ANNALS OF THE UNIVERSITY OF ORADEA

FASCICLE OF TEXTILES, LEATHERWORK

PHYSICO-CHEMICAL PARAMETERS OF RESIDUAL WATER

FROM DIFFERENT SCOURING TREATMENTS OF HEMP/COTTON
FABRIC

DOCHIA Mihaela1, GAVRILAȘ Simona2

1
”Aurel Vlaicu” University of Arad, Research Development Innovation in Technical and Natural Science
Institute, Postal address, 310330, 2-4 Elena Dragoi Street, Arad, Romania, E-Mail: [email protected]

2
”Aurel Vlaicu” University of Arad, Faculty of Food Engineering, Tourism and Environmental Protection, Department of
Technical and Natural Sciences, Postal address, 310330, 2-4 Elena Dragoi Street, Arad, Romania, E-Mail:
[email protected]

Corresponding author: Gavrilaș, Simona, E-mail: [email protected]

Abstract: Impact of economic development - ecological balance rises numerous and complex problems for the
textile industry. It is known that all textile processes need important quantities of water and chemicals. This
situation generates large amounts of wastewater which cannot be further use without additional treatments
because of the environmental problems. The issue of environmental protection has become an essential part of
the textile industry development strategy. Many studies in the field present alternatives for the conventional
scouring to reduse water pollution. The applied ecological strategy is focused on process optimization and
pollution prevention.
The paper presents a comparison of the physico-chemical parameters of the wastewater resulted from the
various scouring treatments applied on a cotton/hemp fabric. Three types of scouring treatments have been
carried out: two with enzymes for which a commercial enzyme product, a washing agent and EDTA or sodium
citrate as complexing agents were used, and one classical scouring treatment with sodium hydroxide. The
main physico-chemical parameters of the residual water analyzed were: pH, salinity, turbidity, TDS (total
dissolved solids), conductivity, chemical oxygen demand (CCOMn), total dissolved oxygen and dry residue.
From the two enzymatic treatments, the values of physico-chemical parameters of the residual water were in
accordance with the legislation in case were the sodium citrate was used. For the alkaline treatment, the data
were even with 100 % higher compared to enzymatic treatments. For some parameters, higher values were
registered also for the enzymatic scouring where EDTA was used as a complexing agent.

Key words: wastewater, physico-chemical analysis, pretreatment, ultrasound, commercial enzyme product.

1. INTRODUCTION

Cotton fibres are characterised by a trilamellar structure. It is considered that the second
layer has in its composition de-esterified pectins. Those may be a result or contribute to the fibre
cells elongation [1]. Both cotton and hemp fibres are characterised by a certain amount of native
pectin. For further utilisation in the textile industry it is mandatory to remove all noncellulosic
components, along with other impurities: lignin, waxes, natural pigments, or organic acids.
Independent of the classical method chosen (acid, alkaline or peroxide scouring) the main objectives
of the treatment are to be non harmful for cellulose fibre and remain with less impurities residues. In
1
case of the hemp fibres it was shown that a scouring treatment which includes sodium hydroxide and
sodium sulphite is recommended for the removing of both lignin and pectin and also to reduce the
treatment time [2].
Using a conventional pretreatment on cotton/hemp fabric with high temperatures (80-90 0C)
and aggressive alkaline (pH ≥ 10) will have a major negative impact on the ecosystems. In this
situation the wastewaters resulted have to be subject to additional purge steps to accomplish the
environmental requirements [3].
Impact of economic development - ecological balance rises numerous and complex
problems for the textile industry. Textile ecological technologies occupy an important place in the
research projects developed at national and international levels. The issue of environmental
protection has become an essential part of the textile industry development strategy. Many studies in
the field present alternatives for the conventional scouring. The applied ecological strategy is
focused on process optimization and pollution prevention. The suggested treatments imply the
utilization of enzymatic products which are not harmful, are suitable for the process, economically
advantageous by decreasing the quantity of energy, water and chemicals used, and eco friendly [4].
Other advantages of using an enzymatic treatment are the lower fibres damage degree and the
utilisation of biodegradable chemicals. Replacement of the classical scouring treatment with the
enzymatic one reduces the pollution factors and also streamlines the technological process from an
economic point of view. Another aspect which should be taken into account is the lower quantity of
effluents resulted after bioscourig treatment [5,6].
It is known that all textile process needs important quantities of water and chemicals. This
situation generates large quantities of wastewater which cannot be further use without additional
treatments due to the fact that they will probably cause environmental problems. The specific
regulations demand a serious of precise determinations for: COD, pH, turbidity, salinity, TDS, and
others. Good results have been reported in case of using different physical methods for wastewater
treatment. In case of the ultrafiltration-electrodialysis system the values of the determined
parameters were lower than the detection limit. This suggests that the treated water could be
reintegrated in the technological process [7].
Independently of the method used for the wastewater treatment (coagulation-flocculation,
oxidation, photocatalytic, chlorination, adsorption, electrocoagulation-ozone) all present different
inconvenient and requires additional costs. This suggests a different approach of the problem. A
development of modern techniques and technologies for reducing the amount of pollutants in the
resulting effluents are needed. A possibility is the development of an ecological process for the
pretreatment of the fabrics by using enzymes and biodegradable reagents. The main advantages of
using enzymes are associated with less severe reaction conditions, lower processing temperatures,
reduced treatment time, non-toxic and biodegradable products. Also, the water consumption is lower
compared with the classical treatment and the wastewater parameters are in the limits specified by
the legislation. For example, in case of a bioscouring cotton knits the pH and CCOMn values
registered for the waters resulted from the process could be with approximately 50 % lower
compared with the alkaline treatment, and the TDS is 10 % of the one registered for the classical
treatment [8]. The lack of supplementary treatment applied to the waters resulted from the
technology imply the process costs reduction. It is believed that up to one fifth of the water pollution
could be determined by different specific textile processes [9].
The bioscouring treatment applied in our case tends to reduce the aggressive conditions
compared to the conventional one. The working temperature had lower value (55 0C) and the pH was
close to 7. As presented in the literature, also in our study the pectinolytic treatment used show
similar efficiency as the classical one regarding the specific parameters of the fabrics (wettability,
tensile strength, elongation at break, etc.).
 2. EXPERIMANTAL PART

2.1 Materials and experimental procedure

The wastewater analysed was resulted after the bioscouring and alkaline treatment on
cotton/hemp materials with the following characteristics: width (120 ± 3 cm), weight (220 ± 10
g/m2), warp density (10 yarns/cm), weft density B (10 yarns/cm), 100 % of cotton yarn, Nm 14 for
warp direction and 100 % of hemp yarn, Nm 14 for weft direction.
The specific reagents have analytical purity and were purchase from: CHT Bezema
Company (Beisol PRO-pectinolytic product, Denimcol Wash RGN- surfactant), Sigma-Aldrich
(sodium hydroxide, sodium citrate, sodium carbonate, sodium silicate, sodium bisulfite), and Rotta
Company (Sulfolen 148: S-148 alkyl polyglicol ether).
During the bioscouring treatment of the cotton/hemp material were used two different
complexing agents EDTA or sodium citrate and the same enzymatic product (Beisol PRO-mixture
of pectinase) in similar concentration and treatment time after an experimental program (see Table 1
and Table 2). The considered liquid to fabric ratio was 20:1, and the temperature 55 0C. The basic
pH in case of the classical method was ensured with sodium hydroxide.
The pectinolytic product concentration used varied between 1-3 % o.w.f (over weight fiber)
and the action time was between 15 and 55 minutes. The quantity of complexing agents (EDTA or
sodium citrate) was 2 g/L and the surfactant (Denimcol Wash RGN) 0.5 %.
For the bioscouring treatments were used also ultrasound of 45 kHz in an Elmasonic X-tra
basic 2500 ultrasonic bath from Elma Company, Germany. The classical scouring treatment used for
comparison was done with 10 g/L sodium hydroxide, 1 g/L sodium bisulfite, 5 g/L sodium
carbonate, 2 g/L sodium silicate and 2 g/L wetting agent (Sulfolen 148) for 1 hour at 100 0C in an
AATCC Launder Ömeter.

2.2 Wastewater analysis

The wastewater quality indicators determined such as: pH, salinity, turbidity, TDS (total
dissolved solids), conductivity, chemical oxygen demand (CCOMn), total dissolved oxygen and dry
residue were chosen according to the EU specific regulations. A WTW multi-parameter inoLab
Multi 740 was used for conductivity, pH, salinity, TDS, and total dissolved oxygen measurements.
For turbidity determination was used a HI 88713 HANNA Instruments Turbidimeter. The dry
residue was determined gravimetrically as difference in mass before and after the drying process.
For evaporation was used a Pura 14 water bath from Julabo, Germany and dried at (105 ± 5) °C to
constant mass in an oven, according to [10]. The CCOMn (chemical oxygen demand) was
performed by titration with KMnO4 as described by R. Ballance [11].

3. RESULTS AND DISCUSSIONS

The purpose of this research was to study the impact of the wastewater resulted from two
eco-friendly scouring treatments compared to the classical alkaline scouring. Further on will be
presented the comparative results obtain for the investigated parameters in case of using EDTA or
sodium citrate as complexing agents in the bioscouring treatment, and for the traditional scouring
with sodium hydroxide. Table 1 shows a comparative analysis of some quality indicators (pH, TDS,
salinity, conductivity, total dissolved oxygen) of the residual water resulted from classical and
enzymatic pretreatments of the cotton/hemp fabric.
Table 1: Comparative analysis of some residual water quality indicators resulted from classical and
enzymatic treatments of the cotton/hemp fabric
Scouring with enzymes + sodium citrate
Treatment Total dissolved
Enzyme TDS Conductivity
Sample time pH Salinity oxygen
[%] [mg/L] [(μs/cm]
[min. [mg/L]
]
1 1.30 21.00 8.02 1778.00 0.90 1780.00 5.27
2 2.70 21.00 7.81 1932.00 1.00 1936.00 5.43
3 1.30 49.00 8.18 1768.00 0.90 1776.00 5.04
4 2.70 49.00 8.05 1912.00 0.90 1917.00 4.92
5 1.00 35.00 8.53 1778.00 0.90 1785.00 4.82
6 3.00 35.00 7.82 2027.00 1.00 2030.00 4.23
7 2.00 15.00 7.65 1914.00 0.90 1918.00 6.86
8 2.00 55.00 8.30 1856.00 0.90 1863.00 5.27
9 2.00 35.00 8.05 1883.00 0.90 1888.00 5.26
10 2.00 35.00 8.15 1885.00 0.90 1893.00 5.15
11 2.00 35.00 7.93 1916.00 0.90 1923.00 4.91
12 2.00 35.00 7.99 1887.00 0.90 1891.00 4.93
13 2.00 35.00 8.10 1881.00 0.90 1886.00 4.76
Scouring with enzymes + EDTA
1 1.30 21.00 4.849 1072.00 0.50 1071.00 5.34
2 2.70 21.00 4.864 1183.00 0.50 1182.00 5.53
3 1.30 49.00 4.933 1039.00 0.50 1038.00 5.15
4 2.70 49.00 5.082 1199.00 0.50 1197.00 5.65
5 1.00 35.00 4.849 998.00 0.40 997.00 5.71
6 3.00 35.00 4.931 1209.00 0.60 1209.00 5.77
7 2.00 15.00 4.887 1105.00 0.50 1105.00 5.79
8 2.00 55.00 4.920 1107.00 0.50 1104.00 5.64
9 2.00 35.00 4.836 1112.00 0.50 1111.00 6.17
10 2.00 35.00 4.868 1107.00 0.50 1104.00 5.93
11 2.00 35.00 4.927 1101.00 0.50 1101.00 6.26
12 2.00 35.00 5.010 1109.00 0.50 1108.00 6.13
13 2.00 35.00 5.018 1109.00 0.50 1109.00 6.29
Classical alkaline scouring
1 - 60.00 13.50 53000.00 35.00 53000.00 4.16

In the textile processing units, pH is a very important factor and must be adjusted for each
processing step for better results. The pH of the wastewater resulted from the three types of scouring
treatments was found in a big range from ~ 4.50 to 13.50. In the case of pretreatment with sodium
citrate, the pH of the wastewater is almost neutral, being in accordance with the legislation. Not the
same situation is in the case of EDTA where the pH values are below 5, requiring a slight correction.
As for salinity, this shows higher values for sodium citrate treatments. The highest value of pH
shows the residual water resulting from the alkaline treatment (13.50), this being far beyond the
limits allowed.
Electrical conductivity and TDS of wastewater from all enzymatic treatments were found to
be in the range of ~ 1000 to 2000. Lower conductivity and TDS values were obtained in this case for
the enzymatic treatments in which EDTA was used as a complexing agent. The same situation is for
salinity values. Close values have been obtained for total dissolved oxygen in both cases of
enzymatic treatments. In the case of classical alkaline treatment, with the exception of total
dissolved oxygen, the other values obtained for conductivity, TDS and salinity exceed the
admissible values.
In Table 2 is presented a comparative analysis of turbidity, dry residue and chemical oxygen demand
values of the residual water resulted from the classical and enzymatic treatments of the cotton/hemp fabric.

Table 2: Comparative analysis of turbidity, dry residue and chemical oxygen demand of the residual
water resulted from classical and enzymatic treatments
Scouring with enzymes + sodium citrate
Enzyme Treatment time Turbidity Dry residue CCOMn
Sample [mg O2/L]
[%] [min.] [NTU] [mg/L]
1 1.30 21.00 2.85 19.26 19.64
2 2.70 21.00 2.98 26.36 21.71
3 1.30 49.00 2.49 29.28 29.07
4 2.70 49.00 2.61 28.00 32.34
5 1.00 35.00 2.63 25.64 22.86
6 3.00 35.00 2.71 36.70 27.81
7 2.00 15.00 3.31 15.16 18.96
8 2.00 55.00 1.92 57.60 25.28
9 2.00 35.00 2.48 34.96 27.81
10 2.00 35.00 2.60 36.88 22.64
11 2.00 35.00 2.90 35.96 25.28
12 2.00 35.00 3.09 38.40 25.28
13 2.00 35.00 2.74 40.86 28.96
Scouring with enzymes + EDTA
1 1.30 21.00 1.64 34.34 644.64
2 2.70 21.00 1.59 46.56 620.80
3 1.30 49.00 1.49 32.00 379.20
4 2.70 49.00 1.56 60.06 606.72
5 1.00 35.00 1.61 31.06 379.20
6 3.00 35.00 1.41 37.20 442.40
7 2.00 15.00 1.83 20.44 265.44
8 2.00 55.00 1.20 64.82 689.60
9 2.00 35.00 1.36 34.44 151.68
10 2.00 35.00 1.51 35.26 145.36
11 2.00 35.00 1.46 37.98 170.64
12 2.00 35.00 1.84 33.32 139.04
13 2.00 35.00 1.60 36.00 169.60
Classical alkaline scouring
1 - 60.00 84.00 1150 1180.00

Turbidity values are higher for sodium citrate treatments. Instead, similar values were
obtained in the case of dry residue and much lower values for CCOMn compared to the treatments
in which EDTA was used. In the case of classical alkaline treatment, the same high values are
observed for all parameters (turbidity, dry residue, CCOMn) resulting high polluted wastewaters.

4. CONCLUSIONS

The main physico-chemical parameters of the residual water resulted from two types of
enzymatic scouring treatments were analyzed in comparison with wastewater parameters of an
classic alkaline treatment. Based on the experimental data obtained it was concluded that for
enzymatic pretreatments (EDTA or sodium citrate) all the parameters are in the limits with the
exception of the pH for treatments were EDTA was used. We can not say the same thing in the case
of classic alkaline treatment were higher values were obtained for all parameters. A constant
monitoring of water quality is necessary to avoid further dreadful conditions. The effluents which
are toxic in nature are needed imperative treatment before disposal on water bodies to create less
pollution and an eco-friendly environment.

ACKNOWLEDGEMENTS

This work was supported by a grant of the Romanian National Authority for Scientific
Research and Innovation, CNCS-UEFISCDI, project number PN-II-RU-TE-2014-4-1370,
and
„Centru de Cercetare în Științe Tehnice și Naturale-CESTN” co-funded by European Union
through European Regional Development Fund Structural Operational Program “Increasing of
Economic Competitiveness” Priority axis 2. Operation 2.2.1. POSCCE Nr. 621/2014 POS-CCE.

REFERENCES

[1] K. C. Vaughn, R. B. Turley, “The primary walls of cotton fibers contains an

ensheathing pectin layer”, Protoplasma, vol. 209, pp. 226-237, 1999.
[2] H. M. Wang, R. Postle, R. W. Kessler, W. Kessler, “Removing Pectin and Lignin
During Chemical Processing of Hemp for Textile Applications”, Textile Res. J., vol. 73, pp. 664-
669, 2003.
[3] C. R. Holkar, A. J. Jadhav, D. V. Pinjari, N. M. Mahamuni, A. B. Pandi, “A critical
review on textile wastewater treatments: Possible approaches”, J. Environ. Manage., vol. 182, pp.
351-366, 2016.
[4] G. Garg, A. Singh, A. Kaur, R. Singh, J. Kaur, R. Mahajan, “Microbial pectinases: an
ecofriendly tool of nature for industries”, Biotech., vol. 6:47, 2016, DOI 10.1007/s13205-016-0371-
4.
[5] K. Mojsov, “Bioscouring and bleaching process of cotton fabrics-an opportunity of
saving water and energy”, J. Text. I., vol. 107, pp. 905-911, 2016.
[6] F. El-Gohary, N. A. Ibrahim, F. Nasr, M. H. Abo-Shosha, H. Ali, “A new approach to
accomplish wastewater regulation in textile sector: an egyptian case study”, Cellulose Chem.
Technol., vol. 47 (3-4), pp. 309-315, 2013.
[7] R. Lafi, L. Gzara, R. H. Lajimi, A. Hafiane, “Treatment of textile wastewater by a
hybrid ultrafiltration/electrodialysis process”, Chem. Eng. Process., vol. 132, pp. 105-113, 2018.
[8] E. K. Choe, C. W. Nam, S. R. Kook, C. Chung, A. Cavaco-Paulo, “Implementation of
Batchwise Bioscouring of Cotton Knits”, Biocatal. Biotransfor., vol. 22 (5/6), pp. 375-382, 2004.
[9] S. M. A. Hoque, A. Y. M. A. Azim, “Using Enzymes as an Aid of Better and Eco-
Friendly Scouring Processing”, AJER., vol. 6 (5) pp. 167-182, 2016.
[10] DS 204:1980 (in compliance with SFS 3008, NS 4764, and SS 028113);
”Determination of total residue and total fixed residue in water, sludge and sediment”.
[11] R. Ballance, ”Physical and chemical analyses, Water Quality Monitoring”, in J.
Bartram, R. Ballance (Eds), A Practical Guide to the Design and Implementation of Freshwater
Quality Studies and Monitoring Programmes, UNEP/WHO ISBN 0 419 22320 7 (Hbk) 0 419 21730
4 (Pbk), 199.
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