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��ࡱ�>��	24����/01p����������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������������[�	����bjbj����	�Cΐΐ��,��������������t����999� ��"�95s��&@�&�&�&�&v(�(�(�r�r�r�r�r�r�r$�u�sxD�r��(v(v(�(�(�r���&�&��r�6�6�6�(L	��&��&�r�6�(�r�6�6Nd�th�&���� �sB��9�1��e0�rs05s�e��x�4��x`thth��x��i��(�(�6�(�(�(�(�(�r�r�6�(�(�(5s�(�(�(�(���������������������������������������������������������������������x�(�(�(�(�(�(�(�(�(�	�:	@ EQ\x\to(P) EQ\x\to(P)Development of Antimicrobial Textiles Using Zinc Pyrithione
                       Anil Kumar Jain1  & Addisu Ferede Tesema2 

1Textile Expert, Bahir Dar Textile Share Company, Bahir Dar, Ethiopia
P.O.Box:� 1037Bahir Dar/ Ethiopia�Office phone:� +251 583 20 60 30� � ��Fax: +251 582 26 62 46
Email : anilkumarjain220561@gmail.com
2 Scientific Director, Ethiopian Institute of Textile and Fashion Technology [EiTEX]Bahir Dar University
Abstract

An attempt has been made to produce antimicrobial 100% cotton textiles using Zinc Pyrithione. Zinc Pyrithione being bacteriostatic in nature is eco friendly and safe, both for manufacturer to apply and consumer to use. After conducting laboratory trials, bulk trial has also been conducted and efficacy of Zinc Pyrithione as bacteriostatic has been quantitatively determined. The durability of antibacterial finish was also checked before & after repeated domestic laundry. To enhance durability of antibacterial finish with Zinc Pyrithione, use of binder is recommended.
Key words -  Antimicrobial, Antibacterial, Textiles, Bacteriostatic, Zinc Pyrithione.

Introduction

The microorganism�s growth on textiles causes a range of undesirable effects, not only on the textile itself, but also on the user. These effects include the generation of unpleasant odor, reduction in mechanical strength, stains and discoloration and an increased likelihood of user contamination [1]. Therefore, due to the growing public health awareness of the pathogenic effects, over the last few years, intensive research and development have been promoted in order to minimize or even eliminate microbe�s growth on textiles. This microbial contamination is a great concern, mainly for textiles used in hospitals as medical devices or for health and hygienic care, but also in sports clothing, water purification systems, animal feed and the food industry. The infections acquired in hospitals may be caused by several species, such as�Escherichia coli, Staphylococcus aureus.

Two different aspects of antimicrobial protection provided by chemical finishes can be distinguished. The first is the protection of the textile user against pathogenic or odour causing microorganisms (hygiene finishes). The second aspect is the protection of the textile itself from damage caused by mould, mildew or rot producing microorganisms [2&3]. The growth of microorganisms on textiles can lead to functional, hygienic and aesthetic difficulties (for example staining). The most trouble-causing organisms are fungi and bacteria [4]. Under very moist condition, algae can also grow on textiles and are troublesome because they act as nutrient sources for fungi and bacteria. Fungi cause multiple problems to textiles including discoloration, coloured stains, and fibre damage. Bacteria are not as damaging to fibres, but can lead to fibre damage, unpleasant odours and a slick, slimy feel [4].  Often, fungi and bacteria are both present on the fabric in a symbiotic relationship. Substances added to fibres, such as lubricants, antistats, natural-based auxiliaries (for example size, thickener and hand modifiers) and dirt provide a food source for microorganisms. Synthetic fibres too are not totally immune to microorganisms, for example polyurethane fibres and coatings can be damaged [5&6]. Natural fibres are more easily attacked. Wool is more likely to suffer bacterial attack than cotton, and cotton is more likely than wool to be attacked by fungi.
Antimicrobial finishes are particularly important for industrial fabrics that are exposed to weather. Fabrics used for awnings, screens, tents, tarpaulins, ropes, etc. need protection from rotting and mildew. Home furnishings such as carpeting, shower curtains, mattress ticking and upholstery also frequently receive antimicrobial finishes. Fabrics and protective clothing used in areas where there might be danger of infection from pathogens can benefit from antimicrobial finishing. These include hospitals, nursing homes, schools, hotels, and crowded public areas. Textiles in museums are often treated with antimicrobial finishes.
 Sized fabrics that are to be stored or shipped under conditions of high temperature (~ 40 �C or 100 �F) and humidity require an antimicrobial finish to retard or prevent microbial growth fuelled by the presence of warp size. Textiles left wet between processing steps for an extended time often also need an antimicrobial treatment [4].

The use of antimicrobial finishes to prevent unpleasant odours on intimate apparel, underwear, socks and athletic wear is an important market need. The odours are produced by the bacterial decomposition of sweat and other body fluids, and controlling bacterial growth by hygiene finishes reduces or eliminates the problem. 

1.1 Properties of an effective antimicrobial finish

Due to their large surface area and ability to retain moisture, textiles are known as being conducive to microorganisms growth, such as bacteria and fungi, which can be found almost everywhere and are able to quickly multiply, depending on the moisture, nutrients and temperature levels [7]. Some bacteria populations may double every 20�30 min under ideal conditions (36�40 �C, pH 5�9), meaning that one single bacteria cell can increase to 1,048,576 cells in just 7 hours [8]. Therefore, antimicrobial finishes must be quick acting to be effective. In addition to being fast acting, the antimicrobial must kill or stop the growth of microbes and must maintain this property through multiple cleaning cycles or outdoor exposure. The antimicrobial must be safe for the manufacturer to apply and the consumer to wear. The finish must meet strict government regulations and have a minimal environmental impact. The antimicrobial finish must be easily applied at the textile mill, should be compatible with other finishing agents and have little if any adverse effects on other fabric properties including wear comfort, and should be of low cost.   

1.2 Mechanisms of antimicrobial finishes

Most of the antimicrobial agents used in commercial textiles are biocides acting in different ways according to their chemical and structural nature and affinity level to certain target sites within microbial cells. Those different modes of action may be [9]:
Damage or inhibition of cell wall synthesis, which is critical for the life and survival of bacterial species;
Inhibition of cell membrane function, which is an important barrier that regulates the intra- and extra-cellular flow of substances, could result in the leakage of vital solutes for the cells survival;
Inhibition of protein synthesis, which is the basis of cell enzymes and structures, consequently leading to the death of the organism or the inhibition of its growth and multiplication;
Inhibition of nucleic acid synthesis (DNA and RNA) due to the binding of some antimicrobial agents to components involved in the process of DNA or RNA synthesis. This inhibition interferes with normal cellular processes, compromising microbes multiplication and survival;
Inhibition of other metabolic processes, for instance, the disruption of the folic acid pathway, which is essential for bacteria to produce precursors important for DNA synthesis.
Despite the long list of requirements, a variety of chemical finishes have been used to produce textiles with demonstrable antimicrobial properties. These products can be divided into two types based on the mode of attack on microbes. One type consists of chemicals that can be considered to operate by a controlled-release mechanism. The antimicrobial is slowly released from a reservoir either on the fabric surface or in the interior of the fibre. This �leaching� type of antimicrobial can be very effective against microbes on the fibre surface or in the surrounding environment. However, eventually the reservoir will be depleted and the finish will no longer be effective.  In addition, the antimicrobial that is released to the environment, may interfere with other desirable microbes, such as those present in waste treatment facilities [4]. 
The second type of antimicrobial finish consists of molecules that are chemically bound to fibre surfaces. These products can control only those microbes that are present on the fibre surface, not in the surrounding environment. �Bound� antimicrobials, because of their attachment to the fibre, can potentially be abraded away or become deactivated and lose long term durability. Antimicrobial finishes that control the growth and spread of microbes are more properly called bio stats, i.e. bacteriostats,  fungistats. Products that actually kill microbes are biocides, i.e. bacteriocides, fungicides. This distinction is important when dealing with governmental regulations, since biocides are strongly controlled. Textiles with biostatic properties, however, are subject to fewer regulations [4].
The actual mechanisms by which antimicrobial finishes control microbial growth are extremely varied, ranging from preventing cell reproduction, blocking of enzymes, reaction with the cell membrane (for example with silver ions) to the destruction of the cell walls and poisoning the cell from within  [5&6].  An understanding of these mechanisms, although important for microbiologists, is not really a requirement for the textile chemist who applies and evaluates the effectiveness of antimicrobial finishes.

1.3 Chemistry of Antimicrobial Finishes


1.3.1 Antimicrobials for controlled release
Many antimicrobial products that were formerly used with textiles are now strictly regulated because of their toxicity and potential for environmental damage. Products such as copper naphthenate, copper-8-quinolinate, and numerous organo mercury compounds fall into this category. Other materials that still have limited use in specialised areas include tributyl tin oxide, dichlorophene and 3-iodopropynylbutyl carbamate . These products typically show a very broad spectrum of activity against bacteria and fungi, but suffer from application and durability problems.
Some more useful products of this same general type include benzimidazol derivatives, salicylanilides and alkylolamide salts of undecylenic acid (particularly effective against fungi). Application of these materials with resin pre-condensates can improve durability to laundering, but also deactivation by reaction with the resin may occur.
A widely used biocide and preservation product is formaldehyde. Solutions of formaldehyde in water, called formalin, were used for disinfection and conservation, for example, of biological samples for display. Bound formaldehyde is released in small amounts from common easy-care and durable press finishes. Therefore these finishes include � at least until they are washed � a small antimicrobial side effect. This can also be true for some quaternary compounds, for example wet fastness improvers and softeners. But for more effective requirements specific antimicrobial finishes are necessary [4].
One of the most widely used antimicrobial products today is 2,4,4'-trichloro-2'- hydroxydiphenyl ether, known more commonly as �triclosan�. Triclosan finds extensive use in mouthwashes, toothpastes, liquid hand soaps, deodorant products, and the like. Although it is effective against most bacteria, it has poor antifungal properties. Triclosan is also important as a textile finish, but since its water solubility is very low, aqueous application requires use of dispersing agents and binders.
Quaternary ammonium salts have been found to be effective antibacterial agents in cleaning products and for disinfecting swimming pools and hot tubs. However, their high degree of water solubility limits their use as textile finishes.
Research into controlled-release antimicrobials continues with organo-silver compounds and silver zeolites, which are promising candidates for textile finishes. Silver ions, for example, incorporated in glass ceramic, have a very low toxicity profile and excellent heat stability [5&6]. These principles are also used for fibre modification, an alternative to the antimicrobial finishes with high permanence [10].
In recent years a variety of antimicrobial modified fibres have been developed, including polyester, nylon, polypropylene and acrylic types. An example of these fibre modifications is the incorporation of 0.5�2 % of organic nitro compounds (for example based on 5-nitrofurfural) before primary wet or dry spinning.
Regenerated cellulosics can be modified with carboxylic or sulfonic acid groups, followed by immersing in a solution of cationic antimicrobials which are then fixed to the cellulose by salt bonds. A novel approach to the controlled release of antimicrobials is microencapsulation. These capsules are incorporated either in the fibre during primary spinning or in coatings on the fabric surface.

1.3.2 Bound antimicrobials

Several antimicrobial finishes that function at fibre surfaces have been commercialised. One popular product is based on octa-decyl-amino-dimethyl-trimethoxy-silylpropyl-ammonium chloride. This material can be applied by either exhaust or continuous methods. After application, a curing step is required to form a siloxane polymer coating on the fibre surface. This coating immobilises the antimicrobial part of the molecule (the quaternary nitrogen) and provides the necessary durability to laundering. Another bound finish has been developed with PHMB, polyhexamethylene biguanide. PHMB can also be either pad or exhaust applied. This chemical has the proper molecular structure to bind tightly to fibre surfaces, yet still be an effective antimicrobial. The antimicrobial effect of cationically charged materials is thought to involve interaction of the cationic molecule with anionic phospholipids in the microbe�s cell walls. This interaction is believed to increase the permeability of the cell walls to the point of cell death [4].
A new and novel approach to bound antimicrobials was recently introduced. Cotton reacted with methylol-5,5-dimethyldyantoin is then treated with hypochlorite to form chloramines in the fibre. These chloramine sites have antibacterial activity and can function as renewable antimicrobial agents by continued treatment with hypochlorite through household bleaching and washing after reacting with bacteria. Problems with using higher concentrations of chloramines include yellowing with heat (for example ironing) and cellulose fibre damage especially significant strength loss, caused by oxy- and hydrocellulose generated by hypochlorous acid.
Another novel approach is the application of chitosan. This modified biopolymer is manufactured from inexpensive natural waste. Chitin from crustacean shells (e.g. from crabs) is converted to chitosan by alkaline treatment. 
Alkali splits most of them (75�95 %), generating free amino groups that provide fungistatic and bacterostatic effects. This mild antimicrobial activity may be amplified by methylation of the amino groups to quaternary trimethylammonium structures. Chitosan can be applied by microencapsulation or by reactive bonding to cellulose and by crosslinking of chitosan. The advantages of the antimicrobial finish with chitosan include high absorbency properties, moisture control, promotion of wound healing, non-allergenic, non-toxic and biodegradable properties [11].

Antimicrobial Textiles by the Incorporation of Antimicrobial Agents in Fibers

Another approach to develop textiles with an antimicrobial ability is by the incorporation of the antimicrobial agents into the polymeric matrix of the textile fibers. 
The agents may be incorporated into the polymeric granules prior to the production or just added to the chamber during the extrusion or electro spinning process [1]. The sub-micron range of fibers produced by electro spinning reveals several advantages, such as a high surface area to volume ratio, adjustable porosity and the ability to manipulate the nano fiber composition to obtain the desired properties [7].
The direct addition of the biocide agent into the polymers has received considerable attention, especially when using thermoplastic matrices. The main advantage of this method is that it may be easily implemented in the standard and large-scale processing units already designed to prepare particulate-filled polymer composites, which are extensively used in the textile industry. Besides that, when using a low agent content, the resulting mechanical properties of the modified fibers are similar to the unmodified ones. The main disadvantage of this method is the lower antimicrobial power due to the restricted diffusion of the antimicrobial agent molecules through the polymeric matrix. Most of the incorporated agent gets trapped in the matrix, not being available to interact with microorganisms and to perform its biocide or bacteriostatic function. However, the agents� incorporation may provide better durability, as the agent is physically withheld in the polymeric matrix, promoting a slower release during use [1].  .
However, this agent�s incorporation on textile fibers may only be used for some synthetic polymers due to the high standard processing temperature used in an extrusion process. In addition, it is also necessary to carefully select the antimicrobial agent regarding its temperature stability. Therefore, metallic particles or even nano particles are the most used agent in this method, as they do not present degradation when submitted to the standard processing conditions of thermoplastic polymers. There are also some products available on the market in the form of fibers or fabrics based on natural fibers possessing an intrinsic antimicrobial ability, such as Chitopoly��and Crabyon�, which are based on chitosan and cellulose fibers. However, the biocide and bacteriostatic action of these kinds of products is less efficient than the ones that use the most conventional antimicrobial agents presented in this review.
1.5 Zinc Pyrithione as antimicrobial

The antimicrobial chemical used in this work is bacteriostatic and prevents the growth of bacteria on the treated textile. Unpleasant smells due to e.g. decomposition products formed by the transformation of body perspiration are effectively prevented e.g. in sportswear, underwear, active wear, outdoor clothing, socks and stockings etc.
This finish is hygienic for mattress ticking, upholstery, carpets, bed linen and curtains. It increases shelf life of textiles like wipes, shoe materials, awnings etc by preventing their damaging by bacteria and fungi.
This chemical is effective whether on socks which have to be washed often or on a filter nonwoven with a long service life. The product is active over long periods of time and survives a lot of wash cycles. Tests confirmed a very good bacteriostatic effect even after 20 washing processes.
This chemical is well skin-compatible and is eco safe. The chemical structure of Zinc Pyrithione is given in Figure 1 [12&13]. 

             C10H8N2O2S2 Zn

Figure 1. Chemical structure of Zinc Pyrithione
              
The fabric treated by this process has high bacteriostatic and fungistatic activity, and retains antimicrobial properties after repeated laundering.
2.0 Experimental
2.1 Materials
The fabric used for experimentation was 100% dyed cotton with vinyl sulfone type of reactive dyes, having 145 gsm, without any finishing agent. 
The antimicrobial chemical used was Zinc Pyrithione, pre-solubilised in water. 
2.2 Methods 

2.2.1 Determination of % Pick up

The % pick up of 100% cotton dyed fabric, at various pressure readings (2, 3, 4 & 5 bar) and at constant speed of 2.62 metres/minute, was determined using two bowls vertical padding mangle, made by Mathis, Switzerland.
The 100% dyed cotton fabric was weighed before & after padding in water. The difference in the weight of wet and dry fabric expressed as percentage of weight of dry fabric gave the % pick up as per following formula:

W � D x 100 = % Pick up
   D
Where, W is the weight of wet fabric.
             D is the weight of dry fabric.
2.2.2 Application of Antimicrobial

100% cotton fabric was padded with 3, 6, 9 and 12 gm / litre Zinc pyrithione aqueous solution at pH 5 to 6 maintained using 1 gm per litre acetic acid. The following padding conditions were used to ensure 80% pick up: 
Mangle Pressure: 4.5 bar
Speed: 2.62 metres/minute
After padding, the treated fabric samples were dried in SDL � Mini dryer at 1350C for 3 minutes.
2.2.3 Application of Antimicrobial in Bulk
The 100% cotton fabric was treated with  Zinc pyrithione on stenter using following conditions :
Zinc Pyrithione = 12 g/l
Binder  = 20 g/l
Magnesium Chloride = 1 g/l
Acetic acid = 1 g/l
Wetting agent = 1 g/l
The fabric was padded with above solutions followed by drying at 1750C for 2 minutes.
2.2.4 Determination of Bacteriostatic Efficacy 
The quantitative evaluation of antimicrobial activity in four samples treated with various concentrations of antimicrobial finished products was carried out by the JIS L 1902:2008 test method as given in Table 1 (Test Variables).
Test organismsStaphylococcus aureus and Escherichia coliDilution medium usedTryptic soya broth (TSB)Eluting medium usedSterile normal saline (0.85% NaCl)Method of sterilization (pre-cleaning )Autoclave, 121 0C, 15 lbs, 15 minutesSize of swatch per Sample0.4 gUntreated control24 hr contact timeTreated samples24 hr contact timeTable 1- Test variables
Sample identification
C24= untreated control sample inoculated with bacteria for 24 hour contact time. 
3g/l concentration treated sample inoculated with bacteria for 24 hour contact time
6g/l concentration treated sample inoculated with bacteria for 24 hour contact time
9g/l concentration treated sample inoculated with bacteria for 24 hour contact time
12g/l concentration treated sample inoculated with bacteria for 24 hour contact time.
2.2.5 Determination of Permanency of Bacteriostatic effect 

In order to determine the permanency of bacteriostatic effect, the cotton fabric treated with 12gms/litre, Zinc Pyrithione (antimicrobial) chemical was subjected to washing cycles 10 & 20 times employing DIN EN ISO 6330 standard for domestic laundry using launderometer made by Mesdan Lab, Italy under following laundry conditions:
Washing temperature: 400C 
Washing time: 15 minutes
Detergent used: EEC Non Phosphate without optical brightening agent
Detergent concentration: 1.25 g/l
M:L:R ratio: 1:20
Drying temperature: 700C 
Time: 10 minutes
After each washing cycle, the fabric was rinsed thoroughly with tap water, squeezed and dried at 700C for 10 minutes
After completing 10 & 20 washing cycles, the bacteriostatic efficacy test was done using JIS L 1902:2008 test method.
2.2.6 Determination of Colour Fastness to Washing 

The colour fastness to washing of both untreated and treated cotton fabric with 12gms/litre Zinc Pyrithione (antimicrobial) was tested using ISO-2 test employing following conditions in launderometer supplied by Mesdan Lab, Italy and the washed samples were dried in an oven supplied by Mesdan, s.p.a Italy, type M250-VF:
Temperature � 500C 
Time � 45 minutes
Detergent � 5gms/litre (ECE Non Phosphate, SDC reference detergent Type 2)
M:L:R ratio = 1:50
Adjacent Fabric Used: SDC Multi fibre DW
The change in colour and the staining on multi fibre fabric was evaluated using AATCC grey scale both for change in colour and staining respectively.

2.2.7 Determination of Colour Fastness to Crocking

The colour fastness to crocking of both untreated and treated cotton fabric with 12gms/litre Zinc pyrithione (antimicrobial) was tested employing AATCC Test Method-8-2004, using Crock meter supplied by Mesdan Lab, Italy. Both the fabric samples were subjected to 10 rubs cycle with dry cotton and wet cotton cloth respectively using Cotton Lawn Rubbing fabric supplied by SDC enterprise. The staining on cotton rubbed fabric was evaluated using AATCC grey scale for staining. 

2.2.8  Determination of Colour Fastness to Perspiration

The colour fastness to perspiration of both untreated and treated cotton fabric with 12gms/litre Zinc pyrithione (antimicrobial) was tested, employing ISO 105 � EO4 1994 (Acid and Alkaline perspiration), using Perspirometer supplied by Mesdan Lab, Electrical Heat Thermostatic Culture Box., Model DH-4000B, Italy. 
The samples of untreated and treated cotton fabric in contact with the standard SDC multi fibre DW fabric (for colour staining) were immersed in simulated alkaline and acid solution, drained and placed between two plates under a specific load, temperature and time in the perspirometer. Any change in colour of the samples and staining of the multi fibre was then assessed with the corresponding Grey scales for colour change and staining respectively.

2.2.9 Determination of Colour Fastness to Light 

The natural sunlight source was used for determining the colour fastness towards light of both untreated and treated cotton fabric with 12gms/litre Zinc pyrithione (antimicrobial) [14].
The light fastness rating system was based on the rate of fading of eight blue-dyed wool standard samples which are rated from 1 (poor) to 8 (excellent). All the eight blue wool standard samples were exposed to natural sunlight source along with untreated and treated cotton fabric. The light fastness rating was given comparing the fading of blue wool standard no. and tested samples placed parallel to blue wool standard.
2.2.10 Determination of Tear Strength 

The tear strength of both untreated and treated cotton fabric with 12gms/litre Zinc Pyrithione (antimicrobial) was determined, employing ASTM D 1424 method, using SDL Atlas M008E Digital Elmendorf Tester. 
2.2.11 Determination of Tensile Strength 

The tensile strength of both untreated and treated cotton fabric with 12gms/litre Zinc Pyrithione (antimicrobial) was determined, employing ISO-13934/1-EN 13534/1, using Fabric Traction Strip method with Tenso Lab Strength Tester, Mesdan Lab, Italy. 
3.0 Results & Discussions

3.1 Effect of Mangle Pressure on % Pick up

The effect of mangle pressure on %pickup was determined at a mangle speed of 2.62 metres/minute. The results are shown in Figure 2. 
 EMBED Excel.Chart.8 \s 
Figure 2.. Relation Between Mangle Pressure & % Pick up

It can be seen from Figure-2, that with increase in pressure, % pick up reduces and after 4 bar pressure, reduction in %pick up slows down. A mangle pressure of 4.5 bar was selected to get 80% pickup on 100% cotton.

3.2 Effect of Zinc Pyrithione (Antimicrobial) on Bacteriostatic Property

The effect of Zinc Pyrithione (antimicrobial) on bacteriostatic property was studied by determining the bacteria growth on untreated fabric as control fabric against treated fabrics (3, 6, 9 & 12 gm/litre) using JIS L 1902:2008 test method.
The results are given below:
In Table 2, records of the CFU values at plates of different dilutions that was used to determine the bacterial counts per sample of swatches using Staphylococcus aureus are given.

Sample10-110-210-310-410-510-6CFU/sampleC24TNTTNTTNTTNTTNT1751.75x10103TNTTNTTNTTNT2212002.21x1096TNTTNTTNT160301.6x1089TNTTNT12510001.25x10712TNTTNT654006.5x106Table 2. CFU values against Staphylococcus aureus
Where:
CFU= Colony Forming Units per test sample 
TNT= Too numerous to count
CFU/sample= CFU were counted ranging between 25 to 250 at minimum dilution to ensure accuracy of results.

It can be seen from Table 2, that number of Staphylococcus aureus recovered from untreated control sample after 24 hour contact time (C24) was 1.75x1010 CFU/sample. However, the number of Staphylococcus aureus recovered in treated fabric at concentrations of 3, 6, 9, 12 gm/liter show reducing trend with increase in concentration of Zinc Pyrithione.
The percentage reduction in bacteria was calculated using following formula :
Calculation of percent reduction of bacteria in treated specimen 

100 (C � A)/C= R



Where:
R = % reduction
A = the number of bacteria recovered from the inoculated treated test specimen incubated over the 24 hour contact period
C= the number of bacteria recovered from the inoculated untreated control specimen incubated over the 24 hours contact period.
It can be seen from Table 3, that even at 6 gm / liter concentration of Zinc Pyrithione, 99% reduction in Staphylococcus aureus bacteria growth has been achieved.
SampleRecovered bacteria after 24 hr contact time (CFU/Sample)% Reduction in bacteria compared to C24  (untreated fabric),   (Bacteriostatic Effect )C241.75x1010-32.21x10987.3761.6x10899.0891.25x10799.93126.5x10699.96Table 3-  Percent reduction of Staphylococcus aureus (Gram positive bacteria)
It can be seen from Table 4, that average number of Escherichia coli recovered from untreated control sample after 24 hour contact time (C24) was 1.72x1010 CFU/ sample. However, the number of Escherichia coli recovered in treated fabric at concentrations of 3,6,9,12 gm/liter show reducing trend with increase in concentration of Zinc Pyrithione.


Sample10-110-210-310-410-510-6CFU/sampleC24TNTTNTTNTTNT11001721.72x10103TNTTNT1357411.35x1076TNTTNT527005.2x1069TNT520260002.6x10612167000001.67x105Table 4 - CFU against using Escherichia coli
It can be seen from Table 5 that even at 3 gm / liter concentration of Zinc Pyrithione, above 99% reduction in Escherichia coli bacteria growth has been achieved.


SampleRecovered bacteria after 24 hr contact time(  CFU/Sample)% Reduction in bacteria compared to C24  (untreated fabric),
(Bacteriostatic effect )C241.72x1010-31.35x10799.9265.2x10699.9792.6x10699.98121.67x10599.99Table 5- Percent reduction of Escherichia coli ( Gram Negative Bacteria)
          

                                                     
3.3 After wash samples 
It can be seen from Table 6, that average number of Staphylococcus aureus  recovered from untreated control sample after 24 hour contact time (C24) was 2.1x1010 CFU/ sample. However, the number of  Staphylococcus aureus  recovered from 12gm/liter treated sample, after 10 washes were 6.1x109    CFU/ sample.
Staphylococcus  aureusSample10-110-210-310-410-510-6CFU/sampleC24TNTTNTTNTTNTTNT2102.1x101012(10Washes)TNTTNTTNTTNT600616.1x109Table 6- CFU values against Staphylococcus aureus
 It can be seen from Table 7, that after 10 domestic washing cycles, the percentage reduction in growth of Staphylococcus aureus was 70.95% with 12 gm /liter treated sample.
SampleRecovered bacteria after 24 hr contact time(  CFU/Sample)% Reduction in bacteria compared to C24  (untreated fabric),
(Bacteriostatic effect )C242.1x1010-12(10Washes)6.1x10970.95Table 7. Percent reduction of Staphylococcus aureus (Gram Positive Bacteria) 

It can be seen from Table 8, that average number of Escherichia coli  recovered from untreated control sample after 24 hour contact time (C24) was 1.72x1010 CFU/ sample. However, the number of Escherichia coli   recovered from 12gm/liter treated sample, after 10 washes were 6.5x109    CFU/ sample.


Sample10-110-210-310-410-510-6CFU/sampleC24TNTTNTTNTTNT11001721.72x101012 ( 10 W)TNTTNTTNTTNT856656.5x109Table 8. CFU values against Escherichia colis

 It can be seen from Table 9, that after 10 domestic washing cycles, the percentage reduction in growth of Escherichia coli was 62.2% with 12 gm /liter treated sample. 

SampleRecovered bacteria after 24 hr contact time(  CFU/Sample)% Reduction in bacteria compared to C24  (untreated fabric)
(Bacteriostatic effect )C241.72x1010-12 ( 10 W)6.5x10962.2Table 9. Percent reduction of Escherichia coli ( Gram Negative Bacteria)
In both the cases (Staphylococcus aureus & Escherichia coli), the reduction in bacteriostatic efficacy was observed after 10 domestic washing cycles, indicating that the bacteriostatic effect is semi-durable.
 3.4 Bulk treated cotton fabric with Zinc Pyrithione & Binder

It can be seen from Table 10, that average number of Staphylococcus aureus  recovered from untreated control sample after 24 hour contact time (C24) was 2.46x109 CFU/ sample. However, the number of  Staphylococcus aureus  recovered from 12gm/liter treated bulk sample (unwashed) was 1.71x108 and after 20 washes were 5.6x108    CFU/ sample.

Sample10-110-210-310-410-5CFU/sampleC24TNTTNTTNTTNT2462.46x10912gTNTTNTTNT171141.71x108After 20 washesTNTTNTTNT854565.6x108Table 10. CFU values against Staphylococcus aureus 
It can be seen from Table 11, that the percentage reduction in growth of Staphylococcus aureus was above 93% with 12 gm /liter treated bulk sample (unwashed) & after 20 domestic laundry cycles, the percentage reduction in growth of Staphylococcus aureus was above 81%.
SampleRecovered bacteria after 24 hr contact time(  CFU/Sample)% Reduction compared to C24
(bacteriostatic effect )C242.46x109-12 g1.71x10893.05After 20 washes5.6x10881.70Table 11. Percent reduction of Staphylococcus aureus 
It can be seen from Table 12, that average number of Escherichia coli recovered from untreated control bulk sample after 24 hour contact time (C24) was 1.04x1010 CFU/ sample. However, the number of  Escherichia coli  recovered from 12gm/liter treated bulk sample (unwashed) was 2.25x107 and after 20 washes were 1.61x109    CFU/ sample.
Sample10-110-210-310-410-510-6CFU/sampleC24TNTTNTTNTTNTTNT1041.04x101012gTNTTNT22514--2.25x107After 20 washesTNTTNT65045016151.61x109Table 12. CFU values against Escherichia colis
It can be seen from Table 13, that the percentage reduction in growth of Escherichia coli  was above 99% with 12 gms /litre treated bulk sample & after 20 domestic laundry cycles, the percentage reduction in growth of Escherichia coli  was above 84%.
SampleRecovered bacteria after 24 hr contact time(  CFU/Sample)% Reduction compared to C24
(bacteriostatic effect )C241.04x1010-12g2.25x10799.78After 20 washes1.61x10984.52Table 13. Percent reduction of  Escherichia coli 
In both the cases (Staphylococcus aureus & Escherichia coli), above 80% bacteriostatic efficacy was observed even after 20 domestic washing cycles, indicating that the bacteriostatic effect is durable.
3.5 Effect of Antimicrobial on Fabric Properties

As shown in Table 14, the various fabric properties have been compared between untreated and treated. The results are self explanatory and do not show any significant change in fabric properties.
S.No.ParametersUntreated Dyed FabricTreated Dyed Fabric1Colour Fastness to Washing��Change in Colour4 to 54 to 5Staining on Adjacent Fabric4 to 54 to 52Colour Fastness to Rubbing��Staining on Adjacent Fabric��Wet Rubbing4 to 54 to 5Dry Rubbing4 to 54 to 53Colour Fastness to Perspiration��Acidic ��Change in Colour4 to 54 Staining on Adjacent Fabric4 to 54 to 5Alkaline��Change in Colour4 to 54 to 5Staining on Adjacent Fabric4 to 54 to 54Colour Fastness to Light>3�>3�Change in Colour�5Tensile Strength (Newtons)��Warp256259Weft1971926Tear Strength (Newtons)��Warp37.8538.14Weft38.9639.45
Table 14 - Comparison of Fabric Properties between Untreated and Treated Dyed cotton

4.0 Conclusions

The application of 6 g/l Zinc Pyrithione is adequate to get antibacterial effect above 90%, on 100% cotton fabric at 80% pick up followed by drying at 130 to 140�C. However, to get durable effect it is recommended to use Zinc Pyrithione along with binder. The application is simple and can be carried out on Stenter as per the recipe mentioned in materials & method.
There is no adverse effect of Zinc Pyrithione chemical on fabric properties as shown in Table-14. 
The antimicrobial textiles developed in this work, can earn huge export earnings as the antimicrobial textiles market size is estimated to be valued at USD 497.4 Million in 2015 and is projected to reach USD 1,076.1 Million by 2026, at a CAGR of 7.4% from 2016 to 2026 as per the report published in  HYPERLINK "http://www.marketsandmarkets.com" www.marketsandmarkets.com. This finish is in high demand in the Asia-Pacific region, Middle-East & Africa, South & North America and Europe because of increasing end-use applications such as,�medical textiles and apparel. The medical applications are the�largest�segment of the antimicrobial textiles market such as, surgical supplies,�curtains, beddings, and upholstery items. 

5.0 Acknowledgements

The authors are thankful to Mr.Adaneh, Director, Textile Chemistry Research and Innovation Centre, Ethiopian Institute of Textile and Fashion Technology (EiTEX) for giving permission to work in Wet Processing Laboratory.
We are also thankful to Mr. Daniel, Lab Head of Wet Processing Lab for helping us in conducting the experiments and Dr. Takele of Food Microbiology Laboratory, Faculty of chemical & Food Technology, Bahir Dar Institute of Technology for testing bacteriostatic properties.






6.0 References

Shahidi, S. and Wiener,(2012) J., Antimicrobial Agents�Chapter 19: Antibacterial Agents in Textile Industry; InTech: Rijeka, Crotia.
Vigo, T. L., (1983) Handbook of Fibre Science and Technology, Vol. II, Chemical Processing of Fibres and Fabrics, Functional Finishes, Part A, 367�427.
Vigo, T. L., (1994) Textile Science and Technology II, Textile Processing and Properties, Amsterdam, Elsevier, 252�262.
Schindler,  W. D. and Hauser, (2004) P. J.,Chemical finishing of textiles, Woodhead Publishing Limited, Cambridge, England . 

Dring, I.,(2003) �Antimicrobial, rot proofing and hygiene finishes�, in Textile Finishing, D Heywood (ed.) Bradford, Society of Dyers and Colourists, 351�371.

Rajan, J., (1999) Antimicrobial Finishes for Textiles, presented at the Chemical Principles of Textile Finishing Short Course, North Carolina State University, Raleigh, NC.
Gao, Y and Cranston, R., (2008) Recent advances in antimicrobial treatments of textiles.�Text. Res. J., 78, 60�72.
  Zanoaga, M. and Tanasa, F.,(2014) Antimicrobial reagents as functional finishing for textiles intended for biomedical applications. I. Synthetic organic compounds.�Chem. J. Mold, 9, 14�32
Glazer, A.N., and  Nikaido, H.,(2007) Microbial Biotechnology: Fundamentals of Applied Microbiology; Cambridge University Press: Cambridge, MA, USA.
Kawata T,(1988) �First permanently antibacterial and deodorant fibres�, Chemical Fibres International, 48(2), 38�43.
Knittel D and Schollmeyer E, (1988), (2002) �Chitosan  und seine Derivate f�r die Textilveredlung�, part 1,  Textilveredlung, 33(3/4), 67�71 and part 4 Melliand Textilberichte, 83(1/2), 58�61.
Morris, Cletus E. & Wech, Clark M.,  Zinc Pyrithione Process to Impart Antimicrobial properties to Textiles, US patent No. US4443222 A., (1984) April 17. 
Morris, Cletus E. & Wech, Clark M., Antimicrobial Finishing of Cotton with Zinc Pyrithione, British patent No. 1,202,716, (2016) July 02. 
Jinlian, H.U., Fabric testing by Published by Wood head Publishing Limited in association with The Textile Institute Abington Hall, Granta  Park, Great Abington, Cambridge CB21 6AH, England (2008).








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