. .

the less meaningful comparisons between them become. 3. However. The untreated rayon cloth loses strength at the rate of about 1. the decay rates are essentially the same for both cotton and rayon.7%/hr.9%/hr.7%/hr. comparisons of the rates of decay of treated and untreated cloths for times greater than forty hours should be limited to the observation that the treated fabrics degrade at a lesser rate than the untreated fabrics. are found to be about one-half that of the untreated materials. however. It should be noted that. while the treated cloth degrades at a rate of only 0. The treated material. since the parameter being measured is a physical property that is only indirectly related to the chemistry of the cellulose polymer making up the fibers.8%/hr. Strength Retained vs. In addition. as measured by the initial slopes of the lines.Fig. the more curves depart from linearity. it . Baking Time at 150°C for Rayon Cloth. the untreated fabric degrades at a rate of about 1. Beyond forty hours the curves for the untreated material exhibit definite concavity. For cotton. while the treated cloth degrades at only about 0. continues to follow first-order (or psuedo first-order) kinetics to about 120 hr. Thus. The rate of strength loss for the treated materials.

2%/hr). and ‗0‘ when the maximum has been reached. The change in color should be linear with time. it may be seen that there is a very rapid strength loss occurring in the first hour or so of baking. 27. we may write Fig. 36–38. where E is the color. . Ef was determined by measuring the color of samples baked for over 400 hr. where Ef = the color at infinitely long baking times. It was found. we may define the following parameter: Fig. and Eo = the original color. since the fabrics contain some moisture when placed in the oven. Figure 4 shows the plots of (1 – F) vs time for treated and untreated cotton and rayon. Et = the color at time ‗t‘. The value of F is ‗1‘ if there is no color change. and Eo is the original color. Finally. This phenomenon comes about because the color meter cannot detect small differences between large color changes. that the rate of color change did not remain linear with time. This is in keeping with the observation in Part I that the rates of decay appear to be independent of the source of the cellulose. where Et is the color at time ‗t‘. This phenomenon is not unexpected. Thus. 2. . 29. In order to avoid this problem. If [C] remains constant. a plot of (1 – F) vs time should be linear. however. 25. [O] the concentration of oxygen at the surface of the fabric. That the yellowing and darkening of cellulosic . but decreased as the fabric became darker. . 40) that moisture accelerates the rate of degradation. and it has been demonstrated in Part I (and see refs. and [C] the concentration of the cellulose moiety that causes the color change.is of interest to note that the decay rates for both the treated cotton and treated rayon cloths are almost identical (about 0. Of major interest is the fact that there is no apparent difference in the rate of color change for treated and untreated cloth.2 Color Change The assumption that the change in color of the fabrics would be affected only by some chemical species in the cellulose and oxygen allows us to write: Fig.3. then (because [O] is constant).

It should be noted that the result could also be ascribed to the fact that the cotton has a dense cuticle layer which the rayon lacks. Increased surface area would permit a more rapid diffusion of moisture from the fiber. moisture influences the reaction rate. as is likely. which might enhance the rate of reaction at the air/fiber interface if. et al41 who concluded that ―the yellowing tendency of [oxidized] cottons is found to depend solely on the aldehyde groups content. This effect may be due to the higher surface area of the finer rayon fibers compared to the cotton.material is not affected by an alkaline treatment indicates that the species which cause the change in color are not acids. we see that the initial rate of discoloration of the rayon is greater than that of cotton. the ketone and carboxyl groups having no appreciable influence. . 4. This result is in agreement with those of Albeck. Baking Time at 150°C for Cotton and Rayon Cloths. so that these phenomena may be due to a combination of surface area and cuticle.‖ Fig. while at times greater than 40 hr it is the same (about 0.3 units/hr). Normalized Color Change vs. Furthermore.

‖ National Bureau of Standards Research Journal.J.Jones. Parts 1–7. Lucia Tang for her helpful suggestions. of this work. it may be concluded that rinsing new cellulosic textiles in a dilute calcium hydroxide solution enhances resistance to strength loss caused by thermal degradation by about a factor of 2. Permanence/Durability of the Book. 61 (1979).. and the Conservation Analytical Laboratory of the Smithsonian Institution and the University of Maryland for their support. Barrow Research Laboratory.I. Tang. W. M.B..2. V. REFERENCES Summarized descriptions of this research project have appeared in the Preprints of the American Institute for Conservation 1981 Meeting (Philadelphia). ―Changes in Properties of Papers After Treatment with Magnesium Bicarbonate Solution. Shaw.4 CONCLUSIONS FROM THE RESULTS of this work to date. Daniels. W. Wilson. 18. ACKNOWLEDGEMENTS THE AUTHOR WISHES to thank Mrs. Barrow.H.O'Leary.M. 1980. R. of the A.Golding. both financial and moral.Gear.J. R.McLaren and J. L. the darkening of cellulosic textiles appears to proceed through the formation of aldehydes rather than acids. 671 (1938). and M.N. 21. ―The Effects of Wash Water Quality on the Aging Characteristics of Paper.‖ Abstracts of the 178th Annual Meeting of the American Chemical Society. . but has little or no effect on the darkening of the fibers.. Richmond. pp. 37–45 and of the International Institute for Conservation 1982 Meeting (Washington). and that these results are independent of the source of the cellulose. In addition. W.C. Cambridge.. ―Aqueous Deacidification of Paper. pp.C.J. ―Effect of Filling and Sizing Materials on Stability of Book Papers.L.M. Va.A.‖ J. 96–99.‖ The Conservation of Library and Archival Materials and the Graphic Arts.K.

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