Some standard content:
Record number: 2837-1999
HG/T 2970-1999
This standard is revised from the chemical industry standard HG/T2970-1989 "Industrial Phosphorus Trichloride" and the cost standard technical indicators are mainly considered for use needs, and are proposed with reference to the product quality data of relevant enterprises. The main technical differences between this standard and HG/T2970-1989 are: 1. According to the actual quality of domestic production, the index requirements for first-class products and qualified products are improved; 2. The test conditions for phosphorus trichloride content and free phosphorus content are clearly determined; according to the nature of the product, the product marking, packaging, transportation and storage are clearly stipulated; sampling is carried out in accordance with the requirements of GB/T6678 "General Principles for Sampling of Chemical Products". The implementation of the industrial phosphorus trichloride industry standard is of great significance for unifying inspection conditions and indicators and strengthening product quality control. This standard is based on the application requirements for product quality and in accordance with GB/T12707-1991 "Guidelines for the Classification of Industrial Product Quality". This standard will replace HG/T2970-1989 from the date of implementation. This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the technical unit responsible for the standardization of chlor-alkali products of the Ministry of Chemical Industry. The drafting units of this standard are: Jinxi Chemical Research Institute of the Ministry of Chemical Industry, Shandong Pesticide Industry Co., Ltd. The main drafters of this standard are: Hu Liming, Li Furong, Liu Yuanchen, Chen Peiyun, and Wang Shaopeng. 949
Chemical Industry Standard of the People's Republic of China
Phosphorus trichloride for industrial use
Phosphorus trichloride for industrial useHG/T 2970—1999
Replaces HG/T 2970--1989
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation, storage and safety of phosphorus trifluoride for industrial use. This standard applies to phosphorus trichloride for industrial use prepared by the synthesis method of yellow phosphorus and nitrogen. Molecular formula: PCl
Relative molecular mass: 137.33 (according to the 1993 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the feasibility of using the latest versions of the following standards. GB 190--19901
Dangerous goods packaging marking
GB191—1990 Pictorial marking for packaging, storage and transportation
GB/T 601-1988 1
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagentsGB/T 6031988
GB/T 615-1988
GB/T 1250--1989
GB/T 6678—1986
GB/T 6680---1986
Preparation of reagents and products used in chemical reagent test methods (neq1ISO6353-1:1982) General method for determination of boiling range of chemical reagents (neqISO6353-1:1982) Expression and determination method of limit values General rules for sampling of chemical products
General rules for sampling of liquid chemical products
GB/T 6682-1992
3 Requirements
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987) 3.1 Appearance: colorless, transparent or slightly yellow liquid. 3.2 Industrial phosphorus trichloride should meet the requirements of Table 1. Table 1 Requirements
Content of phosphorus trichloride
Free phosphorus content
Superior product
Volume fraction at boiling range (74.5℃~77.5℃) 4 Sampling
Second-class product
Qualified product
4.1 The manufacturer takes the daily output or one packaging unit as a batch, and the user can regard each product received as a batch. Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999 950
Implementation on April 1, 2000
HG/T 2970--1999
4.2 For products packaged in glass bottles and iron drums, the number of sampling units shall be determined in accordance with the provisions of 6.6 in GB/T6678---1986. Use an appropriate sampling tube, slowly insert it into the container, and sample at a depth of 2/3; for products packaged in tank trucks, sample from the top, middle and bottom of the tank truck. Mix the sampled samples evenly, with a total volume of no less than 500ml, and place them in two clean, dry ground-mouth bottles (or sample bottles with stoppers and good sealing). Paste labels on the bottles, indicating the manufacturer's name, product name, product batch number, sampling date and the name of the sampler. One bottle is for inspection and the other is kept for future reference. 4.3 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sample from two times the packaging for verification. If one of the indicators in the verification results does not meet the requirements of this standard, the entire batch of products is unqualified. 5 Test method
5.1 Overview
5.1.1 Factory inspection items: appearance, phosphorus trichloride content, free phosphorus content, boiling range. 5.1.2 The rounded value comparison method specified in 5.2 of GB/T1250-1989 is used to determine whether the test results meet the standard. 5.1.3 The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T6682.
The standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601 and GB/T603.
5.2 Determination of phosphorus trichloride content
5.2.1 Summary of the method
Phosphorus trichloride reacts with water to form phosphorous acid, which is oxidized to orthophosphoric acid with excess iodine. The reaction is reversible. To make the oxidation complete, ammonium borate is used to neutralize the hydrogen iodide generated by the reaction, and the remaining iodine is titrated with sodium thiosulfate standard titration solution. Starch is used as an indicator to determine the end point. The reaction formula is as follows:
PCl.+3H2OH.PO3+3HCl
HPO+H2O+I2-H.PO4+2HI
I2+2Na2S,O-NazSO+2NaI
5.2.2 Reagents and solutions
5.2.2.1 Hydrochloric acid solution: 1+6.
5.2.2.2 Hydrochloric acid solution: 1+12.
5.2.2.3 Ammonium borate solution: cL1/3(NH4): BO.=1mol/L. Preparation: Weigh 20g of boric acid (accurate to 0.01g), dissolve it in 170mL10% ammonia water, transfer it to a 1000mL volumetric flask, dilute it to the mark with water, and shake it well.
5.2.2.4 Iodine solution: c()=0.1 mol/L. 5.2.2.5 Sodium thiosulfate standard titration solution: c(NazSOs) 0.1 mol/I. 5.2.2.6 Starch solution: 5 g/L.
5.2.3 Analysis steps
5.2.3.1 Preparation of sample solution
Use a dry pipette to quickly draw 3 mL of sample, place it in a dry weighing bottle of known mass, immediately cover it tightly, weigh it (accurate to 0.0002 g), and then place it together with the weighing bottle in a hydrolysis bottle containing 300 mL of water, cover the hydrolysis bottle tightly, seal it with water, and shake it gently. After the lid of the weighing bottle is opened and the sample slowly flows out, place the hydrolysis bottle in cold water at about 15°C to cool it, and shake the hydrolysis bottle gently and intermittently. Hydrolyze for about 1 hour. After the hydrolysis is complete, transfer all the solution into a 500 mL volumetric flask, let it stand to room temperature, dilute it to the scale with water, and shake it well. 5.2.3.2 Determination
Pick up 25.00ml of sample solution (5.4.3.1) and place it in an iodine volumetric flask. Accurately add 50.00ml of iodine solution, then quickly add 20ml of ammonium borate solution, immediately cover tightly, seal with water, and place in a constant temperature water bath at (25±2)℃. After standing for 30min away from light, add 10ml of hydrochloric acid (5.4.2.1), immediately back-titrate the excess iodine with sodium thiosulfate standard titration solution, add 3ml of starch solution when it is close to the end point, and continue to titrate at 951
to the end point. Perform a blank test at the same time.
HG/T2970—1999
Blank test: Place 13ml of hydrochloric acid (5.4.2.2) and 12ml of water in an iodine volumetric flask. The rest of the operation and reagent dosage are the same as above. 5.2.4 Expression of analysis results
The phosphorus trichloride content X expressed as mass percentage is calculated according to formula (1): X, = (Vi-V) cX0. 068 67 × 100 = (Vi- V)c× 137.3425
Volume of sodium thiosulfate standard titration solution consumed in the titration blank, mL; Where: Vi—
Volume of sodium thiosulfate standard titration solution consumed in the titration sample, mL; Concentration of sodium thiosulfate standard titration solution, mol/L; Sample mass, g;
·(1)
0.06867Mass of phosphorus trichloride equivalent to 1.00mL sodium thiosulfate standard titration solution Lc(NazS2),)=1.000mol/L], g.
5.2.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute value of the difference between the parallel determination results shall not exceed 0.3%. 5.3 Determination of free phosphorus content. www.bzxz.net
5.3.1 Summary of the method
Free phosphorus in benzene solution can reduce silver salts to precipitate metallic silver. The reaction is as follows: P+3AgNO: +3H2O=H.PO +3Ag+ +3HNO: When an emulsifier is present, the precipitated silver is dispersed into a relatively stable brown-yellow silver colloid, and colorimetry is performed at a certain wavelength to determine the content of free phosphorus.
5.3.2 Reagents and materials
5.3.2.1 Benzene.
5.3.2.2 Silver nitrate solution: c(AgNO:)=1 mol/L. Preparation: Weigh 17.5g of silver nitrate, dissolve in 100mL of water, and shake well. The solution is stored in a brown bottle. 5.3.2.3 Emulsifier (anionic and non-ionic mixed solution 1>): 1+1 benzene solution. 5.3.2.4 Phosphorus standard solution: 0.02mg/mL. Preparation: Weigh 0.2g yellow phosphorus (content greater than 99%) with the oxide film removed, wipe it dry carefully with filter paper under nitrogen flow, place it in a weighing bottle of known mass filled with water, weigh it (accurate to 0.0002g), then take out the phosphorus block and wipe it dry under nitrogen flow, immediately put it into a certain amount of benzene (calculate and measure the amount of benzene based on the weighed yellow phosphorus, according to 1mg/mL yellow phosphorus), dissolve it completely, and set aside. When using, dilute it with benzene to 0.02mg/mL at room temperature. 5.3.3 Instruments and equipment
General laboratory instruments.
Spectrophotometer: with a colorimetric III with a thickness of 1cm. 5.3.4 Drawing of standard curve
5.3.4.1 Preparation of standard reference solution
Add 4.0mL of emulsifier to each of six dry 25mL volumetric flasks, and then add 0.0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, and 5.0mL of phosphorus standard solution, dilute to the mark with benzene, and shake to hook. 5.3.4.2 Determination of standard reference solution
Add 1 drop of silver nitrate solution to each standard reference solution, shake vigorously for 10s, and let stand for 8min. Immediately adjust the zero point of the spectrophotometer at 520nm using a 1cm cuvette with the standard reference solution to which 0.0mL of phosphorus standard solution was added, and measure the absorbance of the remaining standard reference solutions within 7min.
Note: 1) Type 0201B is a suitable one. 952
5.3.4.3 Drawing of standard curve
HG/T2970—1999
Draw the standard curve with the mass (mg) of phosphorus contained in 25 ml of standard reference solution as the horizontal axis and the corresponding absorbance as the vertical axis. 5.3.5 Analysis steps
5.3.5.1 Preparation of sample solution
Put 4.0 ml (6.3 g) of sample into a separatory funnel containing 20.0 ml of benzene, add 300 ml of water, cover tightly, shake for 2 min, let stand and separate, and discard the aqueous phase. Repeat the operation until the aqueous phase is neutral. 5.3.5.2 Determination of sample
According to the free phosphorus content, take a quantitative amount of sample solution, put it into a 25 ml volumetric flask, add 4.0 ml of emulsifier, dilute to the mark with benzene, and shake well. Add 1 drop of silver nitrate solution, shake vigorously for 10 seconds, let stand for 8 minutes, immediately adjust the spectrophotometer zero point at 520nm with a 1m colorimetric dish and a blank solution without sample, and measure the absorbance of the sample solution within 7 minutes. 5.3.6 Expression of analysis results
Free phosphorus content X expressed as mass percentage. Calculate according to formula (2): x- m×0.001 ×100 m
Where: V--volume of sample solution absorbed, mL.; mass of sample, g;
m-mass of phosphorus found on the standard curve, mg. 5.3.7 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute value of the difference between the parallel determination results shall not exceed: superior product: 0.0002%;
standard product: 0.0008%;
qualified product: 0.003%.
5.4 Determination of boiling range
According to GB/T615, the following improvements are made according to the characteristics of this product: 5.4.1 The distillation device can be connected with a standard ground joint; 5.4.2 Use an internal standard thermometer without temperature correction; 5.4.3 The heat source is a water bath or directly heated by a 300W voltage regulating electric furnace. 6 Marking, packaging, transportation, storage
6.1 The packaging container of industrial phosphorus trichloride should have firm and obvious markings, including: manufacturer name, product name, trademark, net weight. And there should be firm and obvious "toxic" and "corrosive items" signs specified in GB190. 6.2 Each batch of industrial phosphorus trichloride shipped from the factory should be accompanied by a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, and implementation standard number. 6.3 The packaging container of this product can be clean and dry glass bottles, iron barrels, tank trucks and other suitable containers. When using glass bottles for packaging, the bottle stoppers (caps) should be well sealed and placed in corresponding iron barrels or sturdy wooden boxes. The outside of the bottle should be filled with soft cushioning materials that do not change with the contents. When using iron barrels for packaging, the barrels should have screw caps, washers and other sealing parts, and be in good condition. Tank truck packaging must be well sealed and comply with relevant regulations. 6.4 Phosphorus trichloride products are hazardous chemicals. They must be loaded and unloaded gently during transportation, and measures must be taken to prevent rain, snow and exposure. 6.5 Products must be stored in a cool, dry and well-ventilated warehouse. Stacking is not allowed. 7 Safety
Phosphorus trichloride is a toxic and highly corrosive substance. It reacts violently with water and can cause an explosion. When contacting phosphorus trichloride, you must wear protective equipment such as glasses and rubber gloves. Contact with water is strictly prohibited. 9530mL phosphorus standard solution, adjust the spectrophotometer zero point, and measure the absorbance of the remaining standard reference solutions within 7 minutes.
Note: 1) 0201B is a suitable one. 952
5.3.4.3 Drawing of standard curve
HG/T2970—1999
Draw the standard curve with the mass (mg) of phosphorus contained in 25 ml standard reference solution as the horizontal axis and the corresponding absorbance as the vertical axis. 5.3.5 Analysis steps
5.3.5.1 Preparation of sample solution
Put 4.0ml (6.3g) of sample in a separatory funnel containing 20.0ml benzene, add 300ml water, cover tightly, shake for 2 minutes, let stand and separate, and discard the water phase. Repeat the operation until the water phase is neutral. 5.3.5.2 Determination of sample
According to the free phosphorus content, aspirate a quantitative sample solution, place it in a 25mL volumetric flask, add 4.0mL emulsifier, dilute to the mark with benzene, and shake well. Add 1 drop of silver nitrate solution, shake vigorously for 10s, let stand for 8min, immediately adjust the spectrophotometer zero point at 520nm with a 1m cuvette and a blank solution without sample, and measure the absorbance of the sample solution within 7min. 5.3.6 Expression of analysis results
Free phosphorus content X expressed as mass percentage. Calculate according to formula (2): x-m×0.001×100 m
Where: V--volume of sample solution aspirated, mL.; mass of sample, g;
m-mass of phosphorus found on the standard curve, mg. 5.3.7 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute value of the difference between the parallel determination results shall not exceed: superior products: 0.0002%;
standard products: 0.0008%;
qualified products: 0.003%.
5.4 Determination of boiling range
According to GB/T615, the following improvements are made according to the characteristics of this product: 5.4.1 The distillation device can be connected with a standard ground joint; 5.4.2 Use an internal standard thermometer without temperature correction; 5.4.3 The heat source is a water bath or directly heated by a 300W voltage regulating electric furnace. 6 Marking, packaging, transportation, storage
6.1 The packaging container of industrial phosphorus trichloride should have firm and obvious markings, including: manufacturer name, product name, trademark, net weight. And there should be firm and obvious "toxic" and "corrosive items" signs specified in GB190. 6.2 Each batch of industrial phosphorus trichloride shipped from the factory should be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, and implementation standard number. 6.3 The packaging containers of this product can be clean and dry glass bottles, iron barrels, tank trucks and other suitable containers. When using glass bottles for packaging, the bottle stoppers (caps) should be well sealed and placed in corresponding iron barrels or sturdy wooden boxes. The outside of the bottle should be filled with soft cushioning materials that do not change with the contents; when using iron barrels for packaging, the barrels should have screw caps, washers and other sealing parts, and the matching should be intact; tank truck packaging must be well sealed and comply with relevant regulations. 6.4 Phosphorus trichloride products are dangerous chemicals. During transportation, they must be loaded and unloaded lightly, and measures must be taken to prevent rain, snow and exposure. 6.5 The product must be stored in a cool, dry and well-ventilated warehouse, and it is not allowed to be stacked. 7 Safety
Phosphorus trichloride is a toxic and highly corrosive substance. It reacts violently when it comes into contact with water and can cause an explosion. When contacting phosphorus trichloride, protective equipment such as glasses and rubber gloves must be worn, and contact with water is strictly prohibited.0mL phosphorus standard solution, adjust the spectrophotometer zero point, and measure the absorbance of the remaining standard reference solutions within 7 minutes.
Note: 1) 0201B is a suitable one. 952
5.3.4.3 Drawing of standard curve
HG/T2970—1999
Draw the standard curve with the mass (mg) of phosphorus contained in 25 ml standard reference solution as the horizontal axis and the corresponding absorbance as the vertical axis. 5.3.5 Analysis steps
5.3.5.1 Preparation of sample solution
Put 4.0ml (6.3g) of sample in a separatory funnel containing 20.0ml benzene, add 300ml water, cover tightly, shake for 2 minutes, let stand and separate, and discard the water phase. Repeat the operation until the water phase is neutral. 5.3.5.2 Determination of sample
According to the free phosphorus content, aspirate a quantitative sample solution, place it in a 25mL volumetric flask, add 4.0mL emulsifier, dilute to the mark with benzene, and shake well. Add 1 drop of silver nitrate solution, shake vigorously for 10s, let stand for 8min, immediately adjust the spectrophotometer zero point at 520nm with a 1m cuvette and a blank solution without sample, and measure the absorbance of the sample solution within 7min. 5.3.6 Expression of analysis results
Free phosphorus content X expressed as mass percentage. Calculate according to formula (2): x-m×0.001×100 m
Where: V--volume of sample solution aspirated, mL.; mass of sample, g;
m-mass of phosphorus found on the standard curve, mg. 5.3.7 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute value of the difference between the parallel determination results shall not exceed: superior products: 0.0002%;
standard products: 0.0008%;
qualified products: 0.003%.
5.4 Determination of boiling range
According to GB/T615, the following improvements are made according to the characteristics of this product: 5.4.1 The distillation device can be connected with a standard ground joint; 5.4.2 Use an internal standard thermometer without temperature correction; 5.4.3 The heat source is a water bath or directly heated by a 300W voltage regulating electric furnace. 6 Marking, packaging, transportation, storage
6.1 The packaging container of industrial phosphorus trichloride should have firm and obvious markings, including: manufacturer name, product name, trademark, net weight. And there should be firm and obvious "toxic" and "corrosive items" signs specified in GB190. 6.2 Each batch of industrial phosphorus trichloride shipped from the factory should be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, implementation standard number. 6.3 The packaging containers of this product can be clean and dry glass bottles, iron barrels, tank trucks and other suitable containers. When using glass bottles for packaging, the bottle stoppers (caps) should be well sealed and placed in corresponding iron barrels or sturdy wooden boxes. The outside of the bottle should be filled with soft cushioning materials that do not change with the contents; when using iron barrels for packaging, the barrels should have screw caps, washers and other sealing parts, and the matching should be intact; tank truck packaging must be well sealed and comply with relevant regulations. 6.4 Phosphorus trichloride products are dangerous chemicals. During transportation, they must be loaded and unloaded lightly, and measures must be taken to prevent rain, snow and exposure. 6.5 The product must be stored in a cool, dry and well-ventilated warehouse, and it is not allowed to be stacked. 7 Safety
Phosphorus trichloride is a toxic and highly corrosive substance. It reacts violently when it comes into contact with water and can cause an explosion. When contacting phosphorus trichloride, protective equipment such as glasses and rubber gloves must be worn, and contact with water is strictly prohibited.
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