Photo Documentation

Before Treatment: recto

Before Treatment: verso

Before Treatment: recto

After Treatment: recto

After Treatment: verso

After Treatment: recto

Treatment Record Documentation

Title:  A sheet of music manuscript from His Book, p.39-40
Date/Period:  18th century 

Artist/Maker: Francis Hopkinson (1737-1791)  
Owner: Music Division, Library of Congress

Catalog Number: ML96 .H83 no. 1

Background Information:

Francis Hopkinson(1737-1791), signer of the Declaration of Independence, a scholar, inventor, harpsichordist and organist, and a graduate of first class at University of Virginia, is credited with scoring the first secular music in the colonies. This handwritten notated manuscript is contained in the bound volume, His Book, by Francis Hopkinson. The non-original binding contains over 200 leaves of cellulose acetate-laminated notated music manuscript pages.

 

Full treatment of the entire book including cellulose acetate delamination, washing, complexing, alkalinizing, and resizing steps is proposed as a multi-year project for the Library of Congress Music Division. The treatment of this sheet will help inform and guide the overall treatment protocol. Treatment of works laminated with cellulose acetate is guided generally by treatment steps determined by senior paper conservator Susan Page.  Treatment of works composed or drawn in iron gall ink is guided by the Protocols for Iron-Gall Ink Treatment written by Julie Biggs and other paper conservators in the Library of Congress Paper conservation laboratory. The documentation below describes the music sheet from the page 39-40. 

DESCRIPTION

A cellulose acetate laminated sheet of music (p.39-40) from His Book, a book of music mostly composed by Francis Hopkinson in his hand in iron gall ink. The book contains 206 pages, all of which are laminated between tissue and cellulose acetate. The book contains the first secular music composed in the United States.

MATERIAL AND MEDIA

Media: Probably two types of iron gall inks were used for writing the music. The ink of the music notes is much darker, while the writing of the text is paler.

 

Support: Medium weight of laid paper.

 

Stamps: A blue ink stamp which reads “23” can be found at the bottom left corner of p.39. The blue ink “23” is stamped directly upon the paper surface, indicating that the numbering occurred prior to the cellulose acetate lamination.

 

CONDITION

Staining: The manuscript is discolored overall. There is a large stain that extends across half the sheet of paper, possibly due to previous water damage. This brown staining correlates with an increase in UV absorption, suggesting the spread of soluble Fe2+ ions in the paper sheet during the water incident.

 

Media: The ink is in fair condition. However, there is localized, moderate discoloration surrounding the ink. There is also localized, minor burn-through of the ink.

 

Former Treatment: None on record. The music sheet was laminated as a preservation method. The paper was sandwiched between two pieces of tissue and then the whole thing was laminated between sheets of cellulose acetate film.

SPOT TESTING

Solubility of cellulose acetate film: The solubility of the cellulose acetate was tested with acetone. The test showed that the cellulose acetate film is soluble in acetone.

Solubility of the film: The laminate was tested with acetone and water to confirm the film was cellulose acetate, and to determine the solubility of cellulose acetate. A small piece of only the laminate was cut off from the edge of the object for testing.

 

Solubility of ink:

(1) Iron gall ink:

Before delamination, the solubility of iron gall ink was tested with acetone.

 

After delamination, the solubility of iron gall ink was tested with deionized water adjusted to pH7 with Ca(OH)2, deionized water : ethanol 3:1, deionized water : ethanol 1:1 and 100% ethanol. The test showed that the ink is not soluble in deionized water, mixture of deionized water and ethanol and 100% ethanol after a large droplet of the solution was applied for 20 seconds. Inks were slightly soluble in 100% deionized water conditioned to pH 7.5 with calcium hydroxide. Mixtures of 25%, 50%, 75% ethanol in deionized water conditioned to pH 7.5, and at 100% ethanol showed no ink solubility.

 

(2) Blue Stamp ink:

Before delamination, the solubility of the blue stamp ink was tested with acetone.

 

After delamination, the solubility of blue ink was tested with acetone, deionized water, deionized water, mixture of deionized water and ethanol (3:1,1:1) and 100% ethanol. The test showed that the ink is not soluble in 100% ethanol, but slightly soluble in 100% deionized water or mixture of deionized water and ethanol. Since the stamp number is not original to the object and no bleeding was seen while testing, it is decided that the slightly discoloration of the blue stamp ink is acceptable.

 

Wettability of the paper: Deionized water was absorbed in areas that had been heavily inked. Deionized water sat on the surface of the paper, with no ink, for about 30 seconds before being absorbed.

 

Fe2+ Test:

After delamination, the iron (II) content of the iron gall ink was tested with iron (II) indicating paper. It is found that the ink tested positively and iron (II) is fairly present in the dark brown ink.  

Note: In order to conduct the test, an indicator paper made from Whatman filter paper coated in 0.1% 4,7-diphenyl-1,10-phenanthreline (also known as, bathophenanthreline) in ethanol was used. A small square of the indicator paper was cut and wetted with deionized water. Then it was blotted on one side of the paper to remove excess moisture. The indicator paper was placed on the ink and covered with a piece of Mylar and a weight, for 30 seconds. If the test is positive, the indicator paper will turn magenta.

 

Surface pH:

After delamination, the surface pH was tested using a pH strip with a drop of deionized water. The top left edge (fore-edge) of p.39 and the bottom right edge (gutter) were tested. Both were around pH 3.5.

Note: To conduct the pH test, a piece of Mylar was placed under the area to be tested and drop a spot of distilled water on paper surface. Then placed the pH test strip of 4-7 scale color-side down on the wet area of the paper. A piece of Mylar was placed on top of the strip to ensure that the strip makes full contact with the paper surface. After 30 seconds, the test strip was picked up and compared with the color code on the box.

TREATMENT PROPOSAL

  1. Remove the cellulose acetate film and paper laminates by following the delamination protocol using acetone.

  2. Wash the object in conditioned water to remove cellulosic degradation products. Ethanol-modified solutions will be used as necessary to preserve water-soluble inks.

  3. Immerse the object in a complexing solution using calcium phytate to remove soluble iron compounds and to chelate the free Fe2+ ions, followed by alkalinization with calcium bicarbonate solution. Ethanol-modified solutions will be used as necessary to preserve water-soluble inks.

  4. Resize the paper with gelatin and ethanol.

 

TREATMENT

1.  Delamination: The cellulose acetate film and paper, along with any remaining cellulose acetate in the interstices of the object’s paper fibers were removed in a succession of six 300ml baths of acetone. Each bath was 3 minutes long.

--In bath #1, the object was immersed in acetone for approximately 1 minute before carefully peeling off the cellulose acetate film and paper from both sides of the object.

--In bath #2, the object was immersed in 100% acetone for another 3 minutes. At the mean time, the majority of residual cellulose acetate was scraped off carefully with a small piece of blotter.

-- Then the object was placed in another four successive baths of 100% acetone while brushing the surface with a hake brush to remove any residual cellulose acetate. Also, the baths were agitated frequently to allow for the acetone to flow around the object.

--After the sixth and final bath, the object was taken out and briefly placed on Mylar to check for any residual cellulose acetate. The acetone was allowed to evaporate from the object. This procedure was performed in the fume hood.

Note:

--Usage of acetone: In order to make the use of acetone more cost effective, baths four, five and six were done with fresh acetone, while bath one, two, three were done with used acetone from the previous baths.

--Usage of Hollytex and Mylar: The object was placed on Hollytex (spun polyester web) during baths one two and three, and on a sheet of Mylar (Polyethylene Terephthalate) during baths four, five and six. The use of Mylar sheet provides an easy way for checking any residual cellulose acetate. After the acetone evaporate, residual cellulose acetate on the Mylar sheet will leave white marks.

2. Testing after delamination: the object was pH tested showing pH3.6 on the blank area and pH 3.4 on the ink area. The iron gall ink was tested with mixtures of ethanol and deionised water adjusted to pH7 with calcium hydroxide.

3.Washing: The object was pre-wet by spraying with 100% ethanol. Then it was immersed in a bath of 1:1 ethanol and deionized water, which was conditioned to pH7.5 with calcium hydroxide(Ca(OH)2) for 20 minutes. Then the object was immersed into another bath of 40% ethanol in deionized water conditioned to pH 7.5 for 20 minutes. Half way through the baths, the object was turned over. After immersion, the object was sprayed with 100% ethanol to help speed up the drying process. The object was then blotted, placed between new Hollytex (spun polyester web) and dried between blotter and felts.

4. Calcium phytate treatment: The object was sprayed with 100% ethanol and immersed in a bath of 60:40 calcium phytate solution conditioned with NH4OH to pH 5.6: ethanol for 20 minutes to complex the reactive Fe2+ ions. The object was placed in a second bath of 70:30 calcium phytate: ethanol for 20 minutes. After the complexing treatment, the object was alkalinized by immersing in a bath of 70:30 calcium bicarbonate: ethanol for 20 minutes. After alkalinizing, the object was taken out and sprayed with 100% ethanol to help speed up the drying process. The object was then blotted, placed between new Hollytex (spun polyester web) and dried between blotter and felts.

5. Testing after phytate treatment: A Fe2+ test was conducted after the object was dried. All inks were very slightly positive for Fe2+ so the treatment was not repeated.

6. Resizing: The object was sprayed in 100% ethanol and placed in a tray between Hollytex. Warm 70:30 0.5% gelatin: ethanol was brushed onto both the recto and verso of the object, with a hake. The object was then blotted, placed between new Hollytex (spun polyester web) and dried between blotter and felts.

PREPARATION OF SOLUTIONS

Calcium phytate solution 

6.9g phytic acid solution   

1.32g calcium carbonate 

24mL 3% ammonium hydroxide  

3L chilled deionized water   

 

Calcium carbonate was slowly added to the phytic acid and stirred. The mixture was added to 3L of chilled deionized water with a stirring rod. 3% ammonium hydroxide was added to the solution until the pH reached pH5.7. The solution was put back in the refrigerator to keep it chilled. The chilled calcium phytate solution was modified with chilled ethanol, so that the final solution would be 60:40 calcium phytate: ethanol. For each sheet of music manuscript, 1L solution was used for the phytate treatment.

 

Calcium bicarbonate

1.0g calcium carbonate

900mL chilled deionized water

 

The calcium carbonate was added to chilled deionized water and then placed in the SodaStream for carbonation. The calcium bicarbonate solution was placed back in the refrigerator to keep it chilled. The chilled calcium bicarbonate solution was modified with chilled ethanol, so that the final solution would be 70:30 calcium bicarbonate: ethanol. When using it in the bath, the calcium bicarbonate was poured slowly so that the precipitate was not poured into the bath. For each sheet of music manuscript, 1L solution was used.

 

0.5% Gelatin

5g Polistini Gelatin Type B 200 Bloom

700mL deionized water

300mL ethanol

 

Added 5g gelatin into 700ml deionized water. Allowed the swelling of the gelatin in the deionized water for an hour. Then fully dissolved the gelatin by warming. Before use, the gelatin was warmed up again and 300ml Ethanol was added into the Gelatin solution.

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