硅钼蓝分光光度法测定铁矿石中二氧化硅含量测量不确定度评定

应用测量不确定度评定理论,结合日常工作和实验方法,分析硅钼蓝分光光度法测定铁矿石中二氧化硅含量的影响因素,计算和评定测定过程各不确定度分量,最终给出分析结果的测量不确定度.     

Chiral Discrimination Mechanisms by Silylated-Acetylated Cyclodextrins: Superficial Interactions vs. Inclusion

Cyclodextrin derivatives constitute a powerful class of auxiliary agents for the discrimination of apolar chiral substrates. Both host–guest inclusion phenomena and interactions with the derivatizing groups located on the surface of the macrocycle could drive the enantiodiscrimination; thus, it is important to understand the role that these processes play in the rational design of new chiral selectors. The purpose of this study is to compare via nuclear magnetic resonance (NMR) spectroscopy the efficiency of silylated-acetylated α-, β-, and γ-cyclodextrins in the chiral discrimination of 1,1,1,3,3-pentafluoro-2-(fluoromethoxy)-3-methoxypropane (compound B) and methyl 2-chloropropionate (MCP). NMR DOSY (Diffusion Ordered SpectroscopY) experiments were conducted for the determination of the bound molar fractions and the association constants, whereas ROESY (Rotating-frame Overhauser Enhancement SpectroscopY) measurements provided information on the hosts’ conformation and on the interaction phenomena with the guests. Compound B, endowed with fluorinated moieties, is not deeply included due to attractive Si-F interactions occurring at the external surface of the cyclodextrins. Therefore, a low selectivity toward the size of cyclodextrin cavity is found. By contrast, enantiodiscrimination of MCP relies on the optimal fitting between the size of the guest and that of the cyclodextrin cavity.     

The adsorption of methyl nitrite on the Au(111) surface

The interaction of the methyl nitrite molecule (CH₃ONO) with the gold(111) surface has been studied by means of density functional calculations. The perfect Au(111) surface has been represented by a rather large cluster model, Au₂₂, that was in turn used to extract information about the preferred adsorption geometry of the CH₃ONO species. Vibrational frequencies and adsorption energy are also reported. The calculated adsorption energies are 31.2 kJ/mol with respect to gas phase cis-conformer and 35.1 kJ/mol with respect to trans-methyl nitrite, very close to the experimental adsorption energy of 33.5 kJ/mol. From the analysis of vibrational frequencies of gas phase and adsorbed species it is concluded that only the cis-conformer is present at the Au(111) surface.     

丁苯胶乳_苯乙烯_甲基丙烯酸甲酯核壳乳液接枝共聚的研究

以过氧化苯甲酰(BPO)-Fe~(2+)为引发体系,硬脂酸钾和歧化松香酸皂为乳化剂,硫醇为调节剂,于600mL釜内、70℃下进行丁苯胶乳-苯乙烯-甲基丙烯酸甲酯(SBR-S-MMA)的核壳乳液接枝共聚。研究认为本体系的反应机理为:Fe~(2+)与乳化剂结合为部分油溶性化合物,再与溶解在乳胶粒中的BPO反应,生成自由基与Fe~(3+),Fe~(3+)被雕白块还原为Fe~(2+)后完成一个循环。在乳胶粒相产生的自由基与单体反应或进攻橡胶链,从而引起链引发和链增长反应。S和MMA接枝聚合的初始速率(R_(PO))与[BPO]~(0.5)成正比,R_(PO)随反应温度的升高而增大,随硫醇用量的增加而减小。该体系S和MMA两步接枝反应的表观分解活化能分别为16.56kJ/mol和17.50kJ/mol。     

超声降解铬黑T及亚甲蓝的实验研究

尝试采用超声波技术对铬黑T及亚甲基蓝两种模拟染料废水进行降解实验。以脱色率为指标,分别考察pH值、超声功率强度、超声时间和温度等因素对两种模拟染料废水脱色作用的影响。结果表明:超声波技术对铬黑T及亚甲基蓝两种模拟染料废水具有一定的脱色能力,随着pH值的增大,脱色能力减弱。常温下,在pH=1.79附近、超声时间120min,超声功率0.7kw时,亚甲基蓝模拟染料废水的脱色率为27.60%,铬黑T模拟染料废水的脱色率为20.33%。进一步地采用超声波与水合二氧化锰联用技术,可以极大提高有机染料的降解效率,水合二氧化锰投加量为40mg/L时,亚甲基蓝模拟染料废水的脱色率达到92.48%。     

锌酸盐镀锌层的三价铬蓝色钝化

以外观、醋酸铅点滴实验和中性盐雾实验（NSS）为评价标准，通过正交实验和单因素实验，得到了一种三价铬钝化膜的最佳工艺条件：0．1mol／L CrCl3，0．2mol／L有机羧酸CM，0．24mol／LNaNO3，0．01mol／L Co（NO3）2，8g/LNa2SiO3，pH为1．2，钝化温度为10℃，钝化时间为30s。探讨了配合物CM浓度、硝酸钠浓度、氯化铬浓度、硝酸钴浓度、硅酸钠浓度及钝化液pH、钝化温度、钝化时间的影响。在上述条件下得到的钝化膜呈蓝色，均匀，能通过48h NSS实验。     

Polymer-grafted cellulose fibers. I. Enhanced water absorbency and tensile strength

To enhance the water absorbency of wood fibers, various acrylic monomers were grafted to these fibers using cerium IV initiation followed by base hydrolysis. The absorbent capacity of hydrolyzed methyl acrylate- or acrylonitrile-grafted wood pulp fibers was an order of magnitude greater than ungrafted pulp fibers. A portion of this enhanced absorbency could be attributed to graft-induced osmotic forces. Enhanced absorbency was relatively independent of wood fiber type. Paper handsheets incorporating 20% grafted fibers had a fivefold increase in absorbent capacity, a twofold increase in dry tensile strength, a threefold or greater increase in wet tensile strength, and were more stretchable. In addition to enhanced absorbent capacity, the rate of absorbency was approximately 50% greater. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65:1463–1469, 1997     

Preparation of monoglycerides by guanidine-catalyzed processes

Glycerolysis of methyl stearate and tristearin has been carried out in the presence of alkylguanidines—strong nonionic bases—as catalysts. When applied at 10 mol%, 1,5,7-triazabicyclo [4.4.0]dec-5-ene, 1,2,3-tricyclohexylguanidine, and 1,3-dicyclohexyl-2-n-octylguanidine give monoglycerides in more than 90% selectivity, in a maximum of 6 h reaction time.     

Ni(Ⅳ)引发丙烯酸甲酯与三元尼龙接枝共聚反应的研究

以二过碘酸合镍(Ⅳ)钾〔Ni(Ⅳ)〕为氧化剂,共聚尼龙上的弱的还原基团(酰胺基)为还原剂,组成氧化还原引发体系,于碱性介质中直接在共聚尼龙分子骨架上产生接枝点,引发丙烯酸甲酯(MA)的接枝共聚合反应,获得了较高的接枝效率(可达90%以上)。探讨了引发剂浓度、单体浓度、反应温度对接枝参数的影响,结果表明:当c〔Ni(Ⅳ)〕=8×10-4mol/L,c(MA)=1 5mol/L,θ=35℃时,接枝效率和接枝百分比可达到最高值。用红外光谱、X射线衍射、扫描电镜对接枝共聚物进行了表征,提出了建立在镍(Ⅳ)还原为镍(Ⅱ)的过程为两步单电子转移的基础之上的引发机理。将所得接枝共聚物用作尼龙/聚甲基丙烯酸甲酯体系的增容剂,通过扫描电镜分析表明:该共混体系的相容性得到一定程度的改善。     

酯交换法合成D-异抗坏血酸棕榈酸酯及其抗氧化性能

24℃下,2.9gD 异抗坏血酸和3.8g棕榈酸甲酯分别缓慢加入到14mL的浓硫酸中,搅拌反应24h。反应混合物加入到冰水中,用乙醚萃取,洗涤,除去乙醚,粗产品用甲苯重结晶,得到4.6gD 异抗坏血酸棕榈酸酯,产率79%。用FTIR对产品进行了表征。按国标(GB/T5009.37—1996)方法将产品用于新鲜茶籽油进行抗氧化性能实验,结果表明,D 异抗坏血酸棕榈酸酯是一种比L 抗坏血酸棕榈酸酯更好的油溶性抗氧化剂。