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Chapter 10
Barrow and Alkalization

The Yellowing Phenomenon in Laminated Modern Paper

One study of the history of the chemical causes of paper deterioration provides an interpretation of Barrow's motivation in the early years. Richard D. Smith, engineer and expert in paper alkalization, cataloged the history of alkalization research in his dissertation, "Nonaqueous Deacidification of Paper and Books". He claims that Barrow had to alkalize the acid in paper because his laminating equipment darkened acidic paper to the point of obscuring its text. The rate of paper deterioration is increased proportionally with increases in the temperatures to which it is exposed. Acid in paper also increases its rate of deterioration. The combination of high temperatures and high acid has very rapid deteriorative effects on paper. Smith argued that the darkening Barrow encountered was caused by the high temperature to which Barrow's laminator heated the document sandwich. High temperatures, as high as 400° F, were necessary to create his lamination product, therefore Barrow had to break this temperature/acid cycle by lessening the acid (Smith 1970, 68-69).

Present findings only partially corroborate Smith's conclusions. The actual story is more complex. Barrow identified the practical importance of acid hydrolysis as the primary cause of paper deterioration by a combination of study, product research, and coincidence. High acid modern papers yellowed when laminated under high heat. Barrow saw yellowing in samples using adhesive coated acetate sheeting he tested. He encountered yellowing again in samples he made for NBS' tests using acid paper supplied by NBS.

On 3 January 1939, Scribner informed Barrow that the Eastman Kodak Company of Rochester, New York, had developed a "new type of acetate sheeting for covering paper . . . thermoplastic Kodapak ™. . . coated on one side with a heat-sealing adhesive . . . applied at a temperature of 300° F to 350° F" (Scribner 3 January 1939). Barrow wrote Eastman Kodak asking technical questions about their new product (Barrow 18 January 1939).

Barrow expressed his interest in the new Eastman Kodak product to Scribner. He asked to be kept informed of any additional findings NBS may have had on the product, "Since it is coated only on one side, it eliminates the use of tissue," thus cutting the time and costs of lamination even further (Barrow 18 January 1939).

Within a month, Barrow reported to Scribner additional information about Kodapak™: "Enclosed you will find samples laminated with this material and please note the yellowing in each sheet. the newspaper seems worse than the [bond] paper....They remained in the heating unit about twenty seconds....This yellowing makes me question the permanency of this material, and I feel it should be tested quite thoroughly before using it on documents of value" (Barrow 6 February 1939). Scribner assured him that NBS was "making a heat test of the bond paper sample and will let you know the results" (Scribner 11 February 1939). Barrow continued his own tests of Kodapak™, and reported to Scribner: "All specimens yellowed considerably; the [bond] paper . . . and that of 1722 the least, and the cheap book paper the most. [At higher temperatures] . . . the yellowing increased . . . [At lower temperatures] the yellowing decreased" (Barrow 13 February 1939). Kodapak™ lamination showed yellowing when applied to paper of varying quality and age. Barrow rejected Kodapak™ for his use because of this propensity to yellow documents, and not because of its chemistry or its interaction with the chemistry of the paper (Barrow 13 February 1939).

During late 1938, Barrow followed another line of product testing, this time on mold-caused deterioration. He solicited technical information from a local medical researcher about the possible effect of lamination on mold. "Dr. [Frederick W.] Shaw, of the Medical College of Virginia, Richmond, a noted authority on mould, stated he felt sure all mould spores would be killed when a document was laminated. to prove this we are making tests" (Barrow 6 September 1938). Barrow hypothesized that the high heat of the lamination process would sterilize the product against mold. He sought corroboration so he would be accurate when he promoted his lamination product as also being able to protect documents from mold. at that time he seems to have thought mold was an important, if not the only important, cause of the deterioration he witnessed in paper. on 11 January 1939, Barrow sent Shaw some deteriorated paper samples to test for the viability of mold after the presumed sterilizing effect of lamination (Barrow 11 January 1939).

Shaw reported to Barrow on 21 March 1939 that the deterioration of the sample papers was chemically rather than biologically caused. "To date I have been unable to prove that the deterioration of the papers submitted has been due to either mold or bacteria. It appears to be a chemical process" (Shaw 21 March 1939). Barrow up to this time had not been concerned about chemically caused deterioration, specifically, acid hydrolysis. He had almost all of his restoration experience working with old papers, county records from the 1700s. Such papers, although highly acidic from iron gall ink in the writing areas, were relatively free from excess acids due to modern manufacturing methods and materials common during the mid 1800s, including the use of alum rosin size.

In a letter to Briggs, Barrow mentions his lack of experience with laminating modern paper that was more likely to be sized with alum and rosin. "I will be very glad to prepare specimens for your proposed test. If you could send one or two extra pieces of each type of paper to be laminated, it would be greatly appreciated. Since my work consists of laminating papers made before 1800, I would like to check the adhesion before laminating the modern papers" (Barrow 31 March 1939). Scribner sent him enough samples of the modern paper to be laminated for the research project (Scribner 26 April 1939).

On 29 April 1939, Barrow noted a yellowing phenomenon when he returned the laminated samples to Scribner. "A temperature of 295° F to 300° F was used on all samples with the exception of the rag book paper which was laminated at 285° F to 290° F decided yellowing occurred on the samples containing resin [sic] sizing" (Barrow 29 April 1939). Both the old papers and these modern paper samples, which had yellowed when laminated, were made from rags, that is, from cotton or linen fiber. Thus from the beginning of Barrow's practical knowledge of the deteriorative effects of acid hydrolysis, it appeared that the yellowing was a factor of high acid and not a question of the fiber content of the paper. Barrow apparently had not concerned himself with the effects of acid deterioration, until Scribner assured him that the yellowing phenomenon he noticed was important enough to add to their investigation. "We have noticed the discoloration of some of the papers which you mentioned and propose to make some investigation to find whether this is due to the paper itself, or whether it is some chemical reaction between the contents of the paper and those of the sheeting" (Scribner 4 May 1939). Barrow answered Scribner, again stressing that the yellowing was a new phenomenon and not a result of his own restoration method that had never been used with modern alum rosin sized paper. "I will be very much interested in the results of your test to determine the cause of the discoloration [yellowing] of some of the papers. This is the first time I have had this to [sic] happen. Practically all my lamination work has been on old papers [,] which leads me to think it might possibly be the sizing" (Barrow 12 May 1939).

Acid Hydrolysis and Alkalization

The practical demonstration of the yellowing phenomenon in test samples followed closely Shaw's letter pointing out that the cause of the visible paper deterioration was probably chemical rather than biological. Apparently Barrow put these clues together and saw the need to learn about acid's effects and adapt its control to his lamination process. Thus, Barrow was spurred on to a new phase of product development. Shaw assured him that a laminated document would not mold (Shaw 21 March 1939). Therefore, lamination combined with control of acid caused deterioration (acid hydrolysis) through alkalization would produce the stable restoration product that Barrow desired.

Barrow wrote Scribner of his renewed interest in paper research on the differences in acidity between old and modern papers and therefore on the importance of acidity in paper deterioration. "The results of the test of old paper sent me through Mr. Briggs['s] office was most interesting and I appreciate your sending it to me. This makes me all the more desirous to accepting your invitation to study the methods used in making these tests" (Barrow 12 May 1939).

In the summer of 1939, Barrow probably visited NBS and GPO to initiate his instruction on test methods to study the effects of acidity on paper longevity. The chemists at NBS and GPO were able to instruct Barrow fully on both the literature and contemporary techniques involved in alkalizing acid paper. Herbert F. Launer, a chemist from NBS, wrote acknowledging Barrow's study visit during August 1939 (Launer 23 August 1939). Although there is no direct documentary evidence available that Barrow first learned of alkalization from chemists at NBS and GPO, William K. Wilson, a chemist hired in the Paper Section of NBS in 1940, remembers that Scribner reported instructing Barrow on acid hydrolysis and alkalization (Wilson 1988).

Information on acidity, paper permanence, and standard tests for detection of acid in paper was widely distributed by 1939. This information was so well known that when Barrow wrote to chemical products companies about test equipment and supplies to measure acidity in paper the information sent to him on acid hydrolysis was treated as routine promotional material. a company secretary answered one of his letters accurately and articulately using information quoted from a company-produced report, "pH and Its Practical Application." the letter states, "the properties of the finished paper are greatly influenced by residual acidity in the fibers . . . it has been found that an acid paper deteriorates very rapidly". The letter also describes the two standard tests for paper acidity, the cold extraction method (from the Swedish Model) and NBS's own hot extraction method (Welch 18 August 1939, 1).

Barrow adapted alkalization to the scale and economics of his restoration shop between August and December 1939. Alkalization of paper after sheet formation brought the pH of the paper up to neutral or slightly above neutral into the basic range. It left a residual amount of alkaline material in the paper to buffer future deposits of acid absorbed from air pollution and from continued, but slowed, deterioration. Alkalization had the dual effect of lessening the yellowing of documents when heated during lamination, and the more important effect of slowing dramatically the rate of deterioration of the paper. Barrow reported his adaptation of the alkalization process to Scribner on 6 December 1939.

Calcium carbonate may be precipitated by submerging the document in a solution of calcium bicarbonate. The bicarbonate reverts to the carbonate when the paper is dried. The process is very simple and a number of documents could be treated in relative [sic] short time....My best results have been obtained with a bottle used in making carbonated water in one's home. Calcium Carbonate is added far in excess of its point of solubility and CO2 [sic] is added. The pressure produced seems to accelerate the formation of the bicarbonate, as well as agitation of the solution. a solution of one-half of one per cent bicarbonate can be produced in this manner which is sufficient to give a very acid paper a PH [sic] of over seven [into the basic range]. (Barrow 6 December 1939)

Barrow described to Scribner the steps he planned to use to incorporate alkalization in an economical manner into his restoration method and asked, "Can you suggest a simpler method of preparing this bicarbonate of calcium? If a satisfactory method of preparing this bicarbonate could be worked out it would simplify the mechanical operations. As the documents could be sandwiched between screen wires in the solution and when removed could be dried on the wire. The document then would be subjected to the minimum physical stresses" (Barrow 6 December 1939). Barrow eventually used bronze screens as described above and continued using this method with only very minor changes during his entire career.

His initial experience with alkalization persuaded him of the merits of this treatment as he reported to Scribner: " . . . the papers of high acidity decreased in folding considerable [sic] after heating....the discoloration after heating was very noticeable as well as the ink on an old manuscript faded slightly after the heat treatment....[Following alkalization] there was no discoloration after heating and the folding endurance was good" (Barrow 6 December 1939). Based upon these initial test results, Barrow wanted to add alkalization to his restoration method even if it decreased his profit margin; as he wrote to Scribner: "A process of this nature would consume considerable time in washing which would be costly. However, it appears from these tests that it is very advantageous to neutralize the acids in these papers" (Barrow 6 December 1939). Scribner answered Barrow's letter enthusiastically: "Apparently the treatment has an excellent effect with regard to the stability of the papers, and the results you obtained are of very much interest. I believe that the method you used for preparing the calcium bicarbonate is about the simplest way in which this could be done. I hope that you will keep me informed of your further results and [we] shall keep you informed of our further developments here" (Scribner 14 December 1939).

Prior Patent Claims and Barrow's Accommodations

At about the same time that Barrow was adapting alkalization to his restoration process during the fall of 1939, he received a letter of inquiry about his laminator and restoration process from A. E. R. Westerman, Director of Chemical Research, Ontario Research Foundation (ORF), Toronto, Canada. He sent Westerman samples of laminated documents and information on the costs of the laminator and his restoration process.

The cost of equipment will depend upon the size of machine, etc. the State of Maryland expects to install a machine this year, and the cost will be around $3200.00. This includes the equipment, instructions in its operation, and the use of my patent if granted. I have not applied for a patent in Great Britain which means that you would not be affected by the patent I have applied for in this Country. If you purchased a machine from me there would be a small reduction due to the patent situation. However, one could not expect a great reduction as the machine is custom built and is naturally a costly item when it can not be built on a production basis. (Barrow 9 October 1939)

Westerman's answer on 16 October 1939 further discussed the possibilities for cooperation and distribution of Barrow's laminator in Canada and England.

I have discussed the matter with our Director, Dr. H. B. Speakman, and as a matter of public interest, if for no other reason, he is prepared to consider the installation of the necessary equipment at the [Ontario Research] Foundation, doing enough commercial work to help carry the fixed charges.
At the same time, the Foundation would be interested in helping to develop the process in Canada, and possibly England, and Dr. Speakman suggests that, if too long a time has not elapsed since your [patent] application, that we submit it to Ottawa at once to get a date established. When this is done, we can then discuss the conditions under which you would assign your Canadian patent to us, if one were granted. As matters stand now, the Foundation would be willing to assume the costs of the application at Ottawa in return for an assignment. (Westerman 16 October 1939)

Barrow told Westerman that it was too late to apply for a Canadian patent simultaneously with his U. S. patent application. "I regret that I did not know of your interest sooner in order that an application could have been made in routine manner. Since the Libraries and other institutions in Canada do not have sufficient material for a machine in each institution, I think the plan you have outlined will be of great value to these institutions. Similar conditions exist here in my own state" (Barrow 26 October 1939). Barrow wrote Sutton about obtaining a Canadian patent, and Sutton was ready to apply on his behalf (Sutton 30 October 1939). Apparently, no other communication came from ORF's initial interest in lamination or from Barrow's Canadian patent application at this time. the interaction between Barrow and Westerman is important because of the role ORF played in Barrow's attempts to patent his restoration process and perhaps even a larger role it played in his future reputation and career.

At the beginning of January 1940, Barrow again wrote Scribner asking his advice on the proper concentration of alkalization solution he should use:

I am enclosing the results of tests recently completed relative to the neutralization of acid in old papers. The calcium bicarbonate appears to have the desired effect . . . You will notice one group was submerged in 0.6 per cent CA(HCO3)2 [sic] and the other in 0.30 per cent. This is the maximum and minimum solutions obtained with the apparatus used in making the bicarbonate. I propose to use a solution of about 0.50 per cent as this can be made in about 40 minutes and appears to be the simplest method of preparation, judging from the enclosed test. Do you not think this will be sufficient? . . . Your comments on this proposed method of preservation of documents will be appreciated. (Barrow 3 January 1940)

One of Barrow's chief concerns, as shown by this letter, is the time required mixing the alkalization solution. This time element carries as much weight as the test results in the reasons he gives for selecting a 0.5 percent solution. Scribner immediately answered, and gave Barrow his expert opinion on the chemical question of the proper solution concentration. He also gave his support for Barrow's efforts: "We are very much interested in the data you forwarded with your letter of January 3 concerning the use of calcium bicarbonate for the preservation of papers. The data indicate that the treatment has a decided protective effect. It would seem that a 0.5 per cent solution of bicarbonate would be sufficient" (Scribner 9 January 1940).

Sutton informed Barrow in February 1940 that his patent application needed revision.

At a conference which I had yesterday with the Primary and Assistant Examiners in charge of your application, they took the position that the disclosure of your application is inadequate because you are not sufficiently specific as to material that can be used. Your specification states "For preservative materials I preferably use cellulose acetate, ethyl cellulose or other cellulose derivative that are thermo-plastic," and then for purposes of illustration cellulose acetate is referred to in the following description. The Examiners take the position that cellulose acetate itself cannot be used in the way described, but that some material which, though containing cellulose acetate, must also contain other ingredients, such as plasticizer, would be necessary in order for the invention to be carried out as described....the answer to the question involved is one of fact. If you use pure cellulose acetate, the controversy can be promptly terminated by filling an affidavit to that effect. If you do not use pure cellulose acetate, then I would like to have a full and complete explanation of what is used and I can then gauge what should be done in order to meet the issue raised by the Examiners. (Sutton 8 February 1940)

Celluloid Corporation would not release information on the plasticizer or other proprietary ingredients of their brand of cellulose acetate foil. Barrow again referred Sutton to Scribner as an expert on cellulose acetate foil. Barrow did not get ingredient information from Celluloid Corporation, thus he further informed Sutton that a permanent plastic foil was found by testing, not by listing ingredients. "As you no doubt know the unit of measure for determining a suitable foil for the preservation of documents consists of an accelerated aging process developed at the Bureau of Standards, which consists of heating for seventy-two hours at 100° C. Physical and chemical tests are then made to determine whether there has been any noticeable deterioration. This is an accepted method for determining the suitability of a foil rather than naming the various ingredients" (Barrow 14 February 1940).

By March of 1940, Barrow was ready to incorporate fully alkalization into his method of document restoration, but he also continued to seek reassurance from Scribner for each of his decisions. "At present I am working on apparatus for installing this [alkalization] process and to be used on documents before lamination. Do you think sufficient tests have been made to be safe in using this treatment for deteriorated documents of value? the results obtained in your laboratory for calcium carbonate as . . . filler indicate, as well as mine, that the papers containing this compound have good stability" (Barrow 4 March 1940). Scribner again encouraged Barrow and his adaptation of alkalization. He offered Barrow no further technical information, and apparently turned future testing over to him. "We are much pleased to have your letter of March 4 and the accompanying data concerning the treatment of acid papers with calcium bicarbonate. Like the data you have previously given us, it appears that the treatment has a very beneficial effect of the papers. We would be pleased to have any further information of this kind that you may obtain" (Scribner 8 March 1940).

At this time, Barrow was actively promoting this painstakingly researched alkalization process. His descriptions of the complex chemistry underlying alkalization were very informal. for example, a newspaper article reported: "When a document comes in . . . it first of all is given a bath. This is done in a solution which takes out impurities, or renders them inert, and keeps the paper from going to pieces....Laminating a piece of paper without first giving it a bath, he [Barrow] explained, is like mixing good apples with rotten apples. The decay from the bad soon will spread to the good" (Barrow invents unusual job [1940]).

Despite the submission of additional facts, Barrow's patent application, "Barrow, Serial No. 211,705 - Methods for Preserving Documents and Other Fibrous Materials," was rejected on 28 August 1940 (Sutton 30 September 1940, 1) for lack of disclosure about the foil used and lack of novelty, as Sutton explained:

there is little by way of invention in this case as filed over what has been developed by the Government in preserving its documents . . . while if we are standing upon the particular qualities of the film material to make your process work and do something cheaply that has not heretofore been done, then the application has failed to be sufficiently explicit in teaching the art, just what is the material and what are its characteristics that enable you thus to do more cheaply and more expeditiously what has heretofore been done by more expensive procedure. (Sutton 30 September 1940, 3)

Sutton advised Barrow that if he wished to continue to pursue a patent he would have to start over again. "it is time for us to stop and make a very frank analysis of the entire situation, what is the novelty and what is the scope of protection to be expected thereon? for this your detailed analysis of the patents cited and a comparison thereof with your invention is necessary. Then comes the question what can we do by further disclosure to sharply differentiate your invention from the prior art" (Sutton 30 September 1940, 3).

Apparently, Barrow's lack of disclosure and his ignorance of the processes and materials he used did not deter him from wanting to try again, this time with the addition of alkalization. in a letter dated October 14, 1940, Barrow asked Sutton if he was infringing on any prior patents for the alkalization process he had adapted with the assistance of NBS and GPO (Barrow 14 October 1940, 5). The evidence indicates that Barrow was by now better taught and informed in the state of the art in paper permanence and alkalization research and findings. "It is advantageous financially to proceed with my application....I seem to have been bitten by the invention bug and have developed another process to be used before the lamination of a document. Will you please have it investigated and render an opinion on the enclosed process . . . If you could have copies of patents in this field [alkalization] by the time I visited you [third week of October] it would be appreciated" (Barrow 14 October 1940, 1).

Barrow was now aware of the importance of prior patents to the success of his own patent applications, and he was beginning to understand the relationship of patents and research. Patents have been an important source of scientific information that is not necessarily repeated in the research literature; thus, patents are part of the communication system used by scientists and technicians. "Many of the solutions to problems have been recorded only in the patent documents....[Patents are] unique and carefully recorded history of the resolution of technical problems as they have been dealt with through time" (Walker 1988, 6).

In Barrow's comments to Sutton on the new addition of alkalization, he again emphasized his own independent research and knowledge and minimized the role of the chemists at NBS and GPO.

In September 1939 I discovered that all papers in a deteriorated condition were highly acid (low pH).
A high acidity in paper has been known for some time to be very deleterious to the permanency of cellulose fibers. This acid would also have an adverse effect on the old fibers and any new materials used in reinforcing or strengthening the old paper.
Several alkali solutions, such as sodium bicarbonate, were used to neutralize this acidity but they all proved to have a harmful effect on cellulose fibers as well as paper becoming acid again on aging.
Two papers made over 200 years ago which were found to be in excellent physical condition and were free of acid were found to contain approximately 3/4 of one per cent calcium carbonate. The Bureau of Standards recently found that when calcium carbonate was used as . . . filler in paper it exerted a protective effect on paper when aged. Therefore, calcium carbonate was selected to be the ideal compound for neutralizing acidity in old papers. (Barrow 14 October 1940, 4)

In this same letter to Sutton, Barrow reveals that he knew about an earlier patent granted to Otto Jansen Schierholtz, U.S. Patent 2,033,452 on 10 March 1936, "Chemical Stabilization of Paper and Product". The patent assignor was the laboratory of the Ontario Research Foundation, the institution that had been interested in Barrow's lamination process and equipment in 1939. Schierholtz states specifically that his process was done primarily to stop the tarnishing of metallic paints used on acid paper, but that it also stabilized the paper and contributed to its permanence.

While this test determines only the tarnishing properties of the paper, it has been found that it is also a fairly accurate indication of the stability of the paper because ordinarily a paper which will tarnish is also unstable. However, instability, that is, tendency of the paper to deteriorate, particularly in strength, with age may not be directly proportional to the tarnishing properties of the paper and this may be determined by the so-called oven test. This [accelerated aging] test is not as delicate as the tarnishing test, but has been found to show that paper which has been stabilized in accordance with the present invention generally suffers only about one-half as much in loss of strength as untreated papers, other than those of the type of high grade filter paper, which are inherently non-tarnishing and stable. (Schierholtz 1936, 2)

It is clear that Schierholtz knew, and expressed in his patent, the positive effect of alkalization on paper permanence. Up to 1936, alkalization of paper after sheet formation had been documented in the chemical literature as being possible and desirable but no practical means had been invented to do it. Schierholtz's patent contained a practical alkalization process. Schierholtz made alkalization of acid paper possible (Schierholtz 1936, 2).

Schierholtz may have anticipated the alkalization process Barrow wished to claim as his own. Barrow asked Sutton about ways to differentiate his patent application to avoid being anticipated. "Am I infringing on Schierholtz Patent by using Ca(HCO3)2 [sic]? . . . Schierholtz tries to make his paper neutral pH 6.5 and uses .10 to .15 per cent solution. I attempt to leave an excess of CaCO3 [sic] to neutralize any future acidity and obtain a pH of above 7.5. My solution is .35 per cent bicarbonate in strength" (Barrow 14 October 1940, 3).

Barrow arranged to visit Sutton in Washington on 25 October 1940, to discuss Sutton's letter of 18 October 1940 in which he discouraged Barrow's attempt to patent his version of alkalization:

So far as I can see, your procedure for neutralizing out any hope to you of obtaining worthwhile g the acidity in old documents is substantially anticipated by the patent to Schierholtz . . . You will note that the procedure here disclosed is concerned with the treatment of paper which has already been made with a sizing, and while the patent does not specifically refer to the treating of old papers, the Patent Office would not in my judgement give any respect to the degree of antiquity of the paper. As the process for neutralizing the acidity is the same whether the paper is one day old, . . . or one century old, the Patent Office would almost certainly rule that there is no distinction in substance and no possible line of demarcation for antiquity to be drawn between the Schierholtz procedure and what you are doing. Accordingly, I cannot hold out any hope to you of obtaining worthwhile patent protection on this invention. (Sutton 18 October 1940, 1)

Sutton continued to analyze Schierholtz's patent with the intent of showing Barrow the limits of his possible application for a patent in the face of Schierholtz's prior claims.

Schierholtz does not specify how he makes the calcium bicarbonate solution, other than specifying that he uses CO2 [sic] gas, but I take it from your letter that you do not place your invention in how you make the bicarbonate solution[,] perhaps you have merely adopted some known earlier procedure in this respect, and therefore we have not attempted to develop the state of the art on this particular phase of the procedure.
Schierholtz does not disclose any particular apparatus for dipping and drying the paper, but as you are undoubtedly aware there is a wide variety of structures that could be used for this purpose, there is nothing broadly new in dipping and drying by means of a screen frame, and even if you have a specifically new structure for holding the documents during dipping and drying, I would not recommend the seeking of patent protection thereon because any protection obtained would have to be very specific to the exact structure which you use and as is apparent a wide variety of structures could be used for this purpose. (Sutton 18 October 1940, 1-2)

Barrow decided, during the late fall, to drop altogether his claim of invention for the alkalization process he used. He replaced his earlier application with one that stressed his entire restoration process instead of just the equipment or any one process. By 11 December 1940, Sutton informed him that his new patent application, "Methods for Preserving Documents and the Like", was ready for his notarized signature in order to be filed (Sutton 11 December 1940, 1-2).

On 21 February 1941, Barrow wrote Westerman with a proposal for cooperation, that is, he wanted to use Schierholtz's patented alkalization process in exchange for their use of Barrow's pending patent on his restoration method. "I am interested in obtaining permission to use your patent in my shop and also in libraries and archives in the U.S.A., that install my laminating equipment....I would like to know your fee for permission to use this process....If you are still interested in the installation of a laminating machine, I had thought that it might be possible to make some form of exchange . . . " (Barrow 21 February 1941, 1). in this letter, Barrow again stresses his own research role in the development of his restoration method including alkalization.

I have developed a process for rendering these old papers relatively stable before applying the protecting and strengthening acetate foil. My patent attorney found that your organization was granted a patent . . . similar to the method I developed for old documents.
The principles of the two processes are practically the same. However, I have had to devise special equipment [screens] for handling fragile paper while subjecting it to the solutions of bicarbonate of may be of interest to you that I have found that all deteriorated papers have a high acidity. The pH varies from 4.0 to 4.4 which is not considered a good condition for permanent papers. I will be glad to furnish you the test data obtained from my experiments with old papers . . . and the treatment with calcium bicarbonate. Would you like to have a copy of an analysis of 10 old papers made by the Bureau of Standards relative to alpha, beta, gamma cellulose, copper number, retention of folding endurance under accelerated aging, acidity, sizing and ash content? (Barrow 21 February 1941, 1-2)

Initially Westerman's response to Barrow's request was positive. "Like you, we have had difficulty in getting any of the libraries, etc., to commit themselves to even modest expenditures, so the matter has just been held in abeyance. However, it should be possible to keep one unit operating in Canada and, possibly, such a unit could be justified on the basis of our Schierholtz patent and an arrangement with you" (Westerman 28 February 1941).

During the fall of 1942, Barrow's patent application went through its final revision. "Method for Preserving Documents and the Like" was approved on 1 November 1942, as U. S. Patent number 2,301,996.

After 1940, Barrow's interactions with NBS and GPO lessened, and stopped completely when his restoration method was finally patented. Almost a year passed between letters to Scribner, then Barrow followed up a visit to NBS in 1941 with one of his last letters in which he gives Scribner the citation for Schierholtz's patent. "The patent covering the treatment of acid papers with the alkaline earth metal bicarbonate is number 2,033,452 dated March 10, 1936, and granted to Otto J. Schierholtz, Assignor to Ontario Research Foundation, Toronto, Ontario, Canada" (Barrow 4 March 1941). Barrow wrote Launer, at NBS, thanking him for his time during the visit and commented on meeting William K. Wilson (Barrow 6 March 1941). Wilson reported Launer had written that Scribner had earlier told Barrow about Schierholtz's patent and had been Barrow's principal source on acid hydrolysis and its possible mitigation through alkalization (Launer 3 March 1941, Wilson 30 December 1987). It is unclear whether Barrow first learned of Schierholtz's patent from Sutton or from Scribner.

It is clear however that Barrow discussed Schierholtz's patent at length with the several NBS chemists. a letter from Launer dated 19 March 1941 illustrates their exchanges about Schierholtz's patent; Barrow apparently wanted to gather support for not having to pay a fee for the use of Schierholtz's patent by saying that Schierholtz had used barium not calcium to alkalize acid paper. ". . . barium (also calcium & strontium) bicarbonate Ba(HCO3)2 [sic], is unstable in air in the solid state and reverts to BaCO3 [sic], so that any stability gained by the introduction of the bicarbonate into paper is due to the subsequent presence of the normal carbonate. The author, therefore, really introduces these alkaline earth carbonates into paper after it has left the wire, and therein lies the novelty" (Launer 19 March 1941). Launer thus supported that Schierholtz had prior claim to the alkalization process even if he did not recommend calcium. His claim covered all alkaline earth carbonates.

ORF turned over Barrow's request for an exchange of services to Howard A. Poillon, their representative in the United States. Poillon asked Barrow some pointed business questions. "We assume that you intend to try to commercialize your process and if so we would like to know to whom you intend to address yourself and what method you contemplate using in your plan of operation? Further, on what will your charges be based and what will be their order of magnitude?" (Poillon 20 March 1941)

Barrow's response was filled with comments about the small scale of his business and his limited market for his products.

I am not an employee of the State of Virginia but am in business for myself. The Virginia State Library furnishes quarters [he was back in Richmond in the new State Library building now] for my workshop in order that their valuable documents will not have to leave the building to be repaired....I have no employees [,] as the volume of work has never been beyond the amount that I could do....Being unable to purchase a steam heated hydraulic press [for lamination] on account of its expense ($6500.00) I developed . . . [my own] equipment. The late Dr. James A. Robertson, of the Maryland Hall of Records, encouraged me to apply for a patent on this process in order that he might secure similar equipment. at that time . . . a price of $3200.00 was placed on the installation of this equipment; three weeks' instruction in its operation; and the use of my patent if granted....I have estimated that the saturation point for this process in this country will be about eight institutions....I then decided to raise the cost of my laminating equipment to $3500.00 to cover the cost of equipment for giving the documents a bath in the bicarbonate solution. (Barrow 26 March 1941, 1-2)

Barrow concluded his answer with an apparently disingenuous comment of his business intentions: "I could not see where I could make a profit on this part of the process as most institutions of this nature have a very hard time raising the money for a laminator. It was then decided to make this process available without profit but would be an added service to Archives installing a laminator." Barrow then asked, "What would your price be to allow the before mentioned types of institutions the use of this process in connection with the lamination of their deteriorated documents?" He ends the letter with a list of prominent men, including Scribner, who would "be glad to give you an idea of my status in the restoration field" (Barrow 26 March 1941, 2).

Poillon answered Barrow by sending him a contract: "The fee . . . will be $100.00 per machine, payable by you at the time of the sale of a machine in the future and payable now on any such machines now in use, including your own" (Poillon 2 July 1941). The original contract is still unsigned in the Barrow Papers in the Virginia Historical Society. There is no evidence to indicate that Barrow ever paid a fee to ORF or its representatives. There is no other mention of the ORF in any of Barrow's published or private writings following 1943 (Barrow 1943, 152) until the 1961 edition of his Procedures and Equipment (Barrow 1961 Procedures and equipment . . . , p. 6), although it was left out again from the 1965 and final edition (Barrow 1965 Barrow method of restoration . . .). The unsigned contract may be the reason why Barrow rarely acknowledged Schierholtz's patent.

Barrow wrote Kantrowitz to thank him for extra copies of his annotated bibliography (Kantrowitz, Spencer, and Simmons 1940) to inform restoration customers of the research basis of his alkalization method. "Since visiting your office about two years ago, I have been working on a method of washing and neutralizing the high acidity in old deteriorated papers. Should you be in Richmond at any time I hope you will visit my shop and look over some of the work I have been doing on this new process" (Barrow 5 May 1941).

At the beginning of May 1941, Barrow attempted to sell his laminator to the Library of Congress. He sent this potential customer a copy of Kantrowitz's annotated bibliography. He told them that some of the chemical studies supported his own research and findings, not the other way around, which was in fact the case. "This last one [presumably (Jarrell, Hankins, and Veitch 1936)] was of particular interest to me as the findings of high acidity in all of the deteriorated papers were the same results of my tests. The one paper that seemed to hold up well contained the same compound I am using in my work of freeing the paper of acidity" (Barrow 5 May 1941). Most of his writings and advertising between 1941 and the late 1950s were informal with few references to the chemical literature. Barrow may have not cited his sources out of ignorance of academic traditions of citation, traditions that may have been inappropriate or at least unusual in advertising and promotional writing. Nevertheless, it is also well documented as early as 1939 that he was willing to promote himself as a scientist and inventor. He assumed this prestigious role when he dealt with people, especially his customers and social acquaintances, who were unlikely to be aware of the chemical literature (Barrow invents unusual job [1940]). By the 1960s, with the establishment of the Barrow Laboratory and his association with Verner W. Clapp, he was widely regarded in the library and archives fields as an original researcher in the chemistry of paper (Council on Library Resources 1961).

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