Dicerium trisulphide

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 16 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:

Dicerium trisulphide

EC Number:

234-603-7

EC Name:

Dicerium trisulphide

Cas Number:

12014-93-6

Molecular formula:

Ce2S3

IUPAC Name:

dicerium trisulphide

Test material form:

solid: granular

Details on test material:

- Name of test material (as cited in study report):Cerium sulfide
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 150 µg Ce/l: r = 0.9998
Accuracy at 0.1, 100 and 100 mg test item/l: 96, 104 and 93%
Repeatability at 0.1, 100 and 100 mg test item/l: 2.0, 8.7 and 1.4%
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 Ce/l: stable

Any other information on results incl. tables

Specificity results:

Background reponse of the element is detected in the blank QC sample. The contribution of the response to the LOQ level is 0.011%. 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 reponse and analytical standard concentration in the range of 1 - 150 µg Ce/l. Since the coefficient of correlation (r) is >0.99 ( r = 0.9998) and the black calculated accuracies of the data points are in the range 85 -115% the calibration is accepted.

An additional calibration curve is prepared and alaysed to perfirm the research on an additional set of GC samples with a nominal concentration of 100 mg test item /l. The calibration curve is similar to the validation curve and fell within the criteria range.

Accuracy and repeatability:

The mean accuracy at a concentration level of 0.1 mg test item/l met the criterion of 70 -110%. The mean accuracy at a concentration level of 100 mg test item/l; however, does not fall within the criterion of 70 -110%. QC samples at 100 mg test item/l are re-prepared and similar results are obtained. As the control of the spike solution used for the preparation of the QC samples have a recovery of 110% and 124% respectively, the QC samples are corrected for this recovery and results are accepted. The coefficient of variation is ≤ 20% for all QC samples. Therefore the analytical method is accepted for the analysis of the test item in water in the target concentration range of 0.1 -100 mg test item/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 sustem and end solutions:

Since the coefficient of variation at all concentration levels is ≤ 20%, the analytical system and end solutions are stable over at least a 2.99 hour time interval.

Additional data on the stability of the analytical system and end solutions is obtained with the analysis of the additional QG samples of 100 mg test item/l. The results are similar to the validation results and feel within the criteria range.

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 150 µg Ce/l: r = 0.9998
Accuracy at 0.1, 100 and 100 mg test item/l: 96, 104 and 93%
Repeatability at 0.1, 100 and 100 mg test item/l: 2.0, 8.7 and 1.4%
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 Ce/l: stable

Executive summary:

An analytical method was validated for dicerium trisulfide 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-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).

 

The analytical method is validated for the following parameters:

Specificity: specific

Calibration curve in the range of 1 to 150 µg Ce/l: r = 0.9998

Accuracy at 0.1, 100 and 100 mg test item/l: 96, 104 and 93%

Repeatability at 0.1, 100 and 100 mg test item/l: 2.0, 8.7 and 1.4%

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

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