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Page 1 2017 Easy REACH Example Pigment Report v2.docx Analytical Report Characterisation of an Example substance Client Example Report Contact Example Report Author Example Report Date - 2017

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Page 1 2017 Easy REACH Example Pigment Report v2.docx

Analytical Report

Characterisation of an Example substance

Client – Example Report

Contact – Example Report

Author – Example Report

Date - 2017

Page 2 2017 Easy REACH Example Pigment Report v2.docx

Contents 1. Study Summary Page 3

2. Samples/Appearance Page 5

3. Analytical Methods & Results Page 6

3.1 FT-IR Spectroscopy Page 6

3.2 Qualitative 1H NMR Spectroscopy Page 8

3.3 UV-Vis Spectroscopy Page 16

3.4 Elemental Analysis for C, H and N Content Page 19

3.5 Organic Components Page 20

3.6 Impurities Page 23

3.7 Coulometric Water Content Determination Page 27

4. Conclusion Page 28 Appendix Page 30 XXXXXX Page 42

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1. Study Summary The chemical structure of Example substance was characterised by the standard spectrographic analytical methods; UV-vis, FT-IR, and NMR Pigments are by definition insoluble in most solvents therefore standard chromatographic analytical procedures to establish the purity of the substance and impurities cannot be used. Text removed for Example report – other methods used. Example substance is a monoazo pigment, manufactured by a diazotisation and coupling reaction. In this type of reaction, the xxxxxx xxxxxxxxx xx xx xxxxxx xxx xxxxxxxx xx x xxxxxx xxxxxx.

Manufacturing process

Removed for Example Report

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Text removed from Example Report

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2. Samples/Appearance

Sample Name Ref No Ref No Appearance

Example substance Example

substance Example Report Example substance

Product Name C.I. Example substance CAS Number Example substance EC Number Example substance Chemical Name Example substance Structure:

Molecular formula = Example substance

Molecular weight = Example substance

Structure removed for Example Report

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3. Analytical Methods & Results All volume determinations were made using autopipettors unless stated otherwise.

3.1 FT-IR Spectroscopy

FTIR with ATR accessory

Instrument Example Report

ATR accessory Example Report

Scan Range / cm-1 Example Report

No. of Scans Example Report

Background subtraction Example Report

Resolution Example Report

A spatula was used to transfer sufficient sample to cover the ATR window.

The sample was compressed down on to the window then scanned using the method shown above.

Full Spectrum:

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400 – 2000 cm-1;

2000 – 4000 cm-

As the peaks are primarily found in the fingerprint region of the FTIR spectrum (<1500 cm-1) definitive assignment is difficult. A broad assignment of peaks is shown below:

Wavenumber / cm-1 Assignment

3251 NH2 amides

3079 OH + ArCH

1668 C=O amide

1592 Ar

1540 NH secondary amide

1410 – 1500 NH amide, Ar, C-N

1322 Ar-OH

1230 – 1260 C-N

1150 – 1210 C-C-N, C-OH

1000 – 1110 C-N

650 - 900 ArCH + Ar-Cl

FTIR is consistent with the proposed structure

Removed for Example Report

Removed for Example Report

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3.2 Qualitative 1H NMR Spectroscopy

NMR Parameters – 1H

NMR model Example Report

Frequency Example Report

Probe Example Report

Pulse program Example Report

Size of FID Example Report

Solvent Example Report

Number of Scans Example Report

Dummy scans Example Report

Sweep Width Example Report

Decay FID Res Example Report

Acquisition time Example Report

Receiver gain Example Report

Dwell time Example Report

Pre-scan delay Example Report

Temperature of acquisition Example Report

Delay time, D1 Example Report

Nucleus Example Report

90o pulse width Example Report

Freq of observed channel Example Report

20 mg of sample was weighed into a 7 ml vial and 1 ml of text removed from example report was added using a pipette.

The vial was capped and sonicated for 20 mins to aid dissolution of the sample. Approximately 0.6 ml of the resulting solution was then transferred to an NMR tube for analysis.

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1H NMR – Full Spectrum:

Removed for Example Report

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7.5 – 9.5 ppm: Text and interpretation removed from example report.

Removed for Example Report

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Text removed from Example Report

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Text removed from Example Report

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Text removed from Example Report

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3.3 UV-Vis Spectroscopy

UV/Vis Spectroscopy – Scan Mode

Instrument Example Report

Cuvette Type Example Report

Scan Type Example Report

Scan Range Example Report

Temperature / oC Example Report

Scan Rate / nm min-1 Example Report

Average Time / s Example Report

Data Interval Example Report

Source changeover / nm Example Report

An approximate 1mM stock solution of sample was prepared by accurately weighing approximately 4.36 mg of sample into a 10 ml volumetric flask (actual mass = 4.33 mg).

The flask was made to volume with text removed from example report, capped and sonicated for 10 mins to ensure dissolution of the sample. The flask was then well mixed.

Text removed for example report.

0.9975 g of the ~1mM stock solution was weighed into a 10 ml volumetric flask, made to volume with text removed from example report.

An aliquot of the resulting solution was transferred to a 1 cm Quartz UV cuvette and scanned using the text removed from example report diluent for the baseline correction.

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Blank Spectrum: Sample Spectrum:

Graph removed for Example Report

Graph removed for Example Report

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Extinction Co-efficient Data:

I.D Number

Analytical Solution

Concentration / ppm

Analytical Solution

Concentration* / mM

Wavelength / nm

Absorbance ε / Abs. M.cm-

1

Example Report xx.xx x.xxxxx

xxx.x x.xxx Xx,xxx

xxx.x x.xxx Xx,xxx

xxx.x x.xxx Xx,xxx

xxx.x x.xxx Xx,xxx

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3.4 Elemental Analysis for C, H and N Content

CHN Elemental Analysis

Instrument Example Report Helium Fill Time / seconds Example Report Helium Purge Time / seconds Example Report Helium Pressure / psig Example Report Oxygen Pressure / psig Example Report Combustion Time / seconds Example Report Combustion Furnace Temp / oC Example Report Reduction Furnace Temp / oC Example Report Profile Scale / mV Example Report

Approximately 1.6 – 1.8 mg of sample was accurately weighed to 35 mg tin capsules, which were

washed with acetone (laboratory grade, Fisher) and dried prior to use. The capsules were then cold-

sealed and seated into nickel sleeves. Prior to use, the nickel sleeves were heated to 1000oC in a muffle

furnace for 1 hour to remove any trace solvents/impurities. The samples were then analyzed via the

above CHN EA method shown above with an empty capsule as the blank, text removed for example

report as the standards.

Results:

Sample I.D Calculated % Observed % Difference %

C H N Rest C H N Rest C H N Rest

Example Report

x.xx x.xx x.xx x.xx xx.xx x.xx x.xx xx.xx x.xx x.xx x.xx x.xx

The elemental analysis is very close to the theoretical values which indicates the material is the correct compound

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3.5 Components All info removed for example report.

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Text removed from Example Report

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3.6 Impurities All Text removed for Example Report. Text removed for Example Report.

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Text removed from Example Report

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Text removed from Example Report

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Text removed from Example Report

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3.7 Coulometric Water Content Determination

Oven Coulometry

Instrument Example Report

Hydranal Reagent Example Report

Gas Flow Rate (air) / ml/min Example Report

Oven Temperature / oC Example Report

Extraction time / seconds Example Report

Coulometer Generator type Example Report

Coulometer Generator current / mA Example Report

Start Conditions – Pause / seconds Example Report

Start Drift / µg min-1 Example Report

Titration rate Example Report

Stop Criterion Example Report

Standard and Sample Preparation: Prior to sample analysis, approximately 100 mg of Apura Water Standard Oven 1% (VWR, 0.98% H2O ± 0.03%) was weighed to coulometric vials and analysed via the above coulometry method. The mean blank was determined to be 83.06 µg. Following this analysis, approximately 100 mg of sample was weighed to coulometry vials in triplicate and analysed via the coulometric above method. The results are shown below: Results: Water Standard Results:

Standard #

Standard Mass / mg

Water Content (Abs) / µg

Water Content / ppm

Water Content / %

1 xx.xx xxxx.xx xxxxx.x x.xx 2 xxx.xx xxxx.xx xxxxx.x x.xx 3 xxx.xx xxxx.xx xxxx.x x.xx

Mean x.xx

Analytical Sample Results:

Sample I.D Sample

# Sample Mass

/ mg Water Content

(Abs) / µg Water Content

/ ppm Water

Content / %

Example Report

1 xxx.xx xxxx.xx xxxxx.x x.xx 2 xx.xx xxxx.xx xxxxx.x x.xx 3 xxx.xx xxxx.xx xxxxx.x x.xx

Mean x.xx

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4. Summary of Results and Conclusion:

Analytical Technique Result

FTIR Example Report 1H NMR Example Report

UV/Vis / max + Extinction coefficient (Abs M-1 cm-1)

Example Report Example Report Example Report Example Report

Elemental Analysis

C / % Example Report

H / % Example Report

N / % Example Report

Rest / % Example Report

Xxxxx Impurities Example Report

Xxxxx Impurities Example Report

Water Content / %w/w Example Report

FTIR

Key functional groups identified are as expected from a substance with the structure given

1H NMR

Text removed for Example Report. UV/Vis

Text removed for Example Report.

Elemental Analysis

Text removed for Example Report.

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Impurities

Text removed for Example Report. Water Content

Text removed for Example Report.

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Appendix