YC/T 243-2008 English PDF (YCT243-2008)

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YC/T 243-2008: Tobacco and tobacco products. Determination of 1, 2-propylene glycol and glycerol. Gas chromatographic method
YC/T 243-2008
TOBACCO INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.160
X 87
Record number: 23582-2008
Tobacco and tobacco products - Determination of 1,2-
propylene glycol and glycerol - Gas chromatographic
method
ISSUED ON: APRIL 14, 2008
IMPLEMENTED ON: APRIL 14, 2008
Issued by: State Tobacco Monopoly Administration
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents and materials ... 4 
5 Apparatus ... 5 
6 Analytical procedure ... 6 
7 Calculation and expression of results ... 7 
8 Detection limit and recovery rate ... 8 
9 Test report ... 8 
Appendix A (Informative) Recommended chromatographic columns ... 9 
Appendix B (Informative) Examples of chromatograms ... 10 
Tobacco and tobacco products - Determination of 1,2-
propylene glycol and glycerol - Gas chromatographic
method
1 Scope
This Standard specifies the gas chromatographic determination method for 1,2-
propylene glycol and glycerol in tobacco and tobacco products.
This Standard applies to the determination of 1,2-propylene glycol and glycerol
in tobacco and tobacco products.
2 Normative references
The following documents contain provisions which, through reference in this
Standard, constitute provisions of this Standard. For the dated references, their
subsequent amendments (excluding corrections) or revisions do not apply to
this Standard. However, the parties who enter into agreement based on this
Standard are encouraged to investigate whether the latest editions of these
documents are applicable. For undated reference documents, the latest
editions apply to this Standard.
GB/T 5606.1 Cigarettes - Part 1: Sampling
GB/T 19616 Tobacco - Sampling of batches of raw material - General
principles (GB/T 19616-2004, ISO 4874:2000, MOD)
YC/T 31 Tobacco and tobacco products - Preparation of test sample and
determination of water content - Oven method
3 Principle
USE a methanol solution with an internal standard to extract the 1,2-propylene
glycol and glycerol in the test sample. USE a gas chromatograph equipped with
a hydrogen flame detector for determination.
4 Reagents and materials
4.1 Unless otherwise required, analytical grade reagents shall be used.
35% biphenyl-65% polydimethylsiloxane. See Appendix A for other suitable
chromatographic columns.
6 Analytical procedure
6.1 Sampling
Cigarette samples are taken according to GB/T 5606.1.
Tobacco samples are taken according to GB/T 19616.
6.2 Preparation of test sample
Prepare test samples according to YC/T 31.
6.3 Sample extraction
WEIGH about 2 g of sample, accurate to 0.01 g; PLACE it in 150 mL conical
flask. USE a pipette or an automatic liquid dispenser to add 50 mL of extractant
(4.4); oscillate with plug to extract for 2 h. After that, the extract is allowed to
stand for 10 min~15 min. TAKE the supernatant for gas chromatographic
analysis.
6.4 Determination procedure
6.4.1 Apparatus preparation
According to the manufacturer's operation manual, operate the gas
chromatograph. The chromatographic conditions used shall be such that 1,2-
propylene glycol and glycerol can be completely separated from other
substances. The following gas chromatographic analysis conditions are
available for reference. When other conditions are adopted, their applicability
shall be verified:
a) Temperature:
1) Inlet temperature is 250°C;
2) Detector temperature is 275°C;
3) Initial temperature: 110°C; KEEP for 1 min;
4) Temperature programming 1: At a rate of 10°C/min, increase from
110°C to 150°C and maintain for 3 min;
5) Temperature programming 2: At a rate of 30°C/min, increase from
150°C to 220°C and maintain for 5 min.
b) Airflow rate: According to the apparatus operation manual and the
experience of the analyst, set the airflow rate. The suitable airflow rate is
as follows:
1) Carrier gas: Helium, 0.7 mL/min;
2) Make-up gas: Helium or nitrogen, 30 mL/min;
3) Hydrogen: 30 mL/min;
4) Air: 400 mL/min.
c) Injection mode: Injection volume is 2 μL; split injection. Split ratio is 50:1.
6.4.2 Making of standard curve
Perform chromatographic determination of the working standard solution (4.7.2).
Calculate the peak area ratio of 1,2-propylene glycol and glycerol to internal
standard in each standard solution. MAKE a standard curve of 1,2-propylene
glycol and glycerol concentration to peak area ratio; or calculate to obtain a
regression equation. The standard curve shall be linear. The correlation
coefficient R2 shall not be less than 0.99. The standard curve is produced once
a day. After every 20 sample determinations, a medium-concentration working
standard solution shall be added. If the measured value differs from the
previous value by more than 5%, the entire standard curve shall be made again.
6.4.3 Determination
Determine the sample extract (6.3). Calculate the peak area ratio of 1,2-
propylene glycol and glycerol to internal standard. From the regression
equation, calculate the concentration (c) of 1,2-propylene glycol and glycerol in
the extract.
Conduct gas chromatographic analysis on the standard solution and sample
extract. The resulting gas chromatograms are as shown in Appendix B, Figure
B.1 and Figure B.2.
7 Calculation and expression of results
The content of 1,2-propylene glycol and glycerol in the sample is denoted as
mass fraction w. The value is expressed in % and calculated according to
formula (1):