Tall oil, sodium salt

Boiling point

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

weight of evidence

Study period:

2010-09-09 to 2010-11-11

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

ASTM E537-86

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

> 673 K

Atm. press.:

102.1 kPa

Decomposition:

yes

Remarks:

Loss of volatiles (probably water) was noticed at approximately 100°C

Decomp. temp.:

ca. 100 °C

Key result

Boiling pt.:

> 400 °C

Atm. press.:

102.1 kPa

Decomposition:

yes

Remarks:

Loss of volatiles (probably water) was noticed at approximately 100°C

Decomp. temp.:

ca. 100 °C

Screening test:

Thermograms for Determinations 1 and 2 are in Tables 3 and 4. The thermograms are shown in figures 1 and 2 attached.

Table 3: Thermographic Data – Determination 1

Thermal Event	Interpretation	Temperature
		°C	K
Onset of endotherm	Extrapolated onset of loss of volatiles	102	375

Atmospheric pressure: 101.27 kPa

Table 4: Thermographic Data – Determination 2

Thermal Event	Interpretation	Temperature
		°C	K
Onset of endotherm	Extrapolated onset of loss of volatiles	105	378

A significant endotherm event at approximately 100°C which was investigated by isolating the main body of the test item from the test liquor. DSC determination was performed on the main body of the test item and the test liquor separately.

Definitive test:

Thermal analysis for Determination 3 is shown in Table 5 below. The thermograms for Determinations 1, 2 and 3 are shown in figures 3, 4 and 5 attached.

Table 5: Thermographic Data – Determination 1 and 2

Thermal Event	Interpretation	Temperature
		°C	K
Endotherm	Boiling temperature	101	374

Atmospheric pressure: 102.10 kPa

The boiling temperature of the test material was determined to be greater than 400°C (>673 K). The test item liquor boiling temperature was determined to be 374± 0.5 K.

Conclusions:

A boiling temperature of > 673 K (>400°C) at 102.10 kPa was determined for the substance in a study conducted according to OECD 103 and in compliance with GLP. The result is considered to be reliable.

Reference 2

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2010-10-01 to 2010-11-15

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

ASTM E537-86

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

> 673 K

Atm. press.:

101.42 kPa

Decomposition:

yes

Remarks:

Loss of volatiles (probably water) was noticed at approximately 100°C

Decomp. temp.:

ca. 100 °C

Key result

Boiling pt.:

> 400 °C

Atm. press.:

101.42 kPa

Decomposition:

yes

Remarks:

Loss of volatiles (probably water) was noticed at approximately 100°C

Decomp. temp.:

ca. 100 °C

Screening test:

The thermograms and thermographic data for screening test determinations 1, 2 and 3 are in Table 3 and figures 1 -3 attached.

Table 3: Thermographic data

Determination	Thermal event	Interpolation	Temperature		Atm. Pressure (kPa)
			°C	K
1	Onset of endotherm	Extrapolated onset of loss of volatiles	58.17	331	99.51
2	Onset of endotherm	Extrapolated onset of loss of volatiles	44.13	317
3	Onset of endotherm	Extrapolated onset of loss of volatiles	59.51	316	99.51

There was an evidence of loss of volatile fraction from the test item on heating for all determinations; however, significant residues also remained on completion, indicating the loss is only partial. The variability of the onset temperature can be attributed to the essentially open system used in the screening test determinations i.e manually pierced crucibles, which may allow premature evaporation of volatiles on heating. Such step was essential to allow free atmospheric exchange during investigation under nitrogen atmosphere as required to distinguish between thermal and oxidative processes during preliminary screening. For the definitive test, two significant changes were made to the analytical conditions. The first was a change to pre-perforated crucible lids. These laser drilled lids eliminate premature elimination, and test item vapour leaves the crucible only when the internal pressure rises exponentially at the true boiling temperature of a substance. The second change to the analytical conditions was an acceleration in the heating rate to 20°C/minute which is also to minimise any impact of premature evaporation.

Definitive test:

The analysis of the isolated liquor from the test item resulted in the loss of a volatile fraction from approximately 373 K (100°C). Increase of the onset temperature with respect to those observed during the screening tests was as expected following the changes to the experimental procedure to eliminate premature evaporation. The significant amount of residue remaining on completion of this analysis, indicated that the fraction lost may have been a minority, with further components present in the liquor having a boiling temperature >400°C (>673K).

On analysis of the homogenised test item, the apparent onset temperature increased, possibly due to the volatile substance identified in the isolated liquor which is now being present in a negligible proportion. The erratic baseline following the initial loss of the volatile substance was typical of decomposition processes, and in the case of determination 3, the test item was expelled from the crucible during heating which possibly resulted in the endotherm at approximately 150°C.

Thermal analysis for Determinations 1, 2 and 3 are shown in Table 4 below and figures 4 - 6 attached.

Table 4: Thermographic data for Determination

Determination	Thermal event	Interpolation	Temperature		Atm. Pressure (kPa)
			°C	K
1	Onset of endotherm	Extrapolated onset of loss of volatiles	99.64	373	101.42
2	Onset of endotherm	Extrapolated onset of loss of volatiles	99.78	372	101.42
3	Onset of endotherm	Extrapolated onset of loss of volatiles	98.86	372	101.42

The analysis of the isolated liquor from the test item resulted in the loss of a volatile fraction from approximately 373 K (100°C). Increase of this onset temperature with respect to those observed during the screening tests was as expected following the changes to the experimental procedure to eliminate premature evaporation. The significant remaining residue on completion of this analysis however indicated that the fraction lost may have been a minority, with further components present in the liquor have a boiling temperature >400°C (>673 K).

On analysis of the homogenised test item, the apparent onset temperature remained the same. Variability in the duplicate samples may have resulted from homogeneity issues with respect to the very small sample masses as required for DSC analysis, irrespective of the steps taken to homogenise the test item. The erratic baseline following the initial loss of this volatile substance was typical of decomposition processes and in the case of determination 2 and 3, the test item was expelled from the crucible during heating (possibly resulting in the significant endotherm at approximately 150°C).

To further aid the interpretation of the thermograms, a visual assessment of the homogenised test item on heating was attempted. Aliquots was taken in a test tube and heated in an oil bath. However, at a temperature of 98°C (371 K), the test item expanded as a foam. The test was aborted to prevent loss of the test item from the test tube.

Overall, the homogenised test item lost a volatile fraction from approximately 372 K (99°C) at 101.42 kPa, with decomposition of of the test item believed to occur as heating continued. However, in all cases, the loss of the volatile item was limited and a significant residue with a boiling temperature >673 K (>400°C) was retained in the crucibles on completion of each determination. Where the test item liquor is isolated and/or present at a higher concentration, the onset temperature may be reduced, with a value of 373 K (100°C) being obtained for isolated liquor on analysis.

Conclusions:

A boiling temperature of > 673 K (>400°C) at 101.4 kPa was determined for the substance in a study conducted according to OECD 103 and in compliance with GLP. The result is considered to be reliable.

Reference 3

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

weight of evidence

Study period:

2010-10-01 to 2010-11-12

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

ASTM E537-86

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

> 673 K

Atm. press.:

101.8 kPa

Decomposition:

yes

Remarks:

Loss of volatiles (probably water) was noticed at approximately 100°C

Decomp. temp.:

ca. 100 °C

Key result

Boiling pt.:

> 400 °C

Atm. press.:

101.8 kPa

Decomposition:

yes

Remarks:

Loss of volatiles (probably water) was noticed at approximately 100°C

Decomp. temp.:

ca. 100 °C

Screening test:

Thermograms and thermographic data for the screening test determinations 1, 2 and 3 are in the table below and figures 1 -3 attached.

Table 3: Thermographic data

Determination	Thermal event	Interpolation	Temperature		Atm. Pressure (kPa)
			°C	K
1	Onset of endotherm	Extrapolated onset of loss of volatiles	57.26	330	99.63
2	Onset of endotherm	Extrapolated onset of loss of volatiles	33.27	306
3	Onset of endotherm	Extrapolated onset of loss of volatiles	42.55	316	100.01

There was an evidence of loss of volatile fraction from the test item on heating for all determinations; however, significant residues also remained on completion, indicating the loss is only partial. The variability of the onset temperature can be attributed to the essentially open system used in the screening test determinations i.e manually pierced crucibles, which may allow premature evaporation of volatiles on heating. Such step was essential to allow free atmospheric exchange during investigation under nitrogen atmosphere as required to distinguish between thermal and oxidative processes during preliminary screening. For the definitive test, two significant changes were made to the analytical conditions. The first was a change to pre-perforated crucible lids. These laser drilled lids eliminate premature elimination, and test item vapour leaves the crucible only when the internal pressure rises exponentially at the true boiling temperature of a substance. The second change to the analytical conditions was an acceleration in the heating rate to 20°C/minute which is also to minimise any impact of premature evaporation.

Definitive test:

Thermograms and thermographic data for definitive test determinations 1, 2 and 3 are shown in the table below and in figures 4-6 attached.

Table 4: Thermographic data for Determination

Determination	Thermal event	Interpolation	Temperature		Atm. Pressure (kPa)
			°C	K
1	Onset of endotherm	Extrapolated onset of loss of volatiles	92.02	365	101.81
2	Onset of endotherm	Extrapolated onset of loss of volatiles	99.78	373	101.81
3	Onset of endotherm	Extrapolated onset of loss of volatiles	103.04	376	101.81

The analysis of the isolated liquor from the test item resulted in the loss of a volatile fraction from approximately 365 K (92°C). Increase of the onset temperature with respect to those observed during the screening tests was as expected following the changes to the experimental procedure to eliminate premature evaporation. The significant amount of residue remaining on completion of this analysis, indicated that the fraction lost may have been a minority, with further components present in the liquor having a boiling temperature >400 C (>673K).

On analysis of the homogenised test item, the apparent onset temperature increased, possibly due to the volatile substance identified in the isolated liquor which is now being present in a negligible proportion. The erratic baseline following the initial loss of the volatile substance was typical of decomposition processes, and in the case of determination 3, the test item was expelled from the crucible during heating which possibly resulted in the endotherm at approximately 160 C.

To further aid the interpretation of the thermograms, a visual assessment of the homogenised test item on heating was attempted. An aliquots was taken in a test tube and heated in an oil bath. However, at a temperature of 105°C (378K), the test item expanded as a foam. The test was aborted to prevent loss of the test item from the test tube.

Overall, the homogenised test item lost a volatile fraction from approximately 373 K at 101.81 kPa, with decomposition of the test item believed to occur as heating continued. However, in all cases, the loss of the volatile item was limited and a significant residue with a boiling temperature >673 K (>400°C) was retained in the crucibles on completion of each determination. Where the test item liquor is isolated and/or present at a higher concentration, the onset temperature may be reduced, with a value of 365 being obtained for isolated liquor on analysis.

 

Conclusions:

A boiling temperature of > 673 K (>400°C) at 101.8 kPa was determined for the substance in a study conducted according to OECD 103 and in compliance with GLP. The result is considered to be reliable.

Description of key information

Boiling Point: >673 ± 0.5 K at 101.4 - 102.1 kPa (OECD 103)

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

673 K

Additional information

Three reliable boiling point studies have been determined on three samples of the registered substance. Boiling point value of >673 K (>400°C) at 101.4 - 102.1 kPa was obtained for the substance in all three studies conducted using differential scanning calorimetry in accordance with OECD Test Guideline 103 and in compliance with GLP. During the studies, loss of volatile fractions from approximately 373 K (100°C) was observed as heating continued. However, in all cases, the loss of volatile item was limited and a significant residue with boiling temperature of >673 K was retained in the crucibles. The results are considered to be reliable and are used as weight of evidence.