YC/T 373-2010 English PDF (YCT373-2010)

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YC/T 373-2010: Determination of benzene, toluene, ethylbenzene and xylene in polypropylene fiber tow and polypropylene fiber tow filter rod. Gas chromatography-mass spectrometry method
YC/T 373-2010
YC
TOBACCO INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.160
X 85
Record number: 30430-2011
Determination of benzene, toluene, ethylbenzene and
xylene in polypropylene fiber tow and polypropylene
fiber tow filter rod - Gas chromatography-mass
spectrometry method
ISSUED ON: DECEMBER 01, 2010
IMPLEMENTED ON: JANUARY 01, 2011
Issued by: State Tobacco Monopoly Administration
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents ... 4 
5 Instrument, equipment and conditions ... 6 
6 Analysis steps ... 7 
7 Calculation and expression of results ... 8 
8 Recovery rate, detection limit and quantification limit ... 9 
9 Test report ... 9 
Appendix A (Informative) Example chromatogram ... 10 
Determination of benzene, toluene, ethylbenzene and
xylene in polypropylene fiber tow and polypropylene
fiber tow filter rod - Gas chromatography-mass
spectrometry method
1 Scope
This Standard specifies the determination method of benzene, toluene,
ethylbenzene and xylene in polypropylene fiber tow and polypropylene fiber tow
filter rod -- Gas chromatography-mass spectrometry method.
This Standard applies to the determination of benzene, toluene, ethylbenzene
and xylene in polypropylene fiber tow and polypropylene fiber tow filter rod.
2 Normative references
The following documents are indispensable for the application of this document.
For dated references, only the dated version applies to this document. For
undated references, the latest edition (including all amendments) applies to this
document.
GB/T 15270-2001, Tobacco and tobacco products - Polypropylene fiber tow
filter rod
YC/T 27-2002, Polypropylene fiber tow for cigarette
3 Principle
Use the n-pentane solution that contains internal standard substance to extract
benzene, toluene, ethylbenzene and xylene in the sample; use the gas
chromatography-mass spectrometry method to determine the content of
benzene, toluene, ethylbenzene and xylene in the extract; then, calculate the
residual amount of benzene, toluene, ethylbenzene, and xylene in the sample.
4 Reagents
Except for special requirements, analytical reagents shall be used.
4.1 Reagents
4.1.1 N-hexane (C6H14), Super Pure grade or pesticide residue grade.
4.1.2 N-pentane (C5H12), chromatographic grade.
4.1.3 Benzene (C6H6), purity ≥99%.
4.1.4 Toluene (C7H8), purity ≥99%.
4.1.5 Ethylbenzene (C8H10), purity ≥99%.
4.1.6 O-xylene (o-C8H10), purity ≥99%.
4.1.7 M-xylene (m-C8H10), purity ≥99%.
4.1.8 P-xylene (p-C8H10), purity ≥99%.
4.1.9 2-hexanone (internal standard), if other substances are used as internal
standard, the applicability shall be verified.
4.2 Preparation of internal standard solution
4.2.1 Internal standard stock solution: weigh 0.1 g of 2-hexanone (4.1.9)
(accurate to 0.1 mg) in a 50 mL volumetric flask; use n-hexane (4.1.1) to dilute
to the mark; mix well, to obtain an internal standard stock solution whose
concentration is 2 mg/mL. Seal and store the internal standard stock solution in
a refrigerator at 0 °C ~ 4 °C; the validity period is 3 months.
4.2.2 Internal standard solution: accurately pipette 2.5 mL of internal standard
stock solution (4.2.1) into a 50 mL volumetric flask; use n-hexane (4.1.1) to
dilute to the mark; mix well to obtain an internal standard solution whose
concentration is 100 μg/mL. Seal and store the internal standard solution in a
refrigerator at 0 °C ~ 4 °C; the validity period is 1 month.
4.3 Preparation of standard solution
4.3.1 Mixed standard stock solution: respectively weigh 0.1 g of benzene (4.1.3),
toluene (4.1.4), ethylbenzene (4.1.5), o-xylene (4.1.6), m-xylene (4.1.7), p-
xylene (4.1.8) (accurate to 0.1 mg) in the 100 mL volumetric flasks; use n-
hexane (4.1.1) to dissolve them and dilute to the mark; mix well, to obtain the
mixed standard stock solution, of which the concentration of each component
is 1 mg/mL, respectively. Seal and store the mixed standard stock solution in a
refrigerator at 0 °C ~ 4 °C; the validity period is 3 months.
4.3.2 Mixed standard solution: use n-hexane (4.1.1) to gradually dilute the
mixed standard stock solution (4.3.1) to obtain a mixed standard solution whose
concentration is 5 μg/mL. Formulate this solution when needed.
Perform selective ion scanning on the standard working solution; calculate the
peak area ratio of benzene, toluene, ethylbenzene, and xylene in each standard
solution to the internal standard 2-hexanone; draw the standard working curve
of concentration-to-peak area ratio of benzene, toluene, ethylbenzene and
xylene. The standard working curve shall be straight line relationship; the
correlation coefficient shall be R2>0.99.
A standard working curve shall be made for each test. After every 20 samples,
add a medium-concentration standard working solution. If the measured value
differs from the original value by more than 10%, the standard working curve
shall be made again.
6.5 Sample determination
Measure the sample solution (6.2) according to the instrument test conditions;
repeat the measurement twice for each sample. At the same time, make a set
of blanks for each batch of samples.
7 Calculation and expression of results
Calculate the residual amount (X) of benzene, toluene, ethylbenzene, p-xylene,
m-xylene and o-xylene in the sample according to Formula (1):
Where:
X -- the residual amount of benzene, toluene, ethylbenzene, p-xylene, m-xylene
and o-xylene in the sample, in milligrams per kilogram (mg/kg);
c -- the concentration of benzene, toluene, ethylbenzene, p-xylene, meta-
xylene and o-xylene in the sample solution that is read from the standard
working curve, in micrograms per milliliter (μg/mL);
c0 -- the concentration of benzene, toluene, ethylbenzene, p-xylene, m-xylene
and o-xylene in the blank test that is read from the standard working curve,
in micrograms per milliliter (μg/mL);
m -- sample mass, in grams (g).
The final residual amount of xylene in the sample is the sum of the residual
amounts of p-xylene, m-xylene and o-xylene.
Take the average of two parallel determinations as the final determination result,
accurate to 0.01 mg/kg.