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(Rubber and rubber products. Determination of 3,3'-dichloro-4,4'-diaminodiphenylmethane. Meteorological chromatography-mass spectrometry)
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Basic data
| Standard ID | SN/T 5272-2019 (SN/T5272-2019) |
| Description (Translated English) | (Rubber and rubber products. Determination of 3,3'-dichloro-4,4'-diaminodiphenylmethane. Meteorological chromatography-mass spectrometry) |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | G34 |
| Classification of International Standard | 83.040 |
| Word Count Estimation | 7,725 |
| Date of Issue | 2019 |
| Date of Implementation | 2020-07-01 |
| Issuing agency(ies) | General Administration of Customs |
SN/T 5272-2019: (Rubber and rubber products. Determination of 3,3'-dichloro-4,4'-diaminodiphenylmethane. Meteorological chromatography-mass spectrometry)
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
2019-12-27 release
2020-07-01 Implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organization of this standard. Fuzhou Customs of the People's Republic of China.
The main drafters of this standard. Chen Minshi, Tang Huanyu, Chen Xiangming, Li Xiaojing, Lou Yu, Lai Jiajia, Wang Wei, Wu Minjian, Chen Qinglan.
Determination of 3,3'-dichloro-4,4'-diaminodiphenylmethane in rubber and rubber products
Gas chromatography-mass spectrometry
1 Scope
This standard specifies the gas chromatography-mass spectrometry method for the determination of 3,3'-dichloro-4,4'-diaminodiphenylmethane in rubber and rubber products.
This standard applies to the determination of 3,3'-dichloro-4,4'-diaminodiphenylmethane in rubber and rubber products.
The lower limit of determination in this standard is 20.0 mg/kg.
2 Method summary
The sample was ultrasonically extracted with ethyl acetate, the extract was centrifuged and filtered, and the filtrate was determined by gas chromatography-mass spectrometer and quantified by internal standard method.
3 Reagents and materials
3.1 Ethyl acetate. chromatographically pure.
3.2 3,3'-Dichloro-4,4'-Diaminodiphenylmethane (C13H12Cl2N2, CAS number. 101-14-4). Purity ≥ 98.8%.
3.3 Deuterated perylene (C20D12, CAS number. 1520-96-3). purity ≥ 99.0%.
3.4 Standard stock solution (1 g/L). accurately weigh 0.1 g (accurate to 0.1 mg) 3,3'-dichloro-4,4'-diaminodiphenylmethane (3.2)
Dissolve the standard substance in a 100 mL volumetric flask with ethyl acetate (3.1) and dilute to the mark. Store it in a sealed and dark place at 0 ℃ ~ 4 ℃.
It is valid for one month.
3.5 Internal standard solution (0.5 g/L). accurately weigh out 0.05 g deuterated perylene (3.3) in a 100 mL volumetric flask, and dissolve it with ethyl acetate (3.1)
Solve and dilute to the mark. Store in a sealed and dark place at 0 ℃ ~ 4 ℃. The validity period is one month.
3.6 Standard working solution. draw an appropriate amount of standard stock solution (3.4) and internal standard solution (3.5), and use a stepwise dilution method.
Ethyl acetate (3.1) is formulated into 3,3'-dichloro-4,4'-diaminodiphenylmethane with a concentration of 0 mg/L, 2 mg/L, 5 mg/L, 10 mg/L,
A series of standard working solutions of 20 mg/L, 50 mg/L and the internal standard concentration of 20 mg/L.
4 Apparatus and equipment
4.1 Gas chromatography-mass spectrometer. equipped with EI source.
4.2 Analytical balance. Sensitivity 0.1 mg.
4.3 Ultrasonic oscillator. the power is not less than 220 W.
4.4 Centrifuge. the speed is not less than 2 500 r/min.
4.5 Pipette gun. 1 000 μL.
4.6 Pipette. 1 mL, 2 mL, 5 mL, 20 mL.
4.7 Plastic centrifuge tube with lid. 50 mL.
4.8 Needle organic filter. 0.45 μm.
4.9 Cutting tools. cutting knives, scissors, sharp knives or other suitable tools.
5 Sample preparation
Use the cutting tool (4.9) to make the sample into a sample of about 1 mm, and use it for the test after mixing.
6 Analysis steps
6.1 Extraction
Accurately weigh 0.5 g (accurate to 0.1 mg) of the sample into a plastic centrifuge tube (4.7) with a lid, and accurately add 20 mL of ethyl acetate (3.1),
Immediately cover and seal, mix well, ultrasonically extract at room temperature for 20 minutes, then centrifuge at 2500 r/min for 3 minutes, and take the upper layer of centrifugal liquid with needle organic
The filter head (4.8) filters. Accurately pipette 0.2 mL internal standard solution (3.5) into a 5 mL volumetric flask, dilute to the mark with the filtrate, and mix well
It is then tested by gas chromatography-mass spectrometer.
6.2 Blank test
Except that no sample is added, follow the above steps to obtain a blank sample solution.
6.3 Determination
6.3.1 Reference conditions for gas chromatography-mass spectrometry
The reference conditions are as follows.
a) Chromatographic column. HP-5MS, 30 m×0.25 mm (inner diameter)×0.25 μm (film thickness), or equivalent;
b) Heating program. initial temperature 60 ℃, keep for 2 min; increase temperature at 20 ℃/min to 270 ℃, keep 1 min; at 30 ℃/min
min Raise the temperature to 300 ℃ and keep it for 10 min;
c) Carrier gas. helium, purity ≥ 99.999%;
d) Flow rate. 1 mL/min;
e) Inlet temperature. 280 ℃;
f) Diversion mode. Diversion ratio, 5.1;
g) Injection volume. 1 μL;
h) Chromatography-mass spectrometry interface temperature. 280 ℃;
i) Ion source temperature. 230 ℃;
j) Quadrupole temperature. 150 ℃;
k) Ionization method. EI;
l) Ionization energy. 70 eV;
m) Solvent delay. 4 min;
n) Measurement method. Selected ion monitoring (SIM), the SIM parameters are shown in Table 1.
6.3.2 Standard working curve drawing
Inject the standard working solution (3.6) in order of concentration from low to high, and inject according to the reference conditions of gas chromatography-mass spectrometry (6.3.1)
Measure the concentration ratio of the target substance to the internal standard substance in the standard working solution (3.6) as the abscissa, and use the peak area of the corresponding quantitative ion
The ratio is the ordinate, and the standard working curve is drawn.
6.3.3 Qualitative
Compare the measurement results of the standard working solution (3.6) with the sample solution to be tested. If the retention time of the chromatographic peak in the sample solution to be tested is compared with that of the standard solution
The selected ion abundance ratio of the target compound in the sample solution to be tested is consistent with that of the standard working solution (3.6) (within ±2.5%).
If the abundance ratio of the solution (3.6) is consistent, and the relative abundance deviation does not exceed the regulations in Table 2, then it can be judged that there is a target in the sample solution to be tested.
Compound. 6.3.4 Quantitative
Test the blank sample solution and the sample solution to be tested in turn to obtain the quantitative ion peak area ratios of the target and the internal standard.
The curve obtains the concentration of the target substance in the sample solution. The response value of the target in the sample solution should be within the linear range of the standard working curve.
Out of the linear range, use ethyl acetate (3.1) to dilute to the concentration contained in the linear range.
7 Result calculation
The calculation result is expressed as the arithmetic average of two independent measurement results obtained under repeatability conditions, and the result is kept to one decimal place.
8 Precision
Under repeatability conditions, the absolute difference between the two independent determination results is not more than 10% of the arithmetic mean; under repeatability conditions,
The absolute difference between the results of the two laboratories is not more than 15% of the arithmetic mean.
Appendix A
(Informative appendix)
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