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Water solubility

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Reference
Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
04 April - 11 December 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.6 (Water Solubility)
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 105 (Water Solubility)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7840 (Water Solubility)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
flask method
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Source: Provided by the Sponsor
- Batch No.of test material: AN-0400-113
- Expiration date of the lot/batch: 01 January 2019
- Purity: 100%

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: Frozen at approximately -20 °C, under nitrogen, in the dark
Key result
Water solubility:
ca. 0 g/L
Temp.:
20 °C
Remarks on result:
other: Limit of detection
Remarks:
2.0 x 10^-6 g/L

Preliminary test: estimate = 4.97 x 10^-7 g/L at 25°C

Validation

The linearity of the detector response regarding concentration was assessed over th the concentration range: 5.22 x 10^-2 - 10.4 mg/L.

The results were satisfactory with a first order correlation coefficient (r) of 0.999 being obtained.

Recovery of analysis of the sample procedure was assessed at a fortification level of nominally 0.05 mg/L and proved adequate for the test. Concentrations were not corrected for recovery of analysis (Figure 3).

Chromatographic review of the analysis of the flask method showed a broad multiplet peak n all the samples at the approximate retention times expected for the test material. This was seen to correlate with increasing shaking time from Samples 1 -6 and was thought to be due to oxidation of the test material. GC-MS spectral analysis of Sample 6 (Figure 4) was used to obtain a spectrum of this species, which showed a significant broad multiplet from approximately 5.6 -7.5 minutes. The complex spectrum produced has fragments with mass/charge (m/z) ratios of 318, 302, 287, 271, 257, 243 and many others.

Conclusions:
The water solubility of the test substance, Terpenes and Terpenoids, turpentine-oil, limonene fraction, polymers with 1-methyl-4-(1-methylethenyl)cyclohexene and turpentine-oil β-pinene fraction terpenes, was determined to <4 x10^-6 g/L of solution at a temperature of 20.0°C ± 0.5C.
Executive summary:

The water solubility of the test substane, Terpenes and Terpenoids, turpentine-oil, limonene fraction, polymers with 1 -methyl-4 -(1 -methylethenyl)cyclohexene and turpentine oil β-pinene fraction terpenes, was determined via the flask method in a process compatible with Method A6 Water Solubility of Commission Regulation (EC) No. 440/2008 (30 May 2008), Method 105 of the OECD Guidelines for Testing of Chemicals (27 July 1995) and Method 830.7840 of the OCSPP Guidelines (March 1998).

In preliminary test, the water solubility of the test material was estimated by specialised software WSKOW. The water solubility was initially carried out via the slow stir procedure, where samples were taken after an equilibration period of at least 30 days. A significant erroneous peak was seen in the chromatography of all the samples at the same retention time as the test substance, therefore it was considered that the test substance may have oxidised during testing. The test was subsequently performed via the flask method with slow shaking (100 rpm) for six days. Mixtures of test material and purified water were added to six separate flasks and then the test material was carefully added to the sufrace of the purified water and the headspace was purged with nitrogen. Once the equilibration period was completed, the samples were clear and colourless with excess test substance present on the surface. The solutions were sampled, whilst avoiding excess test substance prior to filitration through a 0.2 µm Nylon filter. The filtrates were also clear and colourless with no Tyndall beam effect. An instrument response was seen in the solvent blank (hexane) and sample matrix blank (procedural blank) at the approximate retention time of the test substance. The solvent blank response was included in the calibration as a zero concentration point and sample concentrations were corrected for concentration relating to the sample matrix blank. The concentration of the test material in the sample solutions was determined via gas chromatography-mass spectrometry.

The test material produced a spectrum with signficant fragments with a m/z 272, 229 and 119, which were present but not predominant in the mass spectrum of the multiplet. It is therefore thought that these species may have formed during testing via oxidation. The limit of detection was determined to be 2.0 x10^-6 g/L and the water solubility of the test substance was determined to 4 x10^-6 g/L over the concentration range 4.92 x10^-7 - 3.6 x 10^-6 g/L at a temperature of 20.0°C.

Description of key information

The water solubility of the test substane, Terpenes and Terpenoids, turpentine-oil, limonene fraction, polymers with 1 -methyl-4 -(1 -methylethenyl)cyclohexene and turpentine oilβ-pinene fraction terpenes, was determined via the flask method in a process compatible with Method A6 Water Solubility of Commission Regulation (EC) No. 440/2008 (30 May 2008), Method 105 of the OECD Guidelines for Testing of Chemicals (27 July 1995) and Method 830.7840 of the OCSPP Guidelines (March 1998).

In preliminary test, the water solubility of the test material was estimated by specialised software WSKOW. The water solubility was initially carried out via the slow stir procedure, where samples were taken after an equilibration period of at least 30 days. A significant erroneous peak was seen in the chromatography of all the samples at the same retention time as the test substance, therefore it was considered that the test substance may have oxidised during testing. The test was subsequently performed via the flask method with slow shaking (100 rpm) for six days. Mixtures of test material and purified water were added to six separate flasks and then the test material was carefully added to the sufrace of the purified water and the headspace was purged with nitrogen. Once the equilibration period was completed, the samples were clear and colourless with excess test substance present on the surface. The solutions were sampled, whilst avoiding excess test substance prior to filitration through a 0.2 µm Nylon filter. The filtrates were also clear and colourless with no Tyndall beam effect. An instrument response was seen in the solvent blank (hexane) and sample matrix blank (procedural blank) at the approximate retention time of the test substance. The solvent blank response was included in the calibration as a zero concentration point and sample concentrations were corrected for concentration relating to the sample matrix blank. The concentration of the test material in the sample solutions was determined via gas chromatography-mass spectrometry.

The test material produced a spectrum with signficant fragments with a m/z 272, 229 and 119, which were present but not predominant in the mass spectrum of the multiplet. It is therefore thought that these species may have formed during testing via oxidation. The limit of detection was determined to be 2.0 x10^-6 g/L and the water solubility of the test substance was determined to 4 x10^-6 g/L over the concentration range 4.92 x10^-7 - 3.6 x 10^-6 g/L at a temperature of 20.0°C.

Key value for chemical safety assessment

Water solubility:
0.004 mg/L
at the temperature of:
20 °C

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