Environ Monit Assess (2011) 177:2333 DOI 10.

1007/s10661-010-1614-1

Physicochemical characteristics of paper industry effluentsa case study of South India Paper Mill (SIPM)
Ningombam Linthoingambi Devi Ishwar Chandra Yadav Q. I. Shihua Surendra Singh S. L. Belagali

Received: 30 November 2009 / Accepted: 9 July 2010 / Published online: 27 July 2010 Springer Science+Business Media B.V. 2010

Abstract Pulp and paper mills generate varieties of pollutants depending upon type of the pulping process being used. This paper presents the characteristics of wastewater from South India Paper Mill, Karnataka, India which is using recycled waste paper as a raw material. The raw wastewater consists of 8090 mg L1 suspended solid and 1,0101,015 mg L1 dissolved solid. However, pH varied from 5.56.8. The biochemical oxygen demand and chemical oxygen demand ranged from 200210 and 1,1201,160 mg L1 , respectively. Aerobic treatment of raw effluent attribute to significant reduction in suspended solid (range between 25 to 30 mg L1 ) and total dissolved solid (range between 360 to 390 mg L1 ). However, pH, temperature, and

electrical conductivity were found superior after treatment. Copper, cadmium, iron, lead, nickel, and zinc were found in less quantity in raw effluent and were almost completely removed after treatment. The dendrogram of the effluent quality parameters clearly indicate that South India Paper Mill does not meet Minimal National Standard set by central Pollution Control Board to discharge in agricultural field. Keywords Raw effluent Treated effluents Cellulose Central Pollution Control Board Dendrogram Cluster analysis

Introduction Paper industries in India are not as modernized as in Western Countries. In general, Indian paper mills use wide variety of cellulosic and noncellulosic-based raw materials for paper production. The pulp and paper mills in India utilizes various cellulosic-based materials for paper production accounting about 43% from forest wood, 28% from agro-based product, and 29% from recycling of waste paper (Balakrishanan 1999). Industrial pollution is global concern. Among the major industries, the paper industry is notorious polluter of the environment (Baruah et al. 1996; Murugesan et al. 2000). In India, more than 55% of industries do not have any proper treat-

N. L. Devi Q. I. Shihua School of Environmental Studies, China University of Geosciences, 388, Lumo Road, Wuhan, Hubei, 430074, Peoples Republic of China I. C. Yadav (B) S. Singh Center of Advanced Study in Botany, Banaras Hindu University, Varanasi 221005, Uttarpradesh, India e-mail: icyadav.bhu@gmail.com S. L. Belagali Department of Environmental Science, University of Mysore, Mysore 570006, Karnataka, India

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Environ Monit Assess (2011) 177:2333

ment methods and around 20% have partial treatment facilities. All of these industrial effluents are released into the environment without any prior treatment (Srivastava et al. 1994). The volume and characteristics of the pulp and paper mill effluent depends upon the type of manufacturing processes adopted. It is estimated that about 273 455 m3 of water is required per ton of paper produced. Consequently, it generates 300 m3 as waste water (Subrahmanyam 1990). The black liquor effluents is dark brown in color and are associated with high biochemical oxygen demand (BOD), chemical oxygen demand (COD), total solids, and organic carbon (Panesar et al. 1999). Black liquor effluent of pulp and paper mill is a complex colloidal solution of various inorganic components and organic polymeric substances, i.e., lignin, carbohydrates, and their complexes. The direct discharge of these effluents in aquatic systems has spoiled most of our fresh water ecosystems (Kumar et al. 2000). During the last two decades, there has been a tremendous expansion in paper industry, which ranks third in the world in terms of fresh water consumption. Pulp and paper mills requires large volume of water during various operations and in turn release huge amount of effluent in the form of black liquor loaded with many pollutants (Ingle 2000; Yedla et al. 2002). It may constitute organic and inorganic chemicals as well (Baruah et al. 1996). Fazeli et al. (1998) studied accumulation of heavy metals in the paddy crop field irrigated with paper mill effluent and found increased level of heavy metals accumulated in plant tissue. Copper seems to be main contributor among other heavy metals of acute toxicity of the craft mill effluent (Reyes et al. 2009). The present study is aimed to analyze the physicochemical characteristics of waste water effluents of South India Paper Mill (SIPM).

away from Mysore City (Fig. 1). It lies between 12 7 11 North and 76 40 58 East. Sample collection The SIPM effluent was collected from the source at the point of discharge. Sampling was done hourly over a period of 12 h with the hourly samples being combined after the 12-h period. This gave a representative sample of the daily discharge of the plant. About 2-l black liquor samples were collected in plastic cans during Jan 2007 to Feb 2007 in four different phases. Phases I, II, III, and IV was the first, 15th, 30th, and 45th day of effluent collection, respectively. The sample was collected at fortnight interval to see the temporal variation in characteristics of paper mill effluent. The collected effluent was stored at 10 C and was brought to room temperature prior to experimentation. The treated effluent of SIPM was also collected in another plastic can following standard method (Tandon 1993). Physicochemical analysis of effluent The pH and temperature of the SIPM effluents were measured using pH meter and thermo-probe at the site of collection. Color of the effluent was noted by visual observation. The collected sample was then brought to the laboratory at Department of Environmental Science, University of Mysore for the analysis of physicochemical parameters. The conductivity of the effluent was measured by using conductivity meter (Systronics conductivity meter 304 model). Atomic absorption spectrophotometer (GBC Avanta Version 1.31) was used for analysis of heavy metals. Sulfate was analyzed following turbidometric method (Digital Nephelo-Turbidity meter 132 models), while phosphate was analyzed colorimetrically using spectrophotometer (Systronics spectrophotometer 169 model).The remaining effluent characteristics parameter, i.e., suspended solid (SS), dissolved solid (DS), total dissolved solid (TDS), alkalinity, chloride, BOD, and COD were analyzed by volumetrically/titrimetrically as per standard methods (APHA 1976; Manivasakam 1996; Trivedi and Goel 1986).

Materials and methods Study area SIPM spreads over 23-acre areas is located at Chikkayana Chatra (Thandavapura) near Nanjangud Town, Karnataka, India about 20 km

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25

Bijapur Belgaum Hampi Hubli Hospet Bellari

Mangalore

Bangalore Mysore

Fig. 1 Location map of South India Paper Mill, Nanjangud (12 7 11 North, 76 40 58 East)

The data were statistically analyzed using the MS-Excel 2007 software while SPSS (16.0 version) software were used for Pearson correlation coefficient.

Results and discussion The physicochemical characteristics of the SIPM effluent showed dark brown in color and is against the standard limit (MOEF 1993). This may be due to presence of lignin compound (Panesar et al. 1999) present in raw material used for paper production. However, Livernoche et al. (1983) reported that the color of the effluent is pH sensitive and the effect of the pH on the color

of the effluent is reversible. The pH of the raw effluent was measured 6.4 compared to 6.9 in treated effluent. Low pH value may be due to the formation of organic acids resulting from the metabolism of the introduced fungus (Martin and Manzanares 1993). However, slight reduction in pH could be accounted for the metabolic production of acids by indigenous micro flora. The concentration of BOD, COD, TDS, and DS were analyzed and found higher in concentration, i.e., 203 mg L1 , 1,145, 996, and 1,012 mg L1 , respectively, while other parameters such as chloride (45 mg L1 ) and sulfate (8.5 mg L1 ) were within optimal level. The source of sulfate ions in effluent was sodium sulfite used in the pulping process. The high BOD and COD value of the SIPM effluents suggest presence of organic and

26 Table 1 Comparison of treated effluents with standards value Parameter Average values ISI standard for (mg L1 ) irrigation watera Temp. pH ECc COD BOD TDS DS SSc Alkalinity Cl PO3 4 SO2 4 Zn Pb Ni Cu Fe Cd 32.2 C 6.9 20.5 cm1 316.2 45.2 381.2 356.2 27.5 206.3 30.5 0 5.2 0.08 0 0 0 0.1 0.2 5.59.0 2.25 250 100 500 200 10 5.0 0.1 0.05 3 0.01 MINASb 5.59.0 30 100

Environ Monit Assess (2011) 177:2333

Values are arithmetic mean of four replicates a ISI (1983) Standards for irrigation and potable water IS: 10500 b MINAS (1985) c The Environment (Protection) Rules (1986)

inorganic pollutants in higher quantities (Pandey et al. 2003). Phosphate was below detection limit. Similar results were reported by Singhal and Thakur (2009). The others chemical parameter analyzed in the study were also found superior in concentration. The elevated level of some of chemical parameter of paper mill effluent may be due to utilization of various cellulosic-based raw material and chemFig. 2 Percent net reduction in BOD, COD, DS, and TDS after aerobic treatment

icals used during various manufacturing process (Baruah et al. 1996). The average mean value of various heavy metals analyzed and were recorded as Cd (0.09 mg L1 ), Cu (0.07 mg L1 ), Fe (0.3 mg L1 ), Ni (0.05 mg L1 ), Pb (0.007 mg L1 ), and Zn (0.2 mg L1 ). Iron was found comparatively higher in concentration compared to others heavy metals, which reflect toxic nature of paper mill effluents. Iron may be found in wastewater either in dissolved state or in a colloidal state, which may be peptized by organic matter, inorganic or organic complexes, or in relatively coarse suspended particles. The physicochemical characteristics of SIPM effluent after aerobic treatment were also analyzed and compared with standard values (Table 1). The pH value of 6.9 fell within the recommended discharge limit. However, BOD value was well within ISI limit but not within the permissible limit of Minimum National Standard (MINAS) set by Central Pollution Control Board, India to discharge for irrigation. There was sharp reduction in alkalinity, BOD, COD, DS, and TDS value (Fig. 2). The reduction in alkalinity and COD may be due to presence of highly nonbiodegradable cellulose, hemicelluloses, xylose, lignin, phenol compounds, and various toxic substances. However, reduction in SS was optimum.

Cluster analysis Cluster analysis (CA) is an exploratory data analysis tool which aims at sorting different objects into groups in a way that the degree of

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association between two objects is maximal if they belong to the same group and minimal otherwise. It can be used to discover structure in data without providing an explanation/interpretation. Hierarchical clustering is the most common approach in which clusters are formed sequentially, by starting with the most similar pair of objects and forming higher clusters step by step. The Euclidean distance usually gives the similarity between the two samples, and a distance can be represented by the difference between analytical values from both the samples (Otto 1998). Hierarchical agglomerative CA was performed on the normalized dataset by means of the Wards method, using Euclidean distances as a measure of similarity. This method uses the analysis of variance approach to evaluate the distances between clusters, attempting to

minimize the sum of squares of any two clusters that can be formed at each step. Cluster analysis was applied to the effluent characteristics dataset with a view to assess the cohesiveness of cluster formed between similar parameter of both untreated and treated effluent and in the resulted dendrogram. In this study, the efficiency of cluster analysis was applied to evaluate correlation between various effluent parameter of the South India Paper Mill without losing important information. Cluster analysis rendered a dendrogram (Figs. 3 and 4), where all the 18 effluent parameter were grouped into statistically significant clusters at similarity. There are other reports (Parashar et al. 2007; Simeonov et al. 2003; Wunderlin et al. 2001), where this approach has successfully been applied in water-quality program too.

Fig. 3 Hierarchical cluster analysis of dendrogram using average linkage (between groups) of untreated effluent

Similarity

PO43Pb 2+ Cu 2+ Cd 2+ Ni 2+ Zn 2+ Fe 2+ pH SO42Temperature EC Cl SS BOD

Alkalinity

11 14 16 18 15 13 17 2 12 1 3 10 8 5 9 6 7 4

TDS DS COD

28 Fig. 4 Hierarchical cluster analysis of dendrogram using average linkage (between groups) of treated fluent
Similarity

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PO43Pb 2+ Ni 2+ Cu 2+ Zn 2+ Fe 2+ Cd 2+ pH SO42Temperature Cl SS EC BOD TDS DS COD
Alkalinity

11 14 15 16 13 17 18 2 12 1 10 8 3 5 6 7 4 9

Interrelationship Descriptive statistics including the mean, standard deviation, maximum, and minimum values for SIPM effluent is presented in Tables 2. A widely used correlation criterion between two variables is the simple correlation coefficient, which indicates the sufficiency of one variable to predict the other (Davis 1986). The correlation coefficient among physicochemical parameter of treated and untreated effluent were computed and these values are presented in the form of correlation matrix. Tables 3 and 4 illustrate the correlation among various physicochemical parameters of untreated effluent and treated effluent of SIPM. Very good positive correlation found among pH, TDS, Zn,

Cu, and Cd (r = 0.991, 0.999, 0.995, and 0.992, P < 0.01) of untreated effluent of SIPM. However, they are not same with treated effluent. Further, a positive insignificant correlation exists between pH, BOD, Cl , Fe and Ni (r = 0.949, 0.577, 0.522, and 0.867). Whereas high positive correlation exists between Zn, COD, SO2 , and 4 Cd (r = 0.992, 0.993, and 0.996, P < 0.01) of the treated effluent. The temperature with BOD, Fe, Ni, and Cd of treated effluent showed a highly negative correlation (r = 0.978, 0.818, 0.801, and 0.871, P < 0.01). However, EC with DS, Fe and Pb is negatively correlated(r = 0.536, 0.842, and 0.999, P < 0.01) in untreated effluent. The above relationships are identified to be useful in the determining effluent quality for their safe disposal.

Environ Monit Assess (2011) 177:2333 Table 2 Descriptive statistics of untreated and treated effluent quality for SIPM (n = 48) Parameter Temp. pH EC COD BOD TDS DS SS Alkalinity Cl PO3 4 SO2 4 Zn Pb Ni Cu Fe All values are expressed in mg L1 except pH, Temperature, and EC Cd Condition Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Untreated Treated Min. 30 31 5.5 6.8 18 15 1120 300 200 40 985 360 1010 355 80 25 185.7 110 43 30 0 0 0 0 0.010 0.008 0.000 0.00 0.050 0.00 0.025 0.015 0.340 0.110 0.095 0.078 Max. 32 33 6.8 7.0 49 26 1160 325 210 55 1001 390 1015 358 90 30 450 350 46 31 0 0 12 8 0.280 0.110 0.001 0.00 0.060 0.006 0.099 0.035 0.360 0.112 0.100 0.79 Mean 31.0000 32.2500 6.4500 6.9500 26.5000 20.5000 1145.5000 316.2500 203.7500 45.2500 996.5000 381.2500 1012.2500 356.2500 86.0000 27.50000 302.3500 206.3250 45.1750 30.5000 0.0000 0.0000 8.5000 5.2500 0.2088 0.0800 0.0075 0.0000 0.0532 0.00275 0.07600 0.02800 0.3500 0.1113 0.09650 0.2563 Std. deviation 1.1547 0.9574 0.6351 0.1 15.0222 4.5092 17.5404 11.0868 4.7871 6.8496 7.6811 14.3614 2.6300 1.5000 4.5461 2.0817 128.6495 107.4385 1.4569 0.5774 0.0000 0.0000 5.7446 3.5940 0.1326 0.04819 0.00500 0.0000 0.00471 0.00250 0.03451 0.00890 0.00816 0.000957 0.00238 0.3558

29 St. error mean 0.5774 0.4787 0.3175 0.05 7.5111 2.2546 8.7702 5.5434 2.3936 3.4248 3.8406 7.1807 1.3150 0.7500 2.2730 1.0408 64.3248 53.7192 7284 0.2887 0.0000 0.0000 2.8723 1.7970 0.06628 0.02410 0.00025 0.0000 0.00235 0.00125 0.01725 0.00445 0.00408 0.00047 0.00119 0.17790

Effluent treatment process The SIPM have adopted aerobic treatment process to treat the wastewater releasing from paper machine before discharge to the agricultural land. It is based on screening with microfilter, aeration by mechanical aerator followed by primary and secondary clarification. The layout of the effluent treatment process adopted at SIPM is shown in Fig. 5. Paper machine waste water is passed through microfilter and penvalt vibro screen. The pulp collected here is reused in the Mill. The effluent emanating from machine

mixed with waste water of stock preparation and is passed through clarifier. The clarified water is passed through aeration tank and then on to a secondary clarifier. The final clarified water is pumped to storage tank on hillock for final discharge to nearby lands for irrigation. The SIPM effluents directly discharged to agricultural field nearby the mill after treatment can alter the yield potential of paddy crops due to increased uptake of toxic heavy metals into their tissues (Fazeli et al. 1998). Further, this may affect all aspects of the environment, i.e., water, air, and land. Pollution control measures adopted in

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Table 3 Correlation matrix (Pearson) of untreated effluent COD BOD TDS DS SS Alkalinity Cl PO3 4 Zn Pb SO2 4 Ni Cu Fe Cd

Temp.

pH

EC

Temp. pH EC COD BOD TDS DS SS Alkalinity Cl PO3 4 SO2 4 Zn Pb Ni Cu Fe Cd 1 0.204 0.165 0.000 0.056 0.914 0.302 0.091 0.148 0.522 0.461 0.131 0.426 0.073 1 0.520 1 0.897 0.195 1 0.630 0.229 0.902 1 0.210 0.398 0.362 0.300 0.526 0.988a 0.254 0.148 0.990a 0.474 0.945 0.711 0.996b 0.589 0.877 0.586 0.391 0.570 0.587 0.765 0.961a 0.464 0.793 0.518 0.973a 0.702 0.799 0.462 0.850 0.000 0.898 0.832 0.966 0.719 0.801 0.463 1 0.535 0.137 0.266 0.378 0.062 0.277 0.084 0.332 1 0.503 0.599 0.577 0.428 0.703 0.000 0.728 1 0.986a 0.406 0.916 0.952a 0.147 0.951a

1 0.545 0.576 0.362 0.905 0.601 0.110 0.381 0.211 0.654 0.000 0.503 0.555 0.577 0.796 0.535 0.707 0.485

1 0.307 1 0.973a 0.297 1 0.137 0.498 0.069 0.991b 0.433 0.962a 0.629 0.536 0.582 0.854 0.630 0.911 0.548 0.795 0.652 0.276 0.336 0.468 0.636 0.538 0.625 0.978a 0.452 0.983a 0.999b 0.353 0.974a 0.262 0.999b 0.247 0.940 0.492 0.852 0.995b 0.219 0.957a 0.771 0.842 0.745 0.992b 0.186 0.966

1 0.308 1 0.946 0.459 1 0.989a 0.174 0.928 1 0.199 0.184 0.135 0.290 1 0.985a 0.140 0.905 0.998b 0.686 1

a Correlation

Environ Monit Assess (2011) 177:2333

b Correlation

is significant at the 0.05 level (2-tailed) is significant at the 0.01 level (2-tailed)

Table 4 Correlation matrix (Pearson) of treated effluent COD BOD TDS DS SS Alkalinity Cl PO3 4 Zn Pb SO2 4 Ni Cu Fe Cd

Environ Monit Assess (2011) 177:2333

Temp.

pH

EC

Temp. pH EC COD BOD TDS DS SS Alkalinity Cl PO3 4 SO2 4 Zn Pb Ni Cu Fe Cd 1 0.861 0.929 0.576 0.758 0.565 0.651 0.441 0.993b 0.992b 0.286 0.827 0.945 0.353 0.977a 1 0.987a 1 0.527 0.522 1 0.760 0.808 0.050 0.547 0.604 0.332 0.379 0.503 0.192 0.073 0.078 0.286 0.856 0.928 0.479 0.919 0.968a 0.581 0.428 0.436 0.538 0.881 0.870 0.867 0.945 0.964a 0.724 0.699 0.636 0.174 0.949 0.987a 0.555 1 0.957a 1 0.832 0.872 0.082 0.058 0.824 0.655 0.777 0.574 0.841 0.930 0.416 0.136 0.647 0.401 0.753 0.717 0.801 0.598

1 0.870 0.347 0.746 0.978a 0.939 0.406 0.753 0.564 0.302 0.269 0.751 0.824 0.520 0.801 0.860 0.818 0.871

1 0.074 1 0.977a 0.250 0.949 0.156 0.986a 0.064 0.556 0.616 0.801 0.355 0.598 0.463 0.577 0.000 0.240 0.830 0.974a 0.175 0.996b 0.156 0.378 0.753 0.867 0.251 0.973a 0.174 0.522 0.811 1.000b 0.073

1 0.535 1 0.723 0.425 1 0.599 0.325 0.985a 1 0.654 0.286 0.387 0.328 1 0.115 0.733 0.770 0.863 0.200 1 0.389 0.208 0.916 0.971a 0.185 0.958a 1 0.302 0.591 0.412 0.448 0.842 0.313 0.430 1 0.577 0.239 0.974a 0.996b 0.378 0.867 0.973a 0.523 1

a Correlation

b Correlation

is significant at the 0.05 level (2-tailed) is significant at the 0.01 level (2-tailed)

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32 Penvalt Vibro Screen

Environ Monit Assess (2011) 177:2333 Aeration Tank Secondary Clarifier

Wastewater

Micro filter

Clarifier

Underflow
Pulp collected here is reused Supply for land irrigation

Storage Tank

Fig. 5 Flow diagram of effluent treatment plant at SIPM

SIPM are not satisfactory to the level. Therefore, it is wise to setup anaerobic treatment process in SIPM for further degradation of cellulose fibers and other constituents prior to final discharge to the agricultural land. A combination of physical, chemical, and biological treatment processes with optimization can provide a long-term solution. A combination of an anaerobic treatment followed by aerobic treatment can offer better option for SIPM to meet MINAS for irrigation. It is imperative to minimize the wastewater generation rather than implanting control measure. This can be accomplished by optimizing the use of raw materials, by-product recovery, maximizing the reuse of water, process modification, attitude of the management in reducing the pollution, proper operation and maintenance, local regulation regarding the water use and effluent quality, and good housekeeping.

References
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Conclusions The physicochemical characteristic of SIPM effluents revealed that it does not meet MINAS to discharge in agricultural fields set by CPCB. The pollution control measures adopted at SIPM are not satisfactory to the level of CPCB. Statistical analysis, showed lead, nickel, copper, zinc, iron, cadmium, pH, sulfates, temperature, chlorides, and suspended solids were highly intercorrelated while other parameters were seldom correlated.
Acknowledgement Authors are grateful to Mr. M Anand, Assistant Manager, and others staffs of South India Paper Mill for providing necessary and relevant information.

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