ICP—AES法测定稀土—铁—镁合金的成分

本文叙述了用 ICP—AES 法同时测定稀土—铁—镁合金中各元素含量。研究了高含量Fe 对其他元素测定的影响。三个标样的测定结果表明该方法是准确可靠的。     

增效试剂在动力学分析法中的应用研究锰(Ⅱ)—高碘酸钾—氨三乙酸—PAN—Triton X—100催化体系

本文报道了以 Triton X—100为增溶剂,高碘酸钾氧化 PAN 催化光度法测定痕量锰的新体系。方法的检出限为3.6×10~(-3)μg/mL,精密度为2.4%(n=9),线性范围为0.10～1.3μg/25mL,可用于谷物样品中锰的测定。     

Ｓt—AN—PMI乳液共聚物的玻璃化温度与流变性

用ＤＳＣ和ＴＢＡ两种方法测定了苯乙烯－丙烯腈－Ｎ－苯基马来酰亚胺乳液共聚物的玻璃化温度Ｔg ,研究了共聚物的流变性能,测定了共聚物的熔体流动指数n,发现共聚物的熔体流动指数越大,两种方法测定的共聚物的Ｔg的差值越大。     

基于ICP—MS的船用润滑油检测分析

采用电感耦合等离子体质谱法(ICP-MS)测定船用润滑油中元素钼、镍、钒、钛、钡、镉、铜、铅和锰。油液样品经加热蒸发和高温灼烧灰化处理,再加硝酸和过氧化氢湿法消解,消除了有机质对质谱测定的影响。经过优化仪器工作条件,内标校正和干扰方程处理后,所测定元素的标准曲线相关系数达0.9999以上,加标回收率为93~106%,RSD1%。     

Y—Al—Si—O—N氧氮玻璃的介电性质研究

用粉末烧结法制备出Ｙ－Ａｌ－Ｓｉ－Ｏ－Ｎ氧氮玻璃。测定了氧氮玻璃的介电常数和ｔａｎδ,以及钇对玻璃介电常数和ｔａｎδ的影响。发现氧氮玻璃的介电常数随钇含量的减少而减少。对制得的氧氮玻璃进行热处理,加热到９７０℃保温４ｈ,再升温到１２００℃保温１ｈ,随炉冷却。测定并研究热处理后氧氮玻璃的介电性质,用ＸＲＤ方法观测了热处理前后的玻璃结晶状况。     

AA—AM—SAS三元共聚物的合成及其阻垢性能

以水为溶剂，过硫酸盐为引发剂，合成了丙烯酸（ＡＡ）、丙烯酰胺（ＡＭ）和烯丙基磺酸钠（ＳＡＳ）三无共聚物（ＡＡ－ＡＭ－ＳＡＳ）。用ＩＲ、ＮＭＲ和热分析方法对共聚物进行了表征和测定，并对共聚物的阻垢性能进行了测定。结果表明，合成的三元共聚物是一种性能优良的阻垢分散剂。     

BPC—1型冰淇淋膨胀率测定仪设计与研制

膨胀率是冰淇淋制品的理化指标之一。长期以来,这项指标的测定采用容量瓶消泡、滴定的方法,对测试人员的操作技巧要求很高,不仅测定时间长,而且测定结果离散性较大,远不能适应当前食品工业发展的需要。 我厂研制开发的冰淇淋膨胀率测定仪,在1994年上海市冷饮行业生产许可证发放的工作中,以其操作简便、测定准确、快速的特点,受到冰淇淋生产企业和     

氢化物—原子荧光法测定饮用水中砷的方法研究与改进

应用氢化物—原子荧光法测定生活饮用水中的砷含量,实验过程中发现绘制的标准曲线和已知浓度水样的测定结果均存在较大误差,通过分析确定起还原剂和掩蔽作用的抗坏血酸在测定过程中存在干扰。在改进方法后,只用硫脲作为还原剂和稳定剂而不加抗坏血酸后测定的标准曲线的线性相关系数为0.9997、检出限为0.035μg/mL,用砷标准溶液6.00μg/L的浓度测得相对标准偏差RSD=2.67%,加标回收率为96.5%-102.5%。实际水样的测定结果也符合国家标准。证明该改进方法对于测定低含量砷且杂质离子未达到影响结果测定浓度时的水样具有过程简单、可靠性强的优点。     

HPLC—荧光检测测定五种多环芳烃

本文采用HPLC—荧光检测测定五种多环芳烃化合物。在shim-pack CLC-ODS柱上,以70％的乙腈水溶液作流动相,20min内同时分离测定了(艹屈)、苊、蒽、荧蒽、芘等五种多环芳烃。     

SHE—1超速化学镀镍

介绍了一种新的超速的化学镀新工艺，找到了适合于高速化学沉镍的络合剂、稳定剂和加速剂，镀液可心在稳定的条件下以２５～２８μｍ／ｈ的速度沉积出镍层。研究了硫酸镍、次亚磷酸钠、丁二酸、络合剂ＣＬ－１、加速剂ＡＬ－１以及ｐＨ值、温度、时间等因素对化学镀镍速度的影响，并用常镀层的耐蚀性，用扫描电镜测定了镀层的形貌，用Ｘ射线测定了结晶取向。     

微波消解快速测定印染污泥中重金属

建立了微波消解-原子吸收分光光度法测定印染污泥中铜、锌、镍、铅、镉5种金属的检测方法。分别称取0.2g~0.3g标准土壤样品和印染污泥样品进行分析,标准土壤样品测定结果的相对误差为-0.99%～6.69%,5次平行测定结果的相对标准偏差为0.71%～5.66%;印染污泥样品测定结果的加标回收率为84%～113%,相对标准偏差为2.47%～9.26%。本方法具有准确、快速等优点,适用于大批量样品分析测定。     

Effects of Cooling and Dressing Methods on Grinding of Glass

Experiments were designed and conducted to evaluate the effects of cooling and dressing methods and five other factors on the grinding of glass. Surface roughness of the ground samples was measured and microscopic studies of the ground glass surfaces were performed. The column effect method and plotting method were applied to analyze and interpret the experimental results. The results showed that the average surface roughness heights of ground glass were improved by 5-36% and 42-52%, respectively, when an improved coolant system and dressing device were employed. The average surface roughness heights decreased by 52-58% and 30-37%, when smaller grit sizes and a resin-bond grinding wheel rather than a metal-bond grinding wheel were used, respectively. In addition, the surface roughness averages decreased by 18-23% and 13-18% when a smaller table-feed rate was used and truing of grinding wheels was performed, respectively. Moreover, compared with the surface roughness heights of the sample that was ground using the existing coolant system and manual dressing method, the surface roughness heights of the sample ground using both the improved coolant system and device-dressing method were improved by 46-70%, because of the positive interaction of these two factors.     

Quantitation of 4-(4-Chl0R0Phenyl)-2-Pyrr0Lidin0Ne in Baclofen Powder and Tablets

Abstract

A high-pressure liquid chromatography method to quantify 4-(4-chlorophenyl)-2-pyrrolidinone which is present as an impurity in baclofen powder and its dosage forms has been developed. The USP-NF method for the determination of 4-(4-chlorophenyl)-2-pyrrolidinone in powder is based on TLC and is only qualitative. The developed method was successfully used to quantify 4-(4-chlorophenyl)-2-pyrrolidinone in powder (USP-NF limit 1%) and in tablets (USP-NF limit 5%). The method is accurate and reproducible with a percent error of 4% for powder and 3% for tablets.     

An ICP-OES method with 0.2% expanded uncertainties for the characterization of LiA1O2

An improved inductively coupled plasma-optical emission spectrometry (ICP-OES) method has been applied to the determination of Li and A1 mass fractions and the Li/A1 amount-of-substance ratio in representative samples of LiA1O2. This ICP-OES method has uncertainty on the order of 0.2%,(2,3) comparable to the best analytical methods. This method is based on several strategies, which are detailed in this work. The mean measured mass fractions of Li and A1 in eight samples were 0.10151 +/- 0.00016 (+/-0.16%) and 0.41068 +/- 0.00056 (+/-0.14%), and the mean Li/A1 amount-of-substance ratio was 0.9793 +/- 0.0017 (+/-0.17%). The uncertainty is dominated by sample handling and heterogeneity-about a factor of 2 larger than the ICP-OES instrumental uncertainties, which were 0.04% for A1 and 0.07% for Li.     

含油食品中塑化剂快速检测

本试验利用乙腈提取塑化剂,氮吹浓缩后甲醇定容通过气相色谱一质谱联用仪测定。试验结果表明：该测定方法的加标回收率在89．1％-104．8％,RSD为1．01％～3．19％,与GB／T2191-2008标准中规定的方法相比相差无几,但样品的处理时间更短,操作方便、经济、快速,适合在基层实验室做大量样品筛选时选用。     

流动注射化学发光法测定杀扑磷

基于杀扑磷对过氧化氧和鲁米诺在碱性条件下化学发光有抑制作用,本文建立了一种杀扑磷的流动注射化学发光（FI-CL）检测方法。杀扑磷在1．0×10^-7-1．0×10^-3g／mL范围内与发光强度呈良好的线性关系,检测限（S/N=3）为7．3×10^-8g,／mL,测定相对标准偏差（RSD）为1．26％,对柑橘样品进行加标回收率测定,回收率在89．5％-92．6％之间。     

Determination of azathioprine and its related substances by capillary zone electrophoresis and its application to pharmaceutical dosage forms assay

The development of a stability-indicating capillary zone electrophoresis (CZE) method for the determination of the drug azathioprine (AZA) and its related substances in bulk and dosage forms is described. Theophylline was used as an internal standard to improve quantitative results. The method was fully validated in terms of repeatability (n = 10, RSD for migration time and peak area ratio were 0.15% and 0.60%, respectively), reproducibility (n = 5, RSD of peak area ratio was 0.84%), linearity at two ranges of the azathioprine concentration, limits of detection (LOD) and quantitation (LOQ), and robustness. The method was applied for determination of the drug in bulk and a commercial tablet dosage form (recovery 98.3-101.3%) and in powder for injection (recovery 98.7-100.6%). The method was fast and reliable for the analysis of AZA and its related substances in bulk and dosage forms.     

银杏叶中五种黄酮测定方法研究

本文建立了高效液相色谱法同时测定银杏叶提取物中五种黄酮成分的方法。实验结果显示:方法的精密度为1.8%~3.6%,回收率为92.7%~97.9%,样品中目标黄酮芦丁、槲皮素、木犀草素、山奈酚和异鼠李素含量依次为0.47%、0.13%、0.02%、0.09%、0.06%。该法具有分析速度较快、不易堵塞管路及能测定较多黄酮化合物等特点。     

高效液相色谱法测定纺织品中苯并三唑类光稳定剂

以乙酸乙酯为提取溶剂,使用超声波辅助萃取-高效液相色谱测定纺织品中2-（2＇-羟基-3＇,5＇-二叔丁基苯基）-苯并三唑,并对仪器的测试条件进行优化。该方法的平均回收率为93.1%-105%,相对标准偏差小于10%,方法检出限可低至0.1mg/kg。该方法操作简单快速,稳定可靠,适用于纺织品中2-（2＇-羟基-3＇,5＇-二叔丁基苯基）-苯并三唑的日常监测。     

流动注射化学发光法测定伏杀硫磷

基于伏杀硫磷对过氧化氢和鲁米诺在碱性条件下化学发光有抑制作用,本文建立了一种伏杀硫磷的流动注射化学发光(FI-CL)检测方法。伏杀硫磷在1.0×10-7-1.0×10-5g/mL范围内与发光强度呈良好的线性关系,检测限(S/N=3)为3.1×10-8g/mL,相对标准偏差(RSD)为1.21%,对甘蓝样品进行加标回收率测定,回收率在90.2%-97.4%之间。