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The direct use of sewage as fertilizers in agriculture without proper treatment has led to substantial economic environmental and healthy ramifications. Proper treatment as well as adequate environmental management of sewage sludge is a necessity in order to eliminate the negative sequences of its utilization in the agriculture field. In this chapter, a novel organic Schiff base chelator derived from hydroxybenzylidene succinohydrazide (HBSH) has been successfully synthesized and characterized by elemental analysis, 1H-NMR as well as infrared spectroscopy. The effect of sewage treated with varying concentration of the Schiff base chelator (0.8, 1.6 and 2.4 g/L) as well as the untreated sewage on the sludge solid reduction, removal of heavy metals and salmonella pathogens has been investigated. The implementation of raw as well as treated sludge on the growth as well as the heavy metal content of radish plant has been also investigated. It was observed that the treated sample showed a reduction in the total content of Zn, Ni, Cr and Cu and enhancements in the yield, stem length, leaf number and flourishing.
Chemical Engineering Department, Borg El Arab Higher Institute Engineering and Technology, Alexandria, Egypt
Abdou Saad El-Tabl
Chemistry Department, Faculty of Science, Menoufia University, Shebin ElKom, Egypt
*Address all correspondence to: ch_sara2011@yahoo.com
1. Introduction
Sewage sludge is a non-homogeneous material constituting of a combination of various compounds including organic and inorganic materials as well as microorganisms, and moisture [1, 2]. It is counted up as the major by-product resulted from treatment of wastewater. The sludge undesirable content of heavy metals, synthetic organic compounds and pathogenic bacterial and other microorganisms represents a major harmful environmental risk. Therefore, disposal process of this by-product surely lead to unwelcomed environmental impacts including human beings health threats and the possibility of atmospheric polluting, as well as water and soil resources contaminating [1, 3]. The remarkable high phosphorus, nitrogen and potassium nutrients content imparts sewage sludge a property of being used as agricultural fertilizer however a series harmful substances content oppose this beneficial application [4, 5, 6]. Hence the main aim of sewage sludge treatment is to eliminate sludge unfavorable contents while to retain sludge nutrients. The primary two steps in the treatment processes of sewage sludge are thickening and dewatering. The first one is aiming to thickened sludge to lower solid percent, while the other one reduces the water content by (centrifugation, filtration, and/or evaporation) in order to reduce transportation costs of disposal, or to improve suitability for advanced processing [7, 8]. On the other hand, digestion (anaerobic and aerobic), incineration, and composting aim to diminish the organic matter content and the amount of harmful microorganisms existing in the residue matter [9, 10, 11, 12, 13, 14, 15].
The high heavy metal content in the sewage sludge represents another major obstacle against sludge utilization. The non-biodegradability nature, unlike organic contaminants, leads to accumulation of heavy metals in the biota, which involves a health risk and an environmental worry. Although metabolism of living organism needs metal ions in order to carry out many metabolic pathways, higher concentrations can cause expected acute as well as chronic toxicity. Therefore, rigorous parameters have been approved for release of various metal ions in wastewaters to evade health risk and environmental contamination. Various chemical, physical, and biological treatment methods such as chemical precipitation, adsorption, membrane filtration, ion-exchange, electrochemical treatment and microorganisms have been established for removing metal ions from water and wastewaters [16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29]. Among these wide scope of heavy metal treatment methods, utilizing of chelating agents has demonstrated a pronounced impact in eliminating of harmful metals [30, 31]. Challenges of metal ions removal can be represented in that metal ions are adsorbed on soil, so it shows resistance to be removed upon washing by surface and ground water moreover the actual low water solubility of some transition metals hydroxides. The remarkable metal binding capabilities enables chelating agents to overcome these challenges [32, 33, 34, 35, 36]. The most commonly ligand, Ethylenediamine-tetraacetic acid (EDTA), a hexadentate ligand, has the ability to bind most of heavy metals forming very stable complexes [37, 38, 39, 40, 41]. However the problem of non-biodegradability is the main drawback of EDTA utilization, as the degradation of EDTA results in formation of a stable organic pollutant (3- ketopiperazine-N,N-diacetate) [42]. The bio-degradable isomer S,S-ethylenediamine disuccinic acid (S,S-EDDS) has been proposed as a likely alternative chelating agent [43, 44], however its ability to metal ions is inferior and special pH conditions should be taken into consideration as the influential pH range is narrower [45].
In this study a novel organic Schiff base chelator derived from hydroxybenzylidene succinohydrazide (HBSH) has been successfully synthesized and characterized by elemental analysis, 1H-NMR as well as infrared spectroscopy. The ability of this novel Schiff base to decontaminate semi-solid sewage has been investigated. The utilization of the treated sludge has been also tested as a plant fertilizers. The influence of raw as well as treated sludge on the growth and heavy metal content in radish plant have been also investigated.
The C, H and N content in the obtained compounds was analyzed at the Microanalytical Laboratory, Cairo University, Egypt. Metal ion content was determined using Standard analytical methods [46, 47, 48]. Jasco FT/IR 300E Fourier transform infrared spectrophotometer covering the range 400–4000 cm−1 was used to record FT-IR spectra of the ligand and its metal complexes using KBr discs. 1HNMR spectrum was obtained on a JEOL EX-270 MHz FT-NMR spectrometer in d6-DMSO as solvent. Where the chemical shifts were determined relative to the solvent peaks. All metal concentrations were detected using Perkin Elmer ICP (ICP-MS-1).
2.2 Preparation of the Schiff base (HBSH)
The Schiff base, (HBSH) was prepared by refluxing (4 gm, 0.022 mole) of 2,3 dihydroxy succcinohydrazide in ethanol with (4.8 ml) of salicylaldehyde (1: 2 molar ratio), for 5 hours at 80°C (Figures 1 and 2). The formed yellow precipitate was left to cool to room temperature, then filtered off and dried under vacuum over anhydrous CaCl2. [C18H26N4O10]Yield: 75%, Color: yellow. Elemental Anal. Calc.: C, 47.16; H, 5.72; N, 12.22. Found: C, 46.98; H, 5.39; N, 12.10. IR, (KBr, cm-1): 3650,3665,3620,3180 υ(OH/H2O), 3320-2730 υ(H-bonding) 1705, 1690 υ(C=O), 1318,1272υ(COH), 1630,1622 υ(C=N).
Figure 1.
Preparation of the Schiff base 2,3-dihydroxy-N,N4-bis(2-hydroxybenzylidene) succinohydrazide (HBSH).
Figure 2.
Variation in TSS concentrations along raw and treated sewage at 0.8gL−1.
2.3 Settled sludge volume (SV30)
The sludge used in this study was collected from the sewage outcome of the aeration tank of Al kharry waste-water plant, El-Behira Governorate, Egypt. Settled Sludge Volume was estimated using reported standard method [49, 50]. In briefly, 1 L of the sludge sample (raw or treated) was places in settling column and the solid content was uniformly distributed by inverting the covered cylinder for three times, then stirred using stirring rod. The suspension is kept under stirring throughout the experiment. The volume occupied by the suspension was determined for 30 minutes at 2 minutes intervals. The same procedures were carried out in presences of different concentration of the succinohydrazide Schiff base (0.8, 1.6, 2.4) g/L.
2.4 Sludge and radish digestion
Digestion of raw sludge, treated sludge as well as radish plant was carried out by well suspension of 1gm of the dry sample in 100 ml of distilled water. Three milliliter of conc. HNO3, and the mixture was evaporated cautiously to 4 ml, then 5 ml of conc. HNO3 (15.8 M) was added and refluxed for 1 hour. The mixture was cooled then solution of (15 ml of HCl (11.65 M) + 15 ml H2O) was added heated again for 15 minutes then cooled. Finally 100 ml of distilled water was added, the mixture was filtered and the heavy metal was estimated on ICP (ICP-MS-1) - Germany [50].
2.5 Salmonella detection
One gram of the sample was diluted in 9 ml 1% NaCl to a dilution up to 5-10 times. One ml from each dilution was transferred into another five tubes containing buffered peptone water (9 ml). The inoculated tubes were incubated at 37° C for 24 h, then 0.1 ml from each tube showing bacterial growth (turbidity) was transferred into 10 ml of Rappaport-Vassiliadis (RV) broth. The inoculated tubes were incubated at 43.5 ± 1°C for 24 h, then three loops from each tube were taken, the first was streaked out onto bismuth sulfite agar according to [51]. The plates incubated up to about 48 h at 37 ± 0.5°C. Growth of Salmonella on bismuth sulfite agar plates showed are black center, light edges surrounded by a black precipitate with metallic sheen (so-called rabbits or fish- eye). A typical colony was collected and streaked on slants of tryptic soya agar (TSA) (contains 10% glycerol) and stored at 4°C not more than 1 year. Confirmation of Salmonella was carried out using the API E20 Enterobacteriaceae test system and RISA molecular profiling [52].
Table 1 displays the general information regarding heavy metals (HMs), parasite and solid volume contents of the sludge sample accompanied by the Egyptian Code and Environmental Protection Agency allowed standard limits. The content values of lead and cadmium are two- folds the allowed Egyptian code standard limit, in the time that nickel and zinc recorded 801.25, 8275 mg/kg respectively which are about four times more than the allowed Egyptian code standard limit. Iron and chromium are greatly pronounced with 468,750 and 1637.5 mg/kg respectively. The values of the main metal species present in the sludge under experiment are all beyond the Environmental Protection Agency limit values. Sludge volume after 30 min (SV30) recorded 650 cm3/L an average value. The parasitic content evaluation showed a higher presence of salmonella (2.6 × 104 unit/mg). Disposal of such untreated sludge on nearby unused lands would inevitability lead to serious parasitic and heavy metal contaminations accompanied with a dangerous chain of negative effects on human and environment [52].
Physicochemical characteristics of the sewage sludge.
EG referred to (Egyptian Code).
EPA referred to (Environmental Protection Agency).
Sludge volume after 30 min.
3.2 1H-NMR spectrum
The 1H- NMR spectrum of the ligand in deuterated DMSO showed the absence of protons of the amine and aldehyde groups belonging to the 2,3 dihydroxy succcinohydrazide and Salicylaldehyde starting material and the appearance of new peaks at 4.29 ppm corresponding to protons of the two azomethine groups (CH=N-). The chemical shift appeared in the 6.2–7.1 ppm range were assigned to the aromatic protons of the benzene moiety which appearing as multiplets, whereas the chemical shifts observed at 5.35 ppm was assigned to the protons of aromatic C-OH groups. The two protons of -NH recorded a chemical shift at 8.9 ppm, whereas the chemical shift observed at 2.8 ppm corresponded to two protons of the alcoholic OH groups (OHC-COH) [53].
3.3 Infrared spectrum
The infrared spectrum of the ligand showed broad bands at 3650, 3665, 3620 and 3180 cm−1 are assigned to the υ (OH)/H2O groups. The two bands located at 1705 and 1690 cm−1 are assigned to the two (C=O) groups, whereas the other two bands observed at 1630 and 1622 cm−1 are attributed to υ(C=N). Presence of the two (C-OH) groups was further supported by the two vibrational bands observed at 1318, 1272, whereas the presence (N-N) group was supported by the vibrational band observed at 1115 cm−1. The IR spectrum showed a band at 1569 cm−1 which is related to υ (C=C)Ar. [54].
3.4 Effect of different concentration of HBSH on sludge solid reduction
The settleability i.e. settling rate expressed as TSS was measured by collecting samples with time in 1000 cm3 (sampling point) of the settling column. The same amount of raw and the treated sludge with (0.8, 1.6 and 2.4 g/L) HBSH was used to conduct to evaluate the settling performance as compared to untreated sludge. The settling rate as TSS concentration was measured with settling time is illustrated in Figures 2–4. The observed results showed that the 0.8 treated sample, at the first part of the curve (up to 12 min) displayed a slightly higher settlement of TSS than that recorded by the raw sludge. However the settleability was doubled after that time and the overall TSS decreased to about half that in the untreated sludge at the end of 30 min period. The settlement rate was enhanced upon further addition of HBSH (1.6 g/L), the TSS decreased quickly and exceeded the TSS value recorded at 30 min by the untreated sludge within only about 17 min. The figure also shows a sharp reduction of TSS recorded after 10 min of settling then gradual decrease in TSS takes places to reach 230 g/L at 30 min. The faster settling rate was recorded by the 2.4 g/L treated sample. It was noticed that the TSS concentration decreased quickly and within less than 5 min reached the TSS concentration recorded by the raw sludge in 30 min. After such very sharp a decrease in the TSS concentration gradually continued to reach the lowest TSS value (150 g/L) recorded by the samples under experiment. The highest percentage of solids settlement (58.38%) was recorded by the 2.4 g/L HSBH treated sample after about 6 min of settling operation [55].
Figure 3.
Variation in TSS concentrations along raw and treated sewage at 1.6gL−1.
Figure 4.
Variation in TSS concentrations along raw and treated sewage at 2.4gL−1.
3.5 HMs binding capacity of HBSH at different concentration
Figures 5–7 shows the heavy metals (HMs) distribution in the liquid sludge phase before and after treating with the HBSH ligand at three different concentrations (0.8, 1.6 and 2.4 g/L). It was found that heavy metal concentrations were very high in the raw sludge. On the other hand, the heavy metal concentration showed a remarked decrease upon treating with the ligand (HBSH); this finding could be assigned to the ability of the HBSH to chelate the heavy metals ions. The results show that among all the HBSH concentrations used, Cd extraction efficiencies are noticeably the highest. The concentration of the chelator is inversely correlated with the general trend of HMs removal. As the concentration of HBSH raised from 0.8 to 2.4 g/L, removal of lead, cadmium, copper, zinc and chromium showed a continuous progress. This behavior is not the same in case of iron and nickel removal which firstly improved significantly by increasing the addition of HBSH from 0.8 to 1.6 g/L, while there is almost no change occurs upon raising the concentration from 1.6 to 2.4 g/L [56].
Figure 5.
Variation in heavy metals concentrations along raw and treated sewage at 0.8 gL−1 dose.
Figure 6.
Variation in heavy metals concentrations along raw and treated sewage at 1.6 gL−1 dose.
Figure 7.
Variation in heavy metals concentrations along raw and treated sewage at 2.4 gL−1 dose.
Figure 8 depicted the percentage of HMs removal upon addition of varying concentration of the HBSH. At 0.8 g/L, the ligand showed the highest removal potential toward cadmium with percentage 81.25% followed by nickel (66.3%). On the other hand, the lowest removal percentage was recorded for cupper. For other metal species (Pb, Fe, Zn and Cr) the removal percentages was around 50%. Upon further addition of HBSH (1.6 g/L), the removal percentages of all metal species have been enhanced to reach over than: 80% for iron and nickel, 70% for lead and chromium, and 60% for copper and zinc. However there is almost no change in removal percentage of cadmium (1.5%). Finally, further addition of HBSH (2.4 g/L) resumes its ability to remove cadmium content of the sludge to reach 93.75%. Removal of other metal species was elevated to: over than 80% of cupper, iron, nickel and lead and more than 85% for zinc and chromium [57].
Figure 8.
Variation in percentage of heavy metal concentrations along raw and treated sewage.
The results suggest also a higher HBSH lead to more effective extraction of heavy metals, this could be explained on basis that increasing dose of chelating ligand would facilitate the complexing reaction between metal ion and the chelating ligand leading to the formation of a chelate. Enhancing of the removal efficiency could be also related to the reason that there are many substances presented in the sludge beside the studied metal species such as: Ca, and Mg which consequently compete with the targeted metal species to bind the ligand and hence participate in the consumption of HBSH and according a large excess of ligand is required to solubilize the target metal due to the co-solubilization of Ca and Fe. Nowack et al. [29].
3.6 Removal of salmonella pathogens
Specific tests for the presence of Salmonella sp. were carried out, in both raw and dry sludge, we identified the presence of Salmonella spp. Confirmation of Salmonella was carried out using the API E20 Enterobacteriaceae test system and RISA molecular profiling. The data demonstrated that the total count of Salmonella sp. have been markedly lowered upon contacting with Schiff base for 30 min (Figure 9). The total counts for salmonella in the raw sludge recorded an averages of 2.8 × 103 and 1.7 × 104 MPN index/100 ml in the liquid and dray raw sludge respectively. These values have drastically decreased to only (25–28) MPN index/100 ml with successful removing of salmonella by about 99% upon treating with different concentration of Schiff base. From the results, it is clear the Salmonella sp. present in the effluent were in fact successfully being removed or inactivated upon treating with the Schiff base. The removal of Salmonella was clearly observed, however no pronounced effect on the salmonella surviving was shown upon changing the Schiff base concentration from 0.8 to 2.4 g/L.
Figure 9.
MPN index/100 ml of salmonella count in solid, liquid raw sludge as well as treated with varying concentrations (0.8, 1.6, 2.4 g/L) of Schiff base (HBSH).
3.7 Raw and treated Schiff base-sludge as fertilizers for radish plant
Organic fertilizers are used to encounter the requirements of vegetable and plant production. Sewage sludge is an important factor that can be utilized for vegetable and plant production in view of its high organic matter content and rich macro and micro nutrients. However extreme care is to be taken to avoid the entry of the heavy metals and other organic compounds in the food chain. In our study, we investigated the implementation of raw as well as treated sludge with Schiff base at 2.4 g/L on the growth as well as the heavy metal content of radish plant. It was observed that the application of sewage sludge enhanced soil fertility and that crop yield in the treated sludge was higher than in the raw one. The treated sample showed enhancement in the radish yield, stem length, leaves number and flourishing (Figure 10). The total heavy metal content in radish have been also estimated in the radish treated with the raw and Schiff base- sludge. The results showed the application of 2.4 g/L of Schiff base showed a reduction in the total content of zinc (Zn), nickel (Ni), chromium (Cr) and cobber (Cu) in the plant. Concentrations of nickel and chromium ions showed a significantly reduction upon treating the plant with the Schiff base rather than that treated with the raw sludge with 82.75 and 70.96% respectively (Figure 11). Schiff base treating sludge showed also promising results regarding copper and zinc ions [58, 59].
Figure 10.
Effect of (a) raw and (b) treated sludge with 2.4 g/L Schiff base on the growth and flourishing of radish plant.
Figure 11.
Variation in heavy metals concentrations in radish plant fertilized by raw and treated sewage at 2.4 gL−1 of the Schiff base.
A novel organic Schiff base chelator (HBSH) has been successfully synthesized and characterized by elemental analysis. The effect of sewage treated with varying concentration of the Schiff base chelator (0.8, 1.6 and 2.4 g/L) as well as the untreated sewage on the sludge solid reduction, removal of heavy metals and salmonella pathogens has been investigated. The settlement rate was enhanced upon addition of HBSH Schiff base, the faster settling rate as well as the highest percentage of solids settlement (58.38%) was recorded by the 2.4 g/L treated sample. The highest removal potential was recorded toward cadmium with percentage 81.25% followed by nickel (66.3%). The total counts for salmonella in the raw sludge have drastically decreased to only (25–28) MPN index/100 ml referring to successful removing of salmonella by about 99% upon treating with different concentration of Schiff base. The implementation of raw as well as treated sludge on the growth as well as the heavy metal content of radish plant have been also investigated. It was observed that, the treated sample showed a reduction in the total content of Zn, Ni, Cr and Cu and enhancements in the yield, stem length, leaves number and flourishing.
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Written By
Sara Mohamed Yonues and Abdou Saad El-Tabl
Submitted: 11 September 2022Reviewed: 29 November 2022Published: 30 December 2022
Open access peer-reviewed chapter
