GC-FID法同时测定腌制鱼干中9种N-亚硝胺类化合物

在气相色谱-氢火焰检测器的基础上建立了同时测定腌制鱼干中9种N-亚硝胺类化合物的方法。采用碱液加热处理结合二氯甲烷萃取的方法提取腌制鱼干的N-亚硝胺,经棷壳活性炭净化,C₁₈固相萃取(SPE,Solid Phase extraction)小柱富集,样液用DB-WAXETR极性柱(30 m×0.25 mm,0.25 μm)进行色谱分离,柱温采用程序升温。结果显示:该方法下的9种N-亚硝胺类化合物在0.05~5 μg/mL浓度范围内线性良好(R2＞0. 999);检出限和定量限范围分别为0.05~0.29 μg/mL和0.18~0.95 μg/mL;回收率和RSD分别为76.8%~129.5%和2.29%~15.5%。对市售的50种腌制鱼干进行检测,N-亚硝基二乙胺(NDEA,N-nitrosodiethylamine)、N-亚硝基哌啶(NDIP,N-Nitrosopiperidine)N-亚硝基吡咯烷(NPYR,N-Nitrosopyrrolidine)检出率分别达到20%、20%、24%,只有一种样品的N-亚硝基二甲胺(NDMA,N-nitrosodimethylamine)超过国标限量规定(4 μg/kg)。     

衣康酸改性苯丙胶乳及其在阻燃性空气滤纸中的应用

本研究采用衣康酸作为功能性单体对苯丙胶乳进行改性,并将改性苯丙胶乳与阻燃剂复配,以浸渍施胶的方式对阻燃性空气滤纸的性能进行改善。研究表明,经衣康酸改性后的苯丙胶乳颗粒平均粒径为0. 0868μm,比改性前降低34. 7%,机械稳定性、稀释稳定性及固含量均表现良好;当衣康酸用量为2%(占单体总质量)时,浸渍改性苯丙胶乳使纸张透气度降低约2. 27%,挺度及耐破度达最优值,分别为3. 40 mN?m和290 kPa,比浸渍改性前的苯丙胶乳分别提高了27. 8%及18. 4%。将阻燃剂与改性苯丙胶乳按质量比1:1.4进行复配后对空气滤纸原纸浸渍后发现,纸张的挺度、耐破度及极限氧指数达4. 07 mN?m、301 kPa和30. 9%,满足我国有关阻燃性空气滤纸行业标准的性能要求。     

植酸的铵化及其对Lyocell织物的阻燃整理

为提高Lyocell织物的阻燃效果,对天然磷化物植酸进行铵化改性,并以双氰胺为催化剂应用于Lyocell织物的阻燃整理。利用傅里叶红外光谱仪、扫描电子显微镜、热重分析仪,测定了阻燃整理Lyocell织物的特征红外吸收、表面形貌以及热稳定性能。对阻燃织物进行了垂直燃烧实验,测定了织物的燃烧性能,并对整理织物的耐洗性进行了测试。结果表明:与未整理Lyocell织物相比,阻燃整理后织物的吸热降解质量损失率下降了20.11%,800 ℃ 时热解残炭量提高了27.98%,垂直燃烧的损毁长度下降至3.4 cm;极限氧指数高达36.6%,达到难燃的级别;且阻燃织物经20次标准洗涤后,仍能达到国家B2标准。     

Experimental study on flame spread along fuel cylinders in high pressures

Flame spread over solid fuels in high‐pressure situations, such as nuclear containment shells during a pressurized period, has potential to result in catastrophic disaster, thus requiring further knowledge. This paper experimentally reveals the flame spread behaviors over fuel cylinders in high pressures. Polyethylene and polymethyl‐methacrylate cylinders with the diameter of 4.0 mm are used in this study. Ambient gas is air, and total pressures are varied from naturally normal pressure (100 kPa) to elevated pressure (500 kPa). Flame characteristics including flame appearance and flame size and burning rate and flame spread rate are investigated. Results show that in high pressure, the flame appearance is significantly affected. As the pressure increases, the blue flame disappeared, and the color of flame tip changes from luminous yellow to orange as well the orange part extends down towards the base of flame. The dimensionless flame height increases with pressure for pressure below 150 kPa and then decreases with pressure above that level. The burning rates show increasing trend with pressure and are proportional to P^0.6 and P^0.79 for polymethyl‐methacrylate and polyethylene, respectively. Besides, flame spread rates for polymethyl‐methacrylate and polyethylene both were found to be proportional to P^0.5.     

Numerical investigation of the effects of H2/CO/syngas additions on laminar premixed combustion characteristics of NH3/air flame

Co-firing NH₃ with H₂/CO/syngas (SYN) is a promising method to overcome the low reactivity of NH₃/air flame. Hence, this study aims to systematically investigate the laminar premixed combustion characteristics of NH₃/air flame with various H₂/CO/SYN addition loadings (0–40%) using chemical kinetics simulation. The numerical results were obtained based on the Han mechanism which can provide accurate predictions of laminar burning velocities. Results showed that H₂ has the greatest effects on increasing laminar burning velocities and net heat release rates of NH₃/air flame, followed by SYN and CO. CO has the most significant effects on improving NH₃/air adiabatic flame temperatures. The H₂/CO/SYN additions can accelerate NH₃ decomposition rates and promote the generation of H and NH₂ radicals. Furthermore, there is an evident positive linear correlation between the laminar burning velocities and the peak mole fraction of H + NH₂ radicals. The reaction NH₂ + NH <=> N₂H₂ + H and NH₂ + NO <=> NNH + OH have remarkable positive effects on NH₃ combustion. The mole fraction of OH × NH₂ radicals positively affects the net heat release rates. Finally, it was discovered that H radicals play an important role in the generation of NO. The H₂/CO/SYN additions can reduce the hydrodynamic and diffusional-thermal instabilities of NH₃/air flame. The NH₃ reaction pathways for NH₃–H₂/CO/SYN-air flames can be categorized mainly into NH₃–NH₂–NH–N–N₂, NH₃–NH₂–HNO–NO(?N₂O)–N₂ and NH₃–NH₂(?N₂H₂)–NNH–N₂. CO has the greatest influence on the proportions of three NH₃ reaction routes.     

Synthesis of a novel DOPO‐based polyphosphoramide with high char yield and its application in flame‐retardant epoxy resins

A novel and highly effective flame retardant (FR), DOPO‐TPMP oligomer, was synthesized by a simple condensation of 4‐(hydroxymethyl)‐2,6,7‐trioxa‐1‐phosphabicyclo[2.2.2]octane‐1‐oxide and phosphorus oxychloride followed by a polycondensation reaction with 6‐(2,5‐dihydroxyphenyl)‐6H‐dibenzo[c,e][1,2]oxaphosphinine‐6‐oxide. The chemical structure of DOPO‐TPMP was well characterized using Fourier transform infrared and NMR spectra. DOPO‐TPMP was used as an additive‐type FR for epoxy resin (EP). The FR properties of the resultant EP composites were investigated by limiting oxygen index (LOI) test, UL‐94 vertical burning test and cone calorimeter measurements. Specifically, the EP composite containing 10.0% DOPO‐TPMP achieved a LOI value of 36.1%, V‐0 rating in the UL‐94 test and a 58% reduction in peak heat release rate. Further mechanism analysis attributed the enhanced flame retardancy to the increased char yield on the addition of DOPO‐TPMP. © 2019 Society of Chemical Industry     

Study on downward flame spread over extruded polystyrene foam in a vertical channel: Influence of opening area

Experimental methods and theoretical analysis are employed to investigate effects of channel opening area on downward flame spread characteristics of extruded polystyrene (XPS) thermal insulation materials on building facade. The average flame height first drops and then rises as dimensionless opening area (the ratio of sidewall opening area to sidewall area, ie, S^*) increases. As S^* rises, both the average and maximum temperature of the curtain wall decrease, and the decreasing of the average temperature is linear. XPS surface temperature history can be divided into four stages, ie, inapparent rising stage (preheating), significant rising stage (melting), dropping stage (pyrolysis), and rerising stage (ignition). The preheating length first rises and then drops as S^* increases. The XPS flame spreads steadily at the early period while acceleration occurs at the later period. For different opening areas, the difference in spread distance history is not apparent in the early stage while this difference is significant in the later stage. The flame spread rate (V_f) first increases and then decreases as S^* rises. A downward flame spread model for XPS in vertical channel with openings is built. The varied trend of V_f predicted using this model corresponds to the experimental result.     

Verification of the new viscoelastic method of thermal stress calculation in asphalt layers of pavements

The new viscoelastic method of thermal stress calculations in asphalt layers has been developed and published recently by the author. This paper presents verification of this method. The verification is based on the comparison of the results of calculations with results of testing of thermal stresses in Thermal Stress Restrained Specimen Test. The calculations of thermal stresses according to the new method were based on rheological parameters of the Burgers model. The parameters were measured in laboratory at different low temperatures, at long time creep under constant loading. Five asphalt mixes were tested. Three of them were high modulus asphalt concretes and two conventional asphalt concretes. Specimens were prepared in exactly the same way both for rheological creep tests and for the Thermal Stress Restrained Specimen Test. The results of measured thermal stresses were compared with thermal stresses calculated from the new viscoelastic method developed by the author and in most cases a good agreement was found. For comparison, the measured stresses were compared with results of calculations according to the existing methods. The viscoelastic Monismith method failed in prediction of thermal stresses. The prediction from the quasi-elastic Hills and Brien method was underestimated, but better than from the Monismith method and worse than from the new viscoelastic method. The reasons of discrepancies were discussed.     

A model of splats deposition state and wear resistance of WC-10Co4Cr coating

In this research both low temperature high velocity oxygen-fuel flame (LT-HVOF) and high velocity oxygen-fuel flame (HVOF) techniques were employed to prepare WC-10Co4Cr splats and coatings. In situ cutting of WC-10Co-4Cr splats was carried out with focused ion beam (FIB), and a model was proposed to describe how the wear resistance of WC-10Co4Cr coatings was correlated with its residual stress state and the splats deposition state. It was observed that in LT-HVOF spraying process, WC-10Co4Cr splats were slightly melted showing "hill" shape, while in HVOF spraying process, the splats were half melted having the appearance of "concavity". The residual stress of WC-10Co4Cr coatings is determined by the size, melting state, flight speed and temperature gradient of splats. In this paper, the quantitative function formula involving heating temperature and the flight speed of the powder is put forward for the first time to predict the wear resistance of the WC-10Co4Cr coatings. This will provide a theoretical basis for engineering practice and an effective way to save costs.     

二甲醚球形扩散火焰的熄火机理研究

采用改进的PREMIX模型及"化学爆炸模式分析(CEMA)"方法,对二甲醚(DME)球形扩散火焰的熄火机理进行数值诊断,分析环境氧气摩尔分数(X_(O_2))及详细基元反应对熄火极限的影响,利用"爆炸因子"和"分岔因子"的概念,确定控制DME球形扩散火焰熄火的关键反应动力学因素。结果表明:DME冷焰具有比热焰更宽的可燃范围;冷焰对X_(O_2)的敏感性弱很多,热焰中具有正特征值的CEM首次出现在最高温度处;在熄火极限附近,CEM的特征值变为虚数,说明熄火伴随着振荡;热焰的熄火主要由小分子所参与的高温反应所控制,而冷焰熄火主要由大分子所参与的低温反应所控制。