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HJ 2525-2012English339 Add to Cart 3 days [Need to translate] Technical requirement for environmental protection products. Fast analyzer for detergent in gasoline by thin-layer chromatography Valid HJ 2525-2012


BASIC DATA
Standard ID HJ 2525-2012 (HJ2525-2012)
Description (Translated English) Technical requirement for environmental protection products. Fast analyzer for detergent in gasoline by thin-layer chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard N52
Classification of International Standard 71.040.20
Word Count Estimation 13,139
Quoted Standard GB/T 191; GB 9969; GB/T 13306; GB/T 13384; GB 17930; JB/T 9329
Drafting Organization China Environmental Protection Industry Association
Administrative Organization Ministry of Environment Protection
Regulation (derived from) Department of Environmental Protection Notice No. 47 of 2012;
Summary This standard specifies the use of thin-layer chromatographic determination of motor gasoline, ethanol gasoline detergent analyzer technical requirements, test methods, inspection rules, marking, packaging, transportation and storage. This standard is app


HJ 2525-2012 Technical requirement for environmental protection products.Fast analyzer for detergent in gasoline by thin-layer chromatography People's Republic of China Environmental Protection Industry Standard Environmental protection product technical requirements thin layer chromatography car Fastener for measuring detergent in gasoline Technical requirement for environmental protection products Fast analyzer for detergent in gasoline by thin-layer chromatography Published on.2012-7-31 2012-11-1 Implementation Ministry of Environmental Protection released Content Foreword..II 1 Scope 1 2 Normative references 1 3 Terms and Definitions..1 4 Basic requirements 2 5 performance requirements 2 6 Test method 3 7 Inspection rules 4 8 Marking, packaging, transportation and storage..5 Appendix A (informative appendix) How to use the detergent rapid analyzer in gasoline 6 HJ □□□□-201□ Foreword In order to implement the "Environmental Protection Law of the People's Republic of China", reduce emissions of automobile engine pollutants, and supervise motor gasoline. This standard is established by the addition of detergent. This standard specifies the basic requirements, performance requirements, test methods, and methods for the rapid determination of the gasoline detergent for the vehicle. Inspection rules and signs, packaging, transportation and storage. This standard is formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard was first developed. This standard is mainly drafted by. China Environmental Protection Industry Association, Tianjin Yuetai Petrochemical Technology Co., Ltd., Shenzhen Runhe Code Industry Co., Ltd. This standard was approved by the Ministry of Environmental Protection on July 31,.2012. This standard has been implemented since November 1,.2012. This standard is explained by the Ministry of Environmental Protection. Technical requirements for environmental protection products Thin layer chromatography, rapid cleaning agent for motor gasoline tester 1 Scope of application This standard specifies the technical requirements for the determination of detergents for motor gasoline and ethanol gasoline by thin layer chromatography. Inspection methods, inspection rules, marking, packaging, transportation and storage. This standard applies to the detection of automotive gasoline, ethanol gasoline and methanol gasoline whether a sufficient amount of polyisobutylene and Polyetheramine (molecular weight 600-1500) is a rapid tester for detergents of effective detergents. 2 Normative references This standard refers to the terms of the following documents. For undated references, the valid version applies to this standard. GB/T 191 packaging storage and transportation icon GB 9969.1 General instructions for the use of industrial products GB/T 13306 signage General technical conditions for GB/T 13384 mechanical and electrical product packaging GB 17930 motor gasoline JB/T 9329 Basic environmental conditions and test methods for instrumentation transportation, transportation and storage 3 Terms and definitions The following terms and definitions apply to this standard. 3.1 Effective substances in gasoline detergents effective substances in gasoline detergent Among the substances used in gasoline detergents, there are mainly polyisobutylene amines and polyether amines. 3.2 SPE solid phase adsorption column solid phase extraction A small adsorption column for adsorbing or purifying samples. 3.3 thin layer chromatography The stationary phase is uniformly applied to the thin plate to form a thin layer of a certain thickness and has a certain separation activity. Chromatographic separation on a thin layer is called thin layer chromatography. 3.4 ratio shift value Rf value In thin-layer chromatography, the ratio of the distance from the origin to the center of the spot on the thin plate and the distance from the origin to the front of the solvent. 3.5 reference solution A polyetheramine or polyisobutylene amine is formulated into a known amount of solution equivalent to the effective detergent component for detection The performance of the instrument and the quantitative reference standard. HJ □□□□-201□ 4 basic requirements 4.1 Appearance 4.1.1 The surface and decoration of the casing should be free from cracks, deformation, scratches, dirt, burrs, etc. The surface coating should be uniform. No corrosion, rust, shedding and wear. 4.1.2 Under normal operating conditions, it can work smoothly without danger. 4.1.3 The product assembly should be firm, the parts should be tightened without looseness, and the buttons, switch door locks, etc. should be matched with appropriateness, and the control can be flexible. by. Each part is not easy to produce mechanical and electrical faults, and there should be static grounding facilities. 4.1.4 The heat-bonding part of the separation part shall not be deformed or changed by heating. 4.1.5 The whole machine should be easy to maintain and inspect the operation. 4.2 Composition The composition of the detergent in the thin layer chromatography gasoline should include two parts. the pretreatment part and the separation and detection part. The general pretreatment part consists of a vacuum pump, a rotary evaporator and an SPE solid phase adsorption column for concentrating and purifying the sample; The separation and detection sections are composed of a thin layer chromatography plate and an ultraviolet lamp. 4.2.1 The vacuum pump is a circulating water vacuum pump or an oil-free vacuum pump with a vacuum of -0.090 MPa to -0.096 MPa. 4.2.2 Rotary evaporators should ensure the corrosion resistance and life requirements of the sealing system at high temperatures and maintain good temperatures at high temperatures. Sealing; glass accessories should be made of hard glass with high temperature resistance and corrosion resistance; the maximum bath temperature of the evaporator should be greater than 180 °C. It can be adjusted from room temperature to 180 °C. 4.2.3 SPE solid phase adsorption column. 5 ml medical syringe with silica gel (180μm~250μm), loading 500 Mg ± 20 mg. 4.2.4 UV lamp. The short-wavelength UV wavelength should be 254 nm and the long-wavelength UV wavelength should be 365 nm. 4.2.5 Thin-layer chromatography plates. height should be no less than 20cm, width should be no less than 10cm, coating thickness is 0.2mm~0.3mm, HF254 silica gel with a particle size of 10μm to 40μm should be uniform and free of bubbles. 4.3 Environmental conditions The working environment temperature of the thin layer chromatography gasoline detergent analyzer is -5 ° C ~ 45 ° C, the relative humidity is less than 85%, applicable The effective content of the detergent is in the range of 50 mg/L to 800 mg/L. 5 performance requirements Thin layer chromatography for the rapid determination of detergents in motor gasoline should meet the technical requirements of Table 1. Table 1 Performance Index of Detergent Rapid Tester for Vehicle Gasoline by Thin Layer Chromatography Serial number project name performance requirements 1 accuracy test ± 15% 2 repeatability ± 15% 3 Partial vacuum degree -0.090MPa~-0.096MPa 4 Rotary evaporator maximum bath temperature ≥180 °C 5 Rotary evaporator evaporation rate ≥1000mL/h 6 insulation resistance 20MΩ or more 7 thin plate uniform without bubbles 8 Between 50 Hz and 1500V AC voltage between the withstand voltage power supply phase and the casing, there should be no arcing and breakdown. 6 Test methods 6.1 Test conditions 6.1.1 The ambient temperature should be between 0 °C and 40 °C. 6.1.2 Relative humidity is below 85%. 6.1.3 The voltage is 220V±20V. 6.1.4 The power frequency is 50Hz±0.5Hz. 6.2 Test materials 6.2.1 5mL medical syringe 6.2.2 Thin-layer chromatography plates. The coating of silica gel should be uniform and free of air bubbles and dried in an oven at 110 ° C for 2 hours. 6.2.3 Reference solution. Accurately weigh 1.000g (accurate to 0.001g) pure polyetheramine or polyisobutyleneamine, add to 1.0L Gasoline (in accordance with GB 17930, no added detergent), formulated into a 1000mg/L solution, sealed and stored at 0 ° C ~ 5 ° C In the refrigerator, the validity period is 7 days. Dilute 10 times before use to become a reference solution of 100 mg/L. 6.3 Inspection of appearance and composition Check by visual inspection or by looking at the design file. 6.4 Accuracy experiment Under the experimental conditions of 6.1, according to the method in Appendix A, the test is formulated with polyetheramine or polyisobutyleneamine and gasoline. A reference solution having a polyetheramine or polyisobutyleneamine content of 100 mg/L and 700 mg/L was prepared three times each. Calculate the deviation of the mean, Should be less than ±15%. 6.5 Repeatability test Under the experimental conditions of 6.1, according to the method in Appendix A, the test is formulated with polyetheramine or polyisobutyleneamine and gasoline. A reference solution having a polyetheramine or polyisobutyleneamine content of 100 mg/L was prepared 6 times. Calculate the relative standard deviation, which should be less than ±15%. 6.6 Vacuum test Check the working vacuum of the vacuum pump with the calibrated pressure gauge, and connect the nozzle of the vacuum pump to the vacuum hose with the tee. One side of the tee is connected to the pumped container, and the other end is connected to the calibrated vacuum gauge to observe the vacuum gauge reading on the vacuum gauge and the pump. The difference should not be greater than ±0.002MPa; the working vacuum of the vacuum pump should be between -0.090MPa and -0.096MPa. 6.7 Rotary evaporator bath temperature The evaporator bath temperature is checked with a calibrated mercury thermometer, and the maximum temperature should be greater than or equal to 180 °C. 6.8 Evaporation speed Under normal pressure, 1000 mL of distilled water was placed in a rotating bottle, the bath temperature was adjusted to 150 ° C, and the water in the rotating bottle was evaporated. The time should be less than 1h. 6.9 Insulation resistance In a normal environment, turn off the meter and measure it with a nationally specified impedance meter (DC 500V insulation impedance meter). The insulation resistance between the source phase and the chassis (ground). HJ □□□□-201□ 6.10 Withstand voltage Under normal environmental conditions and when the analyzer is turned off, 50 Hz is applied between the power supply phase and the chassis (ground). The 1500V AC voltage lasts for 1 minute and there should be no arcing and breakdown. 7 Inspection rules 7.1 Inspection classification The inspection of this product is divided into factory inspection and type inspection. 7.2 Factory inspection 7.2.1 The equipment shall be inspected one by one according to the specified items and testing methods before leaving the factory. Each set of instruments Product certification and instructions for use should be attached. 7.2.2 The items of factory inspection are as specified in Table 2. 7.3 Type inspection 7.3.1 Type inspection shall be carried out when one of the following conditions is true. a) new product type identification; b) when the product structure, process, or material changes may affect the main performance of the product; c) normal production, once every three years; d) When the product is discontinued for more than one year, when the production is resumed; e) When the factory inspection result is different from the previous type inspection. 7.3.2 Type inspection shall be taken from one of the products that have passed the factory inspection, and the sampling base shall be not less than 5 units. Table 2. 7.4 Decision rules 7.4.1 If the product has been tested and the project meets the requirements of this standard, the batch is judged to be qualified. 7.4.2 If the factory inspection fails, it cannot be shipped. 7.4.3 If the type test fails, the sample shall be doubled and the unqualified item shall be tested; if it is still unqualified, then The batch was judged to be unqualified. Table 2 Tester test items and test methods Serial number item name factory inspection type inspection inspection method 1 Appearance, composition √ 6.3 6.3 2 Accuracy -- √ 6.4 3 Repeatability -- √ 6.5 4 Vacuum degree √ 6.6 5 evaporator maximum bath temperature √ 6.7 6 Evaporator evaporation rate √ 6.8 6.8 7 Thin layer √ 6.3 6.3 8 insulation resistance -- √ 6.9 9 withstand voltage -- √ 6.10 8 Marking, packaging, transportation and storage 8.1 mark TLC method for the rapid determination of detergent in motor gasoline. The product label is set in the obvious part, and the signage should conform to GB/T. Provisions of 13306. The contents of the sign include. a) the name of the manufacturer; b) product name; c) trademark; d) product model or marking; e) date of manufacture, serial number or production lot number; f) the main parameters of the product; g) Power requirements. 8.2 Packaging 8.2.1 The packaging type shall comply with the provisions of GB/T 13384. 8.2.2 There should be a receipt and delivery mark and a storage and transportation mark outside the package, and it should comply with the provisions of GB/T 191. 8.2.3 The instructions shall be included in the package, and the instructions shall comply with the provisions of GB 9969.1. 8.3 Transportation The transport of the detergent rapid analyzer should meet the requirements of JB/T 9329. 8.4 Storage The detergent rapid tester should be stored in a dry and ventilated room and avoid squeezing and collision. HJ □□□□-201□ Appendix A (informative appendix) How to use detergent rapid analyzer in gasoline A.1 Scope The experimental method is suitable for the rapid determination of detergent in vehicle gasoline by thin layer chromatography, and the detection range is effective The net content of the substance is 50 mg/L to 800 mg/L. A.2 Introduction to the method In order to detect whether the gasoline contains the effective substance of the detergent, a certain amount of the sample to be tested is measured and concentrated by vacuum distillation to For a certain amount, the sample is purified by a solid phase extraction column, spotted on a thin layer chromatography plate, and separated, and finally compared with the thin layer plate. No spots or spots are located to determine the amount of detergent active substance in the sample to be tested. A.3 Instruments and reagents A.3.1 Instruments A quick tester for detergents in motor gasoline. A.3.2 Reagents and materials A.3.2.1 Methanol. Analytical purity A.3.2.2 Ether. Analytical grade A.3.2.3 Dichloromethane. analytically pure A.3.2.4 Thin layer chromatography plate. 10 cm × 20 cm, dried in an oven at 110 ° C for 2 hours before use. A.3.2.5 SPE solid phase adsorption column A.3.2.6 5mL medical syringe A.3.3 Reagent preparation A.3.3.1 Preparation of reference solution Accurately weigh 1.000g (accurate to 0.001g) pure polyetheramine or polyisobutylene amine, add to 1.0L gasoline (in accordance with GB 17930, no added detergent), formulated into a 1000mg/L solution, sealed and stored in the refrigerator from 0 ° C ~ 5 ° C, Valid for 7 days. Dilute 10 times before use to become a reference solution of 100 mg/L. A.3.3.2 Preparation of the developing solution Methanol, diethyl ether and dichloromethane were uniformly mixed at a ratio of 58.40.2. A.4 Test procedure A.4.1 Oil sample concentration Use a measuring cylinder to measure 100 mL of gasoline to be tested, pour it into a 500 mL distillation flask, and connect to a rotary evaporator to open the vacuum. The pump (vacuum degree is about -0.090~-0.096MPa), the heating speed after boiling is not too fast, the distillation is near to dry, the heating is stopped and the heating is slowed down. Slowly break the vacuum. After the flask is cooled, some samples will condense at the bottom of the flask and pour the condensed sample into a 5 mL stopper scale. Test tube, volume about 1~1.5mL, take appropriate amount of dichloromethane wash flask (can be carried out in ultrasonic cleaner), wash solution Incorporate into the tube so that the total volume is approximately 2.5 mL. A.4.2 Sample purification Connect a 5 mL medical syringe to the SPE solid phase adsorption column, pour the concentrated sample into the syringe, and push the plunger to make a sample. The product was passed through a SPE solid phase adsorption column and the sample was collected using another 5 mL stoppered graduated tube. A.4.3 Spotting Open the spotting lamp on the spotting table of the UV lamp, spot the sample on the thin layer plate with a micro syringe, and set the center distance from the bottom of the thin layer. The part is about 2cm. The sample volume per point is 5 microliters (note that do not hurt the thin layer when spotting, do not fast the spotting, spotting The spot should not exceed 5mm. To prevent interaction, the distance between the sample points should not be less than 2cm. Each sample is in one Three sample points are placed on the thin layer of the plate. A.4.4 Expand Pour the prepared developing solution into the unwinding cylinder. The dosage is determined according to the size of the unrolling cylinder. The solvent depth is 0.5~0.8cm. The thin layer plate is placed vertically into the unwinding cylinder, and one end of the filter paper is inserted into the solvent liquid surface, and the other end is pressed under the unfolding cylinder head. Unfolding the cylinder The height of the leading edge is about 2cm from the top of the board. Note. Due to the extremely volatile solvent, it is recommended that the test section be placed in a ventilated environment. A.4.5 Observation After the deployment is complete, remove the thin layer and allow to dry. Turn on the UV lamp or use iodide to observe if there are spots of detergent. A.4.6 Representation and calculation of test results As shown in Figure 1, measure the spread distance of the spot and the spread front distance, and calculate the average of the three sample points according to formula A1. The specific shift value is found on the standard curve to find the corresponding effective cleansing substance content. Expand front distance Solute expansion distance ratio shift value = fR A1 HJ □□□□-201□ Figure 1 Schematic diagram of the ratio shift calculation Expanding front edge distance solute expansion distance ......


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