Chromium, 1-[2-[5-(1,1-dimethylpropyl)-2-hydroxy-3-nitrophenyl]diazenyl]-2-naphthalenol 1-[2-[2-hydroxy-4(or 5)-nitrophenyl]diazenyl]-2-naphthalenol ammonium sodium complexes

Surface tension

Administrative data

Endpoint:

surface tension

Type of information:

experimental study

Adequacy of study:

key study

Study period:

07 and 09 April 2008

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affcet the quality of relevant results.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2008

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

EU Method A.5 (Surface Tension)

Deviations:

no

Principles of method if other than guideline:

The surface tension result was not corrected using the Harkins-Jordan correction table as the correction is not applicable to the apparatus used. Once calibrated, the balance and ring assembly used in this test give a direct reading for surface tension that is within the required accuracy (± 0.5 mN/m); this is as a result of the reduced ring dimensions.

This deviation has been considered not to have affected the integrity of the study.

GLP compliance:

yes (incl. QA statement)

Remarks:

Date of inspection: 21/08/07 Date of signature: 15/10/07

Type of method:

ring method

Test material

Test material information

Constituent 1

Reference substance name:

Reaction mass of :Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(Z)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)

EC Number:

700-174-4

Cas Number:

1029600-34-7

Molecular formula:

See structure.

IUPAC Name:

Reaction mass of :Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(Z)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)

Constituent 2

Reference substance name:

Reaction mass of : Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(Z)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)

IUPAC Name:

Reaction mass of : Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(Z)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [3-{(E)-[2-(hydroxy-kO)-5-(2-methylbutan-2-yl)-3-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-4-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-) Sodium or ammonium [1-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO][3-{(E)-[2-(hydroxy-kO)-5-nitrophenyl]diazenyl}naphthalen-2-olato(2-)-kO]chromate(1-)

Details on test material:

Sponsor's identification : VCBK3810
Description : black powder
Lot number : N006746
Date received : 25 February 2008
Storage conditions : room temperature, in the dark

Results and discussion

Surface tension

Surface tension:

68.6 mN/m

Temp.:

21.5 °C

Remarks on result:

other: The surface tension of 90% saturation concentration solution of test material has been determined to be 68.6 mN/m

Any other information on results incl. tables

 Results:

 Sample solution concentration:

The mean peak areas relating to the standard and sample solutions are shown in the following table:

Solution	MeanArea
	Group 1	Group 2
Standard 20.1 mg/l	350.744	193.802
Standard 20.2 mg/l	362.307	200.545
Matrix blank	None detected	None detected
Sample A	353.466	75.262
Sample B	349.371	70.530
Mean sample solution	3.98 x 10^-2g/l	1.49 x 10^-2g/l

 

Calibration factor (f):

The readings, temperatures and the corresponding calibration factors for glass double-distilled water are shown in the following table:

Reading (mN/m)	Temperature (ºC)	Literature Value (mN/m)	Calibration Factor
73.5	21.6	72.5	0.986
72.5	21.6	72.5	1.000
73.0	21.6	72.5	0.993
73.0	21.6	72.5	0.993
73.5	21.6	72.5	0.986
73.0	21.6	72.5	0.993
73.0	21.6	72.5	0.993
73.0	21.6	72.5	0.993
73.0	21.6	72.5	0.993
Mean Calibration Factor = 0.992

 Sample solution readings:

The readings, times and temperatures for the sample solution are shown in the following table:

Time (mins)	Reading (mN/m)	Temperature (ºC)
156	68.5	21.6
166	69.5	21.6
179	68.5	21.6
189	68.5	21.6
200	68.5	21.6
208	68.5	21.6
218	68.5	21.6
230	68.5	21.6

Mean reading                    :   68.6 mN/m
Surface tension                  = reading x calibration factor
                                         = 68.6 x 0.992
                                         = 68.1 mN/m
Temperature                      :   21.5 ± 0.5ºC
pH of sample solution        :   6.7

Validation:

The linearity of the detector response with respect to concentration was assessed over the nominal concentration range of 0 to 50 mg/l. This was satisfactory with a correlation coefficient of > 0.997 being obtained for all groups of analyte monitored.

Discussion:

Substances showing a surface tension lower than 60 mN/m should be regarded as being surface active.

It is evident from the information obtained in the hydrolysis test (see Section 10) and data relating to the pH of the test material in water that negligible hydrolysis of the sample solution occurred during the course of the surface tension test.

In the absence of definitive purity values for the test material, all calculated concentration values have been reported as equivalent test material concentrations. That is, the concentration calculated for any individual group/component is equivalent to that specified concentration of test material having been successfully dissolved. The test material has been quantified separately for the two distinct groups of peaks eluting at approximately 5 minutes and 10 minutes respectively.

On initial assessment, the analytical results for the surface tension sample solution were seemingly high when compared to the water solubility definitive test samples solutions values. However on applying Grubb’s outlier test to the surface tension equivalent test material concentration for both the group 1 components and group 2 components (as defined above) the values were not identified as statistically significant using P = 0.05, even when correcting for the 90% dilution of the sample solution. Therefore the results were confirmed as being within the anticipated statistical spread for the procedure applied to the analysis of the water solubility sample solutions.

Applicant's summary and conclusion

Conclusions:

The surface tension of 90% saturation concentration solution of test material has been determined to be 68.6 mN/m at 21.5 ± 0.5°C. The test material is considered not to be a surface-active material. On analysis the sample solution was determined to contain components in the first eluting group equivalent to 3.98 x 10-2 g/l of test material in solution and components in the second eluting group equivalent to 1.49 x 10-2 g/l of test material in solution.

Executive summary:

Surface Tension: 68.6 mN/m (90% saturated solution) at 21.5 ± 0.5°C, using a ring method based on ISO 304, Method A5 of Commission Directive 92/69/EEC. The test material is considered not to be a surface-active material. On analysis the sample solution was determined to contain components in the first eluting group equivalent to 3.98 x 10^-2g/l of test material in solution and components in the second eluting group equivalent to 1.49 x 10^-2g/l of test material in solution.