29H,31H-phthalocyanine

Biodegradation in water: screening tests

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

biodegradation in water: ready biodegradability

Type of information:

experimental study

Adequacy of study:

supporting study

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Remarks:

Data from reliable source. Though no detailed test report is available, all tests from the Japanese Authorities are performed according to an OECD guideline and GLP.

Qualifier:

according to guideline

Guideline:

OECD Guideline 301 C (Ready Biodegradability: Modified MITI Test (I))

GLP compliance:

no

Specific details on test material used for the study:

- Name of test material (as cited in study report): C.I. Pigment Blue 15
Purity: 99.3 %

Oxygen conditions:

aerobic

Inoculum or test system:

mixture of sewage, soil and natural water

Details on inoculum:

- Source of inoculum/activated sludge (e.g. location, sampling depth, contamination history, procedure): In March, June, September, and December, sludge was sampled at the following 10 places in Japan: 1. Fukogawa city sewage plant, 2. Fukashiba industry sewage plant, 3. Nakahama city sewage plant, 4. Ochiai city sewage plant, 5. Kitakami river, 6. Shinano river, 7. Yoshino river, 8. Lake Biwa, 9. Hiroshima bay, 10. Dookai bay; sampling: 1. City sewage: Returned sludge from sewage plants was taken. 2. Rivers, lake and sea: Surface water and surface soil which were in contact with atmosphere were collected.
- Method of cultivation: About 30 minutes after ceasing aeration to the sludge mixture, supernatant corresponding to about 1/3 of the whole volume was removed. Then the equal volume of dechlorinated water was added to the remaining portion and aerated again, followed by addition of synthetic sewage at a concentration of 0.1% (w/v). This procedure was repeated once every day. The culturing was carried out at 25 ± 2 °C. 5 L of the filtrate of the supernatant of old activated sludge was mixed with 500 mL of the filtrate of the supernatant of new sludge and cultured at pH 7.0 ± 1.0 under sufficient aeration using prefiltered open air. During the cultivation, appearance of the supernatant, precipitability, formation of flock, pH, dissolved oxygen concentration in the solution and temperature were checked and necessary adjustments were made, Microflora in the activated sludge was microscopically observed and sludge with no abnormal symptom was used for the test.
- Concentration of sludge: 30 mg/L

Duration of test (contact time):

14 d

Initial conc.:

100 mg/L

Based on:

test mat.

Parameter followed for biodegradation estimation:

O2 consumption

Details on study design:

TEST CONDITIONS
- Composition of medium: 3 mL each of four stock solutions, as described in JIS K 0102-1986-21, are diluted to 1000 mL with purified water
- pH: 7.0
- pH adjusted: yes
- Suspended solids concentration: determined according to Method Japanese Industrial Standards (JIS) K 0102-1986-14.1

TEST SYSTEM
- Culturing apparatus: Closed system oxygen consumption measuring apparatus (Coulometer: Ohkura Electric Co., Ltd.); 300 mL vessel, absorbent for evolving carbon dioxide Soda lime No .l (extra pure reagent, Wako Pure Chemical Industries, Ltd.).
- Number of culture flasks/concentration: 1
- Measuring equipment: Coulometer, Okhura Electric Co., Ltd.
- Test performed in open system: no
- Details of trap for CO2 and volatile organics if used: soda lime, extra pure, Wako Pure Chemical Industries, Ltd.)

CONTROL AND BLANK SYSTEM
- Inoculum blank: yes
- Abiotic sterile control: yes
- Toxicity control: no

Reference substance:

aniline

Parameter:

% degradation (O2 consumption)

Value:

0

Sampling time:

14 d

Results with reference substance:

71% biodegradation, based on O2 consumption at the day 7

Validity criteria fulfilled:

yes

Interpretation of results:

under test conditions no biodegradation observed

Reference 2

Endpoint:

biodegradation in water: ready biodegradability

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 301 F (Ready Biodegradability: Manometric Respirometry Test)

Principles of method if other than guideline:

Test procedures according to EU Directive 79/831/EEC Annex V, part C: Methods for the Determination of the ecotoxicity degradation - biodegradation, Manometric respirometry test. This method is comparable to the OECD guideline 301 F.

GLP compliance:

no

Specific details on test material used for the study:

- Name of test material (as cited in study report): Kupferphthalocyanin
- Analytical purity: 99.3 %

Oxygen conditions:

aerobic

Inoculum or test system:

activated sludge, domestic (adaptation not specified)

Details on inoculum:

- Source of inoculum/activated sludge (e.g. location, sampling depth, contamination history, procedure): Municipal activated sludge from laboratory wastewater treatment plant fed with municipal sewage and synthetic wastewater
- final dry solids concentration: 30 mg/l
- Laboratory culture: yes

Duration of test (contact time):

28 d

Initial conc.:

107 mg/L

Based on:

test mat.

Parameter followed for biodegradation estimation:

O2 consumption

Details on study design:

TEST CONDITIONS
- pH: at the end 7 - 7.5
- pH adjusted: no
- CEC (meq/100 g):


SAMPLING
- Sampling frequency: daily


CONTROL AND BLANK SYSTEM
- Inoculum blank: yes
- Abiotic sterile control: yes
- Toxicity control: yes

Reference substance:

aniline

Key result

Parameter:

% degradation (O2 consumption)

Value:

< 1

Sampling time:

28 d

Results with reference substance:

> 80% biodegradation, based on THSB

	BW1	BW2	KS	IH	PS1	PS2	PS3	PS4	PS5	PS6	PS7	PS8
Water(mL)	240	240	230	230	240	240	240	240	240	240	240	240
Testsubstance(mg)	0	0	0	26	29	29	28	29	25	25	25	25
Refernecesubstance(mL)	0	0	10	10	0	0	0	0	0	0	0	0
Inoculum(mL)	10	10	10	10	10	10	10	10	10	10	10	10
Volume (mL)	250	250	250	250	250	250	250	250	250	250	250	250
O2 Consumption (%)	-	-	2.7	-1	-4	-4	-4	-4	-1	0	-3	-2

 

BW: Biotic control

KS: Reference substance control

IH: Reference substance + Test substacne control

PS: Test substance replicate

Validity criteria fulfilled:

yes

Interpretation of results:

under test conditions no biodegradation observed

Reference 3

Endpoint:

biodegradation in water: ready biodegradability

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 2003-02-10 to 2003-04-09

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Remarks:

Data from reliable source. Though no detailed test report is available, all tests from the Japanese Authorities are performed according to an OECD guideline and GLP incl. analytics.

Qualifier:

according to guideline

Guideline:

OECD Guideline 301 C (Ready Biodegradability: Modified MITI Test (I))

GLP compliance:

yes (incl. QA statement)

Specific details on test material used for the study:

- Name of test material (as cited in study report): K-1680
- Lot/batch No.: DLM9599
- Stability under test conditions: stable as confirmed by infrared spectrum
- Storage condition of test material: stored in dark and cool place

Oxygen conditions:

aerobic

Inoculum or test system:

activated sludge, non-adapted

Details on inoculum:

- Source of inoculum/activated sludge : Sludges were sampled from 10 sites including sewage plant, river, lake and sea in Japan. Filtrates of sludge samples collected at above sites were mixed together. This mixture of filtrates (5L) was mixed with filtrate of the old sludge (5L) to make a new sludge suspension (10L). This suspension was adjusted to pH of 7.0±1.0 and aerated.
- Method of cultivation: After stopping the aeration of the incubation tank to let the sludge settle for approximately 30 minutes, about 1/3 of the supernatant was replaced by equal amount of dechlorinated water before resuming aeration. After more than 30 minutes of aeration, synthetic sewage water was added to make the concentration in renewed supernatant to be 0.1%. This procedure was repeated daily to prepare the activated sludge culture. The incubation temperature was 25±2 °C.
- Storage conditions: Appearance of the supernatant and formation of the activated sludge was observed, and precipitability, pH, temperature and dissolved oxygen concentration of the activated sludge were recorded. Activated sludge used for the test was observed under an optical microscope as appropriate to confirm that no abnormalities were found in biota.
- Concentration of sludge: Concentraion of suspended sludge was 4900 mg/L.

Duration of test (contact time):

28 d

Initial conc.:

100 mg/L

Based on:

test mat.

Parameter followed for biodegradation estimation:

O2 consumption

Remarks:

BOD

Parameter followed for biodegradation estimation:

test mat. analysis

Details on study design:

TEST CONDITIONS
- Composition of medium: A, B, C and D solutions were composed according to Japanese standard testing method for industrial waste water, biochemical oxygen demand (JIS K 0102-1998-21). Basal medium was prepared by mixing 3mL portions of these solutions and puridied water (Takasugi Pharmaceutical Co., Ltd. The japanese Pharmacopeia) to make a total of 1L. The pH was adujusted to 7.0.
- Test temperature: 25±1°C
- Suspended solids concentration: 30mg/L


TEST SYSTEM
- Culturing apparatus: 300mL glass bottle
- Number of culture flasks/concentration: 3 bottles (activated sludge + test substance)
- Method used to create aerobic conditions: stirring by magnetic stirrer
- Measuring equipment: coulometer
- Details of trap for CO2 and volatile organics if used: soda lime


CONTROL AND BLANK SYSTEM
- Inoculum blank: activated sludge + basal medium
- Abiotic sterile control: test substance + purified water
- Other ( activity control): aniline + activated sludge + basal medium

Reference substance:

aniline

Test performance:

The degree of degrafability based on BOD measurement of aniline were 57% (day 7) and 72% (day 14).

Key result

Parameter:

% degradation (O2 consumption)

Value:

5

Sampling time:

28 d

Remarks on result:

other: BOD

Key result

Parameter:

% degradation (test mat. analysis)

Value:

0

Sampling time:

28 d

Remarks on result:

other: gravimetric analysis

Validity criteria fulfilled:

yes

Interpretation of results:

not readily biodegradable

Description of key information

The substance is not readily biodegradable.

Key value for chemical safety assessment

Biodegradation in water:

not biodegradable

Type of water:

freshwater

Additional information

All substances in the category are inert, insoluble in water and octanol, and unreactive. They do not interact with proteins, have a high molecular weight and are insoluble. Thus, they will not be able to penetrate biological membranes. Therefore, the ready biodegradability of these substances is expected to be the same regardless of the slight structural differences between substances. The available experimental data can be used for read-across to all substances in this category. Ready biodegradability studies are available for the following two substances in the category: CAS 147-14-8 and CAS 12239-87-1.

A study on etrabenzo-5,10,15,20-diazaporphyrinephthalocyanine (CAS 147-14-8) was conducted similar to OECD guideline 301F (Manometric respirometry test). This study used domestic activated sludge as inoculum and was exposed to 107 mg/L test substance. Less than 1% of the substance was degraded after 28 d based on O2 consumption (BASF AG 1988, K2). Therefore, it is concluded that the substance is not readily biodegradable. The conclusion is supported by a GLP study conducted according to OECD test guideline 301C (NITE 1992, K2). A mixture of sewage, soil and natural water was used as inoculum and exposed to 100 mg/L test substance. No degradation was observed in the test condition after 14 d based on O2 consumption. Additionally, a GLP study conducted according to OECD TG 301C is available for the test substance CAS 12239-87-1. This study used non-adapted activated sludge as inoculum and was exposed to 100 mg/L test substance. After 28 days of exposure, 5% of the test substance was degraded based BOD analysis. No degradation of the test substance was observed based on gravimetric analysis (NITE 2003, K1). Therefore, it is concluded that the test substance CAS 12239-87-1 is not readily biodegradable.

Based on the results, it is concluded that all substances in the category are not readily biodegradable.