analytical report · · 2017-11-11page 3 easy reach example report 2017 v3.docx 1. study summary...

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


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


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


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:


FT-Infrared Spectra: Sample Report: Full Spectrum:

400 - 2000 cm-1:

2000 - 4000 cm-1:

Graph removed for Sample Report



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



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


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


UV-vis Spectra: Text removed for sample report

Sample Report:




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


3.3 Qualitative 1H NMR Spectroscopy

Qualitative 1H NMR Spectroscopy


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


1H NMR Spectra: Full Spectrum:

7.3 – 8.4 ppm: 1H NMR Interpretation




text removed for sample report text removed for sample report text removed for sample report


3.4 High Performance Liquid Chromatography

High Performance Liquid Chromatography


Column Sample Report

Column Oven / ºC

Sample Report

Quaternary Pump

Sample Report Sample Report




Gradient Timetable

Sample Report Sample Report Sample Report







Runtime / mins

Sample Report

Injection volume / µl

Sample Report

DAD Detector Sample Report Sample Report


Mass Spectrometry


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.


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:


UV Zoom: TIC UV Overlay: TIC UV Overlay Zoom:





UV Peak Integration List:

Suspected Structure:

Chemical Formula = Example

Removed for Sample Report



Summary of Peak Identification:

Retention Time / mins

Area %

Suspected Formula

Suspected I.D.

xx.xx x.xx Example Report

Text removed for example report

xx.xx xx.xx Example Text removed for example report

xx.xx x.xx Example Report

Text removed for example report


3.4.1 Detailed Analysis of Mass Spectrometry Results: Peak xx.xxx mins: Zoomed: Text removed All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:



Table removed for Sample Report


All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------: Text removed: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:

Text removed: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:





Peak xx.xxx mins: Zoomed: Text removed: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------: All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:





Peak xx.xxx mins: Zoomed:





All text removed for sample report ----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------:




3.5 Semi-Quantitative Inductively Coupled Plasma-Mass Spectrometry

ICP-MS (Semi-Quantitative Mode)


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.


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


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


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:



3.6 Quantitative Inductively Coupled Plasma-Mass Spectrometry

ICP-MS


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




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.


Results: ICP-MS Calibration:




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


3.8 Coulometric Water Content Determination

Oven Coulometry


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-----------------------------------------------------------

---------------------------------------------------.


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


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.


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

analytical report · · 2017-11-11page 3 easy reach example report 2017 v3.docx 1. study summary...

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