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A R T I C LE I N FO A B S T R A C T
Keywords: This study evaluated the triple filtration technology efficiency as a post-treatment of anaerobic reactor effluent.
Post-treatment This study was carried out employing different concentrations of ferric chloride as coagulant and peracetic acid
Triple filtration or calcium hypochlorite as oxidant. The filtration rates used were 150 m3/m2 d and 120 m3/m2 d. The efficiency
Coagulation of the system was evaluated through physicochemical and microbiological parameters. The best conditions
Oxidation
found were those using 20 mg/L ferric chloride, 120 m3/m2 d filtration rate and 0.8 and 1.6 mg/L free chlorine.
Reuse
These conditions resulted in turbidity < 1.0 NTU, Total Organic Carbon < 1.5 mg/L, Chemical Oxygen
Demand < 1.0 mg/L, Biochemical Oxygen Demand < 1.0 mg/L, in addition 100% removal of Total Phosphorus
and Linear Alkylate Sulfonate. The post-oxidation process promoted inactivation of 100% Total Coliforms and E.
coli. The post-treatment was able to produce effluent with characteristics that enable its urban, damming,
creation and maintenance of wetlands, industrial and agricultural reuse proposed by USEPA.
∗
Corresponding author.
E-mail addresses: qaasuepgcleber@gmail.com (C.P. da Silva), campos@uepg.br (S.X. de Campos).
https://doi.org/10.1016/j.jenvman.2018.12.030
Received 13 April 2018; Received in revised form 15 November 2018; Accepted 9 December 2018
0301-4797/ © 2018 Elsevier Ltd. All rights reserved.
C.P. da Silva et al. Journal of Environmental Management 233 (2019) 76–82
2.1. Triple filtration pilot unit operation The pH of coagulation and the range of ferric chloride concentra-
tions employed for the treatment of effluents in the triple filtration pilot
In this study, a pilot unit was assembled at the WWTP Rio das Antas, unit were previously determined in bench tests. Fig. 2 shows the main
Irati, state of Parana, Brazil, which serves a population of approxi- results obtained in tests using jar test equipment.
mately 58,000 inhabitants, with an 80 L/s flow. The system in opera-
tion has primary treatment that includes coarse material containment Table 1
screens and sand removal system. Then the effluent is directed to the Physicochemical and microbiological parameters assessed.
secondary system consisting of two anaerobic reactors working in Parameters Method
parallel with a capacity of 40 L/s each. An equalization box combines
the secondary effluent from the anaerobic reactors, which goes to the Turbidity (NTU) Nephelometric 2130B
Biochemical Oxygen Demand – BOD (mg Oxymetric 5210B
final polishing pond. For the tests carried out in this work, effluent was
O2/L)
collected in the equalization box. Chemical Oxygen Demand – COD (mg/L) Spectrophotometric (Hach 8000®)a
Three filters were used in the study. The first was the upward gravel Free chlorine (mg/L) Spectrophotometric (Alphakit®)a
filter (UGF) (Fig. 1), disposed in four 300 × 150 mm layers, with dif- Total Phosphorus – TP (mg/L) Spectrophotometric (Spectroquant®)a
ferent grain sizes within the following intervals: 19.1 to 38.1; 9.52 to Ammonia Nitrogen – AN (mg/L) Spectrophotometric (Alphakit®)a
Total Nitrogen – TN (mg/L) Spectrophotometric (Spectroquant®)a
19.1; 4.8 to 9.52 and 2 to 4.8 mm. The second was the downward sand Partial Alkalinity – PA (mg CaCO3/L) Potentiometric titration 2320 B
filter (DSF) disposed in a 150 × 700 mm monolayer and 0.30 mm ef- Apparent color (C.U) Spectrophotometric 2120 C
fective grain size with a 0.348 m2/g surface area and 0.00078 cm3/g Total suspended solids - SST (mg/L) Filtration/gravimetric 2540 D
pore volume. The third was the downward charcoal filter (DCF), mea- E. coli (CFU/100 ml) Membrane filter 9222 B
Total coliforms - TC (CFU/100 mL) Membrane filter 9222 B
suring 150 × 700 mm, with a 21.31 m2/g surface area and 0.0601 cm3/
Linear Alkylate Sulfonate - LAS (mg/L) Spectrophotometric (Alphakit®)a
g pore volume. Total Organic Carbon - TOC (mg/L) TOC-L (Shimadzu®)
The UGF was operated with the execution of intermediate fund
a
discharge (IFD) and Final Fund Discharges (FFD), which were carried Kit.
77
C.P. da Silva et al. Journal of Environmental Management 233 (2019) 76–82
A 100 B Table 2
100
removal percentage (%)
Physicochemical results obtained for the anaerobic reactor effluent (Raw) and
90 90 anaerobic reactor effluent post-treatment by triple filtration.
80
80 Ferric COD (mg/L) BOD (mg/L) TOC (mg/L) LAS (mg/L)
70
chloride
60 70
50 20 (mg/L) DCF 12.7 ± 0.6a 5.1 ± 0.9a 2.9 ± 0.2a < 0.1
60 50 (mg/L) 11.9 ± 2.2a 5.7 ± 0.6a 2.4 ± 0.2b < 0.1
40 Turbidity (NTU) Color (C.U) Turbidity (NTU) Color (C.U) 80 (mg/L) 13.1 ± 2.8a 5.7 ± 0.6a 2.7 ± 0.1a < 0.1
30 50 20 (mg/L) DSF 27.96 ± 2.9b 12.7 ± 2.2b 9.5 ± 1.9c 2.2 ± 0.2a
5 6 7 8 9 0 20 40 60 80 100 120 140
50 (mg/L) 23.13 ± 3.2b 9.9 ± 1.2b 8.5 ± 1.4c 2.0 ± 0.3a
pH ferric chloride (mg/L)
80 (mg/L) 25.6 ± 5.2b 9.4 ± 1.1b 8.3 ± 0.93c 0.9 ± 0.1b
Raw 253.6 ± 66.9 100.4 ± 18.2 69.6 ± 3.6 8.4 ± 0.3
Fig. 2. Main results obtained in jar test. A: mixing gradient 300 s−1; time of
mixing 15 s and concentration of ferric chloride 80 mg/L. B: mixing gradient
Parameters with the same superscript letter did not differ statistically.
300 s−1; mixing time 15 s and original effluent pH 6.9 ± 0.2. (Mean ± SD,
(Mean ± SD, n = 6).
n = 3).
78
C.P. da Silva et al. Journal of Environmental Management 233 (2019) 76–82
Table 3
Physicochemical and microbiological results obtained through the study of oxidation-disinfection by triple filtration and for the anaerobic reactor effluent (Raw).
Free chlorine PAA Raw
0.8 1.6 4 8
c b b
COD (mg/L) 11.1 ± 1.9 22.4 ± 3.1 19.3 ± 2.4 28.5 ± 3.7a 269.7 ± 82.25
BOD (mg O2/L) 1.6 ± 0.2c 1.2 ± 0.1c 6.2 ± 0.8a 3.2 ± 0.5b 99.6 ± 5.1
Turbidity (NTU) 0.71 ± 0.02a 0.73 ± 0.08a 0.66 ± 0.07b 0.58 ± 0.03b 108.4 ± 9.0
Color (C.U) < 1.0 1.6 ± 0.6 5.0 ± 1.0 8.0 ± 1.0 832.0 ± 86.0
TSS (mg/L) < 1.0 < 1.0 < 1.0 < 1.0 98.1 ± 18.8
PA (mg CaCO3/L) 97.2 ± 11.9a 46.5 ± 6.4c 114.9 ± 12.29a 67.9 ± 6.2b 304.4 ± 47.5
TP (mg/L) < 0.5 < 0.5 < 0.5 < 0.5 3.19 ± 1.26
E. coli (CFU/100 ml) ND ND ND ND 6.12 ± 6.0
T.C (CFU/100 ml) ND ND 1.4 ± 0.4 1.38 ± 0.6 6.16 ± 8.85
Parameters with the same superscript letter did not differ statistically. Values for E. coli and T.C presented in logarithm. ND: not detected; PA: Partial Alkalinity; TP:
Total Phosphorus; T.C: Total coliforms. (Mean ± SD, n = 3).
contaminant (Zipf et al., 2016). the ferric chloride reacted with the weak acid anions present in the
effluent, producing polymerizable insoluble metal oxides and hydro-
3.2. Evaluation of the efficiency of peracetic acid and free chlorine in xides, which are able to aggregate colloidal particles present in the
oxidation-disinfection effluent (Keeley et al., 2016). Such polymerization was able to generate
flakes that were sedimented or retained in the filters (Cavallini et al.,
The physicochemical and microbiological results for the study on 2016).
oxidation-disinfection using peracetic acid (PAA) and free chlorine, In this study, free chlorine in the form of hypochlorite was added
with a 150 m3/m2 d filtration rate and 20 mg/L and ferric chloride by after the filtration process, and the 0.8 and 1.6 mg/L concentrations
triple filtration are presented in Table 3. were tested for a 30-min minimum contact time. Total inactivation of E.
The results presented in Table 3 show that the addition of oxidants coli and total coliforms was observed with all free chlorine dosages.
increased COD values. The variation observed between chlorine addi- Chlorination is the most used effluent disinfection method in WWTP in
tions was 11.3 mg/L while those for PAA addition were 9.3 mg/L. The the world (Hunter et al., 2018; Tyagi et al., 2010). However, peracetic
addition of 8 mg/L PAA was seen to result in an increase of around acid was also tested, and it has been used in several industrial activities
16 mg/L in the effluent COD, which is in accordance to reports by as an alternative oxidant (Cavallini et al., 2016; Mcfadden et al., 2017).
(Cavallini et al., 2013). Regarding the increase in free chlorine addi- All PAA tests resulted in E. coli total inactivation and values below
tions, a more pronounced increase in COD was observed, since the free 30 CFU/100 ml for total coliforms, which represents inactivation over
chlorine concentrations added were lower than the PAA concentrations, 99.9% for total coliforms and 100% for E. coli. This indicates that the
which agrees with the results obtained by the effluent chlorination disinfection process was efficient, even with lower PAA concentrations.
process (El-Rehaili, 1995).
There was no significant variation of the BOD parameter when free 3.3. Filter operation time
chlorine doses were considered. However, the increase in PAA con-
centration showed a reduction in the BOD value. These results show Fig. 3 shows the turbidity and effluent flow rates for the filtration
that the BOD response in relation to PAA oxidation was stronger in runs at 150 and 120 m3/m2 d rates.
comparison to the chlorine oxidation. However, the lower value ob- For the 150 m3/m2 d filtration rate (Fig. 3-A), high turbidity de-
served in the BOD measures free chlorine might be ascribed to the termined the final of the filtering career of the UGF and DSF in 2.5 h.
oxidation of part of the biodegradable dissolved organic matter. The treated effluent flow during this period was observed to reduce
The removal of turbidity and apparent color was over 99%. This from 2.64 to 2.16 m3/d, requiring intermediate fund discharge in the
efficiency in the turbidity and color removal might be explained by the UGF and washing of the DSF. The turbidity for the DCF was below 1.0
retention of colloidal particles and dissolved solids in the sand and NTU for most of the study time, except for the periods where the tur-
activated charcoal filter, in addition to the effluent residual organic bidity of the DSF was greater than 10.0 NTU, and the filtration course
load mineralization process during the oxidation process (Aguiar et al., was finished in the DCF when the final effluent showed turbidity
2007; Cavallini et al., 2016). value > 1.0 NTU.
In relation to total phosphorus, 100% removal was observed when For the 120 m3/m2 d (Fig. 3-B) filtration rate, the turbidity de-
the 0.5 mg/L quantification limit for the determination method was termined the final of the filtration career of the UGF in 4.0 h, when the
considered. The coagulation process carried out in the post-treatment turbidity was > 15 NTU, causing turbidity increase to values > 1.0 in
initial phase contributed significantly to the total phosphorus removal, the DSF. The execution of an IFD was sufficient to obtain values < 1.0
due to the possible formation of ferric hydrates, in addition to the in- NTU in the DSF again in the following couple of hours. The career in the
corporation of phosphate in hydrated oxide structures, formation of DSF was closed with 12 h of operation when the leak fell to 0.84 m3/d.
mixed cation phosphates and ferric phosphate (Metcalf and Eddy, Regarding the 120 m3/m2 d the filtration rate (Fig. 3-C), the tur-
2013). This condition can be verified when the post-treatment proposed bidity determined the final of the filtration career of the UGF in 7.5 h,
in this study is compared to other technologies already reported in the when turbidity removal decreased to values < 20% and increased
literature, such as the urban effluent treatment with sand filtration turbidity of DSF to values > 1.0 NTU, requiring IFD in the UGF. The
without previous coagulation, which presented up to 65% phosphorus turbidity values of the final effluent after the DCF remained < 0.01
removal (Laaksonen et al., 2017), and to the effluent treatment using NTU. The effluent flow was seen to remain constant, except when
coagulation and fast filtration which obtained about 90% total phos- performing intermediate bottom discharges in the UGF.
phorus removal (Altmann et al., 2016, 2015). The observations suggest that the 150 m3/m2 d rate decreases the
Partial alkalinity reduction ranged between 68.1 and 84.7% in the efficiency of the UGF by the transport of material present in the ef-
treatments using free chlorine and between 62.3 and 77.7% for those fluent, leading to the rapid obstruction of the DSF. At a filtration rate of
using PAA. The alkalinity reduction during treatment occurred because 120 m3/m2 d with initial turbidity of 35.4 to 49.6 NTU, an
79
C.P. da Silva et al. Journal of Environmental Management 233 (2019) 76–82
35
30 1.5
25
20
15
1.0
10
5
0
-5 0.5
0 2 4 6 8 10 12
time in hours
30 2.0
25
flow rate (m3/d)
turbidity (NTU)
20
1.5
15
10
1.0
5
-5 0.5
0 2 4 6 8 10 12 14 16
time in hours
(caption on next page)
80
C.P. da Silva et al. Journal of Environmental Management 233 (2019) 76–82
Fig. 3. Results of turbidity and effluent flow in the triple filtration system using 20 mg/L of ferric chloride. A: 150 m3/m2 d with initial turbidity from 32.4 to 49.1
NTU; B: 120 m3/m2 d with initial turbidity from 35.4 to 49.6 NTU; C: 120 m3/m2 d with initial turbidity from 19.3 to 29.8 NTU; UGF: Upward Gravel Filter; DSF:
Downward Sand Filter; DCF: Downward Charcoal Filter; Δ: Intermediate Fund Discharge from UGF; ×: washing the DSF.
Table 4
Results obtained in anaerobic reactor effluent with a filtration rate reduction.
Free chlorine PAA Raw
0.8 1.6 4 8
COD (mg/L) < 1.0 < 1.0 8.4 ± 1.7 9.6 ± 0.6 176.5 ± 23.3
BOD (mg O2/L) < 1.0 < 1.0 1.7 ± 0.2 2.1 ± 0.3 80.5 ± 7.9
TOC (mg/L) 1.4 ± 0.01c 1.1 ± 0.8c 5.8 ± 0.5b 9.7 ± 0.15a 66.18 ± 4.03
LAS (mg/L) < 0.1 < 0.1 < 0.1 < 0.1 14.0 ± 1.4
Turbidity (NTU) 0.45 ± 0.01a 0.35 ± 0.03a 0.31 ± 0.01a 0.29 ± 0.02a 38.2 ± 2.6
Color (C.U) < 1.0 < 1.0 < 1.0 < 1.0 385 ± 63.14
TSS (mg/L) < 1.0 < 1.0 < 1.0 < 1.0 90.5 ± 7.9
Free chlorine 0.5 ± 0.1 1.1 ± 0.3 < 0.1 < 0.1 < 0.1
TP (mg/L) < 0.5 < 0.5 < 0.5 < 0.5 6.4 ± 0.3
AN (mg/L) 41.5 ± 2.1a 39.5 ± 2.2a 38.5 ± 0.7a 35.5 ± 0.7a 55.0 ± 4.2
Nitrite (mg/L) < 0.01 < 0.01 < 0.01 < 0.01 0.03 ± 0.01
Nitrate (mg/L) < 0.01 < 0.01 < 0.01 < 0.01 0.82 ± 0.04
TN (mg/L) 56.0 ± 1.0a 56.5 ± 8.5a 58.0 ± 12.0a 55.5 ± 3.5a 87.5 ± 11.5
E. coli (CFU/100 ml) ND ND ND ND 6.36 ± 5.75
T.C (CFU/100 ml) ND ND ND ND 6.63 ± 6.18
Parameters with the same superscript letter did not differ statistically. Values for E. coli and T.C presented in logarithm. ND: not detected. AN: Ammonia Nitrogen;
TN: Total Nitrogen; TP: Total Phosphorus; T.C: total coliforms. Filtration rate 120 m3/m2 d and 20 mg/L ferric chloride. (Mean ± SD, n = 3).
improvement of approximately 37% in the filtration career time was chlorination process rapidly oxidizes ammonia. Nitrogen from simple
verified in relation to the 150 m3/m2 d rate. This indicates that the and unsubstituted amino acids is oxidized more slowly. Protein ni-
lower filtration rate decreased the drag of flocculated material in the trogen has an insignificant loss, even after prolonged periods of chlor-
settler and the UGF. For a filtration rate of 120 m3/m2 d with initial ination (Pressley et al., 1972). Inorganic nitrogen compounds have no
turbidity from 19.3 to 29.8 NTU, an improvement of approximately significant effect on PAA decay by oxidation. As for organic nitrogen
46.6% in the filtration run time was verified in relation to the 120 m3/ compounds, only proteins significantly affect the demand of PAA
m2 d turbidity rate with initial turbidity from 35.4 to 49.6 NTU. This (Domínguez Henao et al., 2018). In a summarized way, possibly the
can be explained by the fact that effluents with higher turbidity present removal of organic nitrogen occurred during the coagulation and fil-
higher content of suspended solids, which would require a higher tration process. For the removal of ammonia nitrogen, the oxidation
concentration of ferric chloride in the coagulation. process is expected to be the most relevant.
The 120 m3/m2 d filtration rate resulted in a better quality effluent
when compared to the 150 m3/m2 d rate, since it decreased the organic
3.4. Evaluation of the filtration rate reduction matter dragging in the form of solids between the filter particles, as can
be observed by comparing the results of COD, BOD and TOC in Tables 3
The physicochemical and microbiological results of the treatments and 4.
with reduction in the filtration rate are presented in Table 4. The post-treatment using gravel, sand and activated charcoal fil-
Reduction in the filtration rate enabled the improvement of the COD tration was shown to be a promising alternative to the treatment of
removal to values < 1.0 mg/L using free chlorine and values < anaerobic reactor effluent. The results obtained meet all the parameters
10 mg/L when PAA used. The same trend was seen when the TOC set forth in the reuse handbook US.EPA (2012) for urban reuse, re-
values were compared, with values < 1.5 mg/L for the free chlorine stricted/non restricted damming, creation and maintenance of wet-
treatments and values < 10 mg/L for treatments with PAA. lands, industrial and agricultural reuse. They also partially meet the
LAS, turbidity, color and total suspended solid values were < 0.1 requirements for reuse as drinking water, due to the restriction of
mg/L, < 1.0 NTU, < 1.0 C.U and < 1.0 mg/L, respectively. This in- drinking water quality parameters that were not evaluated in this study.
dicates improvement in the removal of dissolved and suspended ma- The results presented pointed out that the use of activated charcoal
terials. The free chlorine residuals values determined after oxidations contributed to the improvement in the removal of all parameters ana-
were 0.5 and 1.1 considering, respectively, the initial values 0.8 and lyzed in relation to similar studies. In addition, the system proposed
1.6 mg/L, after a 30-min minimum contact time, which ensured the produced an effluent with reuse qualities, employing reduced con-
inactivation of pathogenic microorganisms. centrations of ferric chloride (20 mg/L). These results represent sig-
Regarding the removal of phosphorus, nitrite and nitrate, 100% nificant advances in treatment of anaerobic reactor effluent, when
removal could be verified when a quantification limit of 0.5, 0.01 and compared to similar studies of sand slow filtration carried out by Tyagi
0.01 mg/L was considered, respectively. For the ammonia nitrogen, the et al. (2009) and double filtration proposed by Cavallini et al. (2016)
removal observed ranged between 24.5 and 35.4%. Ammonia can which only obtained suitable conditions for agricultural reuse.
oxidized to chloramines (Pressley et al., 1972). However, chloramine
can be oxidized by chlorine under slightly alkaline conditions in ni-
trogen gas. In addition, other end products such as nitrate and nitrogen 4. Conclusion
trichloramine may be formed during the disinfection process using a
strong oxidizing agent such as chlorine or PAA (Cavallini et al., 2016; The results showed that triple filtration can become an alternative
Mitch and Sedlak, 2002; Pressley et al., 1972; Shah et al., 2015). For the to the post-treatment of anaerobic reactor effluent. The activated
total nitrogen, the removal observed ranged between 21.2 and 24.1%. charcoal filter contributed efficiently to the reduction in the ferric
For the total nitrogen, a pattern of oxidation is observed. The chloride dose, in addition to improving the removal of physicochemical
81
C.P. da Silva et al. Journal of Environmental Management 233 (2019) 76–82
parameters when compared to similar studies. The study obtained a multifunctional wetlands: pollution abatement and other ecological services from natural
treated effluent for reuse with 20 mg/L ferric chloride, which resulted and constructed. In: Nagabhatla, N., Metcalfe, C.D. (Eds.), Multifunctional Wetlands.
Springer International Publishing, Cham, pp. 15–81. https://doi.org/10.1007/978-3-319-
in lower reagent consumption. The post-oxidation-disinfection process 67416-2_2.
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