气相色谱-质谱联用法测定橡胶制品中多环芳烃（蒽）含量不确定度评定

目的对气相色谱-质谱联用仪法测定橡胶制品中多环芳烃（蒽）含量不确定度进行评定,确定影响不确定度的关键因素。方法依据《ZEK01.4-2008 GS认证过程中PAHs的测试和验证》,使用气相色谱-质谱联用仪法测定橡胶制品中多环芳烃（蒽）含量,并对结果的不确定度进行评定,分析影响测量不确定度的各个因素,对各个分量进行计算和合成。结果扩展不确定度U=5.7 mg/kg,置信概率95%。结论该实验的不确定度主要影响因素是曲线校准。     

Construction and evaluation of ion-selective electrodes for potassium and calcium with a summing operational amplifier. Application to wine analysis

Electrodes selective to potassium and calcium with improved senstivity were constructed like conventional electrode (ISEs), but used an operational amplifier to sum the potentials supplied by the four membranes (ESOAs). The results obtained during the evaluation of their working characteristics were compared to those obtained by conventional ISEs and were found to be similar, but with higher precision. The electrodes were used in the potentiometric determination of potassium, calcium and magnesium in wines. The results given by ESOAs were more precise than those from ISEs. The results obtained by potentiometry were in good agreement with those from AES for potassium and AAS for calcium and magnesium.     

干灰化–离子色谱法测定木耳标准物质中的钾、钙、镁

采用离子色谱法对木耳标准物质中的K,Ca,Mg进行测定,对样品消解以及离子色谱分离条件进行了优化。在优化实验条件下,该法对木耳中K,Ca,Mg 3种元素测定结果的相对标准偏差小于1.0%(n=7)。采用该方法对NIST西红柿叶标准物质(SRM1573a)进行测定,测定结果与标准值相符,同时与ICP–OES方法比较验证,两者测定结果一致。对该方法测定结果的不确定度进行了评定,K,Ca,Mg测定结果的相对扩展不确定度(k=2)分别为2.3%,3.3%,1.9%。该方法准确可靠,能够满足标准物质定值的要求。     

烷烃在丝光沸石型分子筛中吸附和扩散行为

采用巨正则系综蒙特卡罗(grand canonical Monte Carlo, GCMC)与分子动力学(molecular dynamics, MD)相结合的方法, 研究烷烃分子在丝光沸石(MOR)型分子筛中的吸附和扩散性质. 采用GCMC 方法研究温度为300 K、330 K时, MOR型分子筛中甲烷、乙烷、丙烷、丁烷的吸附. 研究表明, 随着压力的增加吸附量增加, 随温度的升高吸附量有所降低. 饱和吸附量从大到小依次为: 甲烷>乙烷>丙烷>丁烷. 由模拟所得到的单组分吸附等温线, 通过理想吸附溶液理论(IAST)计算二元混合物的吸附平衡相图, 模拟结果与计算结果一致. 采用分子动力学方法, 研究乙烷、丙烷在MOR分子筛上的扩散性质, 结果表明各个方向上的扩散系数不同, z方向上的扩散系数最大.     

锌矿原料有机物含量监测方法探究

采用测定化学需氧量(COD)法和有机溶剂抽提法分别对企业常用的两种锌矿原料(A,B)有机物进行监测。通过采用测定化学需氧量(COD)法对锌矿原料中含有的有机物进行定性及半定量分析,实验结果表明,矿粉A中COD为84.9mg/L,矿粉B中COD为96.9mg/L,各自进行了3次平行实验,都能得到稳定的结果,同时确定矿粉A和B中分别含有不同量的有机物。采用有机溶剂抽提法来确定锌矿原料中有机物的含量。考察了溶剂种类、溶剂量、抽提时间对矿粉中的有机物提取效果的影响,得到最佳实验条件,对矿粉的测定结果为:矿粉A中有机物含量为7.6‰,矿粉B中有机物含量为10.1‰。在各自的最佳实验条件下,进行了3次平行实验,都能得到稳定的结果,方法准确、可靠。     

不同产地啤酒中无机元素的因子分析与聚类分析

啤酒样品经硝酸消解后,用微波等离子体炬原子发射光谱法(MPT-AES)测定其中无机元素的含量。所得结果用SPSS 17.0科学统计软件进行因子分析和聚类分析。因子分析的结果表明:总方差(52.803%)的贡献来自于代表钴、锶、锰元素的因子1和代表锌、铁、铜元素的因子2,所以这些元素是啤酒中的特征元素。聚类分析的结果表明:9种产地的啤酒可以很好地彼此区别,并以此进行啤酒产地的归属辨别。     

Solution thermodynamics of valnemulin hydrogen fumarate in different pure solvents

Solubility of valnemulin hydrogen fumarate in five pure solvents was determined within temperature range of (278.15 to 323.15) K by a gravimetric method. The results show that the solubility of valnemulin hydrogen fumarate in tested pure solvents increases with the increasing temperature. The solubility values were correlated by the Wilson model, NRTL model and UNIQUAC model. The UNIQUAC volume parameter, area parameter, and Wilson liquid molar volume parameter of valnemulin hydrogen fumarate were estimated by the group contribution method. It was found that the correlated results are in good agreement with the experimental results. Furthermore, the mixing thermodynamic properties of valnemulin hydrogen fumarate in solutions, including the mixing Gibbs energy, the mixing enthalpy and entropy, were determined by using the Wilson model and the experimental solubility results.     

连续流动法同时测定污水中氨氮和总磷

采用连续流动分析法测定污水中氨氮、总磷的含量。比较了污水样品不同的稀释倍数对测定结果的影响。实验结果表明:氨氮和总磷的质量浓度在0.1~8 mg/L范围内线性良好,线性相关系数均为0.99997;测量结果的相对标准偏差分别为2.01%,0.84%(n=7);方法检出限分别为0.012,0.009 mg/L;质控样测量值均在标示值范围内;样品加标回收率为93.4%~101.1%。污水的洁净程度对测定结果影响较大。洁净度高的污水,直接测定与稀释后测定,测定值无显著性差异;而洁净度低的污水,直接测定与稀释后测定结果差异比较大。该法采用全谱直读CCD检测方式,灵敏度高,稳定性好,无光谱干扰,且支持氨氮和总磷同时测定,方便快捷,适合污水中氨氮和总磷的测定。     

Construction and evaluation of ion-selective electrodes for potassium and calcium with a summing operational amplifier. Application to wine analysis

Electrodes selective to potassium and calcium with improved senstivity were constructed like conventional electrode (ISEs), but used an operational amplifier to sum the potentials supplied by the four membranes (ESOAs). The results obtained during the evaluation of their working characteristics were compared to those obtained by conventional ISEs and were found to be similar, but with higher precision. The electrodes were used in the potentiometric determination of potassium, calcium and magnesium in wines. The results given by ESOAs were more precise than those from ISEs. The results obtained by potentiometry were in good agreement with those from AES for potassium and AAS for calcium and magnesium. Received: 27 June 1997 / Revised: 29 September 1997 / Accepted: 3 October 1997     

核磁共振法测定苯乙烯和甲基丙烯酸正丁酯竞聚率的研究

以苯乙烯（Ｓｔ）－甲基丙烯酸正丁酯（ＢＭＡ）共聚体系为研究对象，在共聚单体组成敏感点附近做重复实验，进行了４０、６０、８０、１００，１２０、１４０℃下的共聚合，用ＮＭＲ方法测定共聚物的组成，用Ｍａｙｏ－Ｌｅｗｉｓ微分组成方程的误差变量法计算竞聚率，同时给出竞聚率的９５％可信椭圆区间．并根据竟聚率对温度的依赖关系得到一组合理的竞聚率值．