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Chemistry SL
Chemistry SL
Sample Internal Assessment
Sample Internal Assessment

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Table of content
Rationale
Research question
Background information
Hypothesis
Variables
Consideration
Apparatus used
Procedure
Data collection and analysis
Conclusion
Evaluation
Bibliography

Variation in the effectivity of fixing agents in dyeing process

Variation in the effectivity of fixing agents in dyeing process Reading Time
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Table of content

Rationale

Dyeing is one of the prominent applications of chemistry that people unknowingly observe every day. Dyeing garments is the most important application of dyeing. The clothes people wear has different color and pattern which comes after dyeing the fabric or material of the cloth. My home town, Pune, has one of the oldest dyeing industries in the country. As most of my family members are into this industry, I have decided to decipher few of my interests in the chemistry of dyeing as my chemistry internal assessment. The color fixation is a very vital parameter which involves economic factors of the company as well. Owing to my research, I came across several dye fixing agents that are usually used in several dyeing industries; however, I was more interested to understand an intrinsic factor of the dye fixing agent and its effect on color fixation. As studied in chemical kinetics of IB Chemistry, pH chemical has significant effect in the rate and yield of product of any chemical reaction. Thus, in this exploration, I have decided to build the relationship between the intensity of color fixation and pH of different dye fixing agents used to come up with the best economically favorable dye fixing agent.

Research question

How does the pH of different fixing agents (Sodium bicarbonate, Caustic soda, Potassium hydroxide, Soda ash, and a mixture of one third Caustic soda and two third soda ash) affect the color strength of cotton fabric, which is dyed using Reactive Red Dye?

Background information

Reactive dye

It combines with the cellulose group of cotton fabric by covalent bonds. Reactive dye consists of four parts: chromogen - responsible of coloration; reactive system – responsible for chemically reacting with cellulose group of cotton; bridging system – responsible for connecting chromogen and reactive group; solubilizing group – responsible for solubilizing the dye in water.

Fixing agents

In the process of dyeing, as all the dye molecules couldn’t be fixed on the surface of the fabric, fixing agents were used to fix those molecules on the fabric. As these chemicals are usually alkaline in nature, these are added to the dye bath in the process of dyeing to neutralize the acidic solution and form covalent bonds to fix the unbonded dye molecules with the cellulose of the cotton fabric.

Dyeing process

The process of dyeing consists of four parts. They are as follows:

  • The fabric is treated with water and sodium chloride (salt).
  • The fabric is then dyed as per requirement.
  • Fixing agents are added into the dye bath.
  • Washing of dyed cloth.

Fixing of dye onto cellulose

The chromogen present in the dye forms the coloration. When the reactive system reacts with the terminal hydroxyl group of the cellulose of the cotton material, the chromogen molecules are made fixed with the cellulose molecule of the cotton fabric by covalent bonds. The chromogen molecules which are not bonded a fixed by the fixing agents (alkaline). The acid – base neutralization reaction connects the remaining unfixed chromogen molecules with the cellulose group of the fabric by covalent bonds. Due to this reaction, hydrogen ion and hydroxyl ions are liberated by the breakdown of water molecules present in the dye bath. The liberated hydroxyl ions react with cellulose and forms cellulosate ion which lose the capability of combining with chromogen. Hence, the alkalinity of the fixing agents should sufficiently high so that the cellulosate ions could form and terminate the reaction.

Figure 1 - Reaction Between Reactive System And Hydroxyl Group Of Cellulose

Methodology

The cloth will be firstly dyed using reactive red dye and five different fixing agents. Apart from that, in one trial, no color fixing agents would be used.

 

Spectrophotometer was used to determine the intensity of color fixing in this exploration. The intensity of darkness of color in the fabric was expressed using K/S value where K is the light absorbance of the dyed cloth and S is the scattering of light. The device determines the above-mentioned ratio for light of different wavelengths of the visible spectrum. More the value of K/S, darker is the cloth.

Hypothesis

Null Hypothesis: There is no effect in the color strength of cotton fabric when it is dyed in presence of different fixing agents with varying pH.

 

Alternate Hypothesis: There is significant effect in color strength of cotton fabric when it is dyed in presence of different fixing agents with varying pH.

 

According to the information provided above, it could be stated that dye may not be fixed on the cotton cloth if the fixing agents are either highly alkaline or highly acidic. Hence, the predicted curve would be as follows:

Figure 2 - Estimated Variation Of Color Fixing With Respect To pH Of Fixing Agent

Variables

Independent variable

The pH of fixing agent used during the process of dyeing was considered as the independent variable of the exploration. To vary the pH of fixing agents, those agents were chosen in such a way that their individual pH vary over a significant range. The fixing agents that were used in this exploration along with their pH are as follows:

Fixing Agent
pH
Sodium Bicarbonate
8.09
Soda Ash
10.74
Mixture of one third Caustic soda and two third Soda ash
12.76
Potassium Hydroxide
13.01
Caustic Soda
13.26
Figure 3 - Table On Independent variable

Dependent variable

The color absorbance expressed in terms of K/S value, obtained using a spectrophotometer was considered as the dependent variable of this exploration.

Controlled variable

Controlled Variable
Why was it controlled?
How was it controlled?
Temperature of bath used
Variation in bathing temperature would not allow the fixing agents to work in optimum condition which might result in obtaining unreliable data.
The temperature of the bath was made constant for all the trials using temperature-controlled system.
Amount of dye used
Amount of dye used is directly proportional to the color strength of the dyed cloth. Hence, without changing the pH of the fixing agent (independent variable), the color strength would vary.
0.6 gm of dye was used in all the trials of this experiment.
Amount of fixing agent used
Variation in the quantity of fixing agents might change the color fixation on the dyed cloth. Thus, the effect of pH of fixing agent could not be established.
2.4 gm of fixing agent was used in all the trials of the exploration.
Amount of cloth used as sample
The size and quantity of cloth has a significant effect in color fixation in the process of dyeing. If the amount or size of cloth is more, color fixation would be less and vice versa. Thus, relationship between the color fixation and pH of fixing agents could not be deciphered.
10 gm of cotton cloth sample was used in all the trials of the exploration.
Duration of stirring
Duration of stirring is directly proportional to the color fixation. Hence, it should be controlled in order to establish a relationship between color fixation and pH of fixing agents.
In all the trials, the stirring time was constant.
Type of dye used
Different dye has different binding ratio with the cloth. Hence, without changing the pH of the fixing agent (independent variable), the color strength might vary.
Only Reactive Red Dye was used throughout all the trials in this exploration.
Concentration of solution used
Variation in concentration of solution might resulting in a variation in color fixation of the cloth resulting in establishing an unreliable relationship between the color fixation and pH of fixing agent.
In all the trials, the concentration of solution used was same.
Figure 4 - Table On Controlled Variable

Consideration

Safety considerations

  • Rubber gloves were worn throughout to experiment to avoid skin exposure to any chemical.
  • Aprons and thermal gloves were worn throughout the exploration, to avoid thermal burns while touching any hot or warm object.

Ethical considerations

  • All the materials used in this exploration were purchased and utilized at optimum amount to avoid loss or wastage of chemical products and also to decrease the cost of products.
  • The NaCl (sodium chloride) used in this exploration was obtained dyeing unit treatment plant to avoid wastage of chemical.

Environmental considerations

The experiment was performed in a laboratory with an Effluent Treatment Plant. Hence, all the water used in the dyeing process was purified before disposal or reuse.

Apparatus used

Apparatus
Quantity
Least Count
Uncertainty (±)

Conical Flask (200 cm3)

1
-
-
Dyeing Beaker
24
-
-

Pipette (1 cm3)

1

0.1 cm3

0.05 cm3

Glass rod
4
-
-
Beam balance
1
0.01 g
0.005 g
Spatula
1
-
-
Funnel
4
-
-
Spectrophotometer
1
0.1 K/S
0.1 K/S
Lab Infracolor Dyeing Machine
1
-
-
Figure 5 - Table On Apparatus Used

Chemicals used

Figure 6 - Table On Chemicals Used

Procedure

Salt treatment of cotton RFD cloth

  • Sodium chloride was taken and 8 g of it was measured using a digital mass balance.
  • A beaker was taken and it was washed with distilled water and dried using clean cloth.
  • 100 cm3 of water was added into the beaker.
  • The measured sodium chloride was then transferred into the beaker with 100 cm3 of water.
  • The NaCl solution in the beaker was stirred until dissolved.
  • A cotton cloth was taken and 10 g of it was taken after measuring it using a digital mass balance.
  • The 10 g sample of cotton cloth was kept under running water until it was completely wet.
  • The wet cloth was then transferred into the NaCl solution containing beaker.
  • The solution and the cloth in the beaker were then stirred for 5 minutes at a temperature of 25℃ using a Lab Infracolor Dyeing Machine.
  • The fabric was then taken from the beaker and the excess liquid was rinsed out into the beaker.

Dyeing of cloth

  • In the beaker containing sodium chloride solution, 0.6 g of dye was added.
  • The content of the beaker was stirred for 5 minutes at a temperature of 50℃ in a Dyeing Machine.
  • The content of the beaker was then filtered using a filter paper.
  • The filtrate was then transferred into a separate beaker and kept to cool until it reached to a temperature of 25℃.
  • The sample cloth, drenched in sodium chloride solution was transferred to the beaker and it was stirred for 20 minutes in the Dyeing Machine.
  • The fabric was then taken from the beaker and the excess liquid was rinsed out into the beaker.

Treatment using fixing agent

  • Sodium bicarbonate was taken and 2.4 g of it was measured using a digital mass balance.
  • It was then transferred to the remaining solution of the beaker as obtained in Part 2.
  • The solution was stirred until the sodium bicarbonate has completely dissolved.
  • The sample cloth was again transferred into the beaker and stirred for 5 minutes.
  • The content of the beaker was stirred for 15 minutes in a Dyeing Machine with a gradually increase in temperature till 60℃ (4℃ per minute).
  • The fabric was then removed and washed under running water for five times.

Acid and soaping oil treatment

  • Acetic acid was of 0.1 cm3 volume was pipetted out.
  • A beaker was taken and it was washed with distilled water and dried using clean cloth.
  • The obtained acetic acid was transferred into the beaker.
  • The sample cloth was again transferred into the beaker.
  • The sample cloth was transferred to the beaker and it was stirred for 10 minutes in the Dyeing Machine at a temperature of 35℃.
  • The fabric was then taken from the beaker and the excess liquid was rinsed out into the beaker.
  • Another beaker was taken and it was washed with distilled water and dried using clean cloth.
  • Soaping oil of 0.2 cm3 volume was pipetted out and transferred into the beaker.
  • The sample cloth was transferred to the beaker and it was stirred for 10 minutes in the Dyeing Machine at a temperature of 80℃.
  • The fabric was then removed and washed under running water for three times.
  • The readings of spectrophotometer were noted.

The above steps were repeated four more times for each fixing agent. Furthermore, the entire experiment was repeated by changing the fixing agents as mentioned in the independent variable section (refer to section Variables). Other than that, the experiment was repeated without using any fixing agent which is referred as Control Condition.

Data collection and analysis

Qualitative analysis

Fixing Agents
Observation
Control Condition
Light pinkish red fabric
Sodium Bicarbonate
Faded pink fabric
Soda Ash
Very deep pink fabric
Mixture of one third Caustic soda and two third Soda ash
Deep pink fabric
Potassium Hydroxide
Slightly light pink fabric
Caustic Soda
Slightly light pink fabric with a blotchy look
Figure 7 - Table On Qualitative Analysis

Quantitative analysis

Figure 8 - Table On Variation In K/S Value Of Dyed Cloth For Different Fixing Agents

Sample Calculation for Control Condition:

 

Mean\(\frac{8.5+8.5+8.4+8.5+8.6}{5}\) = 8.5

 

Standard Deviation\(\sqrt{\frac{(8.5-8.5)^2+(8.5-8.5)^2+(8.5-8.4)^2+(8.5-8.5)^2+(8.5-8.6)^2}{5}}\) = 0.1

 

Percentage Uncertainty\(\frac{±0.1}{8.5}\) × 100 = ± 1.2 %

Fixing Agent
pH
K/S value (±0.1)

Control condition

7.24
8.5

Sodium Bicarbonate

8.10
4.6

Soda Ash

10.73
24.1
Mixture of one third Caustic soda and two third Soda ash
12.77
18.0

Potassium Hydroxide

13.02
11.1

Caustic Soda

13.24
9.2
Figure 9 - Table On Variation Of Color Fixation (Measured In K/S Value) With Respect To pH Of Fixing Agents
Figure 10 - Variation Of Color Fixation (Measured In K/S Value) With Respect To pH Of Fixing Agents

Analysis

From the above-mentioned graph, the variation of color fixing (in terms of K/S value) with respect to pH of fixing agent has been established. The intensity of color fixation in K/S was plotted along Y – Axis, and the pH of fixation agent was plotted along X – Axis. The intensity of color fixation increases from a pH of around 8 till a pH of around 11. With further increase in pH of fixing agent, the color fixation decreases. From the graph, it is clearly observed that, when the pH of fixing agent increases from 8 to 11, the intensity of color fixation in K/S ratio increases from 4.6 to 24.1. However, with further increase in pH of fixing agent to 13.3, the color fixation decreases to 9.2. Hence, it could be stated that the color fixation is optimum at a pH of around 11.

Conclusion

How does the pH of different fixing agents (Sodium bicarbonate, Caustic soda, Potassium hydroxide, Soda ash, and a mixture of one third Caustic soda and two third soda ash) affect the color strength of cotton fabric, which is dyed using Reactive Red Dye?

 

The color fixation is greatly affected by the pH of fixing agent used in the dyeing process of cotton fabric using Reaction Red Dye. The color fixation is optimum when the pH of the fixing agent was 10.73. Fixing agent having a pH of less or greater than that has yield in less color fixation.

  • The color fixation of cotton fabric dyed using Reactive red dye in terms of K/S value when no fixing agent was used was 8.5.
  • The color fixation of cotton fabric dyed using Reactive red dye in terms of K/S value sodium bicarbonate was used was 4.6.
  • The color fixation of cotton fabric dyed using Reactive red dye in terms of K/S value when soda ash was used was 24.1.
  • The color fixation of cotton fabric dyed using Reactive red dye in terms of K/S value when a mixture of one third of caustic soda and two third of soda ash was used was 18.0.
  • The color fixation of cotton fabric dyed using Reactive red dye in terms of K/S value when potassium hydroxide was used was 11.1.
  • The color fixation of cotton fabric dyed using Reactive red dye in terms of K/S value when caustic soda was used was 9.2.
  • The color in the fabric were most deep when the mixture of one third of caustic soda and two third of soda ash was taken which came out to be very deep pink.
  • The color in the fabric were least deep when no fixing agent was taken which came out to be light pink.

Evaluation

Strength

The experiment was performed in a Lab Infracolour Dyeing Machine which is why all the external and internal conditions was controlled efficiently.

 

The materials required in this exploration was obtained from valid sources which provide chemicals and dyeing agents to various dyeing industries so that the exploration could be error free and reliable.

 

The pH of fixing agents mentioned in the Variable section were measured using pH meter prior to the experiment.

 

Method of triangulation was obtained while collecting raw data. Five trials for each fixing agent were obtained and the mean of the trials were considered for the exploration to nullify the random error or other human error. It has made the exploration more coherent.

Limitations

Source of Limitation
How would it affect the exploration?
How could it be controlled?
Sample of cloth
The fabric sample was obtained on the basis of mass. If the thickness of the fabric was different, then it would affect the color fixation.
The area of surface and the thickness of the cloth should be measured using vernier calipers and controlled.
Quantity of fixing agents
As many fixing agents are functional at definite optimum quantity or concentration, that was not obtained in this exploration because in this exploration, all the constant mass of each fixing agent was taken.
Fixing agents should be taken of definite quantity at which its operation strength (yield of reaction) is maximum.
Mixing of dye solution
The sodium chloride solution and the dye solution were manually stirred without using any profound machinery. This might result in improper or not complete dissolving of salt solution and dye solution. This might introduce a systematic error in the exploration.
Efficient machineries should be used to mix or stir solutions.
Figure 11 - Table On Limitations

Extension

In the exploration, a relationship between the pH of fixing agents used and color fixing intensity of reactive red dye on cotton fabric was established. As a lot of variables were controlled in this exploration, which also conveys an idea of the effect of each of those controlled variables on the color fixation (dependent variable). Apart from that, it could also be stated that the pH of the fixing agents would have significant impact on color fixation if any one of those controlled variables was made to be the independent variable. Hence, I would extend the idea of this exploration not only within the boundaries of one dependent versus one independent variable, rather, I would like to further explore the effect of pH of fixing agents on intensity of color fixing for different fabrics such as silk, cotton, polyester, and wool.

 

The research question would be framed as: How does the pH of different fixing agents (Sodium bicarbonate, Caustic soda, Potassium hydroxide, Soda ash, and a mixture of one third Caustic soda and two third soda ash) affect the color strength of cotton fabric, silk fabric, polyester and wool, which is dyed using Reactive Red Dye and hence determining the effect of pH of fixing agent on different fabric material?

 

The procedure would be similar to that of the current exploration. Sample of four different cloth materials of equal mass, thickness and area would be obtained and would be firstly dyed using reactive red dye and five different fixing agents. Apart from that, in one trial, no color fixing agents would be used.

 

Spectrophotometer was used to determine the intensity of color fixing in this exploration. The intensity of darkness of color in the fabric was expressed using K/S value where K is the light absorbance of the dyed cloth and S is the scattering of light. The device determines the above-mentioned ratio for light of different wavelengths of the visible spectrum. More the value of K/S, darker is the cloth.

Bibliography

  • Fixing Agent | Dyeing | NICCA Textile Chemicals. https://nctexchem.com/product/process/dyeing/fixing/. Accessed 20 May 2021.
  • Get Familiar with Your Textile Production Processes | Textile Guide. https://textileguide.chemsec.org/find/get-familiar-with-your-textile-production-processes/. Accessed 20 May 2021.
  • Gutteridge, J. M. ‘Reactivity of Hydroxyl and Hydroxyl-like Radicals Discriminated by Release of Thiobarbituric Acid-Reactive Material from Deoxy Sugars, Nucleosides and Benzoate.’ Biochemical Journal, vol. 224, no. 3, Dec. 1984, pp. 761–67.
  • Reactive Dye - an Overview | ScienceDirect Topics. https://www.sciencedirect.com Accessed 20 May 2021.
  • Tojimirzaev, Sanjar. Woven Terry Fabrics. www.academia.edu, https://www.academia.edu/45640909/Woven_Terry_Fabrics. Accessed 20 May 2021.
  • Valko, E. I. ‘Particle Size in the Vat Dyeing of Cellulose1’. Journal of the American Chemical Society, vol. 63, no. 5, May 1941, pp. 1433–37. ACS Publications, doi:10.1021/ja01850a083.
  • www.fibre2fashion.com. Methods of Dyeing | Process of Dyeing | The Chemistry of the Dyeing Process | Dyeing Machinery and Equipment | Fibre2fashion.Com. http://www.fibre2fashion.com Accessed 20 May 2021.