Method A By drop test

Drop of 0.5g/l methylene blue solution is placed on the fabric surface from a height of 2.5cm with the help of pipette. A stop watch is started as soon as the drop falls on the fabric and stopped no sooner the image of the reflected light disappears at the edge of the drop i.e. the water drop is completely absorbed by the fabric. This is termed as drop absorbency time. A drop absorbency of about 5sec is generally considered satisfactory for well-prepared Cellulosic materials. Method B By sinking time At least 4 samples of the size 1 1 are cut. Each sample is kept on the surface of water taken in 500ml glass beaker. Time taken by the piece to sink just beneath the water surface is measured. A sinking time of about 5sec is generally considered satisfactory for well prepared Cellulosic materials. Method C By capillary rise method A 5cm wide strip is cut across the filling direction. The strip is then cut into 5cm long sections. The numbered specimens are then immersed 1mm deep in 1% aqueous solution of C.I. Direct Blue 86 for 2 sec and then immediately placed on a wire screen. After drying, the capillary rise of the dye solution is measured. The uniformity in absorbency across the width can thus be tested.

I. Raw Materials and other inputs:

1. Water Quality a. Hardness i. bi-carbonate ii. Carbonates. sulphates and chloride b. TDS (Total Dissolved Solids) c. Turbidity d. Other metals iron, copper 2. Quality of Auxiliary Chemicals used. a. Quality of surfactants like wetting, scouring agents i. Wetting time of wetting agents ii. Solid content iii. Ionic nature iv. Cloud point of non-ionic products v. foaming characters b. Quality of sequestering agents i. Chelating power ii. pH iii. solid content c. Quality of leveling/dispersing agents i. Ionic nature ii. concentration required iii. solid content iv. suitability for metal complex dyes d. Quality of Peroxide Stabilizers i. Solid content ii. Concentration required for bleaching e. Quality of peroxide killers i. Whether it is an enzyme or inorganic product ii. concentration required for treatment iii. If it is enzyme, get the test method from the manufacturer himself. f. Quality of Cationic dye fixing agents i. Solid content ii. Free Formaldehyde content iii.. Degree of Change in tone of a shade iv. How much light fastness is affected? g. Quality of Softeners i. Ionic nature ii. Degree of softness acquired for a standard concentration

iii. Degree of tone change of a shade iv. wash Durability. Solid content h. Determination of Acid Value of a product? Detailed method to find out the acid value of a product i. Determination of Polymer content of a binder? Detailed method to find out the polymer content of a binder. j. Quality of Dyestuff: Dyestuff properties and selection method for a combination

2. Quality of Basic Chemicals used and its concentration.

i Caustic soda purity and concentration percentage ii Soda Ash purity and concentration iii. Acetic Acid, Hydrochloric acid, Sulphuric acid, Oxalic acid purity and concentration iv. Hydrogen Peroxide purity and concentration v. Common Salt purity, hardness of a particular concentration vi. Sodium Hypochlorite - concentration 3. Test for Iron and Copper in cotton fiber In order to avoid the quality problems that may arise due to the improper quality of greige (unprocessed) fabric or yarn, the following Quality Assurance measures has to be taken.

1) Physical properties:
Fiber maturity Fiber color Yarn CSP Tensile / tear strength Stains - oil, rust Fungus Appearance of fabric - weft bowing Abrasion marks weft missing / warp missing Number of cut-ends per squire meter

2) Chemical properties:
If found low in tensile/tear strength, fluidity test must be conducted Simple indicator tests to ascertain the damage in cellulose. Test for degree of polymerization. Analysis pf non-cellulosic residues. Tests for sizes Tests for fat and wax content Purity level of fibers or identification of contamination in fibers Methods of determination of maturity: Several methods are available to determine the maturity of cotton. These can be grouped as below: 1. Direct method - caustic soda swelling method 2. Indirect method. 1. Differential dyeing method 2. Causticaire method 3. Polarized light method. 1) Direct method- Caustic soda swelling method It is the most commonly used method A thin tuft of fibers is drawn by means of tweezers from a silver held in a comb sorter. The tuft is laid on a microscope slide., the fibers parallel and separated and a cover slip is put over the middle. Likewise four to eight slides are prepared. There are two steps involved in this method. 1. Treatment with 18% caustic soda. 2. Examination under a microscope to count the mature, half mature and immature fibers. The fibers on the microscope slide are then irrigated with a small amount of 18% caustic soda solution, which has the effect of swelling them. The slide is then placed on the stage of a

microscope and examined. The presence or absence of the convolution is observed and the fibers are classified into three groups. 1. Mature or normal fibers. 2. Half mature or thin walled fibers. 3. Immature or dead fibers. The presence of caustic soda changes the appearance of both mature and immature fibers by swelling. Mature fibers with a well developed cell wall and pronounced convolutions in the raw state become rod like swelling. These rod like fibers are classified as normal or mature fibers. In the case, the lumen is practically absent. Dead or immature fiber appear ribbon like even after swelling. In dead fibers, the wall thickness is less than 1/5th of the ribbon width. Thin walled or half mature fibers are those lying between the other two classes. The fibers are classed as above based on the ratio of lumen width (L) to wall thickness (W) as indicated below: Class Ratio of lumen width to wall thickness ( L / W ) Mature Less than 1 Half mature 1-2 Immature Greater than 2 All the slides are examined as above and the percentage of mature ( N ) half mature ( H ) and the immature ( I ) fibers are calculated. Then the maturity of the cotton fiber is expressed by any one of the following terms: 1. Percentage of Mature fibers , N 2. Maturity ratio , M 3. Maturity co-efficient, Mc

Copper and Iron content in the fiber

Test for Iron on the fiber:
Reagents: Nitric Acid 5% or 10% w/w Analytical grade. Potassium Thiocyanate Solution 10% w/w made by dissolving 10 g Potassium thiocyante in 90 gram distilled water Potassium bisulphate, analytical grade. Hydrogen peroxide 35% w/w. A small sample 0.5 to 1.0 gram of fiber is placed on a watch glass and then spotted with 1-2 drops of nitric acid (5%) and allowed to stand for 2-3 minutes so that any iron present is oxidized to ferric ions. To detect ferric ions, 2 to 4 drops of potassium thiocyanate (10%) are added. If no color forms then no iron is present. A red color indicates iron is present and the intensity of the color indicates the amount. A pink color indicates low concentrations and a wine red color high concentrations. Potassium Ferrocyanide test: A small sample of fabric on a watch glass is spotted with dil Hydrochloric acid(10%). The acidified area of the fabric is then spotted with dil.Pot.ferrocyanide (1% solution freshly prepared). A dark blue color indicates the presence of iron.

Test for Copper:

Copper tetramine test: The fabric sample is properly ashed using an oven and the cooled ash is spotted with 5 to 10 drops of nitric acid (10%) or hydrochloric acid or by melting with pot.bisulphate. Add dil. Ammonia (1:1) until the ash is alkaline. A blue color shows the presence of copper. A white background e.g. a sheet of paper helps in observing the shade changes.

Testing Soda Ash & Hydrogen Peroxide

In Textile Processing the following materials are considered to be basic chemicals or bulk chemicals used in processing. The quality of each product whether basic or auxiliary chemical would certainly affect the final quality of textile processing. So a good dye-house should have a continuous quality monitoring procedure like one shown below. As and when a new product or chemical enters your dye-house, its quality should be compared with the previous supply without fail.

Soda Ash:
Weigh accurately 1 gram of Soda ash and dissolve in 50ml of distilled water. Titrate this slowly with 1.0N HCl, using methyl orange as indicator. Total alkalinity as Na2CO3.% by weight = 5.3 x V x 1 / Wt where 'V' is the volume of HCl consumed and 'wt' is the exact weight of soda ash taken for titration. Repeat the above titration for 3 times, tabulate and take the average reading as the % concentration of Soda ash as Sodium carbonate.

Hydrogen Peroxide:
Take 10ml of Hydrogen Peroxide solution and dilute it to 500ml using distilled water. From this diluted solution of Hydrogen peroxide take 10ml and add 20ml of 1.0N H2SO4.. Titrate against 0.1N KMNO4 (potassium permanganate). The end point is the appearance of light pink color. Repeat this titration 3 times and tabulate the readings. Find out the average titration value (V). [Hope the reader would be aware of the volumetric titration principles. Titrating two solution of standard known strength and unknown
strength, one can easily find out the strength of the other. The simple formulae used for this purpose is;

V1N1 = V2N2
where V1 = Volume of Standard Solution, N1 = Normality of Standard solution, V2=- Volume of unknown solution, N2 = Normality of unknown solution. Concentration of the unknown solution in grams / liter = Normality of unknown solution x Equivalent weight of the substance.] In the above example, if V is the volume of KMnO4 consumed for titrating 10 ml of 10/500 or 1/50 ml of H2O2; Eq.Wt of H2O2 = 17. Applying the formula

V1N1 = V2N2

N1 = V2N2 / V1 Normality of H2O2 [N] = V [KMnO4] x 0.1 / [1/50]

Strength of Hydrogen Peroxide = V x 0.1 x 50 x 17/ 10 x 3.03 [volumes]. Commercially Hydrogen Peroxide is available in two concentration - viz., 35% and 50%. In the above calculation please note that 1 ml of 0.1N KMNO4 is equal to 0.0017g 100% H2O2. To find out the concentration of Hydrogen Peroxide in terms of % strength, follow the simple procedure below: About 1.5 gram of H2O2 is accurately weighed and made up to 250 ml in a standard flask. To 10 ml of this solution, 50 ml distilled water and 30 ml of 20% Sulphuric acid added. The mixture is then titrated against 0.1 KMNO4 .
%

H2O2

Calculation: Volume of KMNO4 X N x 17 = / Weight of Sample in 10 ml The result is in percentage strength.

X 10

Determination of Hydrogen Peroxide content in bleach bath:

Hydrogen Peroxide content can be determined by titration against standard potassium permanganate solution. Procedure: To carry out the titration, measure 100ml dilute (10%) Sulphuric acid solution into a 250ml conical flask. Titrate with KMNO4 (0.1N) to a faint pink color. Pipette a suitable quantity of aliquot (Vml) of hydrogen peroxide bleach bath solution, usually 2 or 10 ml, into the beaker containing the dilute acid and titrate immediately with potassium permanganate to the same faint color. Let the titre be A ml of 0.1N KMNO4. Calculation: Since 1 ml of KMNO4 (0.1N) is equivalent to 0.0017g H2O2 100%, then V ml bleach bath solution will contain 0.0017 x A gram of H2O2 100%. The strength of the bleach bath is therefore = 0.0017 x A x 1000 / V g/l H2O2 100%. Example: Titration of 10 ml of bleach liquor sample required 8.5 ml of 0.1N KMNO4. What is the H2O2 content of the bath in grams/liter? Calculation: H2O2 content = 0.0017 x 8.5 x 1000/ 10 = 1.445 g/l H2O2 100%

Concentration of H2O2
Volume of 0.1N KMNO4 used ml 1 2 3 4 5 6 7 8 9 10 as 100% g/l .85 1.70 2.55 3.40 4.25 5.10 5.95 6.80 7.65 8.50 as 50% g/l 1.7 3.40 5.10 6.80 8.50 10.20 11.90 13.60 15.30 17.00 a 50% ml/l 1.43 2.86 4.29 5.72 7.15 8.58 10.01 11.44 12.87 14.30 as 35% g/l 2.42 4.84 7.26 9.68 12.10 14.52 16.97 19.36 21.79 24.20 as 35% ml/l 2.14 4.28 6.42 8.56 10.70 12.84 14.98 17.12 19.26 21.40

Testing Strength of Acetic acid, Hydrochloric acid , Sulphuric acid and Oxalic acid
Standardisation of Sulphuric Acid: Mol Wt: 98.08 & Eq. Wt: 49.0 49 grams/litre of H2SO4 gives 1N acid. Strength Testing of Sulphuric Acid: Weigh accurately about 1 gram of the acid and transfer to a conical flask with D.D.Water. Add phenolphthalein indicator and titrate against 0.5N NaOH to a permanent pink colour. % of H2SO4 = (Vol. of NaOH x N of NaOH x 49) / (Wt of Acid x 10) Standard Norms = 96.5% to 98% w/w. Acetic Acid Strength Testing: Mol Wt: 60.05 Eq.Wt: 60.05 Freezing Point:16.6 and Boiling Point:118C Weigh accurately about 0.5 gram of the sample and transfer to a conical flask using D.D.Water. The solution is titrated against 0.5N NaOH using phenolphthalein indicator. The end point is permanent pink colour. % of AcOH = (Vol. of NaOH x Normality of NaOH x 60) / (Wt of acid x 10) Standard Norms : 96 to 98% w/w Strength of Citric acid : Eq Wt: 70 Melting Point:153C Weigh accurately 0.5 gram of the sample and dissolve in 50 ml of distilled water. Add phenolphthalein indicator and titrate against 0.5N NaOH to a permanent pink color. Calculation: % of acid = (Vol of NaOH x N x 70)/(Wt of acid x 10) Standard Norms : 95 to 98% w/w. Strength Testing of Hydro Chloric Acid: Mol Wt: = 36.46 Weigh accurately 0.5 gram of the acid and transfer to a conical flask with D.D.water. Add phenolphthalein indicator and titrate against 0.5N NaOH to a permanent pink colour. % of HCl = (Vol of NaOH x Normality of NaOH x 36.5) / Weight of HCl x 10 Standard Hydrochloric acid strength will be 29 to 35 Tri Sodium Phosphate: Eq Wt: 82 About 5 grams of dried sample ( heated to 100C for 2 hours), accurately weighed is dissolved in 50 ml of distilled water. Add 2.5 gram of common salt (vacuum salt) and after to 15C, the solution is titrated to a distinct red color with 1N HCl, using methyl orange as indicator. Calculation: % of T.S.P. = (Vol of HCl X Normality of HCl x 82)/(Wt of the sample x 10) Potassium Permanganate: Mol Wt: 158.04 Wq.Wt = 31.61 Preparation of Standard solution: 3.161 gram of KMNO4 in 500 ml of D.D.water boiled for 30 minutes and made up to 1 litre gives 0.1N solution. Determination of the strength of KMNO4: 20 ml of 0.1N Oxalic acid + 20 ml of 1N H2SO4 are heated to a warm temp. and titrated against KMNO4.

V1N1 = V2N2 N1= V2N2 (0.1 X 20)/burette reading of KMNO4 Oxalic Acid Strength Testing: Mol Wt:126.07 Eq.Wt :63.02 Weigh about 0.5 gram of the acid and transfer to a conical flask containing 50 ml of distilled water. Dissolve the acid completely and titrate against 0.5N NaOH using phenolphthalein as indicator. % of HOOC-COOH.2H2O = (Vol of NaOH x N x 63)/ (wt of acid x 10) Standard Norms = 94 to 98% w/w. Strength of Sodium Bicarbonate: NaHCO3 : About 1 gram of the sample accurately weighed is dissolved in distilled water and made up to 250 ml. a 50 ml of the solution is titrated against 0.1N HCl using phenolphthalein as indicator and the reading noted as Y. Take another 50 ml of the solution and titrate against 0.1N HCl using methyl orange as indicator and the Titre value be X. Caluculation: % of Sod.Bicarbonate = [(X 2Y) x 0.0084 x 100 x Normality of HCl)]/wt of sample in 50ml Standard Norms: 94 to 98%. TABLE OF APPROXIMATE pH OF SOME COMMON ACIDS AND BASES AT VARIOUS CONCENTRATIONS. NORMALITY/ 2N 1N 0.1N 0.01N 0.001N MATERIAL Hydrochloric acid g/l --36.5 3.65 0.37 0.037 HCl pH 0.11 1.08 2.00 3.00 Sulphuric acid g/l 49.0 4.9 0.49 0.049 H2SO4 pH 0.24 1.17 2.05 3.00 Formic acid g/l 92.0 46.0 4.60 0.46 0.046 HCOOH pH 1.61 1.79 2.32 2.85 3.42 Lactic acid g/l 180 90 9.0 0.90 0.09 C3H6O3 pH 1.78 1.97 2.43 2.95 3.50 Acetic acid g/l 120.0 60.0 6.00 0.60 0.06 CH3COOH pH 2.18 2.40 2.87 3.37 3.89 T.S.P.P. g/l --83.0 8.30 0.83 0.083 Na4P4O7 pH 10.5 10.15 9.25 9.01 Soda Ash g/l 106.0 53.0 5.30 0.53 0.053 Na2CO3 pH 11.60 11.50 11.00 10.00 9.80 Ammonia (Hydroxide) g/l 34.0 17.0 1.70 0.17 0.017 NH4OH pH 11.72 11.59 11.16 10.64 10.15 Trisodium phosphate g/l 98.6 49.3 4.93 0.493 0.049 Na3PO4 pH 12.8 12.3 11.40 11.10 10.95

Caustic soda NaOH

g/l pH

---

40.0 13.93

4.00 12.98

0.40 12.00

0.04 11.00

Strength Test for Caustic Soda

In Textile Processing the following materials are considered to be basic chemicals or bulk chemicals used in processing. The quality of each product whether basic or auxiliary chemical would certainly affect the final quality of textile processing. So a good dye-house should have a continuous quality monitoring procedure like one shown below. As and when a new product or chemical enters your dye-house, its quality should be compared with the previous supply without fail. Caustic Soda lye: Take approximately 25 grams of caustic diluted to 500 ml. From this take 20ml and titrate with 1 N, H 2SO4 using phenolphthalein as indicator. Percentage Strength = V x 40 x 100/ 20 x 2 x wt where V is the volume of H2SO4 consumed and wt = 25/500 x 20 grams.

Conversion of Caustic soda concentrations: To convert a weight of a caustic soda solution to a weight of solid caustic soda, multiply by the %w/w content and divide by 100. Example: How much sold caustic soda should be used in place of 12 kg of 100TW caustic soda (% w/w = 47.33)? Calculation: 12 x 47.33/100 = 5.7 kg NaOH solid. To convert a volume of caustic soda solution in to weight of solid caustic soda, multiply the volume, in liters, by the g/l content of the solution. Example: How much solid caustic soda should be used in place of 12 liters of 48.1Be (-710g/l NaOH) caustic solution? Calculation: 12 x 710 = 8520g = 8.5kg of NaOH solid. Specific Gravity and concentration of Caustic Soda solutions at 20C

SG 1.000 1.050 1.100 1.150 1.160 1.170 1.180 1.190 1.200 1.210 1.220 1.230 1.240 1.250 1.260 1.270 1.280 1.290 1.300 1.310 1.320 1.330 1.340 1.360 1.370 1.380 1.390 1.400 1.410 1.420 1.430 1.440 1.450 1.460

Be 0 6.7 13.0 18.8 19.8 20.9 22.0 23.0 24.0 25.0 26.0 26.9 27.9 28.8 29.7 30.6 31.5 32.4 33.3 34.2 35.0 35.8 36.6 38.2 39.0 39.8 40.5 41.2 42.0 42.7 43.4 44.1 44.8 45.4

TW 0 10 20 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 72 74 76 78 80 82 84 86 88 90 92

%W/W 1.05 4.68 9.19 13.73 14.64 15.54 16.44 17.35 18.26 19.61 20.07 20.98 21.90 22.62 23.28 24.65 25.56 26.48 27.41 28.33 29.26 30.20 31.14 33.06 34.03 35.01 36.00 36.99 37.99 38.99 40.00 41.03 42.07 43.12

G/L 10.6 48.9 101.1 157.9 169.8 181.8 194.0 206.4 219.0 231.8 244.9 258.0 271.5 285.2 299.0 312.9 327.1 341.6 256.2 371.1 386.2 401.6 417.2 449.6 456.0 483.2 500.4 518.0 535.6 553.6 572.0 590.8 610.0 629.6

1.470 1.480 1.490 1.500 1.510 1.520 1.530

46.1 46.8 47.4 48.1 48.7 49.4 50.0

94 96 98 100 102 104 106

44.17 45.22 46.27 47.33 48.30 49.44 50.50

646.2 669.2 698.2 710.0 730.4 751.2 772.4