YC/T 207-2014Determination of solvent residuals on papers for cigarette - Headspace-gas chromatography/mass spectrometry (English PDF)
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Issued by
Tobacco Monopoly Administration
Level / Type
National · Recommended
Issue date
December 24, 2014
Implementation date
January 15, 2015
Scope
YC/T 207-2014 (Determination of solvent residuals on papers for cigarette - Headspace-gas chromatography/mass spectrometry) is available as an English-translated PDF.
YC/T 207-2014 — 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.
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Document preview — YC/T 207-2014
National Standard of the People's Republic of China
- ICS
- 65.160
- Classification
- X 85
Issued by: Tobacco Monopoly Administration
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
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009 and
GB/T 20001.4-2001.
This standard replaces YC/T 207-2006 "Determination of volatile organic compounds
in cigarette carton and packet packaging papers - Headspace-gas chromatography".
Compared with YC/T 207-2006, the main technical changes of this standard are as
follows.
- CHANGE the name of the standard to "Determination of solvent residuals on
papers for cigarette - Headspace-gas chromatography/mass spectrometry";
- ADJUST the scope of application, to add cigarette paper such as cigarette tipping
paper and cigarette lining paper;
- MODIFY the instrument detection method and detection indicators.
Please note that some contents of this document may involve patents. The issuing
agency of this document does not assume the responsibility for identifying these patents.
This standard was proposed by the State Tobacco Monopoly Administration.
This standard shall be under the jurisdiction of the Tobacco Materials Sub-Technical
Committee of the National Tobacco Standardization Technical Committee (SAC/TC
144/SC 8).
The drafting organizations of this standard. Shanghai Tobacco Group Co., Ltd.,
Zhengzhou Tobacco Research Institute, China Tobacco Standardization Research
Center, National Tobacco Quality Supervision and Inspection Center, Guangdong
China Tobacco Industry Co., Ltd., Yunnan Tobacco Science Research Institute,
Hongyun Honghe Tobacco (Group) Co., Ltd., Fujian China Tobacco Industry Co., Ltd.,
Hunan China Tobacco Industry Co., Ltd., Hongta Tobacco (Group) Co., Ltd., Henan
China Tobacco Industry Co., Ltd., Jiangxi China Tobacco Industry Co., Ltd., Yunnan
China Tobacco Industry Co., Ltd.
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
3.2.1.10 n-Butanol.
3.2.1.11 Acetone.
3.2.1.12 4-Methyl-2-pentanone.
3.2.1.13 Butanone.
3.2.1.14 Cyclohexanone.
3.2.1.15 Ethyl acetate.
3.2.1.16 n-Propyl acetate.
3.2.1.17 n-Butyl acetate.
3.2.1.18 Isopropyl acetate.
3.2.1.19 2-Ethoxyethyl acetate.
3.2.1.20 1-Methoxy-2-propanol.
3.2.2 Other solvent residue standard samples
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.
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.
4.2 Gas chromatograph, instrument conditions of which are as follows.
4.3 Mass spectrometer, instrument conditions of which are as follows.
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.
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.
5.4 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;
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.
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.
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).
8 Repeatability, recovery, detection limit
The repeatability, recovery, detection limit results of this method are shown in Appendix
C.
9 Test report
The test report shall state.
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
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009 and
GB/T 20001.4-2001.
This standard replaces YC/T 207-2006 "Determination of volatile organic compounds
in cigarette carton and packet packaging papers - Headspace-gas chromatography".
Compared with YC/T 207-2006, the main technical changes of this standard are as
follows.
- CHANGE the name of the standard to "Determination of solvent residuals on
papers for cigarette - Headspace-gas chromatography/mass spectrometry";
- ADJUST the scope of application, to add cigarette paper such as cigarette tipping
paper and cigarette lining paper;
- MODIFY the instrument detection method and detection indicators.
Please note that some contents of this document may involve patents. The issuing
agency of this document does not assume the responsibility for identifying these patents.
This standard was proposed by the State Tobacco Monopoly Administration.
This standard shall be under the jurisdiction of the Tobacco Materials Sub-Technical
Committee of the National Tobacco Standardization Technical Committee (SAC/TC
144/SC 8).
The drafting organizations of this standard. Shanghai Tobacco Group Co., Ltd.,
Zhengzhou Tobacco Research Institute, China Tobacco Standardization Research
Center, National Tobacco Quality Supervision and Inspection Center, Guangdong
China Tobacco Industry Co., Ltd., Yunnan Tobacco Science Research Institute,
Hongyun Honghe Tobacco (Group) Co., Ltd., Fujian China Tobacco Industry Co., Ltd.,
Hunan China Tobacco Industry Co., Ltd., Hongta Tobacco (Group) Co., Ltd., Henan
China Tobacco Industry Co., Ltd., Jiangxi China Tobacco Industry Co., Ltd., Yunnan
China Tobacco Industry Co., Ltd.
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
3.2.1.10 n-Butanol.
3.2.1.11 Acetone.
3.2.1.12 4-Methyl-2-pentanone.
3.2.1.13 Butanone.
3.2.1.14 Cyclohexanone.
3.2.1.15 Ethyl acetate.
3.2.1.16 n-Propyl acetate.
3.2.1.17 n-Butyl acetate.
3.2.1.18 Isopropyl acetate.
3.2.1.19 2-Ethoxyethyl acetate.
3.2.1.20 1-Methoxy-2-propanol.
3.2.2 Other solvent residue standard samples
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.
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.
4.2 Gas chromatograph, instrument conditions of which are as follows.
4.3 Mass spectrometer, instrument conditions of which are as follows.
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.
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.
5.4 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;
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.
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.
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).
8 Repeatability, recovery, detection limit
The repeatability, recovery, detection limit results of this method are shown in Appendix
C.
9 Test report
The test report shall state.
......
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 14 pages — is available in the English PDF.
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