Final Report. Characterisation of Sample Report. Job No 2016/11/12-34 AS No. 1234A. Client Example Contact Sample. Signed Date 2017.

Transcription

1 Final Report Title Characterisation of Job No 2016/11/12-34 AS No. 1234A Client Contact Sample Author report Signed Date 2017 Easy Reach Report 2017 v2.docx 1 of 33

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 HPLC-Mass Spectrometry Page 13 o Detailed Analysis of Mass Spectrometry Results Page Semi-Quantitative Inductively Coupled Plasma-Mass Page 23 Spectrometry 3.6 Quantitative Inductively Coupled Plasma-Mass Spectrometry Page Ashing for inorganics Page Coulometric Water Content Determination Page Conclusion Page 32 Easy Reach Report 2017 v2.docx 2 of 33

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 2017 v2.docx 3 of 33

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 2017 v2.docx 4 of 33

5 FT-Infrared Spectra: : Full Spectrum: cm -1 : Graph removed for cm -1 : Graph removed for Easy Reach Report 2017 v2.docx 5 of 33

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 2017 v2.docx 6 of 33

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 2017 v2.docx 7 of 33

8 UV-vis Spectra: Text removed for sample report Graph removed for : Graph removed for Easy Reach Report 2017 v2.docx 8 of 33

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 2017 v2.docx 9 of 33

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 2017 v2.docx 10 of 33

11 1 H NMR Spectra: Full Spectrum: ppm: Graph removed for 1 H NMR Interpretation Structure removed for Easy Reach Report 2017 v2.docx 11 of 33

12 text removed for sample report text removed for sample report text removed for sample report Easy Reach Report 2017 v2.docx 12 of 33

13 3.4 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 2017 v2.docx 13 of 33

14 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 2017 v2.docx 14 of 33

15 UV Zoom: Graph removed for TIC UV Overlay: Graph removed for TIC UV Overlay Zoom: Graph removed for Easy Reach Report 2017 v2.docx 15 of 33

16 UV Peak Integration List: Removed for Suspected Structure: Structure removed for Sample Report Chemical Formula = Easy Reach Report 2017 v2.docx 16 of 33

17 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 2017 v2.docx 17 of 33

18 3.4.1 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 2017 v2.docx 18 of 33

19 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 2017 v2.docx 19 of 33

20 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 2017 v2.docx 20 of 33

21 Peak xx.xxx mins: Graph removed for Zoomed: Graph removed for Graph removed for Easy Reach Report 2017 v2.docx 21 of 33

22 Graph removed for Graph removed for All text removed for sample report : Easy Reach Report 2017 v2.docx 22 of 33

23 3.5 Semi-Quantitative Inductively Coupled Plasma-Mass Spectrometry ICP-MS (Semi-Quantitative Mode) Instrument Acquisition Mode: Number of Masses xxx Step 1 (Collision gas mode) Mass Element Det. Mode Integration/P Time/Mass oint (s) x-xxx xxx xxx x.xx x.xx Number of Points per Mass Number of Repetitions Total Acquisition time / s x x xxx.xx Stabilization time / s Tune Step 1 xx Tune Step 2 xx Peristaltic Pump Program (Sample introduction + probe Uptake Speed / rps Uptake Time / s Stabilization time / s rinse) Before Acquisition x.xx xx xx Probe Rinse xx Peristaltic Pump Program (Rinse) Rinse speed / rps Rinse on rinse vial /s Rinse on rinse port / s Rinse Vial 1 (2% HNO3) x.xx xx x Rinse Vial 2 (5% HNO3) x.xx xx x Rinse Vial 3 x.xx xx x Semi-quantitative Calibration Solution Preparation: A 100 ppb mixed element calibration stock solution was prepared by pipetting text removed for sample report into a 100 ml plastic volumetric flask. 2.0 ml text removed for sample report) was pipetted into the flask which was made to volume with ultra-pure water and well mixed to give a 100 ppb multielement stock. This stock solution contained the following elements: text removed for sample report A blank solution was prepared by pipetting 1.0 ml of text removed for sample report into a 15 ml plastic centrifuge tube and adding 9.0 ml of ultra-pure water. Easy Reach Report 2017 v2.docx 23 of 33

24 Semi-Quantitative ICP-MS Sample Preparation: Approximately 100 mg of sample was accurately weighed, in triplicate, into microwave digestion tubes. 10 ml text removed for sample report. The solutions were then digested via the microwave method shown below. Microwave Digestion Instrument Rotor + Vessels Approximate Sample Mass / mg Digestion Solution Temperature Program Microwave Power / W Safety Temperature (T2) / O C xxx xxx xxx Following digestion, the sample solutions were quantitatively transferred to 100 ml volumetric flasks, made to volume with ultra-pure water and well mixed. An aliquot of each solution was transferred to ICP tubes for semi-quantitative ICP-MS analysis. o Sample Mass 1 = x g o Sample Mass 2 = x g o Sample Mass 3 = x g Easy Reach Report 2017 v2.docx 24 of 33

25 Semi-quantitative ICP-MS Results: The mean result for any metallic element detected at significantly above background levels is shown below, these values are only semi-quantitative so are only approximate: Table removed for Easy Reach Report 2017 v2.docx 25 of 33

26 3.6 Quantitative Inductively Coupled Plasma-Mass Spectrometry ICP-MS Instrument Acquisition Mode: Number of Masses x Step 1 (No gas mode) Mass Element Det. Mode Integration Time/Mass /Point (s) xx Na Auto x.xx x.xx Step 2 (Collision gas mode) Number of Points per Mass Number of Repetitions Total Acquisition time / s xx Cr Auto x.xx x.xx xx Ge Auto x.xx x.xx Mass Element Det. Mode Integration Time/Mass /Point (s) xx Na Auto x.xx x.xx xx Cr Auto x.xx x.xx xx Ge Auto x.xx x.xx x x xx.xx Stabilization time / s Tune Step 1 xx Tune Step 2 xx Peristaltic Pump Program Uptake Speed / rps Uptake Time / s Stabilization time / s (Sample introduction + probe rinse) Before Acquisition x.xx xx xx Probe Rinse x.xx xx xx Peristaltic Pump Program (Rinse) Rinse speed / rps Rinse on rinse vial /s Rinse on rinse port / s Rinse Vial 1 x.xx xx xx Rinse Vial 2 x.xx xx xx Rinse Vial 3 x.xx xx xx Easy Reach Report 2017 v2.docx 26 of 33

27 Calibration: A 10 ppm text removed for sample report) into a 100 ml plastic volumetric flask, text removed for sample report was added to the flask which was then made to volume with ultra-pure water. A text removed for sample report was added to the flask which was then made to volume with ultra-pure water. To six 100 ml plastic volumetric flasks was pipetted text removed for sample report specified in the table below. The flasks were then made to volume with ultra-pure water and well mixed: ICP Calibration Solution # Volume of the 10 ppm Na ppm Cr stock / ml [Na] / ppm [Cr] / ppm 1 x x x 2 x.x x.x x.x 3 x.x x.x x.x 4 x.x x.x x.x 5 x.x x.x x.x 6 x.x x.x x.x Sample Preparation: To three 100 ml plastic volumetric flasks was pipetted text removed for sample report 1.0 ml of each of the sample stock solutions used for the semi-quantitative analysis was pipetted into each of the flasks which were then made to volume with ultra-pure water and well mixed. Easy Reach Report 2017 v2.docx 27 of 33

28 Results: ICP-MS Calibration: Table removed for Table removed for Easy Reach Report 2017 v2.docx 28 of 33

29 3.7 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 2017 v2.docx 29 of 33

30 3.8 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 2017 v2.docx 30 of 33

31 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 2017 v2.docx 31 of 33

32 4. Conclusion A summary of the results for the sample is shown below: Analytical Technique Result FTIR Spectrum acquired 1 H 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) Semi-Quantitative ICP-MS - Low level Sample report metallic impurities Quantitative ICP-MS for text Sample report removed for sample report Water Content / %w/w Ash Content / %w/w x.xx 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 UV/Vis The peak at text removed is consistent with text removed. Easy Reach Report 2017 v2.docx 32 of 33

33 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 Metals Semi-quantitative ICP-MS showed the only elements detected significantly higher than background levels, other than text removed for sample report Metal Content Quantitative ICP-MS gave 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 2017 v2.docx 33 of 33