Effect of two-step solid solution on microstructure andδphase precipitation of Inconel 718 alloy

Inconel 718 is the most popular nickel-based superalloy and is extensively used in aerospace,automotive,and energy indus-tries owing to its extraordinary thermomechanical properties.The effects of different two-step solid solution treatments on microstructure andδphase precipitation of Inconel 718 alloy were studied,and the transformation mechanism fromγ″metastable phase toδphase was clarified.The precipitates were statistically analyzed by X-ray diffractometry.The results show that theδphase content firstly increased,and then decreased with the temperature of the second-step solid solution.The changes in microstructure andδphase were studied by scanning electron microscopy and transmission electron microscopy.An intragranularδphase formed in Inconel 718 alloy at the second-[100]_(δ)[011]γ step solid solution temperature of 925℃,and its orientation relationship withγmatrix was determined as//and(010)_(δ)//(111)γ.Furthermore,the Vickers hardness of different heat treatment samples was measured,and the sample treated by second-step solid solution at 1010℃ reached the maximum hardness of HV 446.84.

Synthesis and Solid Phase Extraction Performance Study of NNAL-specific Molecularly Imprinted Polymers Using Dummy Templates

Dummy molecularly imprinted polymers （DMIPs） for 4-（methylnitrosamino）-1-（3-pyridyl）-1-butanol （NNAL） were produced using three structural analogues as dummy template molecules. The chosen analogues were 4-（acetymethylamino）-1-（3-pyridyl）-butanol, 4- （methylamino）-1-（3-pyridyl）-1-butanol, and 1-（3-pyridyl）-1,4,-butanediol. The molecular recognition characteristics of the produced polymers were evaluated by X-ray photoelec- tron spectroscopy （XPS） and Fourier transform infrared spectroscopy （FT-IR）. Interactions between NNAL and methacrylic acid should be cooperative hydrogen bonds while the ni- trogen atom of the pyridine ring and the oxygen atom of the nitroso group in NNAL are two of the hydrogen-bond acceptors. It was further demonstrated that DMIP synthesized by 4-（acetymethylamino）-1-（3-pyridyl）-butanol had the best binding performance by XPS and FT-IR. Then dummy molecularly imprinted solid phase extraction （DMISPE） was developed for the determination of the analyte using the hit polymer as the sorbing material. Under optimal conditions, the recovery of NNAL dissolved in standard solution reached 93%. And the investigated polymer exhibited much higher binding of NNAL when nicotine was acted as the competitive molecule. Also the proposed method was applied to the measurement of NNAL spiked in blank urine samples with recoveries ranging from 87.2% to 101.2%.

Solid-phase Synthesis of-Haloaldehydes from Polymer-supported 4-(Phenylseleno)morpholine

Polystyrene-supported 4-(phenylseleno)morpholine was synthesized and could be used as an efficient ?selenenylating agent for saturated aldehydes. ?Haloaldehydes were prepared by reaction of polystyrene-supported ?selenoaldehydes with bromine or sulfuryl chloride in good yield and high purity.

Solid-Phase Stereoselective Synthesis of (E)-1, 2-Disubstituted Ethenes from Polymer-Sopported a-Selenoaldehydes

Reaction of polymer-supported a-selenoaldehydes with Grignard reagents afforded polymer-bound B-hydroxyalkyl selenides, which treated with thionyl chloride and triethylamine leading to (E)-1, 2-disubstituted ethenes in good yield.

Solid-phase Synthesis of Unsaturated β-Dicarbonyl Compounds from Polymer-supported 4-(Phenylseleno)morpholine

The solid-phase synthesis of unsaturated ?dicarbonyl compounds has been reported.

姜花香气成分的SPME-GC-MS分析

姜花原产我国南部、西南部,印度、马来西亚也有分布,姜花为姜科姜花属多年生草本植物,其花香芬芳纯正,沁人心脾,很受人们喜爱.姜花清芬宜人,早已成为提取芳香油的工业原料,用以制备高级化妆品.……

基于电子鼻和GC-MS的不同品牌橄榄油挥发性风味物质研究

本文旨在探讨不同品牌的橄榄油挥发性风味物质的差异,为研究鉴别不同品牌的橄榄油提供参考。方法:运用电子鼻和顶空固相微萃取-气质联用仪(HS-SPME-GC-MS)对不同品牌的橄榄油挥发性物质进行检测和分析。结果表明:电子鼻能灵敏地检测到不同品牌橄榄油气味的差异性。GC-MS在不同品牌的橄榄油中检测出76种挥发性物质,主要为烃类、醇类、醛类、酮类、酯类、酸类及其他化合物。酸类物质是除帆船牌特级初榨橄榄油外其他4种橄榄油都具有的物质,1号曼托瓦特级初榨橄榄油特有的关键挥发性化合物是癸烷、E-2-庚烯、6-乙基-2-甲基辛烷、戊醛、庚醛、辛醇和2-辛酮;2号百一牌特级初榨橄榄油特有的挥发性物质是1-癸烯和2,2,4,6,6-五甲基庚烷;3号福恩牌特级初榨橄榄油特有的化合物是1-十三烯和辛烷;4号帆船特级初榨橄榄油特有的化合物是十二烷、3,5-二甲基辛烷、D-柠檬烯和3,7-二甲基-1-辛醇;5号斯巴达(金)特级初榨橄榄油特有的化合物是(E)-2-己烯醛。不同品牌的橄榄油之间共有的关键风味化合物主要有己醛和壬醛。结论:橄榄油品牌不同,主要的挥发性成分种类及其相对含量有差异。

液相色谱-质谱联用测定乌头碱血药浓度及其药代动力学参数的方法学研究

乌头碱(aconitine)是存在于乌头属多种植物中的一种双酯二萜生物碱,具有镇[1]、抗炎[2]、抗癫痫[3]、抗肿瘤[4]、提高免疫功能[5]等多种生理活性,但因其具有强烈的心脏毒性和神经毒性,安全系数小,治疗剂量与中毒剂量接近(小鼠LD501.8mg/kg,op;人绝对致死量为2～5mg)[7],限制了对该化合物作为药用的进一步研究,目前仅将其作为致心率失常模型的工具药使用,尚未见其药代动力学的报道.在本文中首次应用液相色谱-质谱联用法对乌头碱在大鼠体内的药代动力学进行了研究.……

液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量

建立了同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物残留量的液相色谱-串联质谱分析方法.样品用2 mol/L氢氧化钠溶液水解,盐酸调节pH值后,以乙腈作为提取溶剂,经C18固相萃取柱净化.各待测物分别经0.1％甲酸甲醇溶液和氨化甲醇（0.1％氨水）洗脱,Phe-nomenex Kinetex C1s（100 mm×4.6 mm,2.6 μm）色谱柱进行分离,采用0.1％甲酸（含5 mmol/L乙酸铵）-甲醇作流动相,梯度洗脱,串联质谱法对5种药物含量进行测定.结果表明,5种药物在2 ～ 100 μg/L范围内线性关系良好,相关系数为0.996 2 ～0.999 8.在加标浓度为5～50 μg/kg的禽肉组织中,这5种药物的加标回收率为73.7％ ～92.3％,相对标准偏差（n=5）为3.9％ ～ 16.6％,检出限为0.2～ 3.0 μg,/kg,定量下限为0.7～ 10 μg/kg.方法快速、简便、经济实用,符合法规要求,可满足日常检测的需要.

固相微萃取GC-MS快速分析火场残留物中汽油成分

火场残留物如碳灰、烧残物等通常经过样品预处理后进行分析鉴定.传统的样品预处理方法往往操作繁琐、费时、重复性差,而且需用大量有机溶剂,不利于分析人员的身体健康,对环境也会造成一定污染.……

快速发酵金丝鱼挥发性风味成分的SPME-GC-MS检测

为改善传统咸鱼的风味,通过在腌鱼上接种Lactobacillus plantarum和Staphylococcus xylosus2种微生物,建立快速发酵法生产风味金丝鱼干,并采用固相微萃取—气相色谱—质谱(SPME-GC-MS)联用法分析、鉴定金丝鱼原料和发酵后的风味成分,研究快速发酵对金丝鱼风味的影响。经NIST质谱数据库检索和文献[1]对照,各检出58、75种成分,其中以羰基化合物和醇类为主,醛类、醇类和酮类分别占60.96%和72.41%。3-甲基-1-丁醇、1-戊烯-3-醇、1-辛烯-3-醇、2-丁酮、3-甲基丁酸等是金丝鱼特征香气成分,酮类和短链不饱和醛及含硫化合物是影响发酵鱼制品风味的主要成分。

罗汉果挥发性成分顶空-固相微萃取-气质联用分析

本研究采取顶空，固相微萃取．气质联用对罗汉果的挥发性成分进行了定性和定量分析。结果表明，最佳的分析条件为：15mL萃取瓶中放置0．2g样品，在60℃条件下选择DVB／CAR／PDMS（50／30μm）萃取头萃取30min。本方法初步鉴定出35种化合物，占总峰面积的92．3％。经分析，主要的化合物包括2．丁烯酸丁酯（14．43％），2，4．壬二稀醛（15．49％两种），对丙烯基茴香N（5．40％），2-庚醇乙酸（5．00％）和糠醛（4．88％）。

气相色谱-离子阱二级质谱法测定猪肉中的氢化泼尼松和甲基氢化泼尼松残留

建立了固相萃取-气相色谱-离子阱二级质谱（GC-MS/MS）测定猪肉中氢化泼尼松和甲基氢化泼尼松残留量的分析方法。待测药物用乙腈提取,C18柱净化,K2Cr2O7氧化,GC-MS/MS测定。采用DB-5毛细管柱分离,电子轰击电离源二级质谱监测模式检测,外标法定量。方法的线性关系良好,线性相关系数均大于0.99,线性范围为2-50μg/kg;氢化泼尼松和甲基氢化泼尼松的回收率为56%-84%。两种药物的检测限和定量限均分别为1μg/kg和2μg/kg。

固相萃取-气相色谱-质谱法同时测定水中9种药品及个人护理用品

采用固相萃取-气相色谱-质谱联用技术，建立了水体中9种药品及个人护理用品（水杨酸、萘普生、布洛芬、对乙酰氨基酚、降固醇酸、三氯生、双氯酚酸、酮洛芬和双酚 A）的定量分析方法。水样品经稀盐酸调节至 pH =3后，采用 Oasis HLB 固相萃取小柱进行富集净化；选用三甲基氢氧化硫（ TMSH）为衍生化试剂，在常温条件下对目标物进行快速甲基化；以气相色谱-质谱法选择离子监测模式（GC-MS-SIM）进行检测，由2，4，5-涕丙酸为内标进行定量分析。本实验分别对固相萃取和衍生化等前处理条件进行了系统的研究。在优化的实验条件下，方法的回收率为50.7～115.4％，相对标准偏差均不高于10％，检出限为0.03～0.30μg / L，定量限为0．15～1．50μg / L。利用该方法对东莞市某农田灌溉水进行了分析，4种目标物在样品中有检出，最大质量浓度范围为0.176～0.998μg / L。结果表明该方法操作简便，灵敏可靠。

苯-丙聚合物-SE30复合固相微萃取涂层的研究与应用

以苯乙烯-丙烯酸乙酯共聚物与色谱固定液SE30结合作为固相微萃取头涂层。考察了复合涂层的热稳定性及其与纤维结合能力。自制了 SPME装置。采用HS-SPME-GC技术萃取分析了水中一氯苯、二氯苯、三氯苯。以色谱峰高对浓度作外标曲线,在10-100mg/L范围内,一氯苯、二氯苯、三氯苯的线性相关系数分别为0.9968、0.9976、0.9904,最低检测限分别为0.32 mg／L、0.27 mg／L、0.50 mg/L。样品测试中,相对标准偏差(n=5)分别为5.37％、4.78％、6.63％,加标平均回收率分别为94.4％、96.7％、94.2％。将自制涂层与商品涂层(PDMS、PA)对水中氯代芳烃化合物萃取量进行了比较,实验结果表明苯乙烯丙烯酸乙酯聚合物-SE-30复合涂层对芳烃化合物具有优良的吸附特性。

气相色谱-负化学源质谱联用法测定水产品及食用油中氟乐灵的残留量

建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1～40μg / L 范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02μg / kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验，平均回收率均处于80％～100％之间，RSD≤10.3％；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。

福建姜黄挥发油化学成分的HS-SPME-GC-MS分析

采用水蒸气蒸馏法提取福建姜黄挥发油,应用顶空固相微萃取进样结合气相色谱-串联质谱联用技术(HS-SPME-GC-MS)分析姜黄挥发油的化学成分。结果表明:姜黄挥发油含有量为7.2%(mL/g),从姜黄挥发油中共分出62个色谱峰,初步鉴定出了其中的51种化学成分,占总挥发油总量的98.41%。在鉴定的化合物中,主要为单萜类化合物和倍半萜类化合物,其中新发现一种主要成分为β-柏木烯,相对含量占比高达26.58%,这可作为福建姜黄挥发油的特征成分和主要品质指标。本研究结果将为福建姜黄植物药材的品质评价提供科学依据。

Perovskite Sr0.9Fe0.9Zr0.1O3-δ:Redox-stable Structure,Oxygen Vacancy,Electrical Properties and Steam Electrolysis Performance

Many researchers have studied on perovskite oxide for its unique structure.Perovskite oxides,ABO3-δ,with different A and B metals have shown wide applications in many fields,in particular solid oxide electrolysers.SrFeO3-δ,typical perovskite oxides,in which iron is the mixed-valence cation with the capacity to change the chemical valence,have a wide range of oxygen nonstoichiometry.In this study,Sr（0.9）Fe（0.9）Zr（0.1）O3-δ（SFZO） is synthesized and then treated in 5%H2/Ar and air at high temperature,exhibiting excellent redox stability.Redox-stable structure,oxygen vacancy and electrical properties of SFZO are investigated.Steam electrolysis is then performed with SFZO cathode under 5%H2O/5%H2/Ar and 5%H2O/Ar atmospheres,respectively.The present results indicate that the SFZO is a novel promising cathode material for solid oxide steam electrolyser.

COMPARISON OF VARIOUS CORRELATION ON IRMA FOR CA19-9 AND CA50 IN THE DIGESTIVE SYSTEM TUMOUR

This paper compared various correlation of IMRA for CA19-9 and CA50 in the digestive system tumour antigen, such as linearity, sensitivity, analytical range, precision as well as storage and stability and so on. And it also determined serum level of CA19- 9 and CA50 of patients with different tumours. The results showed it was well correlated to CA19- 9 and CA50 as a marker of digestive system tumour. Particularly high levels of both markers were found in patients with pancreastic colonic cancer. Therefore it is possible to obtain a higher sensitivity and acceptable specificity by combination with CA19-9 and CA50.

A NEW POLYMER-BOUND 1,2-DIOL AS A PROTECTING AGENT FOR SYMMETRICAL DIALDEHYDE

A novel polymer-bound 1,2-diol, 3-polystyrylsulfonyl-1,2-propanediol (6) had been prepared by the reaction of sodium polystyrylsulfinate with allyl bromide, followed by oxidation and. hydrolysis or directly with 3-chloro-1,2-propanediol in the presence of a phase transfer catalyst, n-tetrabutylammonium iodide. The capacity of resin 6 for terephthaidehyde reached 1.43 mmol/g. The aldehydic groups attached to polymer 6 reacted with hydroxylamine hydrochloride or reduced by sodium borohydride giving p-formylbenzaldoxime (yield: 89%)and p-formyl-benzalcohol (yield: 734%), respectively. The high yields of these polymer-supported reactions showed that the polymer 6 possessed the effective isolation of its reactive sites.