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Beating Time as a Variable of Dye AbsorptionAndrew Crone and
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For our project, we tested dye absorption of cotton fibers as a function of beating time. We decided to use fiber reactive dyes in a yellow color to determine if dye absorption was affected by beating time. We hypothesized that the longer the cotton fibers are beaten, the more dye the fibers will absorb because more of the fibers will be open and able to absorb the dye. Although we could not exactly measure absorption, using a colorimeter we were able to measure the hue, chroma, and lightness of each wafer.
As we have learned in our classes and labs, paper is created from long fibers of cellulose. The source of cellulose that we decided to use for this project was cotton. One of the main reasons that we chose to use cotton fibers was because of the large amount of cellulose found in cotton, almost 100% (Bordley Ch. 7 p. 2). Cellulose is made of glucose, which we know to be a simple sugar. Since cotton is almost 100% cellulose, it is also linear, which "allows the cellulose molecules to pack together to form microfibrils and then fibers" (Bordley Paper Chemistry p. 1). During the creation of pulp and paper, the cellulose is beat in water. This beating process is called fibrillation because the "beating causes the outer layers of he fibers to partially detach from the main fibers" (Bordley Paper Chemistry p. 3). This allows the water to hydrate the pulp. To rid the pulp of excess water the pulp is placed in a filter or on a screen. As the excess water drains away "the fibers intertwine and the microfibrils produced during the beating can then form links with other fibers nearby" (Bordley Paper Chemistry p. 3). The pulp is then placed on a board to dry allowing excess water to evaporate. This evaporation causes the fibers to become closer and more intertwined than before. This is the final step that gives paper strength and flexibility.
Once we made the decision to use cotton fibers, we knew that we must choose a dye that would react well chemically with the fibers. Naturally we chose fiber-reactive dyes because these dyes react with cotton fibers and they have advantages in the area of our experiment. Fiber-reactive dyes are available in a large amount of colors and "are capable of imparting deep shades to paper" (Koretsky 34). Also these dyes are capable of forming one of the strongest chemical bonds with cellulose that a dye can. Fiber-reactive dyes are not used very much in commercial paper making because of hydrolysis. In most cases when dye is added to the pulp, the dye will only bind with the fibers and not with the carrier, or water. But with fiber-reactive dyes, hydrolysis occurs causing the dyes to "chemically bond with the water as well as with the cellulose" (Koretsky 34). For this reason a rinsing process is highly needed to get rid of the dyed water. Because of the large amount of dye lost through the rinsing process, in most cases a dye activator is used. The rinsing procedure is also used to rid the pulp of the NaCl that is needed for the dying process.
Controlled factors:
1. Type of fiber (100% cotton)
2. Sample size (150mL)
3. Type of dye (PRO MX Dye Powder)
4. Final beater setting (1)
5. Dye color (yellow)
6. Dye amount (7 grams of powder to create solution & 14mL dye solution for each sample)
7. NaCl amount (1.5 grams for each sample)
8. Dye activator amount (5mL for each sample)
9. Order of operations (1st added dye solution to pulp, 2nd added NaCl to pulp, 3rd separated dyed pulp and dyed water, 4th added dye activator to dyed water, 5th recombined dyed pulp and dye activated water)
10. Rinsed each sample
11. Drying method (board)
Materials
1. 83.8% of a pound of 100% cotton shirts
2. Beater
3. 7 grams of PRO MX Dye Powder (yellow)
4. 1.5 grams of NaCl (per sample)
5. 5mL dye activator (per sample)
6. 14mL dye solution (per sample)
7. Water
8. Labels
9. 12 200mL beakers for samples
10. Saran wrap
11. Bucket (excess pulp)
12. Pan (excess pulp water)
13. Large filter
14. Small filter
15. Water hose
16. Beater cleaning utensils
17. 300mL beaker
18. Funnel
19. Bottle (dye solution)
20. Strainer
21. Magnets
22. Electronic Magnetic Stirrer
23. Wire Screen
24. Tin Can
25. Stand and Ring
26. Pelons
27. Felt
28. 2L Coke Bottle (filled with water)
29. Drying board
30. Colorimeter
31. Graduated cylinder
32. Small vials (NaCl)
Procedures
1. Beater Preparations
a. Ripped apart three 100% Cotton shirts (.838 lbs) into small shreds.
b. Soaked shredded shirts in water.
c. Filled up beater with water until the water level was between the two stickers on the side of the beater.
d. Added shredded shirts.
2. Calibrating the Beater
a. Turned handle until belt was stiff to the point that the pressure was needed to move it.
b. Reset dial to zero.
c. Repeated two more times to make beater accurate.
Shea Leatherman as he calibrates the beater.
3. Beating the Pulp
a. Plugged beater in and started beating on beater setting 20.
b. Lowered beater setting every three minutes until beating setting one is achieved.
4. Collecting the Pulp
a. After beating setting one has been on for three minutes, started five minute interval samples until 60 minutes was reached. This gave twelve different samples.
b. Each sample of pulp was taken in a beaker. 150mL of pulp was used for each sample size and then the beaker was properly labeled according to the time interval.
c. Covered each beaker with saran wrap.
d. Let samples sit for 24 hours.
Sample of beaten pulp after 30 minutes of beating.
5. Beater Clean Up
a. Drained excess pulp water into bucket under beater drain using a filter to catch excess pulp.
b. Once excess pulp was caught in the filter, the excess pulp was then transferred to a large bucket.
c. The excess pulp bucket was then covered with saran wrap and the excess pulp water was disposed of properly.
d. Cleaned beater out with a water hose and utensils making sure to rid beaker of any dried pulp that was left inside of the beater.
Collection of excess pulp after beater clean up.
6. Dye Preparation
a. Discovered the amounts of ingredients needed for creating a dye solution for the samples which was estimated to be one-fifth of a pound of pulp.
b. The dye solution for the 1/5 pound of pulp included 7 grams of PRO MX Dye Powder, and for each sample 1.5 grams of NaCl and 5mL of dye activator.
PRO MX Dye Powder (yellow).
Dye Solution that we created using the dye powder and water.
MX Dye Activator, used with reactive dyes to help replace dye lost during rinsing process.
7. Creating the Dye Solution
a. Placed 250mL of water into a beaker.
b. Placed seven grams of PRO MX Dye Powder into the beaker with the water.
c. Transferred the solution to a new bottle using a funnel. Made sure to hold the funnel in the air so that air could escape from the new bottle.
8. Combining Dye Solution and Pulp
a. Added 14mL of dye solution to each beaker sample of pulp.
b. Added 1.5 grams of NaCl to each sample of dyed pulp.
c. Separated each sample of dyed pulp from the dye solution using a strainer.
d. Added 5mL dye activator to the dye solution.
e. Combined new solution with the dyed pulp.
f. Placed magnet in sample and placed sample on electric magnetic stirrer for one minute and then stirred occasionally.
g. Repeated for all samples.
Seperating dyed pulp and pulp water so that dye activator can be added.
Pulp with dye activator added. Notice the color change.
9. Rinsing the Pulp
a. Ran water through pulp in a filter until filtered water no longer had dye in it.
10. Creating wafers
a. Placed wire screen on stand with tin can on top of the screen.
b. Placed large beaker under screen to catch excess pulp water.
c. Poured sample into tin can, making sure to hold can firmly against wire screen.
d. After drainage was complete, placed wafer on a moist pelon on top of felt.
e. Placed another pelon and more felt on top of wafer and then couched the wafer using a two liter coke bottle.
f. Placed wafer on drying board to dry.
g. Repeated for all samples.
Andrew Crone creating a wafer.
Andrew Crone couching the wafer.
11. Colorimeter Readings
a. Calibrated the colorimeter.
b. Switched the measurements to Munsell.
c. Took measurements for each sample.
Picture of all samples.
Original Pulp Samples (Before Being Dyed)
| Sample Number | Observations |
|---|---|
| 1 (5 minutes) | Pulp color is white. Pulp is slightly chunky and some large fibers are visible |
| 2 (10 minutes) | Pulp color is white. Fibers are still large and uneven |
| 3 (15 minutes) | Pulp color is white. Fibers are becoming thinner than before, but are still somewhat lumpy |
| 4 (20 minutes) | Pulp color is white. Fibers are becoming visibly thinner |
| 5 (25 minutes) | Pulp color is white. Fibers are becoming much more fine throughout |
| 6 (30 minutes) | Pulp color is white. Lumps within the pulp are now minimal |
| 7 (35 Minutes) | Pulp color is white. Fibers are visibly smaller |
| 8 (40 minutes) | Pulp color is white. No chunks of pulp are prevalent at this point |
| 9 (45 minutes) | Pulp color is white. Fibers are now very fine |
| 10 (50 minutes) | Pulp color is white. Length of each fiber has decreased dramatically |
| 11 (55 minutes) | Pulp color is white. Fibers are much more cohesive. |
| 12 (60 minutes) | Pulp color is white. Fibers are finer and much more even throughout than any previous sample |
During Process of Dying
| Sample Number | Observations |
|---|---|
| 1 | Dye was a clear yellow solution before dye activator was added. After dye activator was added, the solution became much darker with an orange/yellow color. Drained quickly. Pulp was yellow/orange before being rinsed of excess dye. |
| 2 | Drained easily. Because of the chunky fibers, the dye took some time to spread throughout the pulp. |
| 3 | |
| 4 | |
| 5 | |
| 6 | Water and dye take much more time time to drain. The dye solution spread easily throughout the pulp |
| 7 | The finer fibers were much easier to stir, allowing the dye to come in contact with the fibers at a faster rate. |
| 8 | |
| 9 | |
| 10 | |
| 11 | Long drainage time due to smaller fibers |
| 12 | Also long drainage time. The fine fibers allowed the dye to quickly cover all of the pulp while being stirred. |
Rinsing Process
| Sample Number | Observations |
|---|---|
| 1 | The water drains well and visibly contains a large amount of dye. The pulp becomes much more of a pale yellow. |
| 2 | Again, quite some time was needed to wash the excess dye from the solution |
| 3 | Some pulp stuck to filter and had to be rolled off. |
| 4 | Increase in drainage time |
| 5 | Water is draining noticeably slower. The amount of water used to wash the pulp has increased slightly. |
| 6 | Pulp is beginning to stick to the filter more frequently. |
| 7 | Rinsing water is very bright yellow/orange. |
| 8 | Drainage time is periodically increasing, as has the amount of water needed in the rinsing process. |
| 9 | Noticeably more rinsing water needed. |
| 10 | Increase in drainage time. |
| 11 | The rinsed pulp is no longer a bright orange/yellow. Much lighter yellow with no orange tint. |
| 12 | The water drains very slowly because the fibers were beaten into smaller pieces. More water was necessary to drain all of the dye from the pulp mix than was necessary with previous samples |
Dryed Samples
| Sample Number | Observations |
|---|---|
| 1 | This wafer took a lot longer to dry than most of the other wafers. The wafer is not very stiff, but rather flexible. The overall color of the wafer is an orange yellow, but the edge has an orange color to it. One side is much lighter than the other. |
| 2 | This wafer took about the same time to dry as the first wafer. This wafer is also flexible, but considerably stiffer than the first wafer. The color of this wafer is also orange yellow with orange edges but the other side is a much lighter yellow that looks almost the same as the majority of the wafers. |
| 3 | This wafer dryed a lot sooner than the first two and has a more true yellow color to it. Both side are about the same color yellow. This wafer also has the orange color around the edges. |
| 4 | This wafer dryed faster than the first three (about at the same time as the majority of the wafers). This wafer is pretty stiff. Both sides are a nice light yellow color and there is no orange color around the edges. |
| 5 | This wafer dryed at the same speed as the one above. This wafer is also quite stiff and has a nice light yellow color on both sides. No orange on the edges, but one edge did run a little. |
| 6 | This wafer dryed at the same speed as the two above. This wafer is stiff but not as stiff as the two above. The wafer has the same light yellow color as the ones above but wtih a hint of orange edges. |
| 7 | Wafer dryed at same speed as three above. This is the stiffest wafer yet. Nice light yellow color on both sides with no orange edges. |
| 8 | Wafer dryed at same speed as the four above. Wafer is pretty stiff. Light yellow color on both sides with no orange edges. |
| 9 | Wafer dryed at same speed as the five above. Wafer is very stiff but quite thin compared to the others. Light yellow color on both sides with no orange edges. |
| 10 | Wafer dryed at slower than the six above, but faster than the first couple. More of an orange yellow color on one side and light yellow on the other. Wafer does have orange edges. |
| 11 | Wafer dryed at the same speed as above. The wafer has an light yellow color to both sides but does have the orange edges. |
| 12 | Wafer dryed at the same speed as the two above. The wafer has the light yellow color to it on both sides but does have the orange edges. Not as stiff as previous two wafers. |
Colorimeter Data/Munsell Color System
| Sample Number | Hue | Lightness | Chroma/Saturation |
|---|---|---|---|
| 1 | 8.1 Y | 8.9 | 10.3 |
| 2 | 6.7 Y | 8.7 | 10.9 |
| 3 | 8.0Y | 8.9 | 9.8 |
| 4 | 1.4 GY | 9.1 | 8.5 |
| 5 | 9.6 Y | 9.2 | 9.0 |
| 6 | 9.0 Y | 9.1 | 9.2 |
| 7 | 9.2 Y | 9.2 | 9.0 |
| 8 | 9.3 Y | 9.2 | 8.8 |
| 9 | 9.5 Y | 9.2 | 8.4 |
| 10 | 7.2 Y | 8.8 | 10 |
| 11 | 8.7 Y | 9.1 | 9.7 |
| 12 | 8.9 Y | 9.1 | 9.1 |
In conclusion, it was discovered that beating time does not affect dye absorption as was hypothesized. This is evident by the measurements taken by the colorimeter. These findings give no pattern as was hoped for, such as a continuous increase or decrease in hue, chroma, or lightness. It would seem to make sense however that as the fibers are beaten for a longer period of time, those fibers would be able to absorb more dye and in doing so change the values found with the colorimeter. Although there was only one variable, there were in fact a lot of constants that may have been accidentally changed throughout the samples. Another problem with the experiment was the time restraints that were encountered. Because of only certain available working times, the pulp might have set in the dye bath for too long or we may have waited to long to add the dye activator. We also believe that we should have taken two colorimeter readings instead of just one: The one we took plus the board side of the wafer. This may have produced a more consistant measurement for all of the samples. We also decided not to heat the dyed pulp which was recommended. Since past projects, dealing with beating time as a variable of dye absorption, that used heat also concluded that beating time does not affect dye absorption, we argue that the heating process may not be important or neccesary.
At first we wanted to test multiple dyes to see which type of dye had the best absorption, but there were a couple of problems with this. What determines if one dye is better absorbed than another except for personal opinion? Also some of the dye types that we wanted to use such as acid dyes would not work with cotton fibers. We originally wanted to use one pound of pulp but instead ended up using 1/5 pound of pulp. In the beginning we were going to make sheets but thought it better to make wafers to consolidate the dye absorption.
Coloring Paper Pulp using PRO MX Reactive Dyes. (http://www.prochemical.com/directions/MX_PaperPulp.htm)
Reynolds, Alison. Dye Absorption in Abaca Pulp as a Function of Beating Time. (http://www.sewanee.edu/chem/chem&art/Detail_Pages/Projects_2004/Reynolds/index.html)
Bordley, John. Chemistry and Art (Draft). Ch. 7. 2005.
Bordley, John. Paper Chemistry. Class notes. 2005.
Koretsky, Elaine. Color for the Hand Papermaker. Carriage House Press. 1983.
PRO MX Reactive Dye Sampler (Cool Pallette). (www.prochemical.com)
We would like to give thanks to Dr. Bordley for his knowledge and expertise. We would also like to give thanks to Dr. Jennifer Bachman for her advise using chemicals. We would like to give thanks to Alison Reynolds for putting the idea for this project into our heads and helping us in creating a starting point for the project. Alison produced an experiment similar to this in one of the previous classes. Alison, however, used abaca pulp instead of cotton pulp. Some of our information, such as the fact that cotton dyes cannot be exhausted, were taken from her web site, and we would like to give her credit for her thorough and clearly written web page. Lastly we would like to give thanks to Syeda Hamadani and Jeremy Anthony for answering any question that we shot at them.