Analysis and Source Analysis of Particle Discharge Materials for Oil Starter
1 experimental section Experimental section 111 sample collection and pretreatment The experimental lubricating oil and diesel oil are all produced by Shanghai refinery. The lubricating oil specification is 15E/ 40CF24. Diesel is the standard light diesel oil for engine detection No. 0. It is made by straight-run diesel fraction and catalytic cracked diesel fraction. , Comparable with European Community Standard Diesel Reference Fuel CEC RF2032A284. Diesel engine pedestal experimental procedure is strictly in accordance with the 13 working condition method in GB17691-2005, and particle sampling adopts a split-flow constant-capacity sampling system. The sample and blank filter paper (for control) was wrapped in a glass fiber filter and put into a 150 mL cable extractor, extracted with 75 mL of methylene chloride (chromatographically pure) at a constant temperature water bath at 48 °C for 14 h, and then the extract was added. KD concentration (Kuderna2Danish evaporation concentrating device referred to as KD concentrated cryopreservation for analysis (organic analysis)). Using a pipette, add 3 mL of the diesel sample to the activated alumina column with dichloromethane, and wash with 100 mL of 20% (by volume) n-hexane plus 80% (by volume) methylene chloride mixture. Take off, take the eluent concentrated after use. The dried sample was crushed into a plastic bottle, accurately added to 50 mL (pipette) ultrapure water and shaken evenly, and placed in an ultrasonic cleaner for ultrasonic extraction for 30 min. After the ultrasonic extraction was completed, the plastic bottle was taken out and left to stand. After diluting the supernatant, it was filtered through an injectable disposable filter for 2 times to obtain the liquid to be analyzed (for inorganic ion analysis). 112 Instrument conditions Instrument: ICS22000 ion chromatograph, GC/MS (Agi2 lent 6890GC25975MSD). Reagents: Potassium hydroxide, methanesulfonic acid (produced by Dai'an, USA). Standard substance: SO 4 2 -, NO 2 -, NO 3 -, F -, Cl - mixed standard produced by Agilent; the water used for preparing the mixed standard is ultrapure water. Ion chromatographic column: cation IonpacCG (5 mm×50 mm) guard column, IonpacCS (5 mm×250 mm) separation column; anion IonPacAII2HC (4 mm×50 mm) guard column, IonPacAII2HC (4 mm×250 mm) separation column. Suppressor current: anion 75 mA; cation 94 mA. Eluent: anion 30 mmol/L potassium hydroxide solution; cation 32 mmol/L methanesulfonic acid solution. Flow rate: 1 mL/min. Detector: conductivity detector. Suppressor: anion ASRS 24 mm; cationic CSRs 24 mm. Column temperature, conductivity cell temperature: cation 40°C, anion 30°C. The GC/MS column was an Agilent HP25MS 5% PhenylMethyl Siloam (30 m×250 μm×0125 μm) capillary column. Injection method: automatic injection 1μL; vaporization chamber temperature: 250°C; program temperature rise: initial temperature 60°C, retention 3 min, 4°C/min to 160°C retention 2 min, then 5°C/min to 200 °C, and then to 4 °C/min to 300 °C; carrier gas: high-purity helium; scanning mode: full scan, mass 50 ~ 550; solvent delay: 5 min; EI ion source temperature 230 °C, quadrupole rod 150 °C; mass spectrometry tuning reference material: perfluorotributylamine (PFTBA); mass spectrometry search library: N IST05 (US National Bureau of Standards). 113 Experimental procedure Preparation of standard solutions Cation: weighed 21542 g of sodium chloride (NaCl), 1908 g of potassium chloride (KCl), 21770 g of anhydrous calcium oxide (CaCl 2 ), sulfuric acid, which had been dried at 120°C for 2 h. Magnesium (MgSO 4) 41953 g, weighed ammonium chloride (NH 4 Cl) 21967 g, were dissolved and transferred to a volumetric flask of LL, and the volume was adjusted to the mark. The mass of the mixed standard sample was 110×10 −3. Take the above-mentioned certain amount of standard stock solution into a volumetric flask and dilute to volume with ultrapure water. Prepare five concentrations of mixed standard solution as the standard curve. The concentrations were 011 mg/L, 110 mg/L, 310 mg/L, 510 mg/L, and 10 mg/L, respectively. Anion: Transfer the purchased F-, Cl-, NO2-, SO42-, and NO3-samples to a polyethylene plastic bottle. Take a certain amount of standard solution and place it in a volumetric flask. Dilute to volume with water and prepare a standard curve with 5 concentrations of mixed standard solution. The mass concentrations were 0105 mg/L, 110 mg/L, 210 mg/L, 510 mg/L, and 10 mg/L, respectively. The filtrate obtained from the above pretreatment was diluted with distilled water and quantified by US Dian ion chromatography with a sample volume of 25 μL. The linear regression equation of the standard curve had a correlation coefficient > 01999. There was a good linear relationship between the ion concentration and the peak area. . 2 Results and Discussion After subtracting the inorganic ion content background of the blank control sample A0, it was found that the exhaust particles did not contain magnesium ions, fluoride ions, and chloride ions. The contents of various anions and cations in 15 samples can be found in 2. According to the results, the mass fraction of sodium ions and ammonium ions in diesel engine exhaust particulate samples is high, with an average of 31093% and 21507%, respectively. The mass fractions of calcium and potassium ions are low, and the average value is 21010%. , 11727%. The cation content of each sample did not change significantly with the change of engine model. It can be seen that the 15 samples have higher sulfate mass fractions, the maximum value is A11 sample, which is 131989%, and the lowest value is A122 sample 91282%. The main reason for this result is that the sulfur content of the used fuel is high. . The diesel used in the bench test was supper-light diesel oil, and its sulfur content was measured as 1112 × 10 -3 (mass fraction). However, to meet the requirements of China's three emission limits, the sulfur content of diesel oil should be lower than 0135 × 10-3 It is clear that the current fuel supply does not meet the requirements of the national emission standards. It is understood that the quality of vehicle fuel oil currently sold on the market cannot fully meet emission requirements, leading to a serious decline in the emission levels of in-use vehicles that meet emission regulations. Take No. 0 diesel as an example, the mass fraction of commercially available diesel sulfur in most parts of the country is 1150×10- 3. 211 Determination of Organic Components After the pretreatment of the organic extract was analyzed, the total ion chromatograms of the 15 samples analyzed in the experiment were not listed here. The total ion chromatogram of one of the samples was selected (1). The integral score report and NIST05 library search report were exported, and the sequence, name, and molecular formula of SOF (Soluble Organic Fraction) components were determined and analyzed. Area normalization method was used for quantification and the results were found. The analysis results show that the SOF components in the diesel engine particulates are mainly composed of C13 to C34 n-alkanes and branched paraffins, of which the alkanes below C24 account for the main part of SOF, the mass fraction of which is 6015%; in addition to the alkanes, they are also detected. There are considerable amounts of polycyclic aromatic hydrocarbons (homologous compounds such as naphthalene, anthracene, phenanthrene, and pyrene), mainly naphthalene and phenanthrene, with a mass fraction of 1413%; in addition, isobutyramide and 2,62 Tert-butyl p-methylphenol (BHT) 311%, 22 hexyl methyl propionate, diisobutyl phthalate (D IBP), dibutyl phthalate (DBP), phthalic acid II Iso-octyl ester (D IOP), tert-hexadecane thiol, 6, 10, 142 trimethyl 222 pentadecanone and other phenols, esters, alcohols, ketones and derivatives, accounting for 2512% of the total components Among them, IBP, DBP, and D IOP can be classified into 1718% of phthalates (PAEs) and 413% of others. 212 Particle Source Analysis 2. 2. 1 Sources of alkane in SOF From the analysis results, the carbon number distributions of the linear and branched alkanes in the SOF components of the diesel exhaust particulates are known, and they are mainly concentrated around C 21, tetradecane, pentadecane, hexadecane, and heptadecane. The proportion of SOF components is relatively small, only 31858%. The main reason is that the four kinds of alkanes are more flammable in fuel, and most of them are burned out. The visible experimental diesel chain length is C10-C30, and the peak value is C18. Most of the diesel engine exhaust particulates have the same alkanes as the diesel component, indicating that the main source of SOF is diesel fuel that is not completely combusted. However, diesel engine exhaust particles contained high-carbon paraffin C34, but no such substances were detected in the diesel () component. The literature points out that the unburned lubricating oil entering the combustion chamber is also one of the sources of SOF. The current domestic research on lubricating oil components is mainly concentrated in the petroleum smelting industry. As industry standards generally only categorize the components of the lubricating oil base oil into saturation. Alkanes, aromatics and colloids are three parts without detailed analysis of specific components. However, the lubricating oil is generally composed of high-boiling, high-molecular-weight hydrocarbons, and the number of carbon atoms is generally C15-C45. Therefore, it is detected in this paper that the C34 in the granules is likely to be derived from unburned lubricating oil that has entered the combustion chamber. 2. 2. 2 analysis of source of other components Comparing the particulate matter component with the diesel component, we can see that the polycyclic aromatic hydrocarbons (homologous compounds such as naphthalene, anthracene, phenanthrene, pyrene, etc.) in the microparticles are similar to the aromatic hydrocarbons in diesel fuel, and most of them are 223 ring PAHs and their derivatives. As a result, low-order aromatic hydrocarbons in SOF originated from unburned diesel. Isobutyramide, 2,62 di-tert-butyl-p-methylphenol (BHT), 22-methyl propionate, diisobutyl phthalate (D IBP), dibutyl phthalate (DBP) Compounds such as diisooctyl phthalate (D I2 OP), tert-hexathiol, 6, 10, 142 trimethyl 222 pentadecanone were not detected in diesel fuel. Since the mass fraction of BHT, D IBP, DBP, and D IOP in diesel engine exhaust particulates accounts for more than 70% of other organic impurities, it has been known that no such hazardous substances were detected in the lubricant base oil. The components are derived from lubricating oil additives. The results of this test should attract the attention of the environmental protection department and the oil smelting industry. Isobutyramide, 22 hexyl methyl propionate, tert-hexadecyl mercaptan, 6, 10, 142 trimethyl 222 pentadecanone These less abundant impurities are neither detected in diesel oil nor are lubricating oil additives In addition, no such compounds have been detected in the lubricant base oils of the existing literature, and it is presumed that this may be an intermediate product of combustion in complex conditions. Based on the above conclusions, the main source of diesel exhaust particulates is diesel 75138%, lubricant additives 21107%, and combustion intermediates 3155%. Inflatable Float,Floating Island,6 Person Inflatable Floating Island,Floating Raft P&D Plastic Manufacture Co., Ltd , https://www.jminflatablepool.com