Reaction product of Fatty acids, C18-unstaturated, dimer with 4,7,10-trioxa-1,13-tridecane-diamine

Water solubility

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

disregarded due to major methodological deficiencies

Reliability:

3 (not reliable)

Rationale for reliability incl. deficiencies:

unsuitable test system

Remarks:

Result was reported at the pH 2.5 and is not relevant to the environmental condition

Qualifier:

no guideline followed

GLP compliance:

no

Type of method:

other: No method described

Specific details on test material used for the study:

The test material was described as being in aqueous solution, but the concentration was not stated. A 1 wt % mixture of the material with distilled water had pH 2.5 ± 0.3.

Key result

Water solubility:

0.95 other: %

Temp.:

23 °C

pH:

2.5

Remarks on result:

other: pH was measured on a 1 wt % mixture of the material with distilled water using ColorpHast strips.

Details on results:

Solubility was reported as 0.95% at 23 °C and pH 2.5 ± 0.3. The same report later stated that the material is in aqueous solution with solubility in water of 100%. This is contridictory to the 0.95% reported. No detail was provided.

Conclusions:

A reported single value of water solubility of 0.95% at 23 °C and pH 2.5 was considered unreliable and disregarded.

Executive summary:

A single value of water solubility of 0.95% at 23 °C and pH 2.5 was reported. The same report later stated that the material is in aqueous solution with solubility in water of 100%, contradictory to the 0.95% reported. No detail was provided regarding to test method, sample preparation and analytical procedure. The validity and reliability of the result can not be verified. In addition, the result was reported at the pH 2.5 and is not relevant to the environmental condition. Therefore, this study was disregarded.

Reference 2

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

July 19, 2019 to November 23, 2019

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

GLP compliance:

yes

Type of method:

flask method

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: 4293484
- Expiration date of the lot/batch: 01Jan 2021

Key result

Water solubility:

31.01 other: mgC/L

Conc. based on:

other: TOC

Loading of aqueous phase:

50 mg/L

Incubation duration:

>= 5 - <= 7 d

pH:

>= 6.8 - <= 7

Remarks on result:

other: at room temperature

Key result

Water solubility:

49.95 other: mgC/L

Conc. based on:

other: TOC

Loading of aqueous phase:

100 mg/L

Incubation duration:

>= 5 - <= 7 d

pH:

>= 7.6 - <= 9.2

Remarks on result:

other: at room temperature

Table 1. Water solubility of MTDID 18990

		TOC (mgC/L)
Loading rate (mg/L)	Days	Rep 1	Rep 2	Rep 3	Mean	RSD%
100	5	51.27	44.89	48.69	48.28	6.65
100	6	50.92	50.09	51.00	50.67	0.99
100	7	50.53	51.04	51.08	50.88	0.60
% diff (day 6-7)		0.8	-1.9	-0.2
% diff (day 5-7)		1.5	-12.8	-4.8
overall					49.95	4.12
50	5	30.06	32.30	31.02	31.13	3.61
50	6	29.77	31.15	31.15	30.69	2.60
50	7	31.73	31.38	30.53	31.21	1.98
% diff (day 6-7)		-6.4	-0.7	2.0
% diff (day 5-7)		-11.1	5.7	3.2
overall					31.01	2.56

 

Conclusions:

The water solubilities of MTDID 18990 were 31.01 mgC/L at loading rate of 50 mg/L and 49.95 mgC/L at loading rate of 100 mg/L at room temperature.

Executive summary:

Water solubility of MTDID 18990 was determined according to OECD 105 with significant modification.

Samples of test article were weighed into 2 mL glass autosampler vials and submerged in vessels containing 1L distilled deionized water. Two loading rates of 50 mg/L and 100 mg/L, each in triplicate, were tested. The vessels were stirred continuously as slowly as possible for 5, 6 and 7 days at ambient temperature. On each of the 5, 6, and 7 days, aliquots of water were removed, and the pH measured, the samples were stored at room temperature until analysis. After stirring for 7 days, the vials were carefully removed from the beaker and dried at ~100 °C in an oven for over ~ 15 hours. The vials were weighed to determine the mass of the residue remaining in the vials. The water samples were diluted 10-fold prior to analysis by TOC analyzer.

Water solubility of MTDID 18990 were 31.01 mgC/L at loading rate of 50 mg/L and 49.95 mgC/L at loading rate of 100 mg/L, based on average measured concentration from day 5 to day 7. Samples reached equilibrium from day 5 to day 7.

Mean mass balances were 50.8% for the loading rate of 100 mg/L and 62.1% for the loading rate of 50 mg/L. It was noted that test article is also composed of non-carbon elements which are not accountable by TOC, therefore, the percentage of these elements will significantly impact the mass balance results.

This is a guideline study conducted under GLP with significant modification. The modification was used to account the insoluble portion for mass balance. The modification did not affect the data quality and reliability.

Reference 3

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

May 1, 2013

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

comparable to guideline study with acceptable restrictions

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

GLP compliance:

no

Type of method:

flask method

Key result

Water solubility:

0.36 mg/L

Conc. based on:

test mat.

Loading of aqueous phase:

1.08 mg/L

Incubation duration:

ca. 18 h

Temp.:

22.4 °C

Remarks on result:

other: pH not determined

Key result

Water solubility:

<= 100 mg/L

Conc. based on:

test mat.

Loading of aqueous phase:

10 000 mg/L

Incubation duration:

ca. 10 h

Temp.:

22.4 °C

Remarks on result:

other: pH not measured

Details on results:

In the first test, 3.6 mg of the original 5.4 mg remained, suggested that 1.8 mg of MTDID 18990 was dissolved into the 5L water. Therefore, the water solubility is 0.36 mg/L (Table 1).
In the second test, MTDID 18990 was a very noticeable opaque white homogeneous emulsion, not clear or dissolved. The emulsion could not be centrifuged out at a speed up to 10,000 rpm. The emulsion was then diluted by a serial 10-fold dilutions in water and evaluated by a HP 5453 UV/VIS spectrophotometer to determine the opacity at 600 nm (A600). The clarity was achieved at a 100-fold dilution. Therefore, the solubility was ≤ 100 ppm (Table 2).

Table 1: Recorded weights of MTDID 18990 during dissolution test

Weight of vial	2.2385 g
Weight of vial + MTDID 18990	2.2439 g
Initial weight of MTDID 18990 in vial	0.0054 g
Volume of water vial submerged into	5.0 L
Weight of MTDID 18990 in vial after dissolution test	2.2421 g
Weight of MTDID 18990 recovered	0.0036 g
Weight of MTDID 18990 dissolved	0.0018 g
Calculated solubility	0.000360 g/L

 

Table 2: Spectrophotometric results in second test

Nominal conc. (mg/L)	A600
10000	1.89950
1000	0.22729
100(a)	0.01546
10	-0.0016479
1	-0.0022950

(a) the maximum solubility based on measurable emulsion still present in sample

Conclusions:

Screening evaluation of MTDID 18990 water solubility resulted in a water solubility from 0.36 mg/L to ≤ 100 mg/L at 22.4 °C.

Executive summary:

The solubility of MTDID 18990 was evaluated in two screening experiments using modified shake flask method.

In the first test, 5.4 mg of MTDID 18990 was accurately weighed into an accurately weighed vial. The open vial with MTDID 18990 was carefully submerged into a vessel of 5 L of ASTM type -1 water. The vessel was stirred at medium speed on a magnetic stir plate for approximately 18 hours at 22.4 °C. The vial was then carefully removed from the vessel and dried at 95 °C for 24 hrs to determine the residue MTDID 18990 remained in the vial. MTDID 18990 lost from the initial 5.4 mg was assumed due to the solubilization into the 5 liters water.

In the second test, 403.8 mg of MTDID 18990 was accurately weighed into a 50 mL Polypropylene centrifuge tube, and then 40 mL of ASTM type -1 water was added, equivalent to 10,000 ppm. The sample was placed on a rotisserie shaker for approximately 10 hours at 22.4 °C. MTDID 18990 formed an opaque white homogeneous emulsion and could not be centrifuged out at a speed up to 10,000 rpm. The emulsion was then diluted by a serial 10-fold dilutions in water and evaluated by a HP 5453 UV/VIS spectrophotometer to determine the opacity at 600 nm (A600).

Result from the first experiment indicated the solubility of MTDID 18990 in water was 0.36 mg/L. Result from the second experiment demonstrated the solubility of MTDID 18990 in water was ≤ 100 mg/L. MTDID 18990 forms a milky emulsion in water at > 100 mg/L.

Both tests were screening evaluations. The results indicate further evaluation of water solubility of MTDID 18990 is needed.

Description of key information

The water solubilities of MTDID 18990 were 31.01 mgC/L at loading rate of 50 mg/L and 49.95 mgC/L at loading rate of 100 mg/L at room temperature.

Key value for chemical safety assessment

Water solubility:

31.01 mg/L

at the temperature of:

25 °C

Additional information

Water solubility of MTDID 18990 was determined according to OECD 105 with significant modification. The modification was used to account the insoluble portion for mass balance. The modification did not affect the data quality and reliability. Samples of test article were prepared at two loading rates of 50 mg/L and 100 mg/L, each in triplicate, and submerged in vessels containing 1L distilled deionized water. The vessels were stirred continuously as slowly as possible for 5, 6 and 7 days at ambient temperature. On each of the 5, 6, and 7 days, aliquots of water were removed, and the pH measured. The water samples were diluted prior to analysis by TOC analyzer. Water solubility of MTDID 18990 were 31.01 mgC/L at loading rate of 50 mg/L and 49.95 mgC/L at loading rate of 100 mg/L, based on average measured concentration from day 5 to day 7. Samples reached equilibrium from day 5 to day 7. This is a guideline study conducted under GLP with acceptable restrictions (Klimisch 2) and a key study.

The solubility of MTDID 18990 was evaluated in two screening experiments using modified shake flask method. In the first test, a vial containing 5.4 mg of MTDID 18990 was submerged into a vessel of 5 L of ASTM type -1 water and stirred for ~ 18 hrs at 22.4 °C. The vial was then removed and dried at 95 °C for 24 hrs and weighed. MTDID 18990 lost from the initial weight was assumed due to the solubilization. Water solubility of MTDID 18990 was 0.36 mg/L. In the second test, MTDID 18990 at 10,000 ppm in ASTM type -1 water was prepared in a centrifuge tube and placed on a shaker for ~ 10 hrs at 22.4 °C. MTDID 18990 formed an opaque white homogeneous emulsion and could not be centrifuged out at a speed up to 10,000 rpm. The emulsion was diluted in water and the opacity was measured by a HP 5453 UV/VIS spectrophotometer at 600 nm. The clarity was achieved at ≤ 100 mg/L. Both tests were screening evaluation and is considered reliable with acceptable restrictions (Klimisch 2) and a supporting study.

A single value of water solubility of 0.95% at 23 °C and pH 2.5 was reported. A contradictory statement of water solubility of 100% was also in the same report. As this is not relevant to the environmental condition, and no information about the test procedure or method was provided, this study is considered not reliable (Klimisch 3) and a disregarded study.