Mittwoch, 24. Februar 2016

Biodegradation in water and sediment



Biodegradation:

Biodegradation in water and sediment: simulation tests.001


Administrative data

Purpose flag:
key study
Study result type:
experimental result
Reliability:
1 (reliable without restriction)

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2005

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 308 (Aerobic and Anaerobic Transformation in Aquatic Sediment Systems)
Deviations:
no
GLP compliance:
yes

Test materials

Identity of test material same as for substance defined in section 1 (if not read-across):
no
Test material identity
Identifier:
CAS number
Identity:
7775-09-9
Details on test material:
Purity: 99.66 %

Further relevant properties: 
Molecular weight: 106.5
Water solubility: 715 g/L
Vapour pressure: < 3.5 10-5 Pa (25 °C)
Log Ko/w: <-1
Hydrolysis: Stable
Solubility in organic solvents: Mixtures of chlorate and organics are explosive

Composition of the product:
H2O = 0.062 %
NaCl = 0.022 %
Ca3(PO4)2 = 0.16 %
Fe2O3 = 0.09 %

Preparation of the test solution: The test substance was dissolved in an appropriate amount of deionised water, allowing addition of 0.2 mL of the stock solution to the aqueous phase of the water sediment system.

Lot/ Batch number: 1E0103WF
Radiolabelling:
no

Study design

Oxygen conditions:
aerobic/anaerobic
Inoculum or test system:
natural water / sediment
Details on source and properties of sediment:
Two sediments were collected from pristine environments:
a) Heveadorp – This was collected from a stream fed with groundwater (Fonteinallee, Heveadorp, The Netherlands). Aerobic samples were taken from a depth of 0-10 cm. These were grey to brown and had a soil-like smell. Anaerobic samples were taken from 10-20cm. These samples were also grey to brown and had a light sulphide smell.
b) OVP – This was taken from the Oostvaardersplassen (Knardijk, Lelystad, The Netherlands) Aerobic samples taken from 0-5 cm. These were a grey to black and had a slight sulphide smell. The anaerobic samples were taken at 15-25 cm, were black, with a sulphide smell.
The sediments were sieved through screens with openings of 2 mm to improve uniformity of the substrate application. Sediments were then preconditioned by incubation for one week at 20 ± 2 °C.
Initial test substance concentration
Initial conc.:
25 mg/L
Based on:
test mat.
Parameter followed for biodegradation estimation
Parameter followed for biodegradation estimation:
Test mat. analysis
Details on study design:
For each sediment, there was one treatment, i.e. test substance added to the water sediment system. The sediment layer was ± 4.5 cm. The test was carried out in 1 L flasks closed with butyl septa (anaerobic incubations) or parafilm (aerobic incubation), which ensured that the water level was maintained for the duration of the test. Degradation of chlorate in the sediment was followed in duplicate bottles. Chlorate was introduced in the water phase. To prevent depletion of oxygen concentration in the overlying water in the aerobic incubations, the overlying water was aerated at such a rate that the overlying water was oxygen saturated throughout the duration of the test. Anaerobic conditions were established at the start of the test by flushing the gas phase with nitrogen gas. Sampling was performed with minimal disturbance of the sediment and the overlying water, using a gas pipe with a diameter of ± 10 mm. 

Incubation temperature: 20 ± 2 °C
pH (sediments and overlying waters) : 6.1 – 7.3
Redox potential (aerobic/anaerobic): -76 to -180 mV *
Oxygen content (aerobic only): High concentrations
Organic carbon content (in overlying water): Decrease from 54-64 mg/L to 26-32 mg/L

* The redox potential of OVP sediment was slightly lower than Heveadorp sediment. The redox potential in the overlying water of the aerobic incubations was always higher than 240 mV.

The initial concentration of the chlorate in the overlying water was calculated by assuming an even distribution of the test substance in the overlying water and the water in the sediment. Due to the immediate start of chlorate reduction and limited mixing of the overlying water at the start of the test, it is not expected that the chlorate concentrations measured at the start agree with the calculated initial chlorate concentration.

Duration of the test: 
OVP: 28 days
Heveadorp: 56 days

Samples of overlying water and sediment: 0, 3, 7, 10, 14, 28, 42 (both sediments) and 56 (Heveadorp). 
The following time intervals were adopted for the anaerobic bottles starting after introducing the anaerobic conditions: day 0, 1, 3, 7, 10, 14, 21, 28 (both sediments) and only 56 (only Heveadorp).
Reference substance
Reference substance:
not required

Results and discussion

Material (mass) balance

% Degradation of test substance
% Degr.:
100
Parameter:
Test mat. analysis
Remarks:
By the end of the study an excess of chloride was produced in the water sediment systems. This excess already strongly indicates that the chlorate added was reduced to chloride.
Transformation products:
yes
Identity of transformation products
No.:
#1
Identifier:
common name
Identity:
Chloride
Details on transformation products:
The complete conversion of chlorate to chloride by the end of the study period indicates that no intermediates were present after 28 or 56 days.
Details on results:
Mass balances of chlorine in water sediment systems may be used to demonstrate the complete conversion of chlorate to chloride. Excess of chloride was produced in the water sediment systems. This excess already strongly indicates that the chlorate added was reduced to chloride. The controls incubated for the determination of the biomass concentration enabled the assessment of the “endogenous” formation of chloride in the sediment water systems. The chloride formed in the control was subtracted from the chloride produced in the sediment water systems with chlorate. The chloride concentrations ranged from 181 to 298 µmol/L. This demonstrates that almost 100 % of the chlorate-chlorine in the aerobic OVP sediment water system is recovered as chloride. The high rates of biodegradation in both water-sediment systems are highly suggestive of the existence of a large and active population of microorganisms capable of reducing chlorate.
The microbial biomass concentrations decreased after an incubation period of 28 days. The active microbial biomass concentrations in aerobic and anaerobic sediment of Heveadorp were 7 and 6 µg/g respectively. The biomass concentration in both sediments of Heveadorp was 5 µg/g after 56 days.
Any other information on results incl. tables:
Table A7_1_2_2_2-3:        Sodium chlorate and sodium chloride concentrations in two sediments and overlying waters incubated under aerobic conditions (average of duplicates)
Time (days)
OVP
Heveadorp
Overlying water
Sediment
Overlying water
Sediment
[NaClO3] (µmol/L)
0
202
434
151
301
3
195
3
214
77
7
138
48
186
138
10
45
3
162
140
14
15
2
141
123
28
0
0
60
42
42
21
12
56
7
6
Time (days)
[NaCl] (µmol/L)
0
780
785
673
704
3
789
1531
681
915
7
1088
1144
782
828
10
1352
1499
857
866
14
1485
1512
883
898
28
1514
1435
931
924
42
1037
973
56
1098
1037

Table A7_1_2_2_2-4:        Sodium chlorate and sodium chloride concentrations in two sediments and overlying waters incubated under anaerobic conditions (average of duplicates)
Time (days)
OVP
Heveadorp
Overlying water
Sediment
Overlying water
Sediment
NaClO3 (µmol/L)
0
162
264
145
289
1
247
0
243
212
3
213
0
234
53
7
145
31
216
182
10
67
14
195
167
14
38
21
186
152
28
0
0
136
122
42
0
0
105
76
56
21
18
Time (days)
NaCl (µmol/L)
0
778
786
671
693
1
787
800
723
685
3
801
1655
692
964
7
1082
1303
809
875
10
1410
1513
907
917
14
1562
1581
923
957
28
1609
1633
930
942
42
1476
1521
981
983
56
1065
1087
Table A7_1_2_2_2-5:        DT50, DT75 and DT90 values of chlorate reduction in two sediments and their overlying water incubated under aerobic and anaerobic conditions.
OVP (high organic carbon content)
Aerobic
Anaerobic
Water
Sediment
Water
Sediment
DT50 (days)
8
3
9
1
DT75 (days)
10
3
12
1
DT90 (days)
12
3
15
1
Heveadorp (low organic carbon content)
DT50 (days)
20
18
29
24
DT75 (days)
31
26
41
36
DT (days)
42
34
54
51
Table A7_1_2_2_2-6:        Chloride concentrations in test and control flasks at the end of the experiments and the chloride formed calculated by subtracting the concentrations measured
Sample id.
Chloride (µmol/L)
Control
Test
Test - Control
Heveadorp anaerobic
132
394
262
Heveadorp aerobic
81
379
298
OVP anaerobic
474
717
242
OVP aerobic
510
692
181
Control (biomass) = without chlorate

Applicant's summary and conclusion

Conclusions:
Complete conversion is also indicative of the conversion of chlorite to chloride, with no remains of chlorite, i.e. chlorite is completely degraded.
Validity criteria fulfilled:
yes



Biodegradation in water and sediment: simulation tests.002


Administrative data

Purpose flag:
key study
Study result type:
experimental result
Reliability:
2 (reliable with restrictions)

Data source

Reference
Reference Type:
other company data
Title:
Unnamed
Year:
2007

Materials and methods

Principles of method if other than guideline:
An investigation into the degradation of chlorine dioxide in aqueous systems was performed using water from three sources – industrial wastewater, surface (river) water and tap (drinking) water. Chlorine dioxide (0, 1, or 3 mg/L) was added to 500 mL of water in a flask which was then Stoppered and stirred. Samples of the solution were removed at 0, 5, 10, 30 and 60 minutes and 20 hours and the level of chlorine dioxide residual measured using a spectrophotometric method at 340 nm. The pH of the test waters was between 7.0 – 7.9 and the temperature was 22 °C.
GLP compliance:
no data

Test materials

Identity of test material same as for substance defined in section 1 (if not read-across):
yes
Test material identityopen allclose all
Details on test material:
Specification: Prepared as an aqueous solution at 32.3 mg/L
Purity: Pure

Preparation of the test solution: Pure chlorine dioxide solution was produced by adding small amounts of sulphuric acid to the Purate® solution (NaClO3 + H2O2) contained in bottle 1. The chlorine dioxide gas formed is adsorbed into the chilled deionized water in bottle 2. Bottle 3 catches any residual chlorine dioxide gas escaping from bottle 2.
Radiolabelling:
no

Study design

Oxygen conditions:
aerobic/anaerobic
Inoculum or test system:
other: Industrial effluent, surface water and tap water
Details on source and properties of surface water:
Industrial effluent: Waste water from a tissue mill. Sample was taken just before being dispatched in the recipient (river Göta Älv). 
Surface water: The River Göta Älv which supplies the Gothenburg Drinking water works with water. Sample was taken in the river outside EKA Chemicals
Tap water: Drinking water from the city of Gothenburg, disinfected with monochloramine (< 0.3 mg/L as Cl2)
Initial test substance concentrationopen allclose all
Details on study design:
Industrial effluent: Waste water from a tissue mill. Sample was taken just before being dispatched in the recipient (river Göta Älv). 
Surface water: The River Göta Älv which supplies the Gothenburg Drinking water works with water. Sample was taken in the river outside EKA Chemicals
Tap water: Drinking water from the city of Gothenburg, disinfected with monochloramine (< 0.3 mg/L as Cl2)

Duration of the test: 0, 5, 10, 30, 60 minutes or 20 hours
Reference substance
Reference substance:
not required

Results and discussion

Material (mass) balance

% Degradation of test substanceopen allclose all
% Degr.:
ca. 100
Parameter:
Test mat. analysis
Sampling time:
5 min
Remarks:
In wastewater effluent, an initial dose of 3 mg/L chlorine dioxide was completely reacted after 5 minutes contact time.
% Degr.:
> 50 - < 100
Parameter:
Test mat. analysis
Sampling time:
60 min
Remarks:
In surface (river) water, residual chlorine dioxide was detected in the test solution 60 minutes after addition of either 1 or 3 mg/L.
% Degr.:
ca. 100
Parameter:
Test mat. analysis
Sampling time:
20 h
Remarks:
No residual chlorine dioxide was detected in the 3 mg/L test solution after 20 hours contact time.
% Degr.:
ca. 40
Parameter:
Test mat. analysis
Sampling time:
20 h
Remarks:
In tap water (drinking water) the initial dose of 1 mg/L was reduced to 0.6 mg/L after 20 hours contact time.
Half-life of parent compound / 50% disappearance time (DT50)open allclose all
Compartment:
other: Tap water
Half-life:
27.7 h
Type:
no data
Remarks (e.g. regr. equ., r², DT90):
1 mg/L initial ClO2 concentration
Compartment:
other: surface water
Half-life:
16 min
Type:
no data
Remarks (e.g. regr. equ., r², DT90):
1 mg/L initial ClO2 concentration
Compartment:
other: surface water
Half-life:
22 min
Type:
no data
Remarks (e.g. regr. equ., r², DT90):
3 mg/L initial ClO2 concentration
Transformation products:
no data
Details on results:
In wastewater effluent, an initial dose of 3 mg/L chlorine dioxide was completely reacted after 5 minutes contact time.
In surface (river) water, residual chlorine dioxide was detected in the test solution 60 minutes after addition of either 1 or 3 mg/L. No residual chlorine dioxide was detected in the 3 mg/L test solution after 20 hours contact time. 
In tap water (drinking water) the initial dose of 1 mg/L was reduced to 0.6 mg/L after 20 hours contact time.
Any other information on results incl. tables:
No standard deviations available

Applicant's summary and conclusion

Conclusions:
Although selective, chlorine dioxide reacts with a number of inorganic and organic substances like iron, sulphur compounds (organic as well as inorganic), phenolic compounds and humus acids. 
Every surface water, ground water, waste water etc. is unique regarding composition of substances that can react with chlorine dioxide. The lab study has consequently to be seen as an example of how chlorine dioxide may decay in the aqueous environment.
No decay of ClO2 could be detected using tap water during the evaluated time frame. The reason for the slow decay in tap water is the low amount of substances that can be oxidized. Still a low amount of ClO2 in the water leaving the water plant is desired in order to prevent recontamination of the water and to avoid bio fouling of the water pipes.




Biodegradation in water and sediment: simulation tests.003








Administrative data

Purpose flag:
key study
Study result type:
experimental result
Reliability:
2 (reliable with restrictions)

Data source

Reference
Reference Type:
other company data
Title:
Unnamed
Year:
2007

Materials and methods

Principles of method if other than guideline:
Testing was performed in the disinfection basin of a conventional activated sludge plant. The chlorine dioxide demand of wastewater entering the basin was measured daily during the study. Chlorine dioxide was produced on site starting from sodium chlorite 25 % w/w solution and hydrochloric acid 33 % with a new concept generator at a production capacity in the range 2000-5000 g/h: the chlorine dioxide production was linked to the water to be treated flow rate to maintain the desired dosage (0.9-1.1 mg/L). Disinfected wastewater was collected at the end of the basin and analysed for residual chlorine dioxide and disinfection by-products.
GLP compliance:
no data

Test materials

Identity of test material same as for substance defined in section 1 (if not read-across):
yes
Test material identityopen allclose all
Details on test material:
Purity: > 97 %
Radiolabelling:
no

Study design

Oxygen conditions:
aerobic/anaerobic
Inoculum or test system:
other: Municipal waste water
Duration of test (contact time):
ca. 18 min
Initial test substance concentration
Initial conc.:
0.9 - 1.1 mg/L
Based on:
test mat.
Parameter followed for biodegradation estimation
Parameter followed for biodegradation estimation:
Test mat. analysis
Details on study design:
Chlorine dioxide was dosed through a diffuser into the wastewater from a conventional activated sludge plant at the entrance to the disinfection basin.
The disinfected water was sampled at the exit of the disinfection basin in clean and sterilized glass bottles: for microbiological analyses sodium thiosulphate was added to destroy any possible chlorine dioxide residue. Many analyses were carried out directly in the plant laboratory. The disinfectant residue was determined immediately after the sampling. All the analyses were, at any rate performed within 24 hours, adopting, for the different parameters, all the procedures required by the analytical methods in terms of sample stabilization.
Each day during the trial water was sampled at the entrance of the disinfection basin and chlorine dioxide demands were performed during the period 12 April – 4 May. The residual chlorine dioxide was determined according to the CPR method (Chlorophenol red method – UNICHIM method.77; I.J.Fletcher, P.Hemmings, Determination of chlorine dioxide in potable water using Chlorophenol red”, Analyst, 1985) dosing 8 mg/L of chlorine dioxide from a stock pure chlorine dioxide 1025 mg/L (prepared in lab according to Standard Methods for the examination of water and wastewater,19th ED, 1995, met. 4500-ClO2 B- Iodometric Method). The residual chlorine dioxide was checked at 15, 30, 45 and 60 minutes and the chlorine dioxide demand calculated.
Reference substance
Reference substance:
not required

Results and discussion

Material (mass) balance

% Degradation of test substance
% Degr.:
100
Parameter:
Test mat. analysis
Sampling time:
18 min
Remarks:
No residual chlorine dioxide was detected at the exit of the disinfection basin on any of the test days.
Transformation products:
yes
Details on results:
No residual chlorine dioxide was detected at the exit of the disinfection basin on any of the test days.
The chlorine dioxide demand of water entering the disinfection basin varied between 4.4 and 7.1 mg/L during the study.
Any other information on results incl. tables:
Table A7_1_2_2_1-2:        Chlorine dioxide demand vs. Time, pH : 6,5-7, temperature 18-21 °C
Time

CHLORINE DIOXIDE DEMAND
  

measure unit
12-April
13-April
19-April
28-April
4 May
15 min
mg/L
4,4
4,7
4,6
4,85
6,18
30 min
mg/L
5,4
5,15
5,2
5,68
6,8
45 min
mg/L
5,9
5,6
5,5
5,79
7
60 min
mg/L
5,95
6
5,75
5,98
7,1
Table A7_1_2_2_1-3:        Chemical and microbiological data of the water after the chlorine dioxide disinfection
Date

12-apr
13-apr
19-apr
19-apr
28-apr
04-may
Sampling time

16,20
10,30
11,30
14,30
11,30
10,30
Chlorine dioxide dosage
0,9
1,0
1,0
1,1
1,0
1,1
pH

6,5
6,5
6,75
6,45
6,5
6,93
Redox potential
mV
298
320
195
200
339
260
conductivity
mS/cm
1275
1200
1026
1056
987
1283
oxygen
mg/L
4
4,3
3,7
3,5
4,6
3
colour
Pt/Co
53
45
47
49
27
83
turbidity
NTU
2
1,9
2
2,1
2,3
3,5
Chlorine dioxide residue
mg/l
nr
nr
nr
nr
nr
nr
Active chlorine
mg/L
0,04
0,05
0,03
0,02
0,02
0,03
COD
mg/L
18
20
25
29
8
25
TOC
mg/L
13
11,5


11
12,5
DOC
mg/L
11,5
11


10,6
12
UV 254 nm
Abs/cm
0,217
0,19
0,212
0,212
0,226
0,187
DUV 254 nm
Abs/cm
0,193
0,178
0,204
0,196
0,215
0,168
fluoride
mg/L
0,15
0,14
0,13
0,16
0,12
0,15
chlorite
mg/L
0,52
0,59
0,56
0,59
0,53
0,54
chloride
mg/L
121
110
103
102
95,2
112,5
nitrite
mg/L
0,13
0,14
0,19
0,12
0,34
0,59
bromide
mg/L
0,17
0,13
0,1
0,11
0,12
0,11
chlorate
mg/L
0,07
0,03
0,07
0,07
0,03
0,05
nitrate
mg/L
18,3
12,8
18,5
22,9
19,7
3,75
sulphate
mg/L
107
110
96
96
90,1
109,8
sodium
mg/L
108
109
91
93,6

101,5
ammonia
mg/L
9,9
14,4
6
6

17,2
potassium
mg/L
16,6
16,7
12,9
12,9

15,7
magnesium
mg/L
18,2
18,4
15,6
15,7

16,6
calcium
mg/L
101
99,4
84
85,5

91
TTHMs
mg/L
1,2
1,2
0,7
1
1,1
1,4
CHCl3
mg/L
1,2
1,2
0,7
1
1,1
1,4
CHCl2Br
mg/L
n.r.
n.r.
n.r.
n.r.
n.r.
n.r.
CHBr2Cl
mg/L
n.r.
n.r.
n.r.
n.r.
n.r.
n.r.
CHbr3
mg/L
n.r.
n.r.
n.r.
n.r.
n.r.
n.r.
Esch. coli
cfu/100 mL
120
400
20
23
50
150
Coli. tot
cfu/100 mL
1,6*10^3
1,8*10^4
4*10^3
4*10^3
7,6*10^2
3,5*10^3
Salmonella spp
nd
nd
Nd
nd
nd
Nd
Acute toxicity
Bioluminescent
 bacteria

No tox
No tox
No tox
No tox
No tox
No tox
nr = not detectable

Biodegradation in water and sediment: simulation tests.004










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