电喷雾解吸电离质谱法用于临床尿样的直接分析

将电喷雾解吸电离质谱(DESI-MS)用于临床尿样的分析, 优化了电喷雾溶剂流速、电喷雾电压和喷雾锥距离等重要参数. 采用普通滤纸作为样品载体, 在不需要样品预处理的前提下同时快速测定了临床尿样中的钾、钠、尿素、尿酸、丙酮酸和肌苷等多种成分, 并对各种成分的主要离子进行了串联质谱鉴定. DESI-MS在进行多组分同时测定时不需要进行样品预处理, 缩短了测定时间, 单个样品的分析时间不到1 min. 同时, 采用内标法对所测定组分进行了半定量分析.     

茶叶中联苯菊酯、毒死蜱残留量的测定能力验证分析

介绍了组织全国多个行业102家实验室参加茶叶中联苯菊酯、毒死蜱残留量的测定能力验证的情况.选用自然基体测试样品,分别采用F检验和t检验法检验样本的均匀性和稳定性,采用稳健统计技术对试验结果进行了分析.时残留量测定的关键技术进行了讨论.     

火焰原子吸收法测定油画颜料中铅含量

采用干灰化法、湿氧化A法和B法分别对油画颜料进行消解后用原子吸收火焰法测定其中的铅含量.通过分析比较3种消解方法测定的结果,发现采用湿氧化法优于干灰化法,湿氧化A法优于B法.采用湿氧化A法对油画颜料进行加标处理后,加标回收率在90%-105%范围,表明采用该方法测定油画颜料中的铅含量是可信的.     

固相微萃取-气相色谱法测定醒脑静注射剂中的麝香酮

中药制剂醒脑静注射剂中的麝香酮含量较低,采用水蒸气蒸馏法需要长时间的提取富集才能进行含量测定.本文采用固相微萃取-气相色谱法（SPME-GC）对醒脑静注射剂中的麝香酮含量进行测定,集样品采集、萃取、浓缩、进样和分析于一体,完成测定的整个过程仅需十几分钟,操作简单,测定结果准确可靠.     

稻谷副产品中脂肪酸的气相色谱-质谱分析

对稻谷副产品脂肪酸的组成和含量进行分析测定. 采用索氏提取法提取了稻谷副产品中的脂肪油, 再进行甲酯化处理, 利用气相色谱-质谱法对其脂肪酸组成及含量进行了分析测定. 结果表明, 从稻糠、稻叶、稻秆中鉴定出的脂肪酸分别占其总检出量的96.72%、 71.77%和92.63%, 不饱和脂肪酸含量分别为72.88%、 45.26%和66.96%.     

ICP-MS测定屠宰场废水中总磷的方法研究

屠宰场废水中有机质含量高且颜色深,采用常规污水分析方法-消解分光光度法测定总磷较为繁琐.通过蒸干-灼烧法对样品进行前处理,使用电感耦合等离子体质谱(ICP-MS)方便快速地测定出屠宰场废水中总磷的含量.经实际样品验证,加标回收率为95.2%~102.0%.方法测定结果准确可靠,测定范围宽且效率高,对分析工作者具有一定的借鉴意义和参考价值.     

不锈钢中铬的X射线荧光光谱分析

以北京钢铁研究院研制的GSB 03-2028系列不锈钢标准物质作为光谱标样,采用基本参数法校正基体效应,建立了X射线荧光光谱测定不锈钢中铬元素的方法.用该方法对标准样品进行分析,分析结果和化学法分析值相吻合,10次制样测量,测定结果的相对标准偏差约为0.14%.     

超高效液相色谱法测定化妆品中孕激素的不确定度

采用分层建模方法建立了超高效液相色谱法测定化妆品中黄体酮结果不确定度评定的数学模型,对测量过程中的不确定度来源进行逐层分析和合成,运用最小二乘法对外标曲线拟合的不确定度进行了评定.超高效液相色谱法测定化妆品中孕激素含量的相对合成标准不确定度为0.022,相对扩展不确定度为0.044.该评定对采用外标法定量的高效液相色谱、气相色谱等测定结果的不确定度评定具有参考作用.     

流动注射——吸光光度法测定自来水中余氯

城市自来水多采用氯化法消毒,余氯含量是自来水质量的重要指标,余氯测定是自来水厂和管网末端水质监控的例行项目.自来水中余氯的测定多采用邻联甲苯胺比色法,其使用的试剂为有毒品,对分析人员的健康不利.本文发现,在稀盐酸介质中余氯可氧化罗丹明6G使其褪色从而使吸光度降低.吸光度的降低值在一定范围内与余氯浓度呈线性关系,可用于余氯的测定.基于上述原理本文对流动注射—吸光光度法测定余氯含量进行了研究.试验结果表明,本法具有灵敏度高、选择性好、分析速     

ICP—AES法直接测定高纯氧化钐中14个稀土杂质元素

本文采用ICP-AES技术,对纯度为99.95%氧化钐中14个稀土杂质元素的直接测定进行了研究.对分析线的选择,工作功率,载气流量,观测高度,进样浓度等条件进行了试验.本法条件下,各分析元素的相对标准偏差均小于8%,标准加入回收率介于92%～108%之间.并对实际样品进行了测定、结果满意.     

阳离子交换树脂分离-铝试剂分光光度法测定土壤中铝形态

研究了铝试剂光度法测定土壤溶液中铝的最佳条件,着重探讨了共存离子,特别是土壤溶液中的无机离子和有机阴离子对测定铝的影响。采用阳离子交换树脂分离,建立了测定土壤溶液及天然水中铝形态方法。用该法可测定总反应性铝、总单核铝和稳定性单核铝。由总反应性铝减去总单核铝求得酸溶性铝。由总单核铝减去稳定单核铝求得不稳定单核铝。与阳离子树脂交换分离-邻苯二酚紫光度法进行了比较。结果表明：邻苯二酚紫光度法灵敏度较高,但铁的干扰较大。铝试剂光度法灵敏度略低,但铁的干扰较少。阳离子树脂交换分离-铝试剂光度法更适合于测定含铁量比较高的土壤溶液中的铝形态。     

Thermal Stability of Sol-Gel Hydrotalcites

Sol-Gel Hydrotalcites were synthesized using magnesium ethoxide and variable aluminum sources: aluminum acetilacetonate, aluminum chloride, aluminum nitrate and aluminum sulfate; in all cases, the gelation was done at pH 10. X-ray diffraction studies show that the crystallinity depends on the aluminum precursor used. The crystallinity was found in the order aluminum acetylcetonate>aluminum chloride>aluminum nitrate>aluminum sulfate. The precursor determines the sintering behavior as well.     

Electrothermal volatilization of aluminum as 1-phenyl-3-methyl-4-benzoylpyrazolone[5] chelate for gaseous sample introduction in ICP-AES

Based on gaseous compound introduction as 1-phenyl-3-methyl-4-benzoylpyrazolone[5](PMBP) chelate of aluminum by electrothermal vaporization in ICP-AES, a method for determination of trace aluminum was developed. Trace aluminum was vaporized at temperature of 1000 degrees C, and the vaporization behavior of aluminum chelate was detailedly investigated. Under the optimum conditions, the detection limit of aluminum was 0.6 ng ml(-1), and the relative standard deviation for 0.1 mug ml(-1) aluminum was 4.7% (n=8). The proposed method was applied to the determination of trace aluminum in rice flour reference materials, and the results well agreed with the reference values.     

Hydrothermal Synthesis of Porous Al2O3/Al Metal Ceramics: II. Mechanism of Formation of a Porous Al(OH)3/Al Composite

The formation of a porous layer of aluminum hydroxide on the surface of aluminum particles and the aggregation of Al(OH)₃/Al composite particles were analyzed theoretically. It was found that the diffusion mass transfer of the hydroxo complexes of aluminum through the porous structure of a growing layer of aluminum hydroxide to the outer surface is a rate-limiting step in the synthesis of the porous composite. A model mechanism of formation of the porous composite was developed, and rate equations were derived for describing the growth of an aluminum hydroxide layer on the surface of an aluminum particle and changes in the degree of aluminum conversion and the contact radius between composite particles. Based on the developed mathematical model and experimental data, the diffusion coefficient of the hydroxo complexes of aluminum in the porous structure of aluminum hydroxide was calculated.     

Preconcentration of trace aluminum from environmental water samples with 5'-chloro-5-dodecyl-2,4,2'-trihydroxyazobenzene impregnated macroporous resin.

5'-Chloro-5-dodecyl-2,4,2'-trihydroxyazobenzene (CDTA) impregnated XAD-4 resin (CDTA resin) was prepared, and applied to the preconcentration of trace aluminum from environmental water samples with satisfactory results. Aluminum was measured by flow-injection analysis (FIA) with fluorescence detection by using lumogallion after the preconcentration of aluminum with CDTA resin. Fe3+ and other coexisting substances had no interference on the determination of aluminum by the present method. Chemical speciation of trace aluminum in environmental water was carried out by using the CDTA resin after the separation of aluminum species with ionic exchangers without changing the pH. About 50% of water-soluble aluminum in Lake Biwa was found to be aluminum organic species (anion species).     

Removal of phosphate by aluminum oxide hydroxide

The development and manufacture of an adsorbent to remove phosphate ion for the prevention of eutrophication in lakes are very important. The characteristics of phosphate adsorption onto aluminum oxide hydroxide were investigated to estimate the adsorption isotherms, the rate of adsorption, and the selectivity of adsorption. Phosphate was easily adsorbed onto aluminum oxide hydroxide, because of the hydroxyl groups. The adsorption of phosphate onto aluminum oxide hydroxide was influenced by pH in solution: the amount adsorbed was greatest at pH 4, ranging with pH from 2 to 9. The optimum pH for phosphate removal by aluminum oxide hydroxide is 4. The selectivity of phosphate adsorption onto aluminum oxide hydroxide was evaluated based on the amount of phosphate ion adsorbed onto aluminum oxide hydroxide from several anion complex solutions. It is phosphate that aluminum oxide hydroxide can selectively adsorb. The selectivity of phosphate onto aluminum oxide hydroxide was about 7000 times that of chloride. This result indicated that the hydroxyl groups on aluminum oxide hydroxide have selective adsorptivity for phosphate and could be used for the removal of phosphate from seawater.     

天然水中可溶性硅酸与铝盐作用机理探讨

通过考察单核铝和溶解铝浓度的变化, 对天然水体中溶解性硅酸与铝盐的反应机理进行研究. 试验过程中, 采用8-羟基喹啉荧光分光光度法测定铝浓度并结合热力学计算进行机理验证. 结果表明: 单体硅酸和聚硅酸主要与溶液中的单核铝反应生成溶解性硅铝酸盐. 单体硅酸与单核铝的结合能力较弱; 聚硅酸与单核铝的结合能力则较强, 反应产物主要为二啮或三啮配合物. 溶液pH对反应过程有着重要影响, 偏碱性环境对硅酸与单核铝间的反应具有促进作用.     

Synthesis and characterization of nanostructured aluminum borate by sol–gel method

Nanostructured aluminum borate was synthesized using sol?Cgel technique. X-ray diffraction study revealed that the synthesized aluminum borate was single crystal. These nanorods have very uniform diameter. High-resolution transmission electron microscope images indicate that aluminum borate is well crystallized. The alternating current (AC) conductivity of the aluminum borate was studied as a function of temperature and frequency. The AC conductivity mechanism of the aluminum borate was found to be proportional to ??^s. The exponent s is almost independent with temperature. This suggests that AC conductivity mechanism of the aluminum borate can be interpreted by localized hopping model.     

化学浸提-分光光度法测定沙棘叶中不同形态铝

利用KCl、NH4Ac、HCl、NaOH四种浸提液将沙棘叶中的铝浸提溶出,得到沙棘叶中铝的不同化学形态,采用分光光度法定量测定,测定结果:沙棘叶中的Al3+为10.7%,Al(OH)2+和Al(OH)+2为2.1%,胶态Al(OH)03为34.3%,有机铝为53.0%.浸提液中铝的回收率为86.9%～101.0%.     

化学浸提法研究中药茯苓中活性铝的形态分布

利用KCl、NH4Ac、HCl、NaOH四种浸提液对中药茯苓中铝的存在形态分别进行浸取溶出,采用分光光度法对不同形态的铝含量进行测定,得到茯苓中活性铝的形态分布,有机铝含量占总量的58.9%;胶态Al(OH)3占总量41.1%;浸提液中铝的回收率为97.0%~109.3%。