Adsorptive Stripping Voltammetric Determination of Nanomolar Concentration of Cerium(III) at a Carbon Paste Electrode Modified by N′‐[(2‐Hydroxyphenyl)Methylidene]‐2‐Furohydrazide

The aim of this work was to obtain an adsorptive stripping voltammetric method for the Ce(III) determination at a carbon paste electrode, chemically modified with N'‐[(2‐hydroxyphenyl)methylidene]‐2‐furohydrazide (NHMF). The electroanalytical procedure comprised two steps: the Ce(III) chemical accumulation at ?200 mV followed by the electrochemical detection of the Ce(III)/NHMF complex, using anodic stripping voltammetry. The factors, influencing the adsorptive stripping performance, were optimized including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The resulting electrode demonstrated a linear response over a wide range of Ce(III) concentration (5.0–90 nmol dm^?3). The detection limit was found to be 0.8 nmol dm^?3 on the basis of a signal to noise ratio of 3. The precision for six determinations of 10 and 55 nmol dm^?3 Ce(III) was 5.6% and 2.1% (relative standard deviation), respectively. Application of the procedure to the determination of cerium in phosphate rock and wastewater samples gave good results.     

莠灭净悬浮剂物理稳定性

通过颗粒平均粒径测定和形貌表征研究了分散剂种类和用量对莠灭净悬浮剂物理稳定性的影响。 结果表明,相同条件下,双子型分散剂马来松香聚氧丙烯-氧乙烯醚磺酸盐（SC-3）可以在农药颗粒表面形成双层吸附,产生双层屏蔽结构,有效阻隔了颗粒与水的接触,抑制了颗粒团聚和奥氏熟化引起的结晶长大。 其用量(质量分数)大于4.0%时,所制备的莠灭净悬浮剂热贮前后颗粒粒径及形貌基本不变,其结晶长大现象得到有效地抑制,体系物理稳定性较好。     

原子吸收光谱法间接测定钼精矿中钼的研究

对于钼精矿中钼的测定,标准方法采用钼酸铅重量法,该方法需要将钼酸铅沉淀反复多次洗涤、过滤,以保证沉淀物中夹带的铅离子洗涤完全,再对沉淀物进行灰化、灼烧等多步操作,步骤较繁琐,分析费时,不能快速配合选矿、冶金的科学研究。应用原子吸收光谱法间接测定钼,建立了钼精矿中钼的快速分析方法。钼精矿样品经硝酸、氯酸钾、硫酸加热溶解后,用酚酞和盐酸调节pH值,加入乙酸-乙酸铵缓冲溶液调节pH值至5～7,再加入一定量且过量的铅标准溶液。基于在室温下,钼酸铅为难溶电解质,难溶电解质在一定温度下能否沉淀完全,通常比较离子积Q_c与溶度积常数K_sp的相对大小,当Q_c>K_sp,溶液过饱和,沉淀物完全析出,钼精矿中钼的含量为40～60%,铅的加入量为0.125 0～0.150 0 g,取最小值计算出溶液中钼酸铅的离子积,Q_c＝[Pb2+][MoO2-₄]=2.51×10-5,K_sp＝1.0×10-13,Q_cK_sp,因此钼酸铅沉淀可以完全析出,待钼酸铅沉淀完全后干过滤,用原子吸收光谱法测定滤液中过量的铅离子,用差减法计算得出钼精矿中钼的含量。文中分别考察了乙酸-乙酸铵缓冲溶液的加入量及其浓度、铅标准溶液的加入量、钼酸铅沉淀完全的时间、加热时间以及常见共存离子如W6+,Sn4+和Cu2+等的最大允许量诸多因素对原子吸收光谱法间接测定钼的影响。与钼酸铅重量法相比,该方法省去了对钼酸铅沉淀反复多次的洗涤、灰化以及灼烧等步骤,操作简便易掌握,分析时间缩短一半,并用钼酸铅重量法与本方法进行对照实验,分析结果进行数理统计,得出结论：本方法具有很好的准确度和精密度,可用于选矿、冶金钼精矿样品中钼的快速分析检测。     

Dissolution and reconstitution of casein micelle containing dairy powders by high shear using ultrasonic and physical methods

The effect of shear on the solubilization of a range of dairy powders was investigated. The rate of solubilization of low solubility milk protein concentrate and micellar casein powders was examined during ultrasonication, high pressure homogenization and high-shear rotor–stator mixing and compared to low-shear overhead stirring. The high shear techniques were able to greatly accelerate the solubilization of these powders by physically breaking apart the powder agglomerates and accelerating the release of individual casein micelles into solution. This was achieved without affecting the structure of the solubilized proteins. The effect of high shear on the re-establishment of the mineral balance between the casein micelles and the serum was examined by monitoring the pH of the reconstituted skim milk powder after prior exposure to ultrasonication. Only minor differences in the re-equilibration of the pH were observed after sonication for up to 3 min, suggesting that the localized high shear forces exerted by sonication did not significantly affect the mass transfer of minerals from within the casein micelles.     

Influence of milk fat globule membrane and milk protein concentrate treated by ultrasound on the structural and emulsifying stability of mimicking human fat emulsions

The primary objective of the present study was to investigate the effectiveness of ultrasonic treatment time on the particle size, molecular weight, microstructure and solubility of milk fat globule membrane (rich in phospholipid, MPL) and milk protein concentrate (MPC). The mimicking human fat emulsions were prepared using modified proteins and compound vegetable oil and the structural, emulsifying properties and encapsulation efficiency of emulsions were evaluated. After ultrasonic treatment, the cavitation caused particle size decreased and structure change of both MPL and MPC, resulting in the enhancement of protein solubility. While, there was no significant change in molecular weight. Modified proteins by ultrasonic may cause a reduction in particle size and an improvement in emulsifying stability and encapsulation efficiency of emulsions. The optimal ultrasonic time to improve functional properties of MPL emulsion and MPC emulsion were 3 min and 6 min, respectively. The emulsifying stability of MPL emulsion was superior to MPC emulsion, which indicated that MPL is more suitable as membrane material to simulate human fat. Therefore, the obtained results can provide basis for quality control of infant formula.     

稳定同位素比质谱法测定苹果和浓缩苹果汁的δ13C值

用从国际原子能机构溯源得到的橄榄油标准物质[Cat No.B 2172-Batch 3130,其δ13CPDB为(-28.51±0.16)‰]作标准,应用稳定同位素比质谱法测定了苹果和苹果汁的δ13 C值,并以此确定国产苹果的δ13 C值的范围和鉴定制成的果汁的质量。苹果样品去皮后切碎,打成糊状,离心后取其上清液,在75℃加热2～3h至呈黏稠状液体,冷却至室温。此时其糖度约为70Brix。浓缩苹果汁样品是黏稠液体,其糖度一般也在70Brix左右。取2μL上述样品置于锡杯中,按方法处理后供质谱分析。标准物质的进样量为2μL。按所测得碳的稳定同位素13C与12C的比值代入所给公式计算δ13 C值。结果表明:方法的精密度较好,其相对标准偏差(n=11)均小于0.021%。根据测定结果发现,我国苹果的δ13C值在-29.1‰～-23.33‰之间。     

球磨对纳米ZrO2水相悬浮体系性质的影响

实验研究了球磨时间对纳米ZrO₂水悬浮液性质的影响。结果表明,粒径小于15nm ZrO₂在SND6800球磨剂的水相中球磨2h制备的悬浮液,可稳定存在14天。在SND6800球磨剂与ZrO₂的质量比为5:95时,球磨时间对粒子粒度、悬浮液的密度和pH值以及沉降率影响不大;但对悬浮液的吸光度、表面张力和黏度有明显的影响。球磨时间50h是悬浮液的吸光度及表面张力最大,而黏度是球磨40h时最大。     

微量悬浮液进样-火焰原子吸收光谱法测定霜类化妆品中的铅

基于悬浮液技术处理霜类化妆品样品,将样品悬浮在1.00g/L琼脂溶液中制成均匀的悬浮液,采用微量进样技术建立了火焰原子吸收光谱法快速测定霜类化妆品中的铅。方法的检出限为0.030μg/mL,回收率为98.8%—101.5%。方法应用于实际样品的测定,结果满意。     

纳米氧化锆水悬浮液的稳定性

通过黏度、表面张力、密度及粒度测试等手段研究了球磨剂、球磨时间、pH值、添加剂等因素对纳米氧化锆水悬浮液稳定性的影响。结果表明:球磨时间2h,球磨剂与氧化锆质量比为3.5%,添加剂可用乙二醇,悬浮液pH值为10.0,氧化锆粒径小于15nm时,纳米氧化锆水悬浮液可稳定30天。     

固体进样一直接测汞仪法测定金精矿粉中微量汞

将金精矿粉样品直接置于石英舟中,在高纯氧气氛中燃烧,释放出汞,与齐化管中的金形成金汞齐,于900℃热释放出汞蒸汽,用直接测汞仪法测定汞的含量。测定结果的相对标准偏差为0．28％～1．57％（n=6）,方法检出限为1．0pg／kg,加标回收率为95．7％～117．4％。用该法对4种土壤标准样品进行了测定,测定结果与标准值相符。该方法适合于金精矿粉中微量汞的测定。