GB/T 24153-2009 English PDF (GB/T24153-2009)

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GB/T 24153-2009: Rubber and Elastomer Materials - Determination of N-nitrosaminess
GB/T 24153-2009
Rubber and elastomer materials.Determination of N-nitrosamines
ICS 83.060
G40
National Standards of People's Republic of China
Rubber and elastomer materials - Determination of N - nitrosamine
2009-06-15 released
2010-02-01 Implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
China National Standardization Management Committee released
Preface
Appendix A of this standard is a normative appendix, Appendix B is an informative appendix.
This standard is proposed by the China Petroleum and Chemical Industry Association.
This standard by the National Rubber and Rubber Products Standardization Technical Committee (SAC/TC35) centralized.
The drafting of this standard. Fujian Putian Entry-Exit Inspection and Quarantine Bureau, Shenyang Rubber Research and Design Institute, Fujian Quanzhou Entry-Exit Inspection and Quarantine Bureau.
The main drafters of this standard. Tong Yugui, Cheng Qun, Lin Bifen, Li Yijun, Liu Huichun, Lin Zhong.
Rubber and elastomer materials - Determination of N - nitrosamine
WARNING. Personnel using this standard should have practical experience in formal laboratory work. This standard does not indicate all possible security issues.
It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with the conditions set forth in the relevant national regulations.
1 range
This standard specifies the use of gas chromatography - mass selection detector (GC-MSD) determination of rubber and elastomer materials in the 12 kinds of N-nitroso
Amine (see Appendix A).
This standard applies to rubber, elastomer materials and their products.
2 principle
The sample was extracted with methanol and the extract was concentrated and purified by C18 solid phase extraction column. The sample was passed into a gas chromatography-mass selective detector
(GC-MSD), the full-scan detection was used to qualitatively select the ions to quantify the external standard method.
3 reagents and materials
Unless otherwise specified, the reagents used are chromatographic pure.
3.1 methanol, the blank test to check the presence of non-interfering substances.
3.2 C18 solid phase extraction cartridge. 500mg/3mL.
3.3 standard stock solution. respectively, accurately weighed the appropriate amount of each N-nitrosamine standards, with methanol were prepared into a concentration of.200mg/L
Of the standard stock solution, installed in a brown reagent bottle, stored in less than 5 ℃ refrigerator, valid for 3 months.
Note. N-nitrosamines are easily decomposed by UV, and the extract or standard solution should be exposed to light sources such as sunlight or fluorescent lamps. Sample or standard solution
It is wrapped in aluminum foil or stored in brown in a dark place below 5 ° C.
3.4 standard working solution. according to the need to take the appropriate volume of standard stock solution (3.3) for mixing, and then diluted with methanol to the appropriate concentration of the standard
Quasi-working solution, installed in the brown reagent bottle, is now with the current use.
4 instruments and equipment
4.1 Gas Chromatograph. Equipped with a mass selection detector (MSD).
4.2 Ultrasonic generator. Operating frequency 40kHz.
4.3 Rotary Evaporator. equipped with a vacuum table (can show the vacuum to 10kPa).
4.4 solid phase extraction device. equipped with a vacuum pump.
4.5 vortex mixer.
4.6 conical flask. brown, with a mouth plug, 100mL.
4.7 Concentrated bottles. brown, 150mL.
4.8 Centrifuge tube. brown, 10mL.
5 Analysis steps
5.1 Preparation and extraction of samples
Take a representative sample, with the appropriate tools to the edge of the length of 3mm below the particles, mix. Weigh the sample from the above mixture
5.0 g (accurate to 0.01 g) was placed in a Erlenmeyer flask (4.6), 30 mL of methanol (3.1) was added, and the ultrasonic generator (4.2)
Extraction for 30 min. The extract was transferred to a concentrated flask (4.7), and 20 mL of methanol was added to the Erlenmeyer flask, and the extract was repeatedly extracted and the extracts were combined.
The concentrated flask was placed on a rotary evaporator (4.3) and the degree of vacuum was controlled at 21.3 kPa to 16.3 kPa, slowly concentrated in a 35 ° C water bath to slightly less
4.5 mL. Remove the concentrated flask and shake it well for 1 min on the vortex mixer (4.5) for easy packing
Liquid), and then the concentrated bottle of sample solution into the 5mL brown volumetric flask. Take another 0.5mL methanol leaching concentrated bottle wall, on the vortex mixer
Full rotation shaking 1min, into the volumetric flask merger, with methanol volume to 5mL, shake.
5.2 purification
The C18 solid phase extraction column (3.2) was placed on a solid phase extraction apparatus (4.4), the C18 column was pre-eluted with 5 mL of methanol, and the effluent was discarded.
Accurately draw 2.0 mL of sample solution (see 5.1) into the column, the effluent is collected in the centrifuge tube (4.8); the liquid level of the sample is lowered to the column packing
The upper surface, then add 2mL methanol for elution, the collection of all the effluent in the centrifuge tube. And then blow it with a slow nitrogen stream
2mL, sample solution shaken after the brown into the sample vial, sealed cold preservation to be tested.
5.3 Determination
5.3.1 Gas chromatography-mass spectrometry conditions
Since the test results depend on the instrument used, it is not possible to give a general parameter for chromatographic analysis. The operating parameters given below have been
Proved to be feasible, only as a reference when measured.
a) Capillary column. DB-5MS 30m × 0.25mm × 0.25μm, or equivalent;
b) Column temperature. 38 ° C (4 min)
8 ° C /
→ 
min
83 ° C (4 min)
15 ° C /
→ 
min
300 ℃ (6min);
c) Inlet temperature. 260 ° C;
d) mass spectrometer interface temperature. 280 ° C;
e) Carrier gas. helium (purity ≥99.999%), flow rate. 1.0 mL/min;
f) ionization mode. EI;
g) ionization energy. 70 eV;
h) mass scanning range. 35 amu ~ 260mmu;
i) Injection method. no split injection;
j) Injection volume. 1 μL.
5.3.2 Qualitative and quantitative analysis of gas chromatography-mass spectrometry
Respectively, take 1μL standard working solution (3.4) and sample solution (see 5.2) into the chromatograph for determination. If the sample is working with a standard working solution
Of the total ion flow diagram, at the same retention time there is a chromatographic peak, by comparing the sample with the standard character of the characterization of the ion, with the choice of
Ion monitoring method for external standard method.
According to the content of the sample in the sample solution, the selected concentration of similar standard working solution, the standard working solution and sample volume and other volume insert
The response values of each N-nitrosoamine in the standard working solution and the sample solution shall be within the linear range of the instrumentation.
Note 1. If the test response value of the sample solution exceeds the linear range of the instrument detection, it can be appropriately diluted and measured.
Note 2. Under the above analysis conditions, see Appendix B for the total ion chromatogram of the 12 N-nitrosamine standards for gas chromatography-mass spectrometry.
6 results calculated
The content of each N-nitrosamine in the sample is calculated from equation (1)
(1)
Where.
The volume of volume in the V - sample solution (see 5.1), in milliliters (mL);
The result of the calculation indicates one after the decimal point. When the results of more than 100mg/kg, said to a bit.
7 Determination of low limit
The limit of this method is 0.5 mg/kg.
8 test report
The test report shall at least give the following.
a) the standard number;
b) sample description;
c) test results;
d) Deviation from this standard;
e) Test date.
Appendix A
(Normative appendix)
Determination of Quantitative Ion by GC/MS of 12 N - nitrosamines and Their Standards
Table A. 1
N-nitrosoamine name English name
Chemical Abstract Number
(CASNo.)
Chemical formula
Quantitative ion /
amu
1 N-nitrosodimethylamine N-nitrosodimethylamine 62-75-9 C2H6N2O 74
2 N-nitrosomethyl-ethylamine 10595-95-6 C3H8N2O 88
3 N-nitrosodiethylamine 55-18-5 C4H10N2O 102
4 N-nitrosopyrrolidine N-nitrosopyrrolidine 930-55-2 C4H8N2O 100
5 N-nitroso-N-methylaniline N-nitroso-N-methylaniline 614-00-6 C7H8N2O 106
6 N-nitrosomorpholine N-nitrosomorpholine 59-89-2 C4H8N2O2 56
7 N-nitrosodipropylamine 621-64-7 C6H14N2O 70
8 N-nitrosopiperidine N-nitrosopiperidine 100-75-4 C5H10N2O 114
9 N-nitroso-N-ethylaniline N-nitroso-N-ethylaniline 612-64-6 C8H10N2O 106
10 N-nitrosodibutylamine N-nitrosodibutylamine 924-16-32 C8H18N2O 84
11 N-nitrosodiphenylamine N-nitroso-diphenylamine 86-30-6 C12H10N2O 169
12 N-nitrosodibenzylamine 5336-53-8 C14H14N2O 91
Appendix B
(Informative)
The total ion chromatogram of GC/MS for N - nitrosamine standards
1 --- N-nitrosodimethylamine
2 --- N-nitrosomethyl ethylamine
3 --- N-nitroso diethylamine
4 --- N-nitroso pyrrolidine
5 --- N-nitroso-N-methylaniline
6 --- N-nitroso morpholine
7 --- N-nitrosodipropylamine
8 --- N-nitroso piperidine
9 --- N-nitroso-N-ethylaniline
10 --- N-nitrosodibutylamine
11 --- N-nitrosodiphenylamine
12 --- N-nitrosodibenzylamine
Figure B 1/N-nitrosamine standards GC/MS total ion flow chart