Reaction products of 1,6-diisocyanatohexane, oligomers with 2-[(2-methacryloyl)oxy]ethyl 6-hydoxyhexanoate and 2-hydroxyethyl methacrylate

Water solubility

Administrative data

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

07 Oct 2009 to 16 Mar 2010

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: UVCB material, test is of solubility of dominant oligomeric components of the material only

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2010

Report date:

2010

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

other: EEC Directive 92/69, A.6, Council Regulation (EC) 440/2008, A.6

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Test material

Reference

Name:

Unnamed

Type:

Constituent

Details on test material:

- Name of test material (as cited in study report): MTDID 8191
- Substance type: UVCB material
- Physical state: Yellowish liquid
- Concentration of oligomers: ≥99%
- Purity test date: 24 January 2010
- Lot/batch no.: MK 12/048
- Expiration date of the lot/batch: 27-Jan-2010
- Stability under test conditions: Not reported
- Storage condition of test material: In the refrigerator at about 5 °C
- Other:

Results and discussion

Water solubility

Water solubility:

0.35 mg/L

Temp.:

20 °C

pH:

5.06 - 5.31

Remarks on result:

other: The standard deviation of the water solubility is 0.03 mg/L.

Details on results:

The standard deviation of the water solubility is 0.03 mg/L.

Any other information on results incl. tables

Results for calibration standards are reported in Table 3. The regression equation of the calibration standards was :

Peak area = 402226 + Concentration * 140265, R^2 = 0.9967 (Fig. 3)

It should be noted that total peak area was added, and that peaks were not consistent between standards and test samples (see Figures 1, 2). This may be explained by the presence of water soluble residual components present in the UVCB reaction mass. The vast majority (>99%) of the notified substance consists of oligomeric materials, and the water solubility value specified in this study summary should be understood as referring to the oligomerics. Amount dissolved on Day 2 (Table 2) was 13% greater than on Day 1 and 4% less than on Day 3. These differences are less than 15%, and the test is satisfactory.

Recovery from spiked samples ranged from 93% to 108%. Individual recoveries were not tabulated.

TABLES:

Table 1, Data of the performance of the water solubility test
Sample Solution No.	1	2	3	4	5	6
Weighed sample of the test item (g)	37.96	33.22	30.17	30.15	30.04	32.94
Added volume of water (mL)	40	40	40	40	40	40
Agitation time at 30°C (h)	72	72	48	48	24	24
Equilibration time at 20 °C (h)	24	24	24	24	24	24
pH value of test item solution	5.31	5.06	5.17	5.17	5.23	5.07
Dilution factor before quantification	0.095	0.095	0.095	0.095	0.095	0.095

Table 2, Results of the Water Solubility of MTDID 8191
Sample No.	Shaking time at 30°C (h)	Concentration (mg/L)		Water solubility (mg/L)^1
		analyzed	calculated
1	72	3.912	0.37
2	72	3.953	0.38
3	48	3.743	0.36
4	48	3.755	0.36
5	24	3.616	0.34	0.35
6	24	2.990	0.28	SD=0.03^2
1. Water solubility is mean of calculated concentrations.
2. SD = standard deviation.

Table 3, Calibration data of MTDID 8191
Concentration (mg/L)	Peak area	Deviation (%)
0.3776	450259	-9.3
0.75532	507332	-0.8
1.8883	670992	1.5
9.4415	1803664	5.8
18.883	3148104	3.7
28.3245	4126359	-6.3

FIGURE 1: TYPICAL HPLC CHROMATOGRAM OF STANDARD --> SEE ATT 1

FIGURE 2: TYPICAL HPLC CHROMATOGRAM OF AQUEOUS SAMPLE --> SEE ATT 2

FIGURE 3: HPLC CALIBRATION CURVE --> SEE ATT 3

Applicant's summary and conclusion

Conclusions:

Interpretation of results (migrated information): slightly soluble (0.1-100 mg/L)
The water solubility of the test substance at 20 °C is 0.35 mg/L

Executive summary:

The water solubility of the test substance (CAS1101874-33-2) was measured using a shake flask method. Test substance (30-38 mg) of test substance was added to 40 mL of water in each six flasks. Duplicate flasks were shaken at about 30°C and 90 rpm for 24 hours, 48 hours or 72 hours, respectively. Afterwards, the flasks were equilibrated for another 24 hours at 20.0 °C, extracted with a solid-phase extraction method, and analyzed using HPLC. The water solubility at 20 °C is 0.35 mg/L.

The study was conducted under internationally-accepted test guideline OECD105 and was compliant with GLP standards. The test substance is a UVCB-material containing mostly oligomeric materials plus a small amount of residual materials, all with differing solubilities. The water solubility report here is reliable with and should be understood as having the restriction that it is applicable to the oligomeric materials only.