Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2304—92
Industrial trifluorotrichloroethane
Published on May 17, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993
WChemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
Trichlorofluoroethane
HG2304—92
This standard specifies the technical requirements, test methods, inspection rules, as well as marking, packaging, transportation and storage of industrial trifluorotrichloroethane.
This standard applies to trifluorotrichloroethane produced by the solid-phase batch method with pentachloride as catalyst and hexachloroethane as raw material and the continuous fluorination method with tetrachloroethylene as raw material. The main uses of this product are raw materials for the preparation of fluorine-containing compounds, refrigerant insulating oil and solvent, foaming agent, cleaning agent, etc.
Molecular formula: CF2CI-CFCl2
Relative molecular mass: 187.39 (according to the 1989 international relative atomic mass) 2 Reference standards
Dangerous goods packaging mark
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents. Preparation of preparations and products used in chemical reagent test methods GB1250
GB6283
GB6678
GB6680
GB8170
3 Technical requirements
Expression and determination methods of limit values Determination of water content in chemical products
Karl Fischer method (general method)
General rules for sampling of chemical products
Liquid chemical General Rules for Product Sampling
Rules for Rounding Off Numerical Values
3.1 Appearance: Colorless, non-turbid liquid
Odor: No peculiar smell
The quality of trifluorotrichloroethane shall meet the requirements of Table 1: Table 1
Evaporation residue
Acidity (in HCI)
Superior product
Approved by the Ministry of Chemical Industry of the People's Republic of China on May 17, 1992 99.9
First-class product
% (m/m)
Qualified product
Implemented on January 1, 1993
W. bzsoso: com4 Test Method
HG2304—92
Unless otherwise specified, the reagents and water used are analytical pure reagents and distilled water or water of equivalent purity. 4.1 Determination of appearance
In a 25mL colorimetric tube, add 25mL of trifluorotrichloroethane at room temperature, wipe the moisture attached to the outer wall of the test tube with a dry cloth, and there should be no turbidity when observed from the axial perspective.
4.2 Determination of odor
Use the sample to be determined for appearance, slowly heat the test tube until it boils slightly, and the steam should have no peculiar smell. 4.3 Determination of purity
This method uses a methyl silicone oil DC200 chromatographic column to separate trifluorotrichloroethane components, uses a thermal conductivity detector, and calculates the content of each component by normalization method.
4.3.1 Materials and Reagents
4.3.1.1 Carrier gas: hydrogen, purity better than 99.5%; 4.3.1.2 Carrier: Chromosorb W, particle size 0.18~0.25mm; 4.3.1.3
Fixed liquid: methyl silicone oil DC200;
4.3.1.4 Solvent: chloroform.
4.3.2 Instruments
4.3.2.1 Gas chromatograph equipped with a thermal conductivity detector using hydrogen as carrier gas, with a sensitivity to benzene better than 800mVmL/mg. 4.3.2.2 Injector: micro-syringe.
4.3.2.3 Chromatographic column: a stainless steel column with a length of 3m and an inner diameter of 3mm. 4.3.2.4 Standard sample: Trifluorotrichloroethane and difluorotetrachloroethane with a purity of 99.99% and tetrafluorodichloroethane with a purity of 99.0%. 4.3.3 Analysis steps
4. 3. 3. 1
Preparation of stationary phase: Weigh 7.5g of methyl silicone oil and place it in a 250mL beaker and dissolve it in chloroform. Then pour 25g of ChromosorbW carrier with a particle size of 0.180.25mm into the beaker and mix well. Dry it under an infrared lamp for later use. 4.3.3.2 Filling and loading amount of chromatographic column: Plug the outlet of the chromatographic column with a little glass wool or copper mesh, then suck from the outlet and load the stationary phase into the chromatographic column under gentle vibration. For a stainless steel column with an inner diameter of 3mm, the loading amount is about 2.66g/m. 4.3.3.3 Aging of chromatographic column: Pass nitrogen gas and age at 150℃ for 10h. 4. 3.3.4
Typical chromatographic conditions are shown in Table 2.
Chromatographic column
Stationary phase ratio
Column temperature, ℃
Vaporization temperature, ℃
Detection temperature, ℃
Bridge current, mA
Recorder range, mv
03mmX300mmstainless steel disc column
Chromosorb W: Methyl silicone oil DC200=100:3050
w.bzsoso:comParameters
Carrier gas flow rate, mL/min
Column head pressure, MPa
Injection volume, μLbZxz.net
Paper speed, mm/min
HG2304—92
Note: The chromatographic conditions should be selected by the user according to different instruments to obtain equal separation degree. 23
4.3.3.5 Determination: Start the instrument and inject samples after the chromatographic operating conditions are stable. The retention time and relative retention value of each component and the chromatogram are shown in Table 3 and Figure 1.
Tetrafluorodichloroethane
Trifluorotriazineethane
Difluorotetrachloroethane
1min58s
6min33s
Figure 1 Typical chromatogram
1-Air; 2-Tetrafluorodichloroethane ((F1u4); 3-Trifluorotrichloroethane (Fns); 4-Difluorotetrachloroethane (F1z) 3
W.4.3.4 Calculation of results
HG2304-92
4.3.4.1 Determine the peak area of each component of trifluorotrichloroethane and calculate the mass percentage of trifluorotrichloroethane by normalization method X1: A
XI=2(Ai+A.+As+A,)
Where:
Three Peak area of trichlorofluoroethane, cm;
A1, A2, As, .., An—peak area of each component. Take the arithmetic mean as the measurement result. 4.3.5 Allowable difference
The difference between two parallel measurement results should not be greater than 0.2%. 4.4 Determination of evaporation residue
This method is to heat the sample in the evaporating tube to boil and evaporate, and measure the mass of the non-volatile residue to obtain the evaporation residue. 4.4.1 Instruments and equipment
4.4.1.1 Evaporator (see Figure 2).
Evaporating tube
500mL mark
F113 sample
Standard tube
Constant temperature water bath
Trichlorofluoroethane evaporator
4.4 .1.2 Constant temperature water bath.
4.4.1.3 Analytical balance.
4.4.1.4 Oven: 105±2℃.
4.4.2 Analytical steps
Place the standard measuring tube in an oven at 105±2℃ to dry for 1h, then cool it in a desiccator and weigh it until it is constant weight. (1)
Connect the standard measuring tube with constant weight to the evaporating tube, immerse part of the evaporating tube (standard measuring tube) in a constant temperature water bath, add 4504
W.HG2304—92
mL of sample, and control the evaporation of the sample within 1.52h. After the evaporation of the sample is completed, add the remaining 50mL of sample to the evaporator for cleaning, then evaporate it on a water bath. After vaporization, until it is evaporated to dryness, put the standard measuring tube in 1 Dry in an oven at 05±2℃ for 1h, cool to room temperature in a desiccator and weigh (accurate to 0.0002g).
The mass percentage X2 of the evaporation residue is calculated according to formula (2): Xm..x10...
Wherein: m1——mass of the standard measuring tube, g; m2——mass of the standard measuring tube after the sample is vaporized, g; p—density of the sample (1.58g/mL at 20℃), g/mL; V is the volume of the sample, mL.
4.4.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.0002%4.5 Determination of acidity
This method uses water to extract the acidic substances in the sample, uses bromocresol green as the indicator solution, and titrates with sodium hydroxide standard solution to obtain the acidity.
4.5.1 Instruments and equipment
4.5.1.1 Separating funnel: 300mL.
4.5.1.2 Erlenmeyer flask.
4.5.1.3 Volumetric flask: 1000mL.
4.5.2 Reagents
4.5.2.1 Bromocresol green indicator solution: 1g/L. 4.5.2.2 Sodium hydroxide standard titration solution: First prepare c (NaOH) = 0.1mol/L sodium hydroxide standard titration solution, prepare and calibrate according to GB601, then accurately dilute the above solution 10 times with distilled water without carbon dioxide to make its concentration c (NaOH) 0.01mol/L.
4.5.3 Analysis steps
Add 100mL of distilled water to the separatory funnel, weigh 100g of sample and add it to the separatory funnel, shake it thoroughly, separate the water layer from the sample, repeat the operation twice, combine the water extracted twice and transfer it to a conical flask, add 2 to 3 drops of bromocresol green indicator solution, and titrate with sodium hydroxide standard titration solution (4.5.2.2) until the blue color is the end point, and perform a blank test at the same time. Acidity X expressed as mass percentage: (in HCI) calculated according to formula (3): Xx = 9 (V1-V) × 0. 036 5 × 100
Wherein: c——actual concentration of sodium hydroxide standard titration solution, mol/L; V,——volume of sodium hydroxide standard titration solution, mL; V.-volume of sodium hydroxide standard titration solution consumed in blank test, mL; m——mass of sample, gs
(3)
0.0365-mass of hydrochloric acid equivalent to 1.00mL sodium hydroxide standard titration solution [c (Na0H) = 1.000mol/L, expressed in grams.
4.6 Determination of water content
Dissolve 20mL of sample in anhydrous methanol solution, and then determine according to the method specified in GB6283. Take the arithmetic mean as the determination result.
4.6.1 Allowable difference
WHG2304—92
The difference between two parallel determination results shall not exceed 0.0003%. 5 Inspection rules
5.1 This product shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory (each packaging volume is a batch) shall be accompanied by a product certificate, including: manufacturer name, product name, product grade, batch number, production date, product quality certificate and implementation standard number. 5.2 The user has the right to inspect the product quality in accordance with the provisions of this standard within three months (calculated from the date of leaving the factory). 5.3 Sampling: Sampling shall be carried out in accordance with the provisions of Table 2 in GB6678. The sampling method shall be carried out in accordance with 2.1.3 in GB6680. 5.4 If one of the test results does not meet the requirements of this standard, samples should be taken from two times the packaging unit for re-testing. If the re-test results of the unqualified items still do not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.5 When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution shall be selected by both parties through consultation. Arbitration shall be conducted in accordance with the inspection methods specified in this standard.
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 and storage
6.1 The packaging containers of industrial trifluorotrichloroethane shall be painted with firm markings, including: manufacturer name, product name, standard number, trademark, quality grade, batch number, net weight and Figure 11 "toxic mark" in GB190. 6.2 Industrial trifluorotrichloroethane shall be packaged in clean and dry barrels or containers, with a net weight of 200±0.5 or 250±0.5kg per barrel. 6.3 During transportation, there should be covers, and loading and unloading should be done with care to prevent rain and sunlight exposure, and to prevent the packaging barrels or containers from being damaged. 6.4 This product should be stored in a cool, dry, and ventilated warehouse. It should not be piled in the open air to avoid sun and rain. Additional notes:
This standard was 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 jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Shuguang Chemical Plant. The main drafters of this standard are Guo Yiyang, Lu Ronghai, Wu Lianbi, and Zhu Jing. This standard refers to the Japanese Industrial Standard JIS K1528-1982 "Fluoroethanes". W.bzsoso.coI
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.