Some standard content:
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T 2426-93
This standard specifies the technical requirements, test methods, inspection regulations and packaging, marking, transportation and storage of tetrabromoethane. This standard applies to tetrabromoethane synthesized from bromine and ethyl. The product is mainly used as a catalyst in the fiber industry, a flame retardant in the plastics industry, etc. Molecular formula: C, H, Br4
Relative molecular weight: 345.70 (according to the international relative atomic mass in 1989) 2 Reference standards
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB 601
Preparation of preparations and products used in test methods of chemical reagents GB 605
GB 618
General method for colorimetric determination of chemical reagents
General method for crystallization point determination of chemical reagents
GB/T 4472
General rule for determination of density and relative density of chemical products GB/T 6680
General rule for sampling of liquid chemical products
GB6682
Specifications and test methods for water used in analytical laboratories
GB/T 9721
GB/T 9722
GB/T 9724
3 Technical requirements
Chemical reagents General principles for molecular absorption spectrophotometry (ultraviolet and visible light parts) Chemical reagents
General principles for gas chromatography
General principles for pH determination
Chemical reagents
Tetrabromoethane should meet the requirements in the following table.
Appearance (visual inspection)
Color.APHA
Relative density, d
Condensation point, center
Inorganic halide content, 10-≤
Note: 1) Qualified products are pyrophoric products.
Test method
Superior quality
2,955~2,970
5. 0~7. 0
Colorless or light yellow transparent liquid without turbidity or precipitation 200
2.950~2.970
The water used in this standard shall meet the specifications of Grade 3 water in GB6682 unless otherwise specified. Approved by the Ministry of Chemical Industry of the People's Republic of China on March 10, 1993 Qualified product
2.900~2.970
Implemented on January 1, 1994
HG/T 2426—93
The standard solutions, preparations and products used in this standard are prepared in accordance with the provisions of GB601 and GB603. 4.1 Appearance determination
Observe by visual inspection.
4.2 Colorimetric determination
Perform according to GB 605.
4.3 Relative density determination
Perform according to GB/T4472, Section 2.3.1, Pycnometer method, with a determination temperature of 25°C. 4.4 Determination of solidification point
Perform according to GB 618. During the determination, seed crystals of the size of rice grains should be added. Stirring should be carried out from the beginning of cooling the sample. 4.5 Content determination
4.5.1 Principle
After the sample and its measured components are vaporized, they enter the chromatographic column simultaneously with the carrier gas. The differences in the physicochemical properties such as solubility and analysis between the measured components and the stationary phase (gas-liquid) are used to form differences in the migration speed of the components in the column for separation. After separation, the components first flow out of the chromatographic column at the bottom and enter the detector, and the corresponding chromatogram is drawn by the recorder. The retention value of each component and the chromatographic peak area or the corresponding peak height value are used as the basis for qualitative and quantitative analysis respectively.
4.5.2 Instruments and devices
Gas chromatograph: in accordance with the provisions of GB/T9722. 4.5.3 Test conditions
4. 5. 3. 1 Detector and its temperature
The detector is a thermal conductivity detector with a temperature of 170-175°C. 4.5.3.2 Carrier gas and flow rate
Hydrogen is used as the carrier gas with a flow rate of 40-60ml./min (measured by a soap film flow meter). 4.5.3.3 Column length, inner diameter and column temperature The length of the chromatographic column is 2m, the inner diameter is 4mm×0.5mm (stainless steel tube), the column temperature is 170℃, 4.5.3.4 Stationary liquid carrier and its stationary liquid content The stationary liquid is 5% SE-30.6201 carrier 180~250m (60~80 days), dissolved in butanol tridecafluoromethane (1+1). 4.5.3.5 The effective plate height Heffective of the chromatographic column
The effective plate number neffective or the effective plate height Heffective (mm) is calculated according to formula (1): neffective=5.54[wa]
holes loaded
wherein tr
adjusted retention time, tm;
Wh2—half-peak width of tetrabromoethane, mm;
Lcolumn length.mm.
4.5.3.6 Vaporization chamber temperature
The vaporization chamber temperature is 210~220℃,
4.5.3.7 Injection volume
The injection volume is 0.2~0.5μl.
4.5.3.8 Separation R of difficult-to-separate substance pairs Taking impurity peak tribromoethane (or tribromoform) as the difficult-to-separate substance: tr,.tr,
R-Wni)+Wan(2)
（2）
Wherein ttry
Retention time of tetrabromoethane, s;
Retention time of tribromoethane, s;
Wa2(1)-—Half peak width of ethane, mm: W(2): Half peak width of tetrabromoethane, mm. HG/T 242693
Note: When calculating, convert seconds (s) into millimeters (mm), or use the tr value of the amine on the spectrum. 4.5.3.9 Sensitivity SS under selected conditions
Wherein: △R——Response signal change value: —Trace amount change value.
4.5.3.10 Bridge flow and other instruments
(3)
Bridge flow is 120~110mA; paper speed is 8~16mm/min, and attenuation ratio is 1/1. Chromatographic data processor (calculated by area normalization method) and result recorder.
4.5.4 Preparation, filling and aging of chromatographic column 4.5.4.1 Preparation of chromatographic column
Weigh 0.7g SF-30 (fixed liquid), 14.0g 6201 carrier 180~250μm (60~80μm), dissolve the weighed SE-30 in butanol 1 trifluoroethane (1+1) with a volume slightly larger than the volume of the carrier, then pour the weighed carrier into it and mix well under infrared lamp, gently stir. After the solvent is completely discharged, place it in an oven at 120℃ to dry for 2~3h, and put it in a desiccator for use. 4.5.4.2 Filling and aging of chromatographic column
The impregnated stationary liquid carrier is loaded into the column by pumping and packing, and the column net end is plugged with glass wool. Then, it is aged for 24 hours under the condition of 30℃ higher than the use temperature, and the nitrogen flow rate is 10mL/min. 4.5.5 Operation steps
Turn on the recorder, preheat the microprocessor, and after the baseline is stable, use a micro syringe to draw 0.2~0.5L of the sample, inject it into the chromatograph for determination, and use the area normalization method of the microprocessor to determine the mass content of tetrabromoethane and other components. 4.5.6 Result calculation
Use the area normalization method to calculate the mass percentage content of tetrabromoethane according to the following formula: AcH,
Where: Ac.HBr
tetrabromoethane chromatographic peak area, cm2;
ZA is the sum of the chromatographic peak areas except the air peak, cm2. When this method is used to determine the content of tetraethane, the standard deviation of the determination should be less than 0.1. 4.6 pH determination
4.6.1 Principle
Shake the sample with boiled fresh distilled water, extract with water, and determine the pH value of the water extract with a pH meter. 4.6.2 Solution
Hydrochloric acid solution: 0.01 mal/l.
Sodium hydroxide solution: 0.01 mol/L.
Preparation of neutral distilled water: Boil 1L of distilled water in a boric acid glass or stainless steel container for about 15 minutes, then cover and cool to room temperature. Titrate 50ml of distilled water with 0.01 mol/l sodium hydroxide solution or 0.01 tuol/L hydrochloric acid solution to pH 7.0-7.3. Calculate the amount of sodium hydroxide solution or hydrochloric acid solution to be added to 950mL of boiled distilled water to adjust the pH to 7.0-7.3 based on the determination results. Pour 1L of neutral distilled water into a 1000ml volumetric flask or water bottle, and sieve. Take 50mL of neutral distilled water and measure its pH value. If the pH value needs to be further adjusted to 7.0~7.3, repeat the above steps.
4.6.3 Instruments and devices
The pH meter complies with the provisions of GB/T 9724.
4.6.4 Operation steps
HG/T 2426—93www.bzxz.net
Pipette 50mL of sample into a 250ml separatory funnel filled with 50mL of neutral distilled water, shake, let stand and separate the layers, and drain the sample layer after two minutes. Use a pH meter to measure the pH value of the water-benzene solution. 4.7 Determination of inorganic halides
4.7.1 Principle
Extract the sample with water, use thioxenic acid powder as a color developer, and measure the absorbance of the complex at a wavelength of 460mm. The reaction formula is: 2C1-+Hg(SCN), ----IIgCl, +2SCN -Fe3++ 3SCN-Fe(SCN)
4.7.2 Solution
4.7.2. 1 Saturated thiocyanate ethanol solution: Dissolve 0.3g thiocyanate in 100mL 95% ethanol. 4.7.2.2 Ammonium ferric sulfate-nitric acid mixture: weigh 120.550g ammonium ferric sulfate and dilute it to 1L with 1+1 nitric acid solution. 4.7.2.3 Fluoride standard solution: accurately weigh 1.6485g spectrally pure sodium chloride, place it in a 1000mL volumetric flask, dissolve it with distilled water and dilute it to the mark, shake it evenly and let it stand. The concentration of this solution is 1000mgCl/L. Use a pipette to transfer 10mL of this solution to a 1000mL volumetric flask, dilute it to the mark with distilled water, shake it evenly and let it stand. The concentration of this solution is 0.01mgCl/L, that is, 10ugL/L chloride standard solution. 4.7.3 Instruments and devices
UV-visible spectrophotometer, in accordance with the provisions of GB/T9721. 4.7.4 Operation steps
4.7.4.1 Preparation of chemical curve
Use a pipette to accurately transfer 1, 2, 3, 4, and 5 mL of chloride standard solution into six 25 mL volumetric flasks. Add 2 mL of ammonium ferric sulfate-nitric acid mixture and 2 mL of saturated ethanol solution of thiothric acid to each volumetric flask. After each addition of reagent, shake thoroughly, dilute to the scale with distilled water, and let stand for 10 minutes. At a wavelength of 460 μm, in a 2 cm absorption cell, measure the absorbance of distilled water, which is the reagent blank value. Sequentially measure the absorbance of chloride standard solution, subtract the reagent blank value, and then draw a working curve for the corresponding nitrogen mass (g). 4.7.4.2 Sample determination
Pipette 25 mL of tetraethyl ethane and 25 mL of freshly boiled and cooled distilled water into a 250 mL separatory funnel, shake and stand to separate. Transfer 20mL of the extraction solution to a 25mL volumetric flask, add 2mL of ammonium ferric sulfate-nitric acid mixture and 2mL of saturated ethanol solution of mercuric thiocyanate. After each addition of the reagent, shake thoroughly and dilute to the scale with distilled water, shake and let stand for 10min, and measure its absorbance at a wavelength of 460μm in a 2cm absorption cell. At the same time, do a blank test. Subtract the blank value from the absorbance of the sample and find the mass (g) of the chlorine to be measured on the working curve. 4.7. 5 Calculation of results
The content of inorganic halide in the sample is:
Inorganic halide (10-, m/m) =
ov×20
Where: m—the mass of chlorine found on the working curve·V——volume of the sample, ml.:
p——density of the sample, g/cm\.
5 Inspection rules
5.1 Among the inspection items of this standard, the pH value and inorganic halides can be inspected once a month under normal production conditions. Chroma, relative density, freezing point and content are factory inspection items. 5.2 Silang ethane should be inspected by the quality supervision department of the factory. The manufacturer should ensure that all products shipped out of the factory meet the requirements of this standard, and each batch of products shipped out of the factory should be accompanied by a quality certificate in a certain format. 5.3 The user has the right to inspect and accept the received products according to the technical requirements specified in this standard. 5.4 Each uniform product packaged once is considered as a batch. 332
HG/T 2426-—93
5.5 Determine the sampling number according to GB/T6680. The random sampling method is adopted, and the upper, middle and lower parts of the dry and clean sampling tube are evenly sampled. The total sampling volume shall not be less than 500g. After being evenly sampled, it is divided into two bottles, and the bottle mouths are sealed and marked with: manufacturer name, product name, batch number, sampling date. ... One bottle is sent to the quality supervision department for inspection and the other bottle is kept for re-inspection. 5.6 If a certain indicator does not meet the requirements of this standard after inspection, samples should be taken from twice the amount of packaging containers for re-inspection. If the re-inspection results still do not meet the requirements of this standard, the batch of products will be downgraded or unqualified. 5.7 When the supply and demand parties have objections to the product quality, the two parties may negotiate to select an arbitration unit. The arbitration unit shall conduct arbitration analysis according to the test methods specified in this standard.
6 Packaging, marking, transportation, storage
6.1 The product is packed in an iron barrel lined with plastic. The outside of the packaging barrel is painted with firm and clear markings, indicating the manufacturer's name, product name, standard number, trademark, grade, net weight, production date, and "toxic", "handle with care", and "do not invert". 6.2 Each packaging barrel must be accompanied by a product certificate: the content includes the manufacturer's name, product name, standard number, grade, batch number, net weight, production date, inspection month and inspector, etc.
6.3 Handle with care during transportation to avoid breakage and leakage. 6.4 The product should be stored in a ventilated, dry, cool and light-proof warehouse. The storage temperature should be maintained at 5-25'C. 6.5 Under the storage and transportation conditions recommended by this standard, the storage period is half a year from the date of production. Additional 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 jurisdiction of the Chemical Research Institute of Sichuan Province. This standard was drafted by Beidao Organic Chemical Factory and Shanxi Chemical Research Institute. The main drafters of this standard are Hao Wensong, Zhang Shu, Jiang Renlei, Zhu Yuanbo,1 Among the inspection items of this standard, the two items of pH value and inorganic halides can be inspected once a month under normal production conditions. Chroma, relative density, freezing point and content are the inspection items of the factory. 5.2 Silang ethane should be inspected by the quality supervision department of the factory. The manufacturer should ensure that all products shipped out of the factory meet the requirements of this standard, and each batch of products shipped out of the factory should be accompanied by a quality certificate in a certain format. 5.3 The user has the right to inspect and accept the received products according to the technical requirements specified in this standard. 5.4 Each uniform product packaged once is considered as a batch 332
HG/T 2426-—93
5.5 Determine the sampling number according to GB/T6680. The random sampling method is used to sample the upper, middle and lower parts of the dry and clean sampling tube. The total sampling volume shall not be less than 500g. After uniform sampling, it is divided into two bottles, and the bottle mouth is sealed and marked with: manufacturer name, product name, batch number, sampling date. …one bottle is sent to the quality supervision department for inspection and the other bottle is kept for re-inspection. 5.6 If any index does not meet the requirements of this standard after inspection, samples should be taken from the packaging container of twice the amount for re-inspection. If the re-inspection result still does not meet the requirements of this standard, the batch of products will be downgraded or unqualified. 5.7 When the supply and demand parties have objections to the product quality, the two parties may select an arbitration unit through negotiation. The arbitration unit shall conduct arbitration analysis according to the test methods specified in this standard.
6 Packaging, marking, transportation, storage
6.1 The product is packed in an iron barrel lined with plastic. The outside of the packaging barrel is painted with firm and clear markings, indicating the manufacturer's name, product name, standard number, trademark, grade, net weight, production date, and "toxic", "handle with care", and "do not turn upside down". 6.2 Each packaging barrel must be accompanied by a product certificate: the content includes the manufacturer's name, product name, standard number, grade, batch number, net weight, production date, inspection month and inspector, etc.
6.3 Handle with care during transportation to avoid breakage and leakage. 6.4 The product should be stored in a ventilated, dry, cool and light-proof warehouse. The storage temperature should be maintained at 5-25'C. 6.5 Under the storage and transportation conditions recommended by this standard, the storage period is half a year from the date of production. Additional remarks:
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 Shanxi Chemical Industry Research Institute. This standard was drafted by Beidao Organic Chemical Factory and Shanxi Chemical Industry Research Institute. The main drafters of this standard are Hao Wensong, Zhang Shu, Jiang Renlei, Zhu Yuanbo, 3331 Among the inspection items of this standard, the two items of pH value and inorganic halides can be inspected once a month under normal production conditions. Chroma, relative density, freezing point and content are the inspection items of the factory. 5.2 Silang ethane should be inspected by the quality supervision department of the factory. The manufacturer should ensure that all products shipped out of the factory meet the requirements of this standard, and each batch of products shipped out of the factory should be accompanied by a quality certificate in a certain format. 5.3 The user has the right to inspect and accept the received products according to the technical requirements specified in this standard. 5.4 Each uniform product packaged once is considered as a batch 332
HG/T 2426-—93
5.5 Determine the sampling number according to GB/T6680. The random sampling method is used to sample the upper, middle and lower parts of the dry and clean sampling tube. The total sampling volume shall not be less than 500g. After uniform sampling, it is divided into two bottles, and the bottle mouth is sealed and marked with: manufacturer name, product name, batch number, sampling date. …one bottle is sent to the quality supervision department for inspection and the other bottle is kept for re-inspection. 5.6 If any index does not meet the requirements of this standard after inspection, samples should be taken from the packaging container of twice the amount for re-inspection. If the re-inspection result still does not meet the requirements of this standard, the batch of products will be downgraded or unqualified. 5.7 When the supply and demand parties have objections to the product quality, the two parties may select an arbitration unit through negotiation. The arbitration unit shall conduct arbitration analysis according to the test methods specified in this standard.
6 Packaging, marking, transportation, storage
6.1 The product is packed in an iron barrel lined with plastic. The outside of the packaging barrel is painted with firm and clear markings, indicating the manufacturer's name, product name, standard number, trademark, grade, net weight, production date, and "toxic", "handle with care", and "do not turn upside down". 6.2 Each packaging barrel must be accompanied by a product certificate: the content includes the manufacturer's name, product name, standard number, grade, batch number, net weight, production date, inspection month and inspector, etc.
6.3 Handle with care during transportation to avoid breakage and leakage. 6.4 The product should be stored in a ventilated, dry, cool and light-proof warehouse. The storage temperature should be maintained at 5-25'C. 6.5 Under the storage and transportation conditions recommended by this standard, the storage period is half a year from the date of production. Additional remarks:
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 Shanxi Chemical Industry Research Institute. This standard was drafted by Beidao Organic Chemical Factory and Shanxi Chemical Industry Research Institute. The main drafters of this standard are Hao Wensong, Zhang Shu, Jiang Renlei, Zhu Yuanbo, 333
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