分光光度法测定高纯度膨润土吸蓝量

以分光光度法测定高含量膨润土吸蓝量,应用正交试验设计对分光光度法的实验条件进行优化,确定的最佳实验条件:煮沸时间为5 min,4%焦磷酸钠溶液加入体积为20 mL,0.01 mol/L亚甲基蓝溶液加入体积为30mL,振荡时间为15 min。该法与滴定法对比,测定值相对误差在4%以内,相对标准偏差为1.04%,可满足高纯度膨润土吸蓝量的分析要求。     

丙烯腈废水中有机物的高压放电法降解机理

利用气相色谱-质谱探讨了丙烯腈废水中有机物的高压放电法降解机理.结果表明:丙烯腈的氰基首先被破坏生成丙烯酸,丙烯酸进一步被氧化生成乙酸,乙酸降解为甲酸,最后生成CO2.丁二腈首先降解为丁二酸,丁二酸再生成丙酸,并逐步降解为乙酸、甲酸,最后生成CO2.二氰乙基胺在降解过程中依次生成丙腈、丙酸、乙酸和甲酸,最后生成CO2....     

纳米催化剂在CO_(2)加氢制甲醇中的研究进展北大核心CSCD

为减缓温室效应,将CO_(2)转换成高附加值的甲醇是减少CO_(2)排放的有效途径,而高效催化剂是CO_(2)加氢制甲醇反应规模化的关键.可调控合成的具有量子尺寸效应的纳米催化剂在该反应上具有独特的优势.因此我们深入探讨了反应机理,综述了纳米材料在CO_(2)加氢制甲醇中的研究进展,最后给出了高效催化剂可能的发展方向.     

Quantitative and selective analysis of lactose by capillary electrophoresis

Summary A CE method has been validated for the analysis of batches of lactose used as a pharmaceutical raw material. This method was shown to be selective for lactose and was found to be quantitative. The separation was achieved due to on-capillary chelation of the lactose with borate ion. The resulting complex was detected at 195nm. An internal standard is employed to improve injection precision and detector linearity. A system peak occurred in the separation and was systematically investigated to show that it was not sample related. The method was validated and successfully submitted to regulatory authorities and is now in routine use in a number of our quality control laboratories.     

硫酸分离–火试金重量法测定碲化铜中的金和银

建立了用硫酸分离-火试金重量法测定碲化铜中的金和银含量的方法。用硫酸溶解碲化铜样品,过滤,除去铜和碲,得到含金、银的沉淀物,沉淀物经灰化、配料、高温熔融制得铅扣。将铅扣灰吹,得到金银合粒,用硝酸溶解分离金,用重量法测定金含量。用金银合粒的质量扣除金粒的质量和分金液、洗液中杂质的质量即为银含量。采用灰皿、残渣熔融法补正,或用含碲、铜物料做基体加入纯金、纯银同试样方法测定,根据金、银的回收率加以补正,从而得到试样中的碲含量。实验结果表明,浓硫酸的加入量为30 mL,残余量应不少于15 mL。火试金中硅酸度为1左右,试样进炉温度以900℃为宜。该方法金、银测定结果的相对标准偏差分别为0.33%~1.97%,0.28%~1.27%(n=9)。金的回收率为98.5%~100.2%,银的回收率为95.5%~101.4%。该法满足生产控制检测和贸易结算的要求。     

Enhancement of the enzymatic digestibility of waste newspaper using tween

Methods of increasing the enzymatic digestibility of waste newspaper by adding Tween (TW)-20 and 80 surfactants were investigated. Tween-series surfactants were selected because these surfactants increase cellulase activity during enzymatic hydrolysis and do not inhibit cell growth in downstream fermentation processes. When surfactant was used in a pretreatment, a benefic effect was expected in the enzymatic hydrolysis stage owing to surfactant carry-over from the pretreatment stage immediately upstream of the hydrolysis. However, because it was necessary to wash the pretreated substrate with water to remove inhibitors produced during pretreatment, no added benefit was obtained. When surfactant was used in the pretreatment only, it was found that it had a marked effect on digestibility and that this effect was higher at lower enzyme loadings. Also, TW-80 was found to be more effective than TW-20, and the addition of enzyme and TW-80 to substrate at the beginning of enzyme reaction was found to most effectively increase digestibility. When TW-80 was added into either the pretreatment stage or the hydrolysis stage the digestibilities of untreated sample increased by approx 40%, whereas an increase of only 45% was observed when TW-80 was added to both stages. These results show that the addition of surfactant to either the pretreatment or the enzymatic hydrolysis stage is sufficient to increase digestibility.     

Dawson型磷钨酸催化合成乳酸月桂醇酯

用Dawson型磷钨酸催化合成乳酸月桂醇酯。实验结果表明:Dawson型磷钨酸有较高的催化活性,反应时间短,酯收率高,工艺简单。最佳工艺条件为:醇/酸摩尔比为1.5:1,催化剂用量为0.3%,带水剂甲苯体积(mL)与反应物质量(g)之比为0.4:1~0.5:1,反应温度为115~140℃,反应时间30~50min。在此条件下,酯收率可超过93% 。     

统计方法在微量金分析中的应用

化探金样品前处理过程中消解、富集、解吸等环节控制不严格,往往会导致最后数据处理产生过高的校正系数。为了降低校正系数,用统计学的方法对实验过程进行了详细分析,确定了主要影响因素。将水浴时间延长并保温3 h以上,泡塑大小改为0.2 g,清洗时间不大于15 s,解吸到上机时间间隔小于5 h。方法改进后,检测结果校正系数有了明显改善,从改进前有40%批次的校正系数大于1.2,降到了全部小于1.2,甚至不用校正。方法改进后降低了实验过程的误差,提高了分析测试结果的稳定性。     

原子吸收分光光度法空心阴极灯一灯多用探讨

利用原子吸收分光光度法分别用钾空心阴极灯测钠、锌空心阴极灯测铜,标准曲线线性良好,相关系数均在0.999以上。钾灯测量钠质控样结果为0.747 mg/L,在质控样标称值范围(0.712±0.049)mg/L之内。锌灯测量铜质控样结果为1.23 mg/L,在质控样标称值范围(1.19±0.05)mg/L之内。钾灯测钠的相对标准偏差为0.47%(n=6),加标回收率为99.8%。锌灯测铜的相对标准偏差为0.53%(n=6),加标回收率为103%。一灯多用在环境监测工作中是可行的。     

PREPARATION OF POLYSULFONAMIDE/TiO2 NANOCOMPOSITES BY SOL-GEL

Polysulfonamide (PSA) was synthesized at room temperature, the polymerization based on terephthaloyl chloride and 3,3 '-diaminodiphenylsulfone in the common solvent N,N -Dimethyl-acetamide (DMAc). Polysulfonamide/titanium oxide nanocomposites were prepared by sol-gel method. Tetrabutyl titanate(TBT) was added into the polysulfonamide solution, at the same time ,some water was mixed to make the TBT hydrolyze. In the process, hydrochloric acid was used to catalyze the reaction. The polysulfonamide chemistry structure was characterized by FT-IR spectrum. Atomic force microscopy (AFM) was employed to observe the microstructure of the composite film. The thermal property was investigated by TGA.The results show that we have succeeded to synthesize the polysulfonamide, TiO2particles were well distributed in the composite film and average size was about 20 nm on average, the heat-resistance of nanocomposite was batter than the pure polysulfonamide.     

甲苯/水双相体系中以稻草为原料合成糠醛

FeCl³为催化剂,在甲苯/水双相溶剂体系中,以稻草为原料经水解反应制备糠醛,其结构经¹H NMR和¹³C NMR确证。通过响应面分析获得的最佳反应条件为：催化剂质量分数23.09%,甲苯60 mL,溶剂比V（甲苯）: V（水）=1 : 1,料液比为67.5 g·L^-1,于177 ℃反应60 min,糠醛收率高达78.92%。     

Development of a novel analytical method for determination of chondroitin sulfate using an in-capillary enzyme reaction

A novel analytical method for determination of total amount of chondroitin sulfate (CS) based on its conversion to desulfated chondro-disaccharide via an enzyme-catalyzed reaction, was developed. Using the in-capillary enzyme reaction, the method was also applied to the successful construction of an on-line analytical system. Within this system, electrophoretic migration was used to mix zones containing the enzyme mixture (chondroitinase ABC, chondro-4-sulfatase, chondro-6-sulfatase and 2-o-sulfatase) and the substrate (CS). The reaction was then allowed to proceed in the presence of a weak electric field and, finally, the product (desulfated chondro-disaccharide) of enzyme reaction migrated to the detector under the influence of an applied electric field. A polyvinyl alcohol-coated capillary was used to reduce protein adsorption. Desulfated chondro-disaccharide was successfully migrated toward the anode in 10 mM Tris-acetate buffer (pH 7.0) under reversed polarity and detected at 232 nm. The established method was validated and demonstrated to be applicable in the determination of total amount of CS in a commercial ophthalmic solution. No interference from the formulation excipients was observed. Good linearity was obtained, with correlation coefficients above 0.999. Recoveries and precisions ranged from 100.0 to 100.5%, and from 0.2 to 0.6% of the relative standard deviation, respectively. Good agreement was obtained between the established method and traditional photometric method based on carbazole reaction. In this study, application of the method to disaccharide compositional analysis was also performed.     

氢醌对胆红素氧化过程的促进作用及其分析意义

研究了氢醌与胆红素的作用过程，发现氢醌在碱性条件下可促使胆红素氧化，且胆红素被氧化成胆绿素，此反应过程被证实为自由基反应，考察了介质条件，抗氧化剂等反应过程的影响及其它酚类物质对胆红素氧化的作用情况。     

Relationship between Scattered Photon Counts and Concentrations of Some Saline Solutions in Compton Scattering

Compton scattering saline solution was researched. Firstly according to the Compton scattering theory the linear relationship between the concentration and the scattered photon counts was obtained. And then it was proved by Compton scattering experiments for some solutions. According to those experiments, it was found that the slope was decreased when the atomic number of the cation was increased for alkali metal chloride solutions and alkaline-earth metal chloride solutions. Based on those relationships, a new method was promoted with which to measure the concentration of saline solution untouched the measured solution.     

固定化脂肪酶活性的X射线微区分析

利用X射线微区分析的方法，对吸附交联法得到的固定化脂肪酶的微观活性进行了分析。结果表明：以合成出的大孔吸附树脂为固定化酶栽体，酶活较高，活性脂肪酶分布较均匀。并得到了固定化脂肪酶的活性定位的最佳条件。     

酸法制备杨木微/纳纤丝及其表征

近二十多年来,如何从天然纤维素中分离微/纳纤丝和用其来增强高分子聚合物受到许多学者的关注。本研究以杨木纤维素为原料,采用硫酸和盐酸的混合液水解、恒温水浴振荡处理制备杨木微/纳纤丝。利用扫描电子显微和X射线衍射仪对制备的杨木微/纳纤丝进行分析表征,结果表明当酸处理条件为杨木纤维3g、浓H2SO4体积分数为15%、浓HCl体积分数为5%、恒温水浴60℃、振荡8h,可得到杨木微/纳纤丝,杨木微/纳纤丝宽度分布在200nm到1μm之间,长宽比约60~120,相度结晶度为77.59%。     

新型两性聚电解质高吸水性树脂CMCTS-g-（PAA-co-PTMAAC）的制备研究

通过氧化还原引发荆引发的接枝共聚反应,使阴离子型单体丙烯酸(AA)和阳离子型单体三甲基烯丙基氯化铵(TMAAC)在羧甲基壳聚糖(CMCTS)的分子链上接枝共聚,制得羧甲基壳聚糖接枝-(聚丙烯酸-co-聚三甲基烯丙基氯化铵)(CMCTS-g-(PAA-co-PTMAAC)两性聚电解质高吸水性树脂.采用红外光谱对产物的结构进行了表征,比较了反应条件对产物吸液性能的影响.发现制备具有良好吸液性能的高吸水性树脂的最优化反应条件为:TMAAC占单体总质量的14.3%,mNNMBA/mAA值在0.014附近,单体总质量为CMCTS质量的9.33倍,丙烯酸中和度在20%～30%之间.研究发现,随外部溶液pH值的变化,两性聚电解质高吸水性树脂的溶胀性能在酸性和碱性条件下各有一个最大值,在等电点处产物的吸液性相对较低.     

温度对Nafion-结晶紫光纤湿度传感器性能的影响

The optical fiber relative humidity sensor based on Nation-crystal violet film was developed.The effect of samplef s temperature in the range from 299.15K to 324.15K on the sensing performance of the sensor was investigated. The mathematical function between temperature and the sensitivity of the sensor was established according to the reactive theory of sensor to the relative humidity, which was validated with the experiment. With the research, the application range of the sensor was extended, which made the sensor keep a good veracity when it was used in situ.     

上海市食品中铝污染情况分析

为了解上海市食品中铝污染情况,采集四个品种94件样品用国标法GB/T 5009.182-2003进行了铝含量的分析。结果表明,按照国标GB 15202-1994判断,饼干合格率达100%,糕点合格率85.7%,馒头合格率81.5%,油条合格率仅53.5%。提出了控制铝污染对策和建议。     

偶联剂对丙烯酸酯改性聚氨酯聚合物接枝率和乳液性能的影响

合成了含双羟基的甲基丙烯酸甘油酯(GM)并将其作为偶联剂用于聚丙烯酸酯(PAC)对水基聚氨酯(PU)的改性.采用核磁共振、红外光谱和气相色谱等对GM进行了表征.分别以该双羟基GM和单羟基的丙烯酸羟乙酯(HEA)与异氰酸酯基(NCO)封端的PU预聚体进行反应以在PU分子链上引入双键,然后再与丙烯酸酯类单体通过自由基聚合制...