Final Report. Characterisation of Sample Report. Job No 2016/11/12-34 AS No. 1234A. Client Example Contact Sample. Signed. Example report.

Transcription

1 Final Report Title Characterisation of Job No 2016/11/12-34 AS No. 1234A Client Contact Sample Author report Signed Date 25 th November 2016 Easy Reach Report of 30

2 Contents 1. Study Summary Page 3 2. Samples/Appearance Page 3 3. Analytical Methods & Results Page FT-IR Spectroscopy Page UV-Vis Spectroscopy Page Qualitative 1H NMR Spectroscopy Page Qualitative 13C NMR Spectroscopy Page HPLC-Mass Spectrometry Page 16 o Detailed Analysis of Mass Spectrometry Results Page Ashing for inorganics Page Coulometric Water Content Determination Page Conclusion Page 29 Easy Reach Report of 30

3 1. Study Summary The chemical structure of was characterised. Spectroscopic analysis included FT-IR spectroscopy, UV-vis spectroscopy and qualitative 1 H and 13 C NMR spectroscopy. HPLC-UV analysis confirmed the purity of the sample. Further analysis by HPLC-MS (TOF) determined the identity of the impurities detected by HPLC-UV. Additional analysis included thermogravimetric analysis to determine the inorganic content and water content determination by oven coulometry. 2. Samples/Appearance Sample Name Batch No Ref No Appearance Lot A /11/12-34 Product Name CAS Number EC Number EU Chemical Name IUPAC Name Molecular Formula Molecular Weight C.I. Structure Structure removed for Easy Reach Report of 30

4 3. Analytical Methods & Results All volume determinations were made using autopipettors unless stated otherwise. 3.1 FT-IR Spectroscopy Fourier-Transform Infrared Spectroscopy with ATR Accessory Instrument ATR Accessory Scan Range / cm -1 No. of Scans Background Subtraction Resolution Sample Preparation: By clean spatula, approximately 50 mg of sample was taken and analysed via the FT-IR method above. The temperature at which this analysis was conducted was 24.0 o C. The resulting spectra are shown overleaf: Easy Reach Report of 30

5 FT-Infrared Spectra: : Full Spectrum: cm -1 : Graph removed for cm -1 : Graph removed for Easy Reach Report of 30

6 FTIR Interpretation: Structure removed for Wavenumber / cm -1 Assignment C=O 1450 OH 1218 C-O C-OH 763 Ar 1488 Ar C=C 1448 C-N C-O + Ar-OH Easy Reach Report of 30

7 3.2 UV-Vis Spectroscopy UV/Vis Spectroscopy Scan Mode Instrument Cuvette Type Scan Type Scan Range / nm Temperature / o C Scan Rate / nm min -1 Average Time / s Data Interval / nm Source Changeover / nm Sample Preparation: An approximate 1000 ppm sample stock solution was prepared by adding 10 mg of sample to 10 ml volumetric flasks, dissolving in text removed for sample report by sonicating for 30 mins, allowing to cool and then making up to volume text removed for sample report buffer solution. 100 µl of the 1000 ppm stock solution was pipetted into a 10 ml volumetric flask and made to volume with text removed for sample report buffer resulting in a 10 ppm sample solution. The resulting solution was then transferred to a quartz UV cuvette and analysed with baseline correction via the UV/Vis method above with text removed for sample report buffer solution as the blank. Sample I.D Sample Report Sample Mass / mg xx.x Solvent text removed for sample report [Sample] / ppm xx [Sample] assuming 100% purity / mm x.xxx Easy Reach Report of 30

8 UV-vis Spectra: Text removed for sample report Graph removed for : Graph removed for Easy Reach Report of 30

9 Extinction Co-efficient Data: Sample I.D Molecular Weight UV Sample Concentration* / mm Sample Report xxx.xx x.xxx Absorbance Wavelength / nm ε / Abs. M.cm -1 x.xxx xxx xxxx x.xxx xxx xxxx x.xx xxx xxxxx x.xxx xxx xxxxx x.xxx xxx xxxxx * text removed for sample report Text removed for sample report Sample I.D Molecular Weight UV Sample Concentration* / mm Sample Report xxx.xx x.xxx Absorbance Wavelength / nm ε / Abs. M.cm -1 x.xxx xxx xxxx x.xxx xxx xxxx x.xx xxx xxxxx x.xxx xxx xxxxx x.xxx xxx xxxxx Easy Reach Report of 30

10 3.3 Qualitative 1H NMR Spectroscopy Qualitative 1 H NMR Spectroscopy Instrument Frequency / MHz Probe Pulse Program Size of FID Solvent Number of Scans Dummy Scans Sweep Width / Hz Decay FID Resolution / Hz Acquisition Time / sec Receiver Gain Dwell Time / µsec Pre-scan Delay / µsec Temperature of Acquisition / K Delay Time / sec Nucleus 90 o Pulse Width / sec Power of Pulse / W Frequency of Observed Channel / MHz Sample Preparation: To a 7 ml vial, approximately 15 mg of sample was accurately weighed and dissolved in text removed for sample report with sonication and gentle heating to ensure maximum dissolution. The resulting solutions was transferred to an NMR tube and analysed via the qualitative 1 H method above and 13 C NMR below: Sample I.D Sample Mass / mg NMR Solvent x.xx xxxx Easy Reach Report of 30

11 1 H NMR Spectra: Full Spectrum: ppm: Graph removed for 1 H NMR Interpretation Structure removed for Easy Reach Report of 30

12 text removed for sample report text removed for sample report text removed for sample report Easy Reach Report of 30

13 3.4 Qualitative 13C NMR Spectroscopy Qualitative 13 C NMR Spectroscopy Instrument Frequency / MHz Probe Pulse Program Size of FID Solvent Number of Scans Dummy Scans Sweep Width / Hz Decay FID Resolution / Hz Acquisition Time / sec Receiver Gain Dwell Time / µsec Pre-scan Delay / µsec Temperature of Acquisition / K Delay Time, D1 / sec Nucleus 90 o Pulse Width / sec Power of Pulse / W Frequency of Observed Channel / MHz 13 C NMR Spectra: Full Spectrum: Easy Reach Report of 30

14 : Graph removed for : Graph removed for 13 C NMR Interpretation Structure removed for Easy Reach Report of 30

15 Report: Text Removed Text Removed Text Removed Report: Text Removed Text Removed Text Removed Text Removed Easy Reach Report of 30

16 3.5 High Performance Liquid Chromatography High Performance Liquid Chromatography Instrument Column Column Oven / ºC Quaternary Pump Gradient Timetable Runtime / mins Injection volume / µl DAD Detector Mass Spectrometry Instrument Source Scan Mode Gas Temperature / ºC Gas Flow Rate / ml/min Nebuliser Pressure / psig Sheath Gas Temperature / ºC Sheath Gas Flow Rate / ml/min VCap / V Fragmentor / V Skimmer / V Acquisition Rate / spectra per sec Mass Range / m/z Sample Preparation: Approximately 200 mg of sample was accurately weighed to 100 ml sealable plastic jars. Approximately 25 ml of text removed for sample report was then added. The vessels were then sealed and sonicated for 20 minutes. To this solution was added Easy Reach Report of 30

17 an additional 50 ml of appropriate solvent followed by sonication for a further 20 minutes. The solutions were then quantitatively transferred to 100 ml volumetric flasks and made to volume with the appropriate solvent, yielding approximate 2000 ppm solutions. The resulting solutions were transferred to HPLC vials and analysed via the above method with water and acetonitrile as the blanks. The table overleaf shows the sample mass and solvent details for each sample: Sample I.D Sample Mass / mg Solvent Mass Spec Ionisation Mode xxx.x example example HPLC-UV-MS Chromatograms: TIC: UV: Easy Reach Report of 30

18 UV Zoom: Graph removed for TIC UV Overlay: Graph removed for TIC UV Overlay Zoom: Graph removed for Easy Reach Report of 30

19 UV Peak Integration List: Removed for Suspected Structure: Structure removed for Sample Report Chemical Formula = Easy Reach Report of 30

20 Summary of Peak Identification: Retention Time / mins Area % Suspected Formula Suspected I.D. xx.xx x.xx Text removed for example report Report xx.xx xx.xx Text removed for example report xx.xx x.xx Report Text removed for example report Easy Reach Report of 30

21 3.5.1 Detailed Analysis of Mass Spectrometry Results: Peak xx.xxx mins: Graph removed for Zoomed: Graph removed for Text removed All text removed for sample report : Table removed for Easy Reach Report of 30

22 Structure removed for All text removed for sample report : Structure removed for Text removed: All text removed for sample report : Table removed for Text removed: All text removed for sample report : Easy Reach Report of 30

23 Peak xx.xxx mins: Graph removed for Zoomed: Graph removed for Text removed: All text removed for sample report : Table removed for All text removed for sample report : Easy Reach Report of 30

24 Peak xx.xxx mins: Graph removed for Zoomed: Graph removed for Graph removed for Easy Reach Report of 30

25 Graph removed for Graph removed for All text removed for sample report : Easy Reach Report of 30

26 3.6 Ashing for inorganics Sample Preparation: Approximately 250 mg of sample was accurately weighed into a pre-dried, weighed porcelain crucible and the total mass recorded. The sample was then placed in a muffle furnace and heated to 750 o C and held at that temperature for 2 hrs. The sample was then allowed to cool and reweighed. Sample Sample Report Empty crucible mass / g xx.xxxxx Crucible + sample mass / g xx.xxxxx Mass of sample / g Mass of crucible + residue / g Mass of Residue / g xx.xxxxx xx.xxxxx xx.xxxxx % w/w Residue x.xx Easy Reach Report of 30

27 3.7 Coulometric Water Content Determination Oven Coulometry Instrument Hydranal Reagent Gas Flow Rate (air) / ml/min Oven Temperature / o C Extraction time / seconds Coulometer Generator type Coulometer Generator current / ma Start Conditions Pause / seconds Start Drift / g min -1 Titration rate Stop Criterion Standard and Sample Preparation: Prior to sample analysis, approximately 100 mg of text removed for sample report was weighed to coulometric vials and analysed via the above coulometry method. Text removed for sample report Following this analysis, approximately 50 mg of sample was weighed to coulometric vials in triplicate and analysed via the coulometric above method. A table of accurate sample masses is shown below: Sample I.D Sample Mass A / mg Sample Mass B / mg Sample Mass C / mg xx.xx xx.xx xx.xx Results: Standard # The water standard results are shown below: Standard Mass / mg Water Content / g Water Content / ppm x xxx.xx xxxx.xx xxxxx.x x.xx* x xxx.xx xxxx.xx xxxx.x x.xx Water Content / % x xx.xx xxxx.xx xxxxx.x x.xx Mean x.xx *Text removed for sample report Easy Reach Report of 30

28 The analytical sample results are shown below: Sample I.D Sample Report: Sample # Sample Mass / mg Water Content / µg Water Content / ppm Water Content / % x xx.xx xxx.xx xxxx.x x.xx x xx.xx xxx.xx xxxx.x x.xx x xx.xx xxx.xx xxxx.x x.xx Mean xxxx.xx x.xx Easy Reach Report of 30

29 4. Conclusion A summary of the results for the sample is shown below: Analytical Technique Result FTIR Spectrum acquired 1 H NMR Spectrum acquired 13 C NMR Spectrum acquired UV/Vis / max + Extinction coefficient (Abs M -1 cm -1 ) Sample report HPLC Area % Purity Sample report Any HPLC Impurities >1% area (Number)? Yes (2) Water Content / %w/w x.xx Ash Content / %w/w x.xx FTIR Key functional groups identified are as expected from a substance with the structure given 1H NMR Interpretation of the peaks confirms the structure and purity 13C NMR Interpretation of the peaks confirms the structure and purity UV/Vis The peak at text removed is consistent with text removed. Easy Reach Report of 30

30 Purity Retention Time / mins The sample has 2 HPLC impurities >1% Area Suspected Suspected I.D. % Formula xx.xx x.xx Sample report Text removed for Sample report xx.xx xx.xx Sample report Text removed for Sample report xx.xx x.xx Sample report Text removed for Sample report Water Content The sample supplied is dry with minimum moisture content Ash Content Small quantity of ash was detected indicating that the sample supplied contain a small amount of inorganic substances Easy Reach Report of 30