GB/T 4615-1984 Determination of residual vinyl chloride monomer content in polyvinyl chloride resin

This standard is a method for determining the residual vinyl chloride monomer (RVCM) content in polyvinyl chloride (PVC) resin by liquid gas chromatography. It is applicable to the determination of residual vinyl chloride monomer in vinyl chloride (VC) homopolymer, copolymer resin and its products. The minimum detection amount of this method is 0.5 mg/kg. The method for determining the residual vinyl chloride monomer content in polyvinyl chloride resin by solid gas chromatography is shown in Appendix A. GB/T 4615-1984 Method for determining the residual vinyl chloride monomer content in polyvinyl chloride resin GB/T4615-1984 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Determination method of residual yinylchloride monomer contents in polyvinyl chloride resin
Determination method of residual yinylchloride monomer contents in polyvinyl chloride Scope of application
UDC 678.743.22
: 678.742.2
GB4615—84
This standard is a method for determining the residual yinylchloride monomer (RVCM) content in polyvinyl chloride (PVC) resin by headspace gas chromatography. It is applicable to the determination of residual yinylchloride monomer in vinyl chloride (VC) homopolymer, copolymer resin and its products. The minimum detection amount of this method is 0.5mg/kg. The method for determining the residual yinylchloride monomer content in polyvinyl chloride resin by headspace gas chromatography is shown in Appendix A. 2 Principle of the method
Dissolve the sample in a suitable solvent and determine the yinyl chloride content by headspace gas chromatography with gas phase sampling. Reagents and materials
Vinyl chloride: Purity greater than 99.5%.
3.2N, N-dimethylacetamide (DMAC): Does not contain any impurities with the same chromatographic retention time as vinyl chloride under the test conditions.
3.3 Air, nitrogen, hydrogen.
4 Storage and preservation of samples
Fill samples with qualified moisture content into wide-mouth bottles according to batch numbers and seal them for storage. The measurement must be carried out within 24 hours. If the storage time exceeds 24 hours, the storage time of the sample must be indicated. Samples of polyvinyl chloride products can be placed in wide-mouth bottles with lids. 5 Instruments
5.1 Gas chromatograph: with hydrogen flame ionization identifier (FID). 5.2 Chromatographic column: The chromatographic column used should be able to completely separate impurities from vinyl chloride in the sample. The chromatographic peak height obtained for a solution containing 0.02 mg of vinyl chloride per liter or per dry gram is at least 5 times the baseline noise. The chromatographic columns and test conditions that can be used are listed in Appendix B (reference). 5.3 Thermostat: 70±1℃, with sampling hole. 5.4 Medical syringes: 1, 5 ml, several. 5.5 Micro syringes: 1, 10, 100μ1, several. 5.6 Sample bottle: 25±0.5ml, operating temperature 90℃, pressure resistance 0.5kgf/cm2, with silicone rubber cover and metal screw sealing cap. As shown in the figure.
National Bureau of Standards 1984-07-30 Issued
1985-05-01 Implementation
Analytical balance: graduation value is 0.1mg.
Stopwatch: graduation value is 0.2s.
5.9 Pressure-resistant fluoroethylene container: 50~100ml. 5.10 Magnetic stirrer.
Electronic calculator.
Graduated magnifying glass or reading microscope.
Safety measures
GB 4615--84
Vinyl chloride is a harmful gas, so when preparing samples and discharging, it must be carried out in a fume hood. Preparation of vinyl chloride standard gas and standard sample
7.1 Preparation of standard gas: Put a few glass beads in the sample bottle, cover it tightly and seal it, and weigh it on an analytical balance (accurate to 0.1mg). Use a syringe to take out 5ml of gas from the vinyl chloride container (wash the syringe with vinyl chloride gas twice when taking gas) and inject it into the bottle, and then weigh it (accurate to 0.1mg). Shake it well and let it stand for 10 minutes, then use it immediately. The gas concentration C is about 400μg/ml. It can be calculated according to formula (1): Ci =
Wz-Wl×106
-weight of the sample bottle with glass beads, g,
-weight of the sample bottle with glass beads after 5ml of vinyl chloride gas is injected, g,-volume of the sample bottle, ml,
-volume of vinyl chloride added, ml.
7.2 Preparation of standard samples: Use a micro syringe to accurately inject 3ml of DMAC into three sample bottles in two series, and then accurately inject 0.5, 5, and 50μl of standard gas respectively, shake well for use. The content of vinyl chloride monomer (VCM) (μg) in each standard sample is calculated according to formula (2):
vcm=c,xV
Where: Ci standard gas concentration, μg/ml, 1.10
V added standard gas volume, ml.
8 Analysis steps
8.1 Preparation of sample solution
GB 4615--84
8.1.1 Weigh two well-mixed samples (0.3~0.5g (accurate to 0.1mg) on ​​an analytical balance, place them in a sample bottle, then place a Φ2mm×25mm galvanized iron wire, and immediately cover it tightly. 8.1.2 Place the above sample bottle on an electromagnetic stirrer, and under slow stirring, accurately inject 3mIDMAC with a syringe to dissolve the sample.
8.2 Sample balance
8.2.1 Place the standard sample and the sample together in a thermostat (70±1℃) for more than 30 minutes, so that vinyl chloride can reach equilibrium in the gas and liquid phases.
8.2.2 Use a syringe to quickly take out 1ml of the upper gas from the balanced standard sample and sample bottle in turn, and inject it into the chromatograph for analysis (when the sample content is low, 2~3ml of gas can be taken, but it is necessary to ensure that there is a standard sample with a similar content, and take the same amount of gas, and analyze it at the same sensitivity of the instrument), and record the peak area (or peak height) of vinyl chloride. Note: The syringe is pre-heated to the same temperature as the sample. 9 Result expression
Residual vinyl chloride monomer (RVCM) content in the sample (mg/kg), calculated according to formula (3): RVCM = -A×C ×V
Wherein: A
The peak area (or peak height) of nitrogen and vinyl in the sample, cm2 (or mm), the peak area (or peak height) of the standard sample with a content close to that of the sample, cm2 (or mm), the concentration of the standard gas, μg/ml,
The volume of the standard sample with a content close to that of the sample, ml; - Sample weight, g.
The arithmetic mean of the results of two parallel tests is taken as the result of this test. 10
Test report
The test report should include the following contents:
Indicate the method adopted in this standard,
The complete mark of the test material (manufacturer, model, grade, batch number and shape), the chromatographic column used and the working conditions,
The results of two parallel tests and their arithmetic mean, the test personnel and the date.
下减造罗
（3）
GB4615-84
Appendix A
Determination of residual vinyl fluoride monomer content in polyvinyl fluoride
resin by solid-state gas chromatography
(reference)
This method is based on the vapor equilibrium established in a closed system between polyvinyl chloride resin, residual vinyl chloride monomer and air. This method is applicable to the determination of residual vinyl chloride monomer (RVCM) content in polyvinyl chloride homopolymer (PVC) resin. The minimum detection limit of this method is 0.2 mg/kg. In addition to the following contents, the reagents and materials, storage and preservation of samples, instruments, safety measures, reporting of test results, chromatographic columns and working conditions, etc. refer to the relevant chapters of the standard text and Appendix B. A.1 Preparation of fluoroethylene standard gas and standard sample A.1.1 Preparation of standard gas
Use a syringe to take 5 ml of chloroethylene gas from a pressure-resistant chloroethylene container and inject it into a sealed sample bottle. Its concentration C2 (ml/ml) is calculated according to formula (A1):
Where: V1-the volume of the sample bottle, 23.5 ml, V2
the volume of the added chloroethylene gas, ml. V2
A.1.2 Preparation of standard sample
Use a microsyringe to accurately inject 1.2, 12 and 120 μl of standard gas into three sample bottles in two series, respectively. The content of vinyl chloride monomer (VCM) in each standard sample (ul/ml) is calculated according to formula (A2), V
VCM =C2×
Wherein: C2
is the volume concentration of vinyl chloride in the standard gas, ml/ml, is the volume of the added standard gas, ml,
is the volume of the sample bottle, ml.
Note: If the content of vinyl chloride in the sample to be tested can be estimated in advance, only one standard sample with a content close to that in the sample to be tested can be prepared, without having to make two standard samples at the same time.
A.2 Analysis stepswwW.bzxz.Net
A.2.1 Sample preparation
Weigh 4±0.5g (accurate to 0.1mg) of the well-mixed resin sample, place it in a sample bottle, and immediately cover it. A.2.2 Sample balance
Put the standard sample and the sample bottle together in a thermostat (90±1℃) and keep the temperature constant for more than 60 minutes to allow the vinyl chloride to reach equilibrium in the gas and solid phases.
A.3 Result expression
A.8.1 The residual vinyl chloride monomer (RVCM) content (mg/kg) in the sample is calculated according to formula (A3): 6.095721 × 10-2
(4.257768 × 10 3+ - 6
Wherein: As——RVCM peak area in the sample, cm2, Rf——-response factor, (standard sample peak area/standard sample volume, cm2/ppm), 112
sample weight,
A.3.2 The test conditions for this method are as follows: room temperature: 22℃ (295K),
equilibrium temperature: 90℃ (363K);
atmospheric pressure: 750mmHg;
sample bottle volume: 23.5ml,
sample water content: less than 0.5%.
GB 4615--84
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B.1 See the table below for applicable chromatographic columns:
Column length, m
Diameter, mm
B.2 Temperature and constant temperature accuracy of each part of the chromatograph: Chromatographic column: 50±0.5℃,
Detection chamber: 120±1℃,
Vaporization chamber: 110±1℃.
B.3 Gas flow rate:
Ammonia: 30ml/minz
Hydrogen: 50ml/min,
Air: 350~400ml/min.
GB 4615--84
Appendix B
Applicable chromatographic columns and working conditions
(reference)
6201 Glazed support
(80-100 days)
407 Organic support
80-100 mesh)
Stationary liquid composition
(weight ratio)
8,β'-oxydipropionitrile:
Silicone oil blood = 2:1
Stationary liquid/support
(weight ratio)
Column temperature, ℃
Additional remarks:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. It is under the jurisdiction of the Chemical Method Sub-Technical Committee of the National Technical Committee for Plastics Standardization.
This standard was drafted by Jinxi Chemical Research Institute. The main drafters of this standard are An Shaohua, Rong Yufang and Zhang Zhenying. 144
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