Reaction mass of Dicerium trisulfide and Dilanthanum trisulfide

Additional physico-chemical information

Administrative data

Endpoint:

other: Validation of an analytical method in water

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 24 July 2015 to 23 February 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Cross-reference

Reason / purpose for cross-reference:

reference to same study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

other: European Commission: Guidance for Generating and Reporting Methods of Analysis in Support of Pre-registration Data Requirements for Annex II (Part A, section 4) and Annex III (Part A, section 5) of Directive 91/414, SANCO/3029/99 rev. 4 (11/07/00).

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Test material

Test material information

Constituent 1

Reference substance name:

Reaction mass of Dicerium trisulfide and Dilanthanum trisulfide

EC Number:

915-048-6

Molecular formula:

N/A

IUPAC Name:

Reaction mass of Dicerium trisulfide and Dilanthanum trisulfide

Test material form:

solid: granular

Details on test material:

-Name of test material (as cited in study report): Reaction mass of dicerium trisulphide and dilanthanum trisulphide
For others details, see "Confidential details on test material" section

Results and discussion

Results:

The analytical method is validated for the following parameters:
Specificity: specific
Calibration curve in the range of 1 to 100 µg La/l: r = 0.998
Accuracy at 0.1 and 100 mg test item/l: 96 and 104%
Repeatability at 0.1 and 100 mg test item/l: 9.8 and 10%
Limit of quantification of this method: 0.1 mg test item/l
Stability analytical system and end solutions at 1.00, 5.00 and 150 µg La/l: stable
Storage stability at 0.1 and 100 mg test item/l: stable

Any other information on results incl. tables

Specificity results:

Background response of the element is detected in the blank QC sample. The contribution of the response to the LOQM level is 0.19%. Since this value is < 30%, the specificity requirements are met and the analytical method is found to be specific for the element of the test item.

Calibration curve:

There is a linear relationship between response and analytical standard concentration in the range of 1.00 - 100 µg La/l. Since the coefficient of correlation (r) is >0.99 ( r = 0.998) and the back calculated accuracies of the data points are in the range 85 -115% the calibration is accepted.

An additional calibration curve is prepared and analysed to perform the research on the storage stability samples. The curve is similar to the validation and fell within the criteria ranges.

Accuracy and repeatability:

The mean accuracy at each concentration level falls in the criterion 70 -110% and the coefficient of variation is ≤20%, the analytical method is accepted for the analysis of the test item in water in the target concentration range of 0.1 -100 mg/l.

Limit of quantification of this method:

The limit of quantification of this method (LOQM) is assessed at 0.1 mg test item/l in water.

Stability of the analytical system and end solutions:

The coefficient of variation at all concentration levels is ≤ 20%, the analytical system and end solutions are stable over at least a 3.89 hour time interval.

Additional data on the stability of the analytical system and end solutions was obtained with the analysis of the storage stability samples. Stability data are similar to the validation curve and fall within the criteria range.

Storage stability of samples:

The mean accuracy of the frozen QC samples falls in the criterion 70 -110%, the samples are stable when stored in the freezer.

Applicant's summary and conclusion

Conclusions:

The analytical method is validated for the following parameters:
Specificity: specific
Calibration curve in the range of 1 to 100 µg La/l: r = 0.998
Accuracy at 0.1 and 100 mg test item/l: 96 and 104%
Repeatability at 0.1 and 100 mg test item/l: 9.8 and 10%
Limit of quantification of this method: 0.1 mg test item/l
Stability analytical system and end solutions at 1.00, 5.00 and 150 µg La/l: stable
Storage stability at 0.1 and 100 mg test item/l: stable

Executive summary:

An analytical method was validated for reaction mass of dicerium trisulphide and dilanthanum trisulphide under GLP-compliant conditions in accordance with a recognized international guideline (European Commission: Guidance for Generating and Reporting Methods of Analysis in support of Pre-Regitration Data Requirements for Annex II (Part A, section 4) and Annex III (Part A, section 5) of Directive 91/414, SANCO/3029/99 rev. 4 (11/07/00).

The analytical method is validated for the following parameters:

Specificity: specific

Calibration curve in the range of 1 to 100 µg La/l: r = 0.998

Accuracy at 0.1 and 100 mg test item/l: 96 and 104%

Repeatability at 0.1 and 100 mg test item/l: 9.8 and 10%

Limit of quantification of this method: 0.1 mg test item/l

Stability analytical system and end solutions at 1.00, 5.00 and 150 µg La/l: stable

Storage stability at 0.1 and 100 mg test item/l: stable