Experimental Assessment of Characterised PCMs for Thermal ...
Analytical Report · · 2017-11-11Page 3 Easy Reach Example Report 2017 v3.docx 1. Study Summary...
Transcript of Analytical Report · · 2017-11-11Page 3 Easy Reach Example Report 2017 v3.docx 1. Study Summary...
Page 1 Easy Reach Example Report 2017 v3.docx
Analytical Report
Characterisation of an Example substance
Client – Example Report
Contact – Example Report
Author – Example Report
Date - 2017
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Contents 1. Study Summary Page 3
2. Samples/Appearance Page 3
3. Analytical Methods & Results Page 4
3.1 FT-IR Spectroscopy Page 4
3.2 UV-Vis Spectroscopy Page 7
3.3 Qualitative 1H NMR Spectroscopy Page 10
3.4 HPLC-Mass Spectrometry Page 13
o 3.4.1 Detailed Analysis of Mass Spectrometry Results Page 18
3.5 Semi-Quantitative Inductively Coupled Plasma-Mass Page 23 Spectrometry
3.6 Quantitative Inductively Coupled Plasma-Mass Spectrometry Page 26
3.7 Ashing for inorganics Page 29
3.8 Coulometric Water Content Determination Page 30 4. Conclusion Page 32
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1. Study Summary The chemical structure of Sample Report was characterised. Spectroscopic analysis included FT-IR spectroscopy, UV-vis spectroscopy and qualitative 1H and 13C 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
Sample Report Lot A123 2016/11/12-34 Sample Report
Product Name C.I. Sample Report
CAS Number Sample Report
EC Number Sample Report
EU Chemical Name Sample Report
IUPAC Name Sample Report
Molecular Formula Sample Report
Molecular Weight Sample Report
Structure
Structure removed for Sample Report
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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 Sample Report
ATR Accessory Sample Report
Scan Range / cm-1 Sample Report
No. of Scans Sample Report
Background Subtraction Sample Report
Resolution Sample Report
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 oC. The resulting spectra are shown overleaf:
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FT-Infrared Spectra: Sample Report: Full Spectrum:
400 - 2000 cm-1:
2000 - 4000 cm-1:
Graph removed for Sample Report
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FTIR Interpretation:
Wavenumber / cm-1 Assignment
1650 - 1550 C=O
1450 OH
1218 C-O
1162 - 1146 C-OH
763 Ar
1488 Ar C=C
1448 C-N
1300 - 1100 C-O + Ar-OH
Structure removed for Sample Report
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3.2 UV-Vis Spectroscopy
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 Mass / mg
Solvent [Sample] /
ppm [Sample] assuming 100% purity / mM
Sample Report
xx.x text removed for
sample report xx x.xxx
UV/Vis Spectroscopy – Scan Mode
Instrument Sample Report
Cuvette Type Sample Report
Scan Type Sample Report
Scan Range / nm Sample Report
Temperature / oC Sample Report
Scan Rate / nm min-1 Sample Report
Average Time / s Sample Report
Data Interval / nm Sample Report
Source Changeover / nm Sample Report
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UV-vis Spectra: Text removed for sample report
Sample Report:
Graph removed for Sample Report
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Extinction Co-efficient Data:
* text removed for sample report Text removed for sample report
Sample I.D Molecular
Weight
UV Sample Concentration*
/ mM Absorbance
Wavelength / nm
ε / Abs. M.cm-1
Sample Report
xxx.xx x.xxx
x.xxx xxx xxxx
x.xxx xxx xxxx
x.xx xxx xxxxx
x.xxx xxx xxxxx
x.xxx xxx xxxxx
Sample I.D Molecular
Weight
UV Sample Concentration*
/ mM Absorbance
Wavelength / nm
ε / Abs. M.cm-1
Sample Report
xxx.xx x.xxx
x.xxx xxx xxxx
x.xxx xxx xxxx
x.xx xxx xxxxx
x.xxx xxx xxxxx
x.xxx xxx xxxxx
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3.3 Qualitative 1H NMR Spectroscopy
Qualitative 1H NMR Spectroscopy
Instrument Sample Report
Frequency / MHz Sample Report
Probe Sample Report
Pulse Program Sample Report
Size of FID Sample Report
Solvent Sample Report
Number of Scans Sample Report
Dummy Scans Sample Report
Sweep Width / Hz Sample Report
Decay FID Resolution / Hz Sample Report
Acquisition Time / sec Sample Report
Receiver Gain Sample Report
Dwell Time / µsec Sample Report
Pre-scan Delay / µsec Sample Report
Temperature of Acquisition / K Sample Report
Delay Time / sec Sample Report
Nucleus Sample Report
90o Pulse Width / sec Sample Report
Power of Pulse / W Sample Report
Frequency of Observed Channel / MHz Sample Report
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 1H method above and 13C NMR below:
Sample I.D Sample Mass / mg NMR Solvent
Sample Report x.xx xxxx
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1H NMR Spectra: Full Spectrum:
7.3 – 8.4 ppm: 1H NMR Interpretation
Graph removed for Sample Report
Structure removed for Sample Report
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text removed for sample report text removed for sample report text removed for sample report
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3.4 High Performance Liquid Chromatography
High Performance Liquid Chromatography
Instrument Sample Report
Column Sample Report
Column Oven / ºC
Sample Report
Quaternary Pump
Sample Report Sample Report
Sample Report Sample Report
Sample Report Sample Report
Sample Report Sample Report
Gradient Timetable
Sample Report Sample Report Sample Report
Sample Report Sample Report Sample Report
Sample Report Sample Report Sample Report
Sample Report Sample Report Sample Report
Sample Report Sample Report Sample Report
Sample Report Sample Report Sample Report
Sample Report Sample Report Sample Report
Runtime / mins
Sample Report
Injection volume / µl
Sample Report
DAD Detector Sample Report Sample Report
Sample Report Sample Report
Mass Spectrometry
Instrument Sample Report
Source Sample Report
Scan Mode Sample Report
Gas Temperature / ºC Sample Report
Gas Flow Rate / ml/min Sample Report
Nebuliser Pressure / psig Sample Report
Sheath Gas Temperature / ºC Sample Report
Sheath Gas Flow Rate / ml/min Sample Report
VCap / V Sample Report
Fragmentor / V Sample Report
Skimmer / V Sample Report
Acquisition Rate / spectra per sec Sample Report
Mass Range / m/z Sample Report
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 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.
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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
Sample Report xxx.x example example
HPLC-UV-MS Chromatograms: TIC:
UV:
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UV Zoom: TIC UV Overlay: TIC UV Overlay Zoom:
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UV Peak Integration List:
Suspected Structure:
Chemical Formula = Example
Removed for Sample Report
Structure removed for Sample Report
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Summary of Peak Identification:
Retention Time / mins
Area %
Suspected Formula
Suspected I.D.
xx.xx x.xx Example Report
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xx.xx xx.xx Example Text removed for example report
xx.xx x.xx Example Report
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3.4.1 Detailed Analysis of Mass Spectrometry Results: Peak xx.xxx mins: Zoomed: Text removed All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:
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Table removed for Sample Report
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All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------: Text removed: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:
Text removed: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:
Structure removed for Sample Report
Structure removed for Sample Report
Table removed for Sample Report
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Peak xx.xxx mins: Zoomed: Text removed: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:
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Table removed for Sample Report
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Peak xx.xxx mins: Zoomed:
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All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:
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3.5 Semi-Quantitative Inductively Coupled Plasma-Mass Spectrometry
ICP-MS (Semi-Quantitative Mode)
Instrument Sample Report
Acquisition Mode: Sample Report
Number of Masses xxx
Step 1 (Collision gas mode) Mass Element Det. Mode Integration/Point
Time/Mass (s)
x-xxx xxx xxx x.xx x.xx
Number of Points per Mass x
Number of Repetitions x
Total Acquisition time / s xxx.xx
Stabilization time / s Tune Step 1 xx Tune Step 2 xx
Peristaltic Pump Program (Sample introduction + probe rinse)
Uptake Speed / rps
Uptake Time / s
Stabilization time / s
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 multi-element 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.
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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 Sample Report
Rotor + Vessels Sample Report
Approximate Sample Mass / mg
xxx
Digestion Solution Sample Report
Temperature Program Sample Report
Microwave Power / W xxx
Safety Temperature (T2) / OC 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
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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 Sample Report
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3.6 Quantitative Inductively Coupled Plasma-Mass Spectrometry
ICP-MS
Instrument Sample Report
Acquisition Mode: Sample Report
Number of Masses x
Step 1 (No gas mode) Mass Element Det. Mode Integration/Point
Time/Mass (s)
xx Na Auto x.xx x.xx
xx Cr Auto x.xx x.xx
xx Ge Auto x.xx x.xx
Step 2 (Collision gas mode)
Mass Element Det. Mode Integration/Point
Time/Mass (s)
xx Na Auto x.xx x.xx
xx Cr Auto x.xx x.xx
xx Ge Auto x.xx x.xx
Number of Points per Mass
x
Number of Repetitions x
Total Acquisition time / s xx.xx
Stabilization time / s Tune Step 1 xx Tune Step 2 xx
Peristaltic Pump Program (Sample introduction + probe rinse)
Uptake Speed / rps
Uptake Time / s
Stabilization time / s
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
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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 + 12.5 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.
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Results: ICP-MS Calibration:
Table removed for Sample Report
Table removed for Sample Report
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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 750oC and held at that temperature for 2 hrs.
The sample was then allowed to cool and reweighed.
Sample Empty
crucible mass / g
Crucible + sample mass / g
Mass of sample /
g
Mass of crucible + residue /
g
Mass of Residue /
g
% w/w Residue
Sample Report
xx.xxxxx xx.xxxxx
xx.xxxxx xx.xxxxx xx.xxxxx x.xx
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3.8 Coulometric Water Content Determination
Oven Coulometry
Instrument Sample Report
Hydranal Reagent Sample Report
Gas Flow Rate (air) / ml/min Sample Report
Oven Temperature / oC Sample Report
Extraction time / seconds Sample Report
Coulometer Generator type Sample Report
Coulometer Generator current / mA Sample Report
Start Conditions – Pause / seconds Sample Report
Start Drift / g min-1 Sample Report
Titration rate Sample Report
Stop Criterion Sample Report
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
Sample Report xx.xx xx.xx xx.xx
Results: The water standard results are shown below:
Standard #
Standard Mass / mg
Water Content /
g Water Content /
ppm Water Content
/ %
x xxx.xx xxxx.xx xxxxx.x x.xx* x xxx.xx xxxx.xx xxxx.x x.xx x xx.xx xxxx.xx xxxxx.x x.xx
Mean x.xx
*Text removed for sample report-----------------------------------------------------------
---------------------------------------------------.
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The analytical sample results are shown below:
Sample I.D Sample
# Sample Mass
/ mg Water
Content / µg Water Content
/ ppm Water
Content / %
Sample Report:
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
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4. Conclusion
A summary of the results for the Sample Report sample is shown below:
Analytical Technique Result
FTIR Spectrum acquired 1H 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 metallic impurities
Sample report
Quantitative ICP-MS for text removed for sample report
Sample report
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
UV/Vis
The peak at text removed is consistent with text removed.
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Purity
The sample has 2 HPLC impurities >1%
Retention Time / mins
Area %
Suspected Formula
Suspected I.D.
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