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Physical & Chemical properties

Water solubility

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Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 105 (Water Solubility)
Deviations:
yes
Remarks:
Standard water pH 8 ISO 6341 OECD TGD 29
GLP compliance:
yes (incl. QA statement)
Type of method:
flask method
Water solubility:
<= 1 µg/L
Temp.:
20 °C
pH:
8

Fe </= 1 µg/L at 1 and 10 g triiron tetraoxide/L

Conclusions:
Interpretation of results (migrated information): insoluble (< 0.1 mg/L)
A very low water solubility was determined according to OECD Guideline 105. With a loading of 10 g triiron tetraoxide to water at pH 8 the dissolved iron was determined to be <1µg/L. With a loading of 1 g triiron tetraoxide to water at pH 8 the dissolved iron was determined to be 1 µg/L.
Executive summary:

A very low water solubility was determined according to OECD Guideline 105. With a loading of 10 g triiron tetraoxide to water at pH 8 the dissolved iron was determined to be <1 µg/L and at a loading of 1 g triiron tetraoxide to water at pH 8 the dissolved iron was determined to be

1 µg/L.

For the determination six test mixtures with two different loading concentrations (1 g/L and 10 g/L) were agitated with a magnetic stirrer for 24 hours at 20 °C. The received suspensions were filtrated through a 0.1 μm (100 nm) membrane filter. Also three blank solutions (standard water pH 8 to ISO 6341, OECD-Guidance-Document 29) were investigated. To determine the dissolved iron in water the amount of total iron was determined employing the graphite furnace atomic absorption spectrometry method. As iron is insoluble in water, in deviation to the guidelines a different procedure for the water solubility test was chosen. Also three blank solutions (standard water pH 8 to ISO 6341, OECD-Guidance-Document 29) were investigated.

Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2018-03-19 to 2018-06-15
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 105 (Water Solubility)
Deviations:
yes
Remarks:
Please refer to "Principles of method if other than guideline"
Qualifier:
according to guideline
Guideline:
EU Method A.6 (Water Solubility)
Version / remarks:
2008
Principles of method if other than guideline:
The water solubility of triiron tetraoxide was assessed according to the OECD-Guideline for Testing of Chemicals No. 105, Water Solubility (flask method) with the following modifications:
- Two vessels were set up in a parallel design at 20.0 ± 1.0 °C, each vessel was sampled several times instead of sampling one single vessel at each point in time
- The study was performed under exclusion of atmospheric oxygen and carbon dioxide under inert gas (argon)
GLP compliance:
yes (incl. QA statement)
Remarks:
signed 2016-05-31
Type of method:
flask method
Key result
Water solubility:
1.52 µg/L
Conc. based on:
test mat. (dissolved fraction)
Loading of aqueous phase:
200 mg/L
Incubation duration:
>= 1 - <= 25 d
Temp.:
20 °C
pH:
>= 6.1 - <= 7.1
Remarks on result:
other:
Remarks:
Filtration through a 0.2 µm membrane and centrifugal filtration (3kDa), Mean of Vessel 1 and 2
Water solubility:
1.1 µg/L
Conc. based on:
element (dissolved fraction)
Loading of aqueous phase:
200 mg/L
Incubation duration:
>= 1 - <= 25 d
Temp.:
20 °C
pH:
>= 6.1 - <= 7.1
Remarks on result:
other:
Remarks:
Filtration through a 0.2 µm membrane and centrifugal filtration (3kDa), Mean of Vessel 1 and 2
Water solubility:
83.1 µg/L
Conc. based on:
test mat.
Remarks:
dissolved and dispersed < 0.2 µm
Loading of aqueous phase:
200 mg/L
Incubation duration:
>= 1 - <= 25 d
Temp.:
20 °C
pH:
>= 6.1 - <= 7.1
Remarks on result:
other:
Remarks:
Filtration through a 0.2 µm membrane, Mean of Vessel 1 and 2
Water solubility:
59.8 µg/L
Conc. based on:
element
Remarks:
dissolved and dispersed < 0.2 µm
Loading of aqueous phase:
200 mg/L
Incubation duration:
>= 1 - <= 25 d
Temp.:
20 °C
pH:
>= 6.1 - <= 7.1
Remarks on result:
other:
Remarks:
Filtration through a 0.2 µm membrane, Mean of Vessel 1 and 2
Details on results:
The iron concentrations of solutions containing Ferroxide Black 86 in the samples filtered through a 0.2 µm membrane and centrifugally filter did not appear to increase during the test. Thus, the overall mean iron concentration during the test was calculated based on iron concentrations from day 1 to day 25, in the dissolved phase (filtered through a 0.2 µm filter and centrifugally filtered samples) with 1.10 ± 0.02 µg Fe/L, corresponding to 1.52 ± 0.02 µg/L triiron tetraoxide (Ferroxide Black 86).

Observations

During the study, the respective test items were homogenously distributed in solution. After sampling and filtering, the samples were clear.

 

Temperature

The mean temperature was 20.6 ± 0.4 °C.

 

Oxygen concentrations

The oxygen concentration was measured over the period of sampling time inside the acrylic glass box with anMicro IC oxygen sensor (Gfg, Dortmund, Germany). No oxygen was measurable.

pH measurements

Table 1: pH of solutions containing the test item and method blanks

 

Test item/sample

Solution pH (min-max)

1d,2dand3d

8dand9d

23d,24d and25d

MethodBlanks

5.76.0

5.96.2

5.75.9

FerroxideBlack86

7.58.5

7.28.0

6.37.0

Turbidity measurement

The turbidity of filtered samples from day 1, 2 and 3 was immediately measured after filtering (centrifugal filtration) with a TURB 550 IR (WTW, Weilheim, Germany) to confirm that measured iron concentrations correspond to the dissolved fraction.

The turbidity was below 0.02 NTU, indicating the absence of particles. Due to the limited volume of test solution, turbidity was measured only on day 1, 2 and 3.

Method validation summary (ICP-OES)

Limits of detection (LODs), limits of quantification (LOQs) and correlation coefficients (r)

Limits of detection (LOD) within all measurement series: < 0.938 µg Fe/ L.

Limits of quantification (LOQ) within all measurement series: < 2.81 µg Fe/ L.

Correlation coefficients (r) within all measurement series: >0.99993

Mean recoveries for certified reference materialTMDA-52.4 (concentration range 16.6 – 66.4 µg Fe/L, n=8): 98.4-100%

Mean recoveries for quality control standard (5 µg Fe/ L, n = 4): 99.4 %

Mean recoveries for internal standard (10 µg / L, n = 4): 97.7 %

Mean recovery of fortified samples (n = 20): 98.6 - 104 %

Conclusions:
Under the conditions of this test (flask method; loading of 200 mg/L), iron concentrations of solutions (filtered through 0.2 µm membrane and centrifugally filter) containing Ferroxide Black 86 did not appear to increase during the test, indicating solubility equilibrium. Mean dissolved Fe concentrations after filtration through a 0.2 µm membrane and centrifugal filtration were determined with 1.1 ± 0.02 µg Fe/L, corresponding to 1.52 ± 0.02 µg/L test item in solution.

Description of key information

A very low water solubility of triiron tetraoxide was determined according to OECD Guideline 105.


Iron concentrations of solutions of solutions containing a loading of 200mg/L containing Ferroxide Black 86 did not appear to increase during the test (25d), indicating solubility equilibrium. Mean dissolved Fe concentrations after filtration through a 0.2 µm membrane and centrifugal filtration were determined with 1.1 ± 0.02 µg Fe/L, corresponding to 1.52 ± 0.02 µg/L test item in solution.


With a loading of 10 g triiron tetraoxide to water at pH 8 the dissolved iron was determined to be <1µg/L. With a loading of 1 g triiron tetraoxide to water at pH 8 the dissolved iron was determined to be 1 µg/L.

Key value for chemical safety assessment

Water solubility:
1.52 µg/L

Additional information