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Analysis of smoke and analytical sciences

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The development of reliable, reproducible and validated analytical techniques is critical to all of our research programmes. From routine analysis of tar, nicotine and carbon monoxide to analysis of emissions from reduced toxicant products, the analytical science programme plays a fundamental role in quantifying constituent levels.

There are many challenges in accurately measuring cigarette smoke constituent levels; these include the need for standardised smoke generation methodologies and techniques to analyse complex and unstable mixtures.

Presently, our analytical capabilities cover tobacco, tobacco smoke, non-tobacco materials and include:-

measurement of common analytes in tobacco such as:- 

  • nicotine;
  • sugars;
  • nitrate; and
  • chloride.
  • European Smokeless Tobacco Council (ESTOC) standard constituents; 
  • machine smoking measurement of tar, nicotine and carbon monoxide;
  • measurement of Hoffmann analytes in smoke; and
  • materials analysis capability for the non-tobacco materials present in our products.

We have a range of methods developed either in-house, or ISO (International Standards Organisation) or CORESTA approved, which have been introduced to meet the specific needs of our scientific community and research programmes. Our work also utilises external contract laboratories where appropriate to complement and increase the range of analyses we offer. A library of many of the analytical methods we use, which can be seen and downloaded below.

As part of our commitment to quality and comparability with other laboratories, we participate in a range of cross-check and proficiency exercises annually.

Participation in industry collaborative work is something we strongly believe in, and we are particularly active through CORESTA. We also aim to present our development activities and research at international scientific conferences, where we encourage active discussion of our science. Furthermore, we provide expert input to standards organisations such as the British Standards Institute and ISO.


Constituent analysis methods for mainstream smoke (Hoffmann Analytes)


Ammonia
  • Lower reporting limit: 0.8µg/cigarette
  • Collection method: 5 cigarettes on a linear smoke engine into 2 impingers containing 20mL of 0.05M sulphuric acid.
  • Extraction method: Combine the impinger solutions and analyse an aliquot.
  • Analysis method: IC with an IonPac CS12A cation exchange column.

PDF: PDF: Method for determination of ammonia... - PDF: Method for determination of ammonia... (293 kb) Opens new window

Aromatic Amines
  • Lower reporting limits:
    • 1-Aminonaphthalene: 0.45ng/cigarette
    • 2-Aminonaphthalene: 0.45ng/cigarette
    • 3-Aminobiphenyl: 0.09ng/cigarette
    • 4-Aminobiphenyl: 0.09ng/cigarette
  • Collection method: 20 cigarettes on RM200 and collect the particulate phase on a 92mm Cambridge filter pad.
  • Extraction method: Extract pad with 5% HCl and internal standards. Filter through a MCX cation exchange SPE cartridge. Add 10mL of ammonium hydroxide solution and filter through a HLB SPE cartridge. Derivatise the solution using heptafluorobutyric anhydride at 80°C.
  • Analysis method: GC/MS in SIM mode using a J&W DB5 MS 30m x 0.25mm x 0.25µm column.

PDF: PDF: Method for determination of aromatic... - PDF: Method for determination of aromatic... (91 kb) Opens new window

Benzo(a)pyrene
  • Lower reporting limit: 0.42ng/cigarette
  • Collection method: 20 cigarettes on a RM200 and collect the particulate phase on a 92mm Cambridge filter pad.
  • Extraction method: Add internal standard to the Cambridge filter pad and extract with 25mL of cyclohexane. Filter through a PAH SPE cartridge and concentrate to 1mL.
  • Analysis method: GC/MS in SIM mode using a J&W DB5 MS 30m x 0.32mm x 0.25µm column.

PDF: PDF: Method for determination of Benzo(a)pyrene... - PDF: Method for determination of Benzo(a)pyrene... (490 kb) Opens new window

Carbonyls
  • Lower reporting limits:
    • Formaldehyde: 0.85µg/cigarette
    • Acetaldehyde: 1.15µg/cigarette
    • Acetone: 1.45µg/cigarette
    • Acrolein: 0.95µg/cigarette
    • Propionaldehyde: 0.95µg/cigarette
    • Crotonaldehyde: 1.10µg/cigarette
    • Methyl ethyl ketone: 1.10µg/cigarette
    • Butyraldehyde: 1.15µg/cigarette
  • Collection method: 2 cigarettes on a linear smoke engine into 2 impingers containing 25mL of 2,4-dinitrophenylhydrazine.
  • Extraction method: Combine the impinger solutions, remove an aliquot and add a buffer solution of sodium hydroxide and glacial acetic acid.
  • Analysis method: HPLC-UV @ 380nm using a C18 250mm x 4.6mm column.

PDF: PDF: Method for determination of carbonyls... - PDF: Method for determination of carbonyls... (135 kb) Opens new window

Hydrogen Cyanide
  • Lower reporting limit: 1.94µg/cigarette
  • Collection method: 5 cigarettes on a linear smoke engine into 2 impingers containing 25mL of 1M sodium hydroxide (front) and 10mL of 1M sodium hydroxide (rear).
  • Extraction method: Combine the impinger solutions and analyse an aliquot.
  • Analysis method: Colorimetric determination using continuous flow analysis.

PDF: PDF: Method for determination of hydrogen... - PDF: Method for determination of hydrogen... (60 kb) Opens new window

Nitric Oxide
  • Lower reporting limit: 10ppm/puff
  • Collection method: Puff by puff on-line analysis of vapour phase smoke.
  • Extraction method: Not applicable
  • Analysis method: Vapour phase is passed through a chemiluminescence detector.

PDF: PDF: Method for determination of nitric... - PDF: Method for determination of nitric... (90 kb) Opens new window

Metals
  • Lower reporting limits:
    • Chromium: 1.17ng/cigarette
    • Nickel: 1.99ng/cigarette
    • Arsenic: 0.97ng/cigarette
    • Selenium: 4.10ng/cigarette
    • Cadmium: 1.93ng/cigarette
    • Mercury: 0.13ng/cigarette
    • Lead: 12.03ng/cigarette
  • Collection method: 10 cigarettes on a linear smoke engine into a dry-ice cooled impinger containing glass packing beads.
  • Extraction method: Extract the impinger with 2 x 25mL of 5% nitric acid containing internal standards. Filter the extract through quartz wool.
  • Analysis method: ICP-MS with collision cell technology.

PDF: PDF: Method for determination of metals... - PDF: Method for determination of metals... (111 kb) Opens new window

Nitrosamines
  • Lower reporting limits:
    • NNN: 0.2ng/cigarette
    • NNK: 0.2ng/cigarette
    • NAT: 0.2ng/cigarette
    • NAB: 0.1ng/cigarette
  • Collection method: 5 cigarettes on a linear smoke engine and collect the particulate phase on a 44mm Cambridge filter pad.
  • Extraction method: Extract the Cambridge filter pad with 20mL of methanol containing internal standards.
  • Analysis method: LC/MS/MS using MRM transitions for identification and quantitation. Positive ESI mode using a C18 100A, 100mm x 2.0mm column.

PDF: PDF: Method for determination of tobacco-specific... - PDF: Method for determination of tobacco-specific... (146 kb) Opens new window

Phenols
  • Lower reporting limits:
    • Catechol: 0.24µg/cigarette
    • Phenol: 0.11µg/cigarette
    • Hydroquinone: 0.19µg/cigarette
    • Resorcinol: 0.06µg/cigarette
    • o-Cresol: 0.03µg/cigarette
    • m-Cresol: 0.03µg/cigarette
    • p-Cresol: 0.07µg/cigarette
  • Collection method: 5 cigarettes on RM20/CSR and collect particulate phase on a 44mm Cambridge filter pad.
  • Extraction method: Extract the Cambridge filter pad with 10mL of TBME containing internal standard. Derivatise the solution using BSTFA at 76°C.
  • Analysis method: GC/MS in SIM mode using a J&W DB-5 60m x 0.25mm x 0.25µm column.

PDF: PDF: Method for determination of phenols... - PDF: Method for determination of phenols... (395 kb) Opens new window

Semi-Volatiles
  • Lower reporting limits:
    • Pyridine: 0.15µg/cigarette
    • Quinoline: 0.02µg/cigarette
    • Styrene: 0.04µg/cigarette
  • Collection method: 5 cigarettes on RM20/CSR and collect the particulate phase on a 44mm Cambridge filter pad. The volatile constituents are collected on an XAD-4 sorbent tube.
  • Extraction method: Combine the Cambridge filter pad and the contents of the XAD-4 tube and extract with 20mL of methanol containing internal standards.
  • Analysis method: GC/MS in SIM mode using a J&W DB-WAX 30m x 0.25mm x 0.25µm column.

PDF: PDF: Method for determination of semi-volatiles... - PDF: Method for determination of semi-volatiles... (151 kb) Opens new window
  

Tar, Nicotine & Carbon Monoxide
  • Lower reporting limits:
    • 0.1mg/cigarette
  • Collection method: 5 cigarettes on a linear smoke engine and collect the particulate phase on a 44mm Cambridge filter pad. Carbon monoxide is collected in vapour phase bags.
  • Extraction method: Extract the Cambridge filter pad with 20mL of propan-2-ol containing internal standards.
  • Analysis method: GC/FID and GC-TCD using Poraplot Q 10m x 0.53mm and WCOT CP-WAX 52CB 25m x 0.53mm columns.

PDF: PDF: Method for determination of tar... - PDF: Method for determination of tar... (107 kb) Opens new window

Volatiles
  • Lower reporting limits:
    • 1,3-Butadiene: 0.32µg/cig
    • Isoprene: 0.41µg/cig
    • Acrylonitrile: 0.16µg/cig
    • Benzene: 0.07µg/cig
    • Toluene: 0.11µg/cig
  • Collection method: 5 cigarettes on linear smoke engine, filter the smoke through a Cambridge filter pad before collecting in chilled methanol.
  • Extraction method: Add internal standard to the chilled methanol extract.
  • Analysis method: GC/MS in SIM mode using a Restek RTX-VMS 30m x 0.32mm x 1.8µm column.

 PDF: PDF: Method for determination of selected... - PDF: Method for determination of selected... (124 kb) Opens new window

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