Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2305—92
Industrial Methyl Methacrylate
Published on May 17, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993Www.bzxZ.net
W Chemical Industry Standard of the People's Republic of China
Industrial Methyl Methacrylate
Subject Content and Scope of Application
HG2305-—92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation, storage, etc. of industrial methyl methacrylate.
This standard applies to methyl methacrylate produced by the acetone cyanohydrin method. This product is mainly used to manufacture organic glass, molding plastics and other synthetic resins.
Molecular formula: CH2C (CH:) COOCHs
Relative molecular mass: 100.12 (according to the international relative atomic mass in 1989) 2 Reference standards
GB1250
GB2366
GB3143
GB4472
GB6283
GB6678
GB6680
GB8170
GB9722
3 Technical requirements
3.1 Appearance
Dangerous goods packaging mark
Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) Preparation of preparations and products used in chemical reagent test methods Methods for expressing and determining limit values Determination of water content in chemical products Gas chromatography Color determination of liquid chemical products (Hazen unit - platinum-cobalt color number) General rules for determination of density and relative density of chemical products Determination of water content in chemical products Karl Fischer method (general method) General rules for sampling of chemical products
General rules for sampling of liquid chemical products
Rules for rounding off values
General rules for gas chromatography
Chemical reagents
Colorless and transparent liquid, without turbidity and suspended matter. 2 Industrial methyl methacrylate should meet the requirements of the following table. 3.2
Chroma (platinum-cobalt), No.
Density (P2O), g/cm3
Acid content (as methacrylic acid), %
Water, %
Methyl methacrylate content, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on 1992-05-17>
Superior product
0.942~0.946
Qualified product
0.938~0.948
Implemented on 1993-01-01
W.4 Test method
HG2305-92
Unless otherwise specified, the reagents and water used in this test method are of analytical grade reagents and distilled water or water of equivalent purity. The standard solutions, preparations and products used in this test method shall be prepared in accordance with the provisions of GB601 and GB603 unless otherwise specified.
4.1 Determination of chromaticity
Perform in accordance with the provisions of GB3143. Use 100mL Nessler colorimetric tube. 4.2 Determination of density
Perform in accordance with the provisions of Article 2.3.3 of GB4472. 4.2.1 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.0005g/cm3, and the arithmetic mean shall be taken as the determination result. 4.3 Determination of acid content
4.3.1 Principle
In ethanol medium, use bromothymol blue as the indicator solution and neutralize with sodium hydroxide standard titration solution. 4.3.2 Reagents and solutions
Ethanol: 95%;
Bromothymol blue indicator solution: 1g/L
c. Sodium hydroxide standard titration solution: c (NaOH) = 0.01 mol/L. 4.3.3 Analysis steps
In a conical flask, add 20-50 mL of ethanol and 2 drops of bromothymol blue indicator solution, use sodium hydroxide standard titration solution to titrate until the color turns blue, use a pipette to add a sample of the same volume as ethanol, and use sodium hydroxide standard titration solution to titrate until the color turns blue. The end point is considered if the color does not fade for 15 seconds. 4.3.4 Expression of analysis results
The acid content (in terms of methacrylic acid) expressed as a percentage by mass (X) is calculated according to formula (1): Xi = V1:0X 0.086
Wherein: Vi is the volume of the standard sodium hydroxide titration solution, mL
is the actual concentration of the standard sodium hydroxide titration solution, mol/L; V, is the sample volume, mL;
-0.943, the sample density, g/cm;
0.086 is the mass of methacrylic acid equivalent to 1.00 mL of the standard sodium hydroxide titration solution [c(Na0H)=1.000 mol/L], expressed in grams.
The arithmetic mean of the values of two replicate measurements is taken as the result. 4.3.5 Permissible difference
The relative deviation of the results of two replicate measurements shall not exceed 10%. 4.4 Determination of moisture
4.4.1 Karl Fischer method (arbitration method)
Determine in accordance with GB6283 using the coulometric titration method. 4.4.1.2 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed 10%, and the arithmetic mean shall be taken as the determination result. 4.4.2 Gas chromatography
Determine in accordance with the provisions of GB2366.
WHG230592
The quantitative method adopts the peak height-percentage standard curve method. 4.4.2.1 Preparation of standard samples
When the moisture content of the product is within the range of 0.05% to 0.1%, a benzene-water equilibrium solution is used and prepared according to Article 5.2.1 of GB2366; when the moisture content of the product is within the range of 0.1% to 0.5%, a weighing sample preparation method is used and prepared according to Article 5.2.2 of GB2366. The base liquid is methyl methacrylate with a known moisture content.
4.4.2.2 Standard curve use cycle
Calibrate once every two months. During this period, when the absolute value of the maximum relative deviation of the four repeated test values is >15%, it should be recalibrated immediately.
4.4.2.3The rest shall be carried out in accordance with the provisions of GB2366, and the instrument part shall be carried out in accordance with the provisions of GB9722. The reference conditions and chromatograms of the chromatographic test are shown in Appendix A.
4.4.2.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed 10%, and the arithmetic mean shall be taken as the determination result. 4.5 Determination of content
According to the organic impurity content determined by gas chromatography and the acid content and water content determined in Article 4.3.4.4, the content of methyl methacrylate shall be calculated.
4.5.1 Reagents and materials
Anhydrous methanol;
Acetone;
Methyl acrylate;
Methyl isobutyrate;
Ethyl methacrylate;
Methyl α-hydroxyisobutyrate: homemade (and calibrated for purity); f.
Methyl methacrylate: excluding water and acid content, purity ≥99.95% Carrier gas: nitrogen with a purity of not less than 99.8%; h.
Fuel gas: hydrogen with a purity of not less than 99.8%; i
Combustion-supporting gas: purified compressed air. j.
4.5.2 Instruments and equipment
4.5.2.1 Gas chromatograph
Any type of gas chromatograph with a hydrogen flame ionization detector, a detection limit D<1×10-g/s, and stability in accordance with the relevant provisions of GB9722.
4.5.2.2 Chromatographic column
Column tube: stainless steel tube with an inner diameter of 3mm and a length of 2m; carrier: Celite545 white diatomaceous earth carrier, particle size 0.18~0.25mm (80~60 mesh); b.
c. Stationary liquid: polyethylene glycol 20M, diisocyanate, phosphoric acid; d.
Preparation and aging of the chromatographic column
Prepare according to the ratio of carrier: polyethylene glycol 20M: diisocyanate: phosphoric acid = 100:1:20:2 (m/m). Dissolve the three stationary liquids prepared according to the above ratio in acetone with a volume greater than that of the carrier, heat it on a water bath until it is slightly hot, stir it to fully dissolve it, pour the carrier into it, stir it gently, and place it in a ventilated place to dry it naturally. Finally, use an infrared lamp to bake it for 20 minutes to make it fully dry.
Pretreat the empty column and pack it according to the relevant provisions in GB9722. The filling amount is 3.5-3.8g/m, and the temperature is gradually raised from low temperature to 110℃ with nitrogen, and aged in stages for more than 36 hours until the baseline is stable. 4.5.2.3 Micro-injector: 1μL.
4.5.2.4 Recorder or chromatography data processor. 3
W.bzsosO.cOHG2305—92
4.5.3 Reference conditions for chromatographic tests, retention time of each component, relative retention value, and chromatogram curve are shown in Appendix B. 4.5.4 Analysis steps
Operate the chromatograph according to the instructions, and set the operating conditions according to Appendix B. Samples can be injected after the baseline of the instrument is stable. Before injection, the column temperature and carrier gas flow must be checked to see if they are consistent with those when preparing the standard curve. If there are any differences, they must be adjusted before injection. The injector must be inserted quickly during injection and pulled out quickly after injection. Use a recorder or chromatography data processor to record signals or process calculation results. 4.5.5 The quantitative method uses the peak height-percentage content standard curve method. See Appendix C for the preparation method of the peak height-content standard curve. 4.5.6 Expression of analysis results
The methyl methacrylate content (X2) expressed as a mass percentage is calculated according to formula (2): X,=100-X-Xw-EX,
Wherein: X,——the acid content measured in 4.3, %; X—the moisture content measured in 4.4, %;
X——the content of chromatographic organic impurities measured in 4.5.5, %. The arithmetic mean of the two parallel determinations is taken as the result. 4.5.7 Allowable error
The difference between the two parallel determination results shall not exceed 0.2%. 5 Inspection rules
5.1 Industrial methyl methacrylate shall be inspected by the quality supervision department of the manufacturer, and the manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, batch number, production date, product quality and this standard number. 5.2 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from the packaging unit of twice the amount for re-testing. If one of the indicators in the re-testing results still does not meet the requirements of the standard, the entire batch of products shall be judged as unqualified. 5.3 Sampling method
Each storage tank is a batch. The number of samples and the sample volume shall be carried out in accordance with the method specified in Article 6.6 of GB6678. Sampling shall be carried out in accordance with the method specified in GB6680, and the sampling volume shall not be less than 250mL. The collected samples shall be divided into two equal parts, placed in clean and dry glass bottles, tightly sealed, and labeled. The product name, batch number, sampling date and sampler shall be indicated on the label. One bottle is for inspection, and the other bottle is sealed and stored for one month for future reference.
The user's own packaging container shall be subject to the sampling of the storage tank of the manufacturer. 5.4 All technical indicators listed in this standard are type inspection items. Under normal production conditions, the density is inspected once every half month, and the other items are factory inspection items.
5.5 The user has the right to inspect and accept the product according to the technical requirements and test methods of this standard. When the supply and demand parties have a dispute over the quality of the product, the supply and demand parties shall jointly agree on arbitration. If there is any objection, it shall be submitted to the manufacturer within 15 days of receiving this product. 5.6 The judgment of the test results shall be carried out according to the rounded value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 The packaging container shall have a mark in accordance with the provisions of GB190, and the product packaging barrel shall be attached with a product certificate, including: manufacturer name, product name, trademark, this standard number, batch number, production date, product net weight, etc. 6.2 The product is packaged in a dry, clean and sealed aluminum barrel or galvanized iron barrel, with a net weight of 180kg per barrel. 6.3 This product is a dangerous and flammable product. It shall not be exposed to sunlight or rain during transportation and storage, and open flames are strictly prohibited. 6.4 This product is easy to polymerize when exposed to light or heat, and should be stored in a cold storage below 10°C. Inhibitors should be added during storage and transportation. If the user requires the product without inhibitors and polymerization occurs, the manufacturer will not be responsible. 4
W.bzsoso.coI Chromatographic Reference Test Conditions
HG2305—92
Appendix A
Reference conditions and chromatograms for chromatographic test of moisture determination (supplement)
Stationary phase: 407 organic carrier, particle size 0.18~0.25mm (80~60 mesh); Chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; Carrier: hydrogen, 25mL/min;
Column temperature: 130℃;
Detector temperature: 130℃;
Vaporization chamber temperature: 160℃;
Injection volume: 5μL;
Bridge current: 180mA;
Attenuation: 1/1.
Retention time (t) and relative retention value (T,) of each component. A2
Methyl methacrylate
te/min
Users can adjust the chromatographic conditions appropriately, but appropriate separation and response values should be obtained. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylate Figure A2
1-Air, 2-Water, 3-Methanol, 4-Methyl methacrylate Appendix B
Content determination chromatographic test reference conditions and chromatograms (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".6 Expression of analysis results
The methyl methacrylate content (X2) expressed as mass percentage is calculated according to formula (2): X,=100-X-Xw-EX,
Wherein: X,——acid content measured in 4.3, %; X—water content measured in 4.4, %;
X——content of chromatographic organic impurities measured in 4.5.5, %. The arithmetic mean of the two parallel determinations is taken as the result. 4.5.7 Allowable error
The difference between the two parallel determination results shall not exceed 0.2%. 5 Inspection rules
5.1 Industrial methyl methacrylate shall be inspected by the quality supervision department of the manufacturer, and the manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, batch number, production date, product quality and this standard number. 5.2 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from the packaging unit of twice the amount for re-testing. If one of the indicators in the re-testing results still does not meet the requirements of the standard, the entire batch of products shall be judged as unqualified. 5.3 Sampling method
Each storage tank is a batch. The number of samples and the sample volume shall be carried out in accordance with the method specified in Article 6.6 of GB6678. Sampling shall be carried out in accordance with the method specified in GB6680, and the sampling volume shall not be less than 250mL. The collected samples shall be divided into two equal parts, placed in clean and dry glass bottles, tightly sealed, and labeled. The product name, batch number, sampling date and sampler shall be indicated on the label. One bottle is for inspection, and the other bottle is sealed and stored for one month for future reference.
The user's own packaging container shall be subject to the sampling of the storage tank of the manufacturer. 5.4 All technical indicators listed in this standard are type inspection items. Under normal production conditions, the density is inspected once every half month, and the other items are factory inspection items.
5.5 The user has the right to inspect and accept the product according to the technical requirements and test methods of this standard. When the supply and demand parties have disputes over product quality, the supply and demand parties shall jointly agree on arbitration. If there is any objection, it shall be submitted to the manufacturer within 15 days of receiving this product. 5.6 The determination of the test results shall be carried out according to the rounded value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 The packaging container shall have a mark in accordance with the provisions of GB190, and a product certificate shall be attached to the outside of the product packaging barrel, including: manufacturer name, product name, trademark, this standard number, batch number, production date, product net weight, etc. 6.2 The product is packaged in dry, clean and sealed aluminum barrels or galvanized iron barrels, with a net weight of 180kg per barrel. 6.3 This product is a dangerous and flammable product. It shall not be exposed to sunlight or rain during transportation and storage, and open flames are strictly prohibited. 6.4 This product is easy to polymerize when exposed to light or heat, and should be stored in a cold storage below 10°C. Inhibitors should be added during storage and transportation. If the user requires the product to be free of inhibitors and polymerization occurs, the manufacturer will not be responsible. 4
W.bzsoso.coI Chromatographic Reference Test Conditions
HG2305—92
Appendix A
Reference conditions and chromatograms for chromatographic test of moisture determination (supplement)
Stationary phase: 407 organic carrier, particle size 0.18~0.25mm (80~60 mesh); Chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; Carrier: hydrogen, 25mL/min;
Column temperature: 130℃;
Detector temperature: 130℃;
Vaporization chamber temperature: 160℃;
Injection volume: 5μL;
Bridge current: 180mA;
Attenuation: 1/1.
Retention time (t) and relative retention value (T,) of each component. A2
Methyl methacrylate
te/min
Users can adjust the chromatographic conditions appropriately, but appropriate separation and response values should be obtained. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylate Figure A2
1-Air, 2-Water, 3-Methanol, 4-Methyl methacrylate Appendix B
Content determination chromatographic test reference conditions and chromatograms (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".6 Expression of analysis results
The methyl methacrylate content (X2) expressed as mass percentage is calculated according to formula (2): X,=100-X-Xw-EX,
Wherein: X,——acid content measured in 4.3, %; X—water content measured in 4.4, %;
X——content of chromatographic organic impurities measured in 4.5.5, %. The arithmetic mean of the two parallel determinations is taken as the result. 4.5.7 Allowable error
The difference between the two parallel determination results shall not exceed 0.2%. 5 Inspection rules
5.1 Industrial methyl methacrylate shall be inspected by the quality supervision department of the manufacturer, and the manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, batch number, production date, product quality and this standard number. 5.2 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from the packaging unit of twice the amount for re-testing. If one of the indicators in the re-testing results still does not meet the requirements of the standard, the entire batch of products shall be judged as unqualified. 5.3 Sampling method
Each storage tank is a batch. The number of samples and the sample volume shall be carried out in accordance with the method specified in Article 6.6 of GB6678. Sampling shall be carried out in accordance with the method specified in GB6680, and the sampling volume shall not be less than 250mL. The collected samples shall be divided into two equal parts, placed in clean and dry glass bottles, tightly sealed, and labeled. The product name, batch number, sampling date and sampler shall be indicated on the label. One bottle is for inspection, and the other bottle is sealed and stored for one month for future reference.
The user's own packaging container shall be subject to the sampling of the storage tank of the manufacturer. 5.4 All technical indicators listed in this standard are type inspection items. Under normal production conditions, the density is inspected once every half month, and the other items are factory inspection items.
5.5 The user has the right to inspect and accept the product according to the technical requirements and test methods of this standard. When the supply and demand parties have disputes over product quality, the supply and demand parties shall jointly agree on arbitration. If there is any objection, it shall be submitted to the manufacturer within 15 days of receiving this product. 5.6 The determination of the test results shall be carried out according to the rounded value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 The packaging container shall have a mark in accordance with the provisions of GB190, and a product certificate shall be attached to the outside of the product packaging barrel, including: manufacturer name, product name, trademark, this standard number, batch number, production date, product net weight, etc. 6.2 The product is packaged in dry, clean and sealed aluminum barrels or galvanized iron barrels, with a net weight of 180kg per barrel. 6.3 This product is a dangerous and flammable product. It shall not be exposed to sunlight or rain during transportation and storage, and open flames are strictly prohibited. 6.4 This product is easy to polymerize when exposed to light or heat, and should be stored in a cold storage below 10°C. Inhibitors should be added during storage and transportation. If the user requires the product to be free of inhibitors and polymerization occurs, the manufacturer will not be responsible. 4
W.bzsoso.coI Chromatographic Reference Test Conditions
HG2305—92
Appendix A
Reference conditions and chromatograms for chromatographic test of moisture determination (supplement)
Stationary phase: 407 organic carrier, particle size 0.18~0.25mm (80~60 mesh); Chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; Carrier: hydrogen, 25mL/min;
Column temperature: 130℃;
Detector temperature: 130℃;
Vaporization chamber temperature: 160℃;
Injection volume: 5μL;
Bridge current: 180mA;
Attenuation: 1/1.
Retention time (t) and relative retention value (T,) of each component. A2
Methyl methacrylate
te/min
Users can adjust the chromatographic conditions appropriately, but appropriate separation and response values should be obtained. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylate Figure A2
1-Air, 2-Water, 3-Methanol, 4-Methyl methacrylate Appendix B
Content determination chromatographic test reference conditions and chromatograms (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".6. Sampling is carried out according to the method specified in GB6680, and the sampling volume is not less than 250mL. The collected samples are divided into two equal parts, placed in clean and dry glass bottles, tightly sealed, and labeled. The label should indicate the product name, batch number, sampling date and sampler. One bottle is for inspection, and the other bottle is sealed and stored for one month for future reference.
Users shall prepare their own packaging containers based on the sampling of the manufacturer's storage tank. 5.4 All technical indicators listed in this standard are type inspection items. Under normal production conditions, the density is inspected once every half month, and the other items are factory inspection items.
5.5 The user unit has the right to accept the product according to the technical requirements and test methods of this standard. When the supply and demand parties have a dispute over the quality of the product, the supply and demand parties shall jointly agree on arbitration. If there is any objection, it shall be submitted to the manufacturer within 15 days of receiving this product. 5.6 The judgment of the inspection result shall be carried out according to the rounding value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 The packaging container should have a mark that complies with the provisions of GB190, and a product certificate should be attached to the outside of the product packaging barrel, including: manufacturer name, product name, trademark, standard number, batch number, production date, product net weight, etc. 6.2 The product is packaged in dry, clean and sealed aluminum barrels or galvanized iron barrels, with a net weight of 180kg per barrel. 6.3 This product is dangerous and flammable. It must not be exposed to sunlight or rain during transportation and storage, and open flames are strictly prohibited. 6.4 This product is prone to polymerization when exposed to light and heat, and should be stored in a cold storage below 10°C. Inhibitors should be added during storage and transportation. If the user requires the product without inhibitors, the manufacturer will not be responsible if polymerization occurs. 4
W.bzsoso.coI Chromatographic Reference Test Conditions
HG2305—92
Appendix A
Reference conditions and chromatograms for chromatographic test of moisture determination (supplement)
Stationary phase: 407 organic carrier, particle size 0.18~0.25mm (80~60 mesh); Chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; Carrier: hydrogen, 25mL/min;
Column temperature: 130℃;
Detector temperature: 130℃;
Vaporization chamber temperature: 160℃;
Injection volume: 5μL;
Bridge current: 180mA;
Attenuation: 1/1.
Retention time (t) and relative retention value (T,) of each component. A2
Methyl methacrylate
te/min
Users can adjust the chromatographic conditions appropriately, but appropriate separation and response values should be obtained. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylate Figure A2
1-Air, 2-Water, 3-Methanol, 4-Methyl methacrylate Appendix B
Content determination chromatographic test reference conditions and chromatograms (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".6. Sampling is carried out according to the method specified in GB6680, and the sampling volume is not less than 250mL. The collected samples are divided into two equal parts, placed in clean and dry glass bottles, tightly sealed, and labeled. The label should indicate the product name, batch number, sampling date and sampler. One bottle is for inspection, and the other bottle is sealed and stored for one month for future reference.
Users shall prepare their own packaging containers based on the sampling of the manufacturer's storage tank. 5.4 All technical indicators listed in this standard are type inspection items. Under normal production conditions, the density is inspected once every half month, and the other items are factory inspection items.
5.5 The user unit has the right to accept the product according to the technical requirements and test methods of this standard. When the supply and demand parties have a dispute over the quality of the product, the supply and demand parties shall jointly agree on arbitration. If there is any objection, it shall be submitted to the manufacturer within 15 days of receiving this product. 5.6 The judgment of the inspection result shall be carried out according to the rounding value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 The packaging container should have a mark that complies with the provisions of GB190, and a product certificate should be attached to the outside of the product packaging barrel, including: manufacturer name, product name, trademark, standard number, batch number, production date, product net weight, etc. 6.2 The product is packaged in dry, clean and sealed aluminum barrels or galvanized iron barrels, with a net weight of 180kg per barrel. 6.3 This product is dangerous and flammable. It must not be exposed to sunlight or rain during transportation and storage, and open flames are strictly prohibited. 6.4 This product is prone to polymerization when exposed to light and heat, and should be stored in a cold storage below 10°C. Inhibitors should be added during storage and transportation. If the user requires the product without inhibitors, the manufacturer will not be responsible if polymerization occurs. 4
W.bzsoso.coI Chromatographic Reference Test Conditions
HG2305—92
Appendix A
Reference conditions and chromatograms for chromatographic test of moisture determination (supplement)
Stationary phase: 407 organic carrier, particle size 0.18~0.25mm (80~60 mesh); Chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; Carrier: hydrogen, 25mL/min;
Column temperature: 130℃;
Detector temperature: 130℃;
Vaporization chamber temperature: 160℃;
Injection volume: 5μL;
Bridge current: 180mA;
Attenuation: 1/1.
Retention time (t) and relative retention value (T,) of each component. A2
Methyl methacrylate
te/min
Users can adjust the chromatographic conditions appropriately, but appropriate separation and response values should be obtained. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylate Figure A2
1-Air, 2-Water, 3-Methanol, 4-Methyl methacrylate Appendix B
Content determination chromatographic test reference conditions and chromatograms (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".25mm (80~60 mesh); chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; carrier: hydrogen, 25mL/min;
column temperature: 130℃;
detector temperature: 130℃;
vaporization chamber temperature: 160℃;
injection volume: 5μL;
bridge current: 180mA;
decay: 1/1.
retention time (t) and relative retention value (T,) of each component. A2
methyl methacrylate
te/min
users can adjust the chromatographic conditions appropriately, but should obtain appropriate separation and response values. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylateFigure A2
1—air, 2—water, 3—methanol, 4—methyl methacrylateAppendix B
Reference conditions and chromatograms for content determination chromatographic test (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".25mm (80~60 mesh); chromatographic column: 2m long, inner diameter Φ3mm stainless steel tube; carrier: hydrogen, 25mL/min;
column temperature: 130℃;
detector temperature: 130℃;
vaporization chamber temperature: 160℃;
injection volume: 5μL;
bridge current: 180mA;
decay: 1/1.
retention time (t) and relative retention value (T,) of each component. A2
methyl methacrylate
te/min
users can adjust the chromatographic conditions appropriately, but should obtain appropriate separation and response values. Peak height (mm)
Water content (%)
Figure A1 Peak height-water content standard curve
B1 Reference test conditions
HG2305-92
Actual sample chromatogram of water in methyl methacrylateFigure A2
1—air, 2—water, 3—methanol, 4—methyl methacrylateAppendix B
Content determination chromatographic test reference conditions and chromatograms (supplement)
The above is 102G gas from Shanghai Analytical Instrument Factory Take phase chromatograph as an example: a.
Column temperature: 100℃;
Detection chamber temperature: 110℃;
Vaporization chamber temperature: 150℃;
Injection volume: 1uL;
Sensitivity: 1000 (equivalent to high resistance 109); Attenuation: 1/8 (-1~+4mV recorder); Carrier gas: nitrogen 20mL/min;
Fuel gas: hydrogen 30mL/min;
Auxiliary gas: air 300mL/min.
Retention time (tr) of each component, relative retention value (rs) n
Acrylic cresol
Methyl isobutyrate
Methyl methacrylate
Ethyl methacrylate
Methyl α-hydroxyisobutyrate
HG2305—92
te/min
The analysis conditions can be adjusted appropriately, and the retention time and spectrum will change accordingly, but the entire chromatographic process should be completed within 6 to 10 minutes with appropriate separation.
Figure B1 Typical chromatogram of methyl methacrylate 1-methanol; 2-acetone; 3-methyl acrylate; 4-methyl isobutyrate 5-methyl methacrylate; 6-ethyl methacrylate; 7-methyl hydroxyisobutyrate 7
HG2305-92
Appendix C
Steps for preparing peak height-content standard curve
(Supplement)
Pipette 8mL of high-purity methyl methacrylate into a small sample bottle with a rubber stopper, and inject the impurity components separately with a microinjector. The content of each impurity is approximately 0.1% for methanol, 0.05% for acetone, 0.1% for methyl acrylate, 0.1% for methyl isobutyrate, 0.15% for ethyl methacrylate, and 0.3% for methyl α-hydroxyisobutyl ester (calculated according to the homemade content). The weight is accurate to 0.0002g. This standard sample is called the mother solution. Then dilute the mother liquor with high-purity methyl methacrylate to 2/3; 1/2; 1/3; 1/4 concentrations to form five standard samples with different concentrations. Under the same chromatographic conditions as the analytical sample, inject three times continuously, take the average peak height as the ordinate and the percentage content as the abscissa to draw the standard curve. If it is found that it does not pass through the origin, it must be recalibrated.
The standard curve needs to be calibrated regularly, once a month. Add ethyl methacrylate to high-purity methyl methacrylate according to the calibration method. The recovery rate should be within the range of 80% to 120%, otherwise it needs to be recalibrated. All calibration must be done once every three months at most. The calibration date and chromatographic conditions used must be noted next to the standard curve for verification during testing. Peak height (mra)
Figure CI peak height-content standard curve
1-acetone, 2-methanol; 3-methyl acrylate; 4-methyl isobutyrate; 5-ethyl methacrylate, 6-methyl hydroxyisobutyrateAdditional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shanhu Chemical Factory. The main drafters of this standard are Jin Baofang, Han Min, Xu Wentao, and Xu Rendi. This standard adopts the Japanese Industrial Standard JISK6716-1989 "Methyl Methacrylate".
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