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GB/T 24153-2009 PDF in English

GB/T 24153-2009 (GB/T24153-2009, GBT 24153-2009, GBT24153-2009)
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GB/T 24153-2009: PDF in English (GBT 24153-2009)

GB/T 24153-2009
ICS 83.060
G 40
Rubber and Elastomer Materials
– Determination of N-nitrosamines
ISSUED ON. JUNE 15, 2009
Issued by. General Administration of Quality Supervision, Inspection and
Standardization Administration of PRC.
3. No action is required - Full-copy of this standard will be automatically &
immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Analytical Procedures ... 5
6 Result calculation ... 7
7 Determination Lower Limit ... 7
8 Test Report ... 7
Appendix A (Normative) 12 Types of N-Nitrosamines Names and their
GC/MS Selective Quantitative Ions ... 9
Appendix B (Informative) N-Nitrosamines Standard Products’ GC/MS Total
Ion Flow Diagram ... 10
This Standard’s Appendix A is normative; while Appendix B is informative.
This Standard was proposed by China Petroleum and Chemical Industry Association.
This Standard shall be under the jurisdiction of National Technical Committee for
Standardization of Rubber and Rubber Products (SAC/TC 35).
Drafting organizations of this Standard. Fujian Putian Entry-Exit Inspection and
Quarantine Bureau, Shenyang Rubber Research and Design Institute, and Fujian
Quanzhou Entry-Exit Inspection and Quarantine Bureau.
Chief drafting staffs of this Standard. Tong Yugui, Cheng Qun, Lin Bifen, Li Yijun, Liu
Huichun, and Lin Zhong.
Rubber and Elastomer Materials
– Determination of N-nitrosamines
Warning. personnel using this Standard shall have practical working experience
in the formal laboratory. This Standard doesn’t indicate all possible laboratory
work. The users shall take responsibility to take appropriate safety and health
measures; and ensure compliance with the conditions set forth in the relevant
national regulations.
1 Scope
This Standard specifies adopting gas chromatography – mass selective detector (GC-
MSD) to determine 12 types of N-nitrosamines (see Appendix A) contents in the rubber
and elastomer.
This Standard is applicable to the rubber, elastomer materials and their products.
2 Principle
The sample was extracted by methanol; after concentrating, the extracting solution
passes through C18 solid-phase extraction column to purify; the sample solution enters
into the gas chromatography – mass selective detector (GC-MSD) to be measured;
qualified by full-scanning detection; select ions to quantify by external standard method.
3 Reagents and Materials
Unless otherwise is specified, all the reagents used are chromatographic pure.
3.1 Methanol, the blank test check there are no interfering substances.
3.2 C18 solid-phase extraction column. 500mg/3mL.
3.3 Standard stock solution. separately and accurately weigh the appropriate amount
of each N-nitrosamines standard products; use methanol to prepare the standard stock
solution with concentration of 200mg/L; inject into the brown reagent bottle; store in
the refrigerator at 5°C below; and valid for 3 months.
NOTE. N-nitrosamines substances are easy to be decomposed by the ultraviolet rays; the
extracting solution and standard solution shall avoid exposing to the sunshine or fluorescent
lamps or other light sources. The sample or standard solution shall be wrapped by aluminum
foil or stored in the dark at 5°C below.
3.4 Standard working solution. take appropriate volume of standard stock solution
(3.3) as required to mix; then use methanol to dilute to the standard working solution
with suitable concentration; inject into the brown reagent bottle; it shall be prepared for
current use.
4 Apparatus
4.1 Gas chromatograph. equipped with mass selective detector (MSD).
4.2 Ultrasonic generator. operating frequency of 40kHz.
4.3 Rotary evaporator. equipped with vacuum gauge (can show the vacuum to
4.4 Solid-phase extraction device. equipped with vacuum pump.
4.5 Vortex mixer.
4.6 Conical flask. brown, with ground stopper, 100mL.
4.7 Concentrated bottle. brown, 150mL.
4.8 Centrifuge tube. brown, 10mL.
5 Analytical Procedures
5.1 Specimen preparation and extraction
Take the representative sample, use appropriate tool to cut it into particles with edges
of 3mm below, mix evenly. Take 5.0g (accurate to 0.01g) of specimen from the above
mixed sample; place into conical flask (4.6); add 30mL of methanol (3.1); perform the
ultrasonic extraction in the ultrasonic generator (4.2) for 30min. Transfer the extracting
solution into the concentrated bottle (4.7); add 20mL of methanol into the conical flask;
extract once again; combine the extracting solutions. Place the concentrated bottle
onto the rotary evaporator (4.3); control the vacuum degree to be 21.3kPa~16.3kPa;
slowly concentrate in the 35°C water bath, so that the volume is slightly less than
4.5mL. Take off the concentrated bottle; rotate and shake fully onto the vortex mixer
(4.5) for 1min (so that the substances attached on the bottle wall can dissolve into the
extracting solution); the transfer the sample solution in the concentrated bottle into 5mL
brown volumetric flask. Take another 0.5mL of methanol to leach the concentrated
bottle wall; after rotating and shaking fully on the vortex mixer for 1min, transfer into
the volumetric flaks to combine; use methanol to make constant volume of 5mL; shake
5.2 Purification
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.