YC/T 207-2014 PDF English (YC/T 207-2006: Older version)
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Determination of solvent residuals on papers for cigarette - Headspace-gas chromatography/mass spectrometry
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| YC/T 207-2006 | English | 70 |
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Determination of volatile organic compounds in cigarette carton and packet packaging papers - Headspace-gas chromatography
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YC/T 207-2014: PDF in English (YCT 207-2014) YC/T 207-2014
YC
TABACCO INDUSTRY STANDARD
ICS 65.160
X 85
Filing No.. 48466-2015
Replacing YC/T 207-2006
Determination of solvent residuals on papers for cigarette -
Headspace-gas chromatography/mass spectrometry
ISSUED ON. DECEMBER 24, 2014
IMPLEMENTED ON. JANUARY 15, 2015
Issued by. Tobacco Monopoly Administration
Table of Contents
Foreword... 3
1 Scope... 4
2 Principle... 4
3 Reagents and materials... 4
4 Instruments and conditions... 6
5 Specimen preparation... 8
6 Analysis steps... 9
7 Calculation and expression of results... 10
8 Repeatability, recovery, detection limit... 11
9 Test report... 11
Appendix A (Informative) Examples of typical residual solvent quantification ions. 13
Appendix B (Informative) Chromatogram example... 14
Appendix C (Informative) Repeatability, recovery, detection limit results of the method
... 16
Determination of solvent residuals on papers for cigarette -
Headspace-gas chromatography/mass spectrometry
1 Scope
This standard specifies the headspace-gas chromatography/mass spectrometry
determination method for solvent residues (benzene, toluene, ethylbenzene, xylene,
styrene, methanol, ethanol, isopropanol, n-propanol, n-butanol, acetone, 4-methyl-2-
pentanone, butanone, cyclohexanone, ethyl acetate, n-propyl acetate, n-butyl acetate,
isopropyl acetate, 2-ethoxyethyl acetate, 1-methoxy-2-propanol, 1-ethoxy-2-propanol,
2-ethoxyethanol, dimethyl succinate, dimethyl glutarate, dimethyl adipate) in cigarette
paper; other solvent residues can make reference to this standard.
This standard is applicable to cigarette rod packaging paper, box packaging paper,
cigarette tipping paper, cigarette lining paper; other cigarette papers can make reference
to this standard.
2 Principle
In a closed container and at a certain temperature, when the solvent residue in the
specimen reaches equilibrium between the gas phase and the matrix (liquid phase or
solid phase), the gas phase is introduced into the gas chromatograph/mass spectrometer
for separation and identification. After matrix correction, the solvent residue in the
specimen is determined.
3 Reagents and materials
Warning - Relevant volatile organic compounds shall not be placed in the
laboratory. Experimenters shall wear protective equipment to ensure safety. Test
waste liquid shall be collected and disposed of uniformly.
Unless otherwise required, reagents of analytical grade or above shall be used.
3.1 Triacetin.
3.2 Solvent residue standard sample
3.2.1 Typical solvent residue standard sample
3.2.1.1 Benzene.
Determined by the qualitative analysis results of cigarette paper specimens.
3.3 Standard solution
3.3.1 Mixed standard stock solution
According to the qualitative analysis results of the solvent residue in the test specimen,
weigh the corresponding solvent residue standard samples (3.2) respectively; dissolve
them in triacetin (3.1), to prepare a mixed standard stock solution.
Recommended preparation method for typical solvent mixed standard stock solution.
Accurately weigh 1000 mg of each of ethanol (3.2.1.7), n-propyl acetate (3.2.1.16), 1-
methoxy-2-propanol (3.2.1.20), 1-ethoxy-2-propanol (3.2.1.21), dimethyl succinate
(3.2.1.23), dimethyl glutarate (3.2.1.24), dimethyl adipate (3.2.1.25) in a 100 mL
volumetric flask, 15 mg of each of benzene (3.2.1.1), toluene (3.2.1.2), ethylbenzene
(3.2.1.3), o-xylene (3.2.1.4), m-xylene and p-xylene (3.2.1.4), styrene (3.2.1.5), 150 mg
each of methanol (3.2.1.6), isopropanol (3.2.1.8), n-propanol (3.2.1.9), n-butanol
(3.2.1.10), acetone (3.2.1.11), 4-methyl-2-pentanone (3.2.1.12), butanone (3.2.1.13),
cyclohexanone (3.2.1.14), ethyl acetate (3.2.1.15), n-butyl acetate (3.2.1.17), isopropyl
acetate (3.2.1.18), 2-ethoxyethyl acetate (3.2.1.19), 2-ethoxyethanol (3.2.1.22),
accurately to 0.1 mg respectively; make up to volume with triacetin (3.1), to prepare a
mixed standard stock solution. The concentration of ethanol (3.2.1.7), n-propyl acetate
(3.2.1.16), 1-methoxy-2-propanol (3.2.1.20), 1-ethoxy-2-propanol (3.2.1.21), dimethyl
succinate (3.2.1.23), dimethyl glutarate (3.2.1.24), dimethyl adipate (3.2.1.25) in the
prepared mixed standard stock solution is 10 mg/mL; the concentration of benzene
(3.2.1.1), toluene (3.2.1.2), ethylbenzene (3.2.1.3), o-xylene (3.2.1.4), m-xylene, p-
xylene (3.2.1.4), styrene (3.2.1.5) is 0.15 mg/mL; the concentration of other substances
is 1.5 mg/mL. The mixed standard stock solution is sealed and stored in the dark at -
18 °C; the validity period is 6 months.
For other solvent residue standards (3.2.2), prepare standard stock solutions according
to actual conditions.
3.3.2 Standard working solutions
The series of standard working solutions shall use triacetin (3.1) as solvent, using mixed
standard stock solutions to dilute and prepare series of standard working solutions. The
series of standard working solutions shall be prepared in at least 5 levels; the appropriate
concentration shall be prepared according to the actual content of the sample. Place it
at room temperature when taking it; use it only after it reaches room temperature.
4 Instruments and conditions
4.1 Static headspace instrument, instrument conditions of which are as follows.
- Headspace bottle. 20 mL;
spectrometry ion fragments of each solvent residue, select ions with higher
specificity and response as quantitative ions; select other 1 ~ 2 fragment ions as
auxiliary qualitative ions. For typical solvent residue ion selection parameters, see
Appendix A.
4.4 Analytical balance, sensitivity 0.1 mg.
4.5 Piston pipette, 1000 μL.
4.6 Paper cutter.
5 Specimen preparation
5.1 General requirements
Take laboratory samples for specimen preparation. For flat sheets of cigarette paper,
samples shall be taken from the middle or from the 4th or 5th layer to prepare the
specimen; for rolls and disks of cigarette paper, at least 3 layers of the surface shall be
discarded before sampling and preparing the specimen. Prepare two parallel specimens
for each sample. For special specifications of cigarette paper, the specimen shall be
prepared according to the sampling area of cigarette paper for corresponding purposes.
Specimen preparation shall be fast and accurate; ensure that the sample is not
contaminated.
5.2 Hard box packaging paper
Take a piece of hard box packaging paper sample; cut a specimen with an area of 22.0
cm × 5.5 cm; the specimen shall include the main packaging surface. Roll the cut
specimen into a tube with the printed surface facing inward; immediately put it into a
headspace bottle; add 1000 μL of triacetin (3.1); seal it for testing.
5.3 Soft box packaging paper
Take a piece of soft box packaging paper sample; cut a specimen with an area of 15.5
cm × 10.0 cm; the specimen shall include the main packaging surface; roll the specimen
into a tube with the printed surface facing inward; immediately put it into a headspace
bottle; add 1000 μL of triacetin (3.1); seal it and wait for testing.
5.4 Strip packaging paper
Take a strip packaging paper sample; cut a specimen with an area of 22.0 cm × 5.5 cm
in the central area of the front of the packaging paper; roll the specimen into a tube with
the printed surface facing inward; immediately put it into a headspace bottle; add 1000
μL of triacetin (3.1); seal it and wait for testing.
5.5 Cigarette tipping paper
Take a tipping paper sample; cut a specimen with an area of 20.0 cm × 4.0 cm. The
specimen shall contain a single edge. Roll the cut specimen into a tube with the printed
side facing inwards. Immediately put it into a headspace bottle. Add 1000 μL of triacetin
(3.1). Seal it and wait for testing.
5.6 Cigarette lining paper
Take a lining paper sample; cut a specimen with an area of 17.0 cm × 10.0 cm. Roll the
cut specimen into a tube with the printed side facing inwards. Immediately put it into a
headspace bottle. Add 1000 μL of triacetin (3.1). Seal it and wait for testing.
6 Analysis steps
6.1 Qualitative analysis
6.1.1 Qualitative identification of typical solvent residues
Use the corresponding cigarette paper base (box packaging paper base, strip packaging
paper base, cigarette tipping paper base, cigarette lining paper base, baked at 80 °C for
2 h before use) as the sample matrix; prepare specimens according to steps 5.2 ~ 5.6;
add typical solvent residue standards (3.2.1); perform headspace-gas
chromatography/mass spectrometry analysis according to instrument conditions (4.1 ~
4.3); determine the total ion flow, retention time, quantitative ion peak of the typical
solvent residue standards. Determine the target compound in the specimen by
comparing the retention time and total ion flow of the reference standard. When the
specimen and the standard appear at the same retention time (±0.2 min), meanwhile the
mass-to-charge ratio of the corresponding mass spectrometry fragment ion is consistent
with that of the standard, its abundance ratio is in accordance with that of the standard.
when the relative abundance is > 50%, a deviation of ±10% is allowed; when the
relative abundance is 20% ~ 50%, a deviation of ±15% is allowed; when the relative
abundance is 10% ~ 20%, a deviation of ±20% is allowed; when the relative abundance
is ≤ 10%, a deviation of ±50% is allowed, then the target analyte can be qualitatively
confirmed.
See Appendix B for the headspace-gas chromatography/mass spectrometry of the
typical solvent residual standard working solution and the specimen.
6.1.2 Qualitative identification of other solvent residues
First, the ion fragments of the chromatographic peak in the total ion flow of the mass
spectrum of the specimen are used, to call the mass spectrum library for reference and
search to obtain the preliminary qualitative results of the solvent residue. Based on the
preliminary qualitative results, the corresponding solvent residue standard sample is
dissolved in triacetin (3.1); the standard sample solution is added to the cigarette
paper/base paper sample, to perform the headspace-gas chromatography/mass
spectrometry analysis according to the instrument conditions (4.1 ~ 4.3). Determine the
target compound in the specimen, by comparing the retention time and total ion flow of
the standard sample. When the specimen and the standard appear at the same retention
time (±0.2 min), meanwhile the mass-to-charge ratio of the corresponding mass
spectrometry fragment ion is consistent with that of the standard, its abundance ratio is
in accordance with that of the standard. when the relative abundance is > 50%, a
deviation of ±10% is allowed; when the relative abundance is 20% ~ 50%, a deviation
of ±15% is allowed; when the relative abundance is 10% ~ 20%, a deviation of ±20%
is allowed; when the relative abundance is ≤ 10%, a deviation of ±50% is allowed; then
the target analyte can be qualitatively confirmed.
6.2 Quantitative analysis
6.2.1 Drawing of standard working curve
Using the corresponding cigarette paper as the sample matrix, prepare the test specimen
according to the requirements of Chapter 5.Add 1000 μL of the series of standard
working solutions (3.3.2) respectively; perform headspace-gas chromatography/mass
spectrometry analysis according to the instrument conditions (4.1 ~ 4.3), to obtain the
total ion flow diagram and quantitative ion peak of the solvent residual standard.
According to the quantitative ion peak area and content of the solvent residue standard
(the mass number of compounds contained in the unit area of paper, mg/m2), a standard
working curve is established. The working curve is forced to pass through the origin;
the linear correlation coefficient of the working curve R2 ≥ 0.995.
A standard working curve shall be prepared for each test. After 20 sample tests, a
medium concentration standard working solution shall be measured. If the measured
value differs from the original value by more than 5%, the standard working curve shall
be prepared again.
6.2.2 Blank test
Use the corresponding cigarette paper base as a sample, prepare a blank sample
according to the requirements of Chapter 5; perform headspace-gas
chromatography/mass spectrometry analysis according to the instrument test conditions
(4.1 ~ 4.3).
6.2.3 Sample determination
Measure the sample according to the instrument test conditions (4.1 ~ 4.3). Each sample
is measured twice in parallel; a group of blanks is made for each batch of samples.
7 Calculation and expression of results
The content of residual solvent in the specimen is calculated according to formula (1).
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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