舰艇用LZN-2型高性能阻尼材料释放物定性定量分析与评价

舰艇舱室多为密闭环境,舱室内使用的非金属材料释放物是舱室污染的主要来源,因此对所选用的非金属材料必须进行常温释放物的定性定量分析。由于舰艇的特殊性,不仅要求非金属材料在常温条件下释放物的浓度符合舰艇舱室容许浓度,还要求材料在高温条件(火灾或爆炸)下不产生高毒性的物质。本文根据有关军用标准和规程对舰船用LZN-2型高性能阻尼材料常温释放物和高温热解物进行定性、定量分析,从而对其使用的安全性进行评估。     

舰船用无溶剂环氧涂料常温释放物及高温热解物分析与评价

涂料作为舰船舱室及其部件的内部防护装饰材料已广泛地应用于舰船舱室,科技的发展使得涂料更新换代的步伐加快。舰船舱室经常处于全封闭状态,为减少舱室空气污染对船员的身心健康和战术技术发挥的不良影响,故对舰船舱室大气环境质量提出了更高更新的要求,因此舰船用涂料的筛选尤为重要。涂料作为常用的一种非金属材料其挥发物具有一定的毒性,尤其是对一些新的、毒性不明的涂料,必须先对其进行使用条件下的安全性评价,以便确定其可否应用于舰船舱室之中。本实验根据有关标准对舰船用低毒无溶剂环氧涂料常温释放物及高温热解物进行分析,并对其作卫生学评价,从而为舰船设计、建造部门在筛选艇用涂料方面提供可靠的科学依据。     

新型导弹驱逐舰舱室大气组分的定性定量分析

新型导弹驱逐舰是我海军主要战斗舰船,因其"全封闭"的环境特点,对舱室空气质量产生不同影响,致使舱室大气组份复杂,浓度差异,只有对其进行全面的定性定量测定,才能正确给予卫生学的分析与评价.     

某潜艇长航期间舱室空气污染物的定性测定

潜艇是一个设备复杂、人员集中的密闭环境,特别是潜艇采用了核动力后,使舱内空气污染问题突出起来,为了弄清污染物的详细组成,我们利用色-质(GC-MS)联用仪和其它仪器设备对某潜艇舱室内空气污染物进行定性分析,以便为毒理学研究及制订<潜艇舱室空气组分容许浓度>军用标准提供科学依据.     

密闭环境中人体自身代谢挥发性有机化合物气相色谱/质谱分析

参考EPA TO－14方法,以稍加改装热解析装置Tekmar6000和吹扫捕集装置Tekmar 3000作为进样系统,对密闭环境中人体挥发性有机化合物（VOCs)进行了GC／MS定性分析和外标定量,初步确定了密闭环境中的生活人员给密闭的生活环境带来的污染成分,为密闭环境的气体净化提供了依据。     

氯气的制备与性质综合实验设计

将氯气制备与多个性质实验及尾气吸收综合在一起进行一体化创新设计,整个装置密闭,操作简单。该实验集微型化和综合性于一体,既节约试剂,现象明显,又可控速率,绿色环保,非常适合课堂演示。     

堆沤腐肥时防止跑氨的一种方法

在堆沤熟化制造腐植酸铵过程中,跑氨现象很普遍。我们用测定酸碱度的试纸测定的方法,对用尼龙胶布覆盖和木板、水泥板封面的密闭池(室)熟化的情况,作了一些调查,发现上述覆盖密闭也不能全部控制跑氨现象。氨很容易挥发,只要稍有孔隙,就钻空而出,特别是填料不足,留有空间的密闭池(室),这些空间就充满氨气,盖门一开,大量跑氨。为解决这问题,我们用腐植酸原料(泥炭、风化煤、煤矸石等)进行封面堆沤。做法是:(1)用砖砌成四壁密闭的氨化池。     

改进溶胶—凝胶法固定酶结构剖析及在苯酚光化学传感器？…

通过光学显微镜比较了用密闭老化法和浸涂法制备的溶胶－凝胶膜的表面状态,从实验上证实了用密闭老化法制备的溶胶－凝胶膜不会破裂,并用透射电子显微镜了包埋根过氧化物酶的溶胶－凝胶膜的内部结构。     

密闭罩

密闭罩用于产生有毒物质的实验,其制作方法为: 取用透明、强度性能良好的塑料薄膜,围成一个密闭的圆台体,台体两底面边缘衬以金属硬圈,起支撑、固定罩的作用。     

锅炉给水中微量溶氧的自动监测

为防止蒸汽锅护的腐蚀、热电厂、蒸汽动力舰船和核电站的高压燕汽锅护的给水要求把溶氧控制在10ppm以下。我们所设计、研制的7258型溶氧分析仪能自动、连续、准确的监测给水中微量的溶氧。该仪表是由隔膜式极谱氧传感器、放大器和多     

Thermal decomposition study of the coordination compound [Fe(urea)6](NO3)3

The thermochemical behavior of the coordination compound [Fe(urea)₆](NO₃)₃ was studied by simultaneous CG–TG–DTG–DTA and mass spectrometry methods non-isothermal conditions. The compound decomposes at 200 °C into a mixture of spinel-type oxides and hematite. The nature and particle size of the final decomposition products are strongly associated with the conditions during the thermal treatments, in particular the heating rate and the calcination temperature. A certain fraction of the products are formed as nanometric particles; they show superparamagnetic behavior at room temperature. The comparably low temperature of the calcination treatments of this compound is a promising perspective to attain small sized magnetic powders.     

Polyethylene glycol （PEG） as a benign solvent for Knoevenagel condensation

The Knoevenagel condensation of aromatic aldehydes with active methylene compound proceeded efficiently in polyethylene glycol at room temperature with L-proline as catalyst. The yield is high and the products had E-isomer dominantly. Polyethylene glycol containing L-proline could be recycled and reused for several times without noticeably decreasing in productivity.     

Brominations of steroidal hormone having alpha,beta-unsaturated ketone, 17-O-acetyltestosterone, in the presence of silver triflate

Bromination of 17-O-acetyltestosterone (17beta-acetoxyandrost-4-en-3-one) (1) was performed with 1, 5, and 10 eq of Br2 in AcOH-Et2O at room temperature. In all cases 2alpha,6beta- (2) and 2alpha,6beta-dibromo-17beta-acetoxyandrost-4-en-3-one (3) were obtained, although the yields were dependent upon the conditions used. Bromination of compound 1 with 10 eq of Br2 in the presence of silver trifluoromethanesulfonate (silver triflate, AgOTf) at room temperature for 12 h gave 2,7alpha-dibromo- (4) and 2,4,7alpha-tribromo-17beta-acetoxy-3-hydroxy-1-methylestra-1,3,5(10)-triene-6-one (5). The formations of the products were inferred on the basis of products obtained under controlled brominations of 1 in the presence of AgOTf, and of those obtained by the brominations of compounds 9-13 also in the presence of AgOTf.     

Chemoenzymatic synthesis of a mixed phosphine-phosphine oxide catalyst and its application to asymmetric allylation of aldehydes and hydrogenation of alkenes

The chemoenzymatic synthesis of a Lewis basic phosphine-phosphine oxide organocatalyst from a cis-dihydrodiol metabolite of bromobenzene proceeds via a palladium-catalysed carbon-phosphorus bond coupling and a novel room temperature Arbuzov [2,3]-sigmatropic rearrangement of an allylic diphenylphosphinite. Allylation of aromatic aldehydes were catalysed by the Lewis basic organocatalyst giving homoallylic alcohols in up to 57% ee. This compound also functioned as a ligand for rhodium-catalysed asymmetric hydrogenation of acetamidoacrylate giving reduction products with ee values of up to 84%.     

Further studies on synthesis of the 12,13-seco norditerpenoid alkaloids

After a series of optimization for the reaction conditions (reagents, reaction temperature, etc.), treatment of the sulfonates 4, 8, 13 and 15 with 8% NaOH (room temperature, 24 h) via a semipinacol rearrangement afforded the corresponding C-nor compounds 5, 9, 12 and 16, as the major of a pair of epimer at C-16, to an excellent extent, in 95%, 92%, 100% and 90% yield, respectively. The 12,13-seco compounds 21 and 22 (23) were obtained in 20% and 60% yield, respectively, by treating 5 with Br(2)-glacial HOAc (room temperature, 24 h). Treatment of the C-nor compounds 5 or 6, 16 or 17, and 28 from 10 with SOCl(2)-anhydrous benzene (room temperature, overnight) afforded the 12,13-seco compounds 24, 26 and 30 in 70% or 100%, 40% and 66% yield, respectively. When treatment of the C-nor compound 29 from 9 under same conditions gave the 12,13-seco products 30, 31 and 32 in 33%, 26% and 20% yield. When treating 21 or 24, and 26 with 5% KOH in EtOH afforded the 12,13-seco compounds 25 and 27 quantitatively, respectively. The compound 31 converted to 30 quantitatively by treatment with Na(2)CO(3) in MeOH. All of the new compounds were isolated and fully characterized.     

梳型接枝共聚物的合成（Ⅲ）——氯代乙酸（降冰片稀基）甲酯的制备

从双环戊二烯与烯丙醇进行Diels-Alder反应合成了5－羟甲基2－降冰片烯2，后者在N.N－二甲基苯胺存在下与a－氯代乙酰氯反应，首次合成了氯乙酸降冰片烯甲酯2，考察了反庆条件（温度、反应物摩尔比等）对各步反应收率的影响，并对各步反应产物结构进行表征。     

酸催化甘油与苯甲醛缩合制备六员环缩醛

比较了对甲苯磺酸（PTSA）、磷钨酸（PWA）、KHSO₄和FeCl₃催化对甘油与苯甲醛的缩合反应收率,及对产物中六元环缩醛5-羟基-2-苯基-1,3-二氧六环(1)与五元环缩醛4-羟甲基-2-苯基-1,3-二氧五环(2)比例的影响。 当以环己烷为带水剂及苯甲醛与甘油的摩尔比为2∶3的情况下,KHSO4为催化剂的缩合产物（1+2）收率较高,为96.8%;PTSA催化的缩合产物中,化合物1的比例最高(m(1)∶m(2)=48.6∶51.4)。 室温下PTSA、PWA、KHSO₄和FeCl₃均可催化化合物2向化合物1的转化。 在-20 ℃下,只有PTSA能催化化合物2向化合物1的转化。 在-20 ℃,PTSA催化化合物[STHZ]2转化成化合物1a,并以晶体形式从苯（40%）-石油醚（60%）中析出。 母液循环转化3次后,化合物1a的累计收率可达91.1%。     

An efficient one-pot synthesis of novel isatin-based 2-amino thiazol-4-one conjugates using MgO nanoparticles in aqueous media

An efficient and green approach for the preparation of novel isatin-based conjugates with 2-amino thiazol-4-ones is described by the one-pot reaction of isatin derivatives, rhodanine, and secondary amines in the presence of magnesium oxide nanoparticles as a heterogeneous catalyst in water as a green solvent at room temperature. This new protocol provides products in good yields and short reaction times using a simple work-up procedure. The structure of one representative compound has been confirmed by X-ray single-crystal analysis.     

GC-MS技术在舰船胶粘材料毒性评价中的应用

胶粘材料简称胶粘剂、粘合剂、粘结剂、接着剂。因其能把各种材料紧密地粘合在一起,并具有各种良好的性能,因而广泛地应用于海军舰船的制造及维修中。应用GC-MS技术对在使用环境及条件下其释放物及高温热解物的定性分析是对其进行使用过程中毒性评价的重要步骤。1实验部分1.1仪器与材料仪器:JMS-D300(日本JEOL);PIATFORMⅡGC-MS。     

2-氨基-3-氰基-4-芳基-6-甲氧基-1,4,9,10-四氢萘并[2,1-b]吡喃衍生物的一步合成

以芳醛、丙二腈和7-甲氧基-1,2,3,4-四氢萘-2-酮为原料,在六氢吡啶催化下以乙醇为溶剂,在室温合成了一系列新的2-氨基-3-氰基-4-芳基-6-甲氧基-1,4,9,10-四氢萘并[2,1-b]吡喃衍生物,反应条件温和,产率较高,并通过IR,1H NMR和元素分析表征产物的结构,还通过单晶X射线衍射分析确证产物的构象.