钼蓝分光光度法测定钼铝与钒铝合金中的硅

采用硝酸、氢氟酸分解试样,钼蓝分光光度法测定钒铝、钼铝合金中的硅量。对试样分解、光度法测定条件及共存元素的干扰等进行了试验。将该法应用于6个钒铝、钼铝试样中硅量(0.04%~0.46%)的测定,结果的相对标准偏差(n=11)在1.2%~4.6%之间,加标回收率为97.4%~102.2%。同时进行了多家实验室间数据比对,结果一致。     

固体进样石墨炉原子吸收光谱法测定船用燃料油中硅、铝含量

建立了固体进样石墨炉原子吸收光谱法测定船用燃料油中微量硅、铝元素含量的快速检测方法。通过选择谱线和背景校正模式,优化了石墨炉条件;根据待测样品及元素特点优化了升温程序。硅、铝的测定波长分别为251.6,394.4 nm,采用塞曼背景校正,样品无需前处理,直接通过石墨舟进样检测。燃料油中硅、铝元素的检出限分别为0.165,0.126 ng;3个浓度水平下,硅元素平均回收率为88%~92%,铝元素平均回收率为93%~95%,测定结果的相对标准偏差为4.2%~10.7%(n=6)。采用本法对实际燃料油样品进行测定,硅、铝元素的测定结果与IP 501方法测定结果基本一致。该方法取样量少、操作简便、快速,检验结果准确度高、稳定性好,适用于船用燃料油中微量硅、铝元素含量的定量检测。     

硅钼蓝分光光度法测定硅肥中有效硅

本文采用硅钼蓝分光光度法测定硅肥中有效硅的含量,通过研究浸取剂、振荡频率以及称样量等条件对有效硅提取量的影响,确定了样品溶解方式。探讨了酸度、显色时间、波长等因素对硅钼蓝吸光度的影响。同时,对优化后的硅钼蓝分光光度法进行精密度和准确度试验,多次重复测定的极差小于0.60%,标准偏差小于0.20%,加标回收率在98.5%~101.3%之间。结果表明优化后的硅钼蓝分光光度法具有良好的重现性和精密度。     

高压密闭消解-钼蓝分光光度法测定钴铬烤瓷合金中硅

在HNO3-HCl-HF混酸中高压密闭消解,采用钼蓝分光光度法测定钴铬烤瓷合金中的硅量。研究了酸体系、消解时间及共存离子对硅测定的影响。方法用于已知样品的测定,相对标准偏差小于3%(n=11),加标回收率为98.9%~101%。方法精密度高、准确度好,能够满足钴铬烤瓷合金中硅含量测定的要求。     

电感耦合等离子体发射光谱法测定镍铜合金中高含量硅

采用电感耦合等离子体发射光谱（ICP-AES）法对镍铜合金中高含量硅进行了测定.方法对样品的溶解和仪器测量条件以及共存元素干扰进行了系统的研究,选定了仪器的最佳测定条件,硅分析线为251.611 nm,内标元素线为371.029 nm.样品以硝酸为主加盐酸溶解,加氢氟酸控制温度溶解硅,在仪器最佳条件进行测量,并与经典化学法（重量法）结果对照一致.硅元素含量在1%~5%范围回收率为99%~102%,RSD为0.77%.     

气体容量法测定单质硅的改进

对测定单质硅的气体容量法进行了改进,在测量装置中增加了恒温系统、柱形称样器,并扩大了量气管的量程。最佳反应碱度为200g·L-1氢氧化钠溶液65mL,反应时间为1h。对不同含量单质硅样品进行测定,测定值的相对标准偏差(n=6)在0.32%~0.47%之间,偏差在-0.45%~0.40%之间。     

气相色谱法同时测定α-乙酰基-γ-丁内酯和甲苯含量

本文对气相色谱法分离α-乙酰基-γ-丁内酯(ABL)的条件进行了系统的考察,建立了校正因子峰面积归一化法测定ABL含量的分析方法,并且当甲苯含量大于0.0005%时能同时准确测定其含量。结果表明:在最佳的分离条件下,甲苯的浓度在0.00055%~0.5239%范围内其浓度与峰面积呈良好的线性关系,相关系数R2为0.9990,检出限为0.000353%;测定甲苯和ABL含量的相对标准偏差分别为1.1%和0.0008%;当甲苯加入量在0.00076%~0.4728%之间时,回收率为96.4%~114.3%。     

磁致冷材料钆硅锗系合金中Si和Gd的重量法联测的研究

参考了HClO4脱水重量法测定Si及草酸盐重量法测定Gd的方法,建立了钆硅锗系合金中主成分Si和Gd联合测定的方法,并详细考查了共存元素及杂质元素对测定的影响。合金共存元素Ge在HCl的存在下,绝大部分可以GeCl4的形式被蒸发,达到与被测元素分离的目的。熔样过程引入的杂质元素Ni可与被测元素Gd,用氨水沉淀分离,残留Ni不足以影响Gd的测定。方法回收率在98.5%以上,Si和Gd的测量相对标准偏差分别在2.6%~3.0%和0.4%~0.5%。     

MPT–AES法测定合金钢中的硅

建立了微波等离子体炬原子发射光谱(MPT–AES)测定合金钢中的硅含量的分析方法。考察了仪器最佳实验条件、溶液酸度和钢中共存离子对测定的干扰,采用相似基体的标准钢样绘制工作曲线。硅的线性范围在0.3~7.0μg/m L之间,检出限为0.05μg/m L。测定结果的相对标准偏差为1.2%~3.1%(n=9),样品加标回收率在97.0%~103.0%之间,该法测定结果与国家标准方法测定结果相符合。MPT–AES法良好的精密度和准确度,可用于测定合金钢中硅的含量。     

食用菌中稀土元素的分离富集-ICP-AES法测定

采用强酸型阳离子交换树脂分离富集-ICP-AES法同时测定食用菌中的稀土元素,排除了高含量的K、Na、Ca、Mg等非稀土元素的基体干扰,并对分析谱线的选择、样品消解方法、仪器工作条件和分离富集条件进行了研究。方法回收率为92.2%~104.2%,相对标准偏差为1.4%~9.7%。     

Determination of micro amounts of uranium by a molybdenum blue method

A new and highly sensitive spectrophotometric method has been developed for the determination of micro amounts of uranium by a molybdenum blue method. The method is based on the observation that at low acidities uranium(IV) reduces ammonium molybdate to molybdenum blue, the absorbance of which is proportional to the amount of uranium present. The variables affecting development of the colour have been investigated and the conditions optimized. Beer's law is found to hold good for uranium concentrations between 1 and 20 ppm, with a precision of 2%. The effect of diverse ions has been studied. The method is useful for the determination of uranium present as an impurity (down to 0.1%) in plutonium, neptunium or thorium.     

测定痕量磷的激光热透镜光谱法--钼蓝法与孔雀绿法的比较

采用激光热透镜光谱法（LTLS）,分别以孔雀绿－磷钼杂多酸缔合物法和磷钼蓝法对痕量磷进行了测定;探讨了测定条件的影响,分析比较了两种测定方法,结果表明,钼蓝法的线性范围较宽,孔雀绿法的灵敏度较高,选择性较好,将孔雀绿LTLS法应用于河水、自来水和土壤样品中痕量磷的分析测定,取得了满意的效果。     

原子荧光光谱法测定煤中砷含量

主要研究了原子荧光光谱法测定煤中砷含量的方法,该法回收率为(95.75~98.34)%,RSD2.36%。通过与砷钼蓝分光光度法测定煤中砷含量比较,和对该法的精密度和准确度进行探讨,结果表明,该法操作简单,快速,灵敏度高,测定砷浓度范围大,适用于煤中砷含量测定。     

The colorimetric determination of silicate with special reference to sea and natural waters

The optimum conditions for the determination of silicate in natural waters by a molybdenum blue method have been investigated p-Methylaminophenol sulphate has a number of advantages over other reducing agents for the reduction of silicomolybdic acid to molybdenum blue. Beer's law is obeyed up to concentrations of at least 3 mg/l.The interference of several inorganic ions has been investigated; none of those encountered in natural waters is likely to cause error. The method has been applied to the analysis of sea-water and the “salt error” correction evaluated.     

磷酸盐缓冲体系中大豆卵磷脂的分析

建立了一种测定磷酸盐缓冲体系中大豆卵磷脂含量的方法。利用无水乙醇－石油醚（６０～９０℃）萃取剂从磷酸盐缓冲溶液中分离出大豆卵磷脂，再用钼蓝法对大豆卵磷脂含量进行测定。该方法操作简便，定量准确，重现性好，用于胰岛素口腔喷剂中大豆卵磷脂含量测定，样品平均回收率为９９．７５％，ＲＳＤ＝３．９３％。     

Investigation of the extraction equilibrium of ion-association complexes of molybdenum (VI) with some polyphenols and thiazolyl blue. extraction-spectrophotometric determination of molybdenum

The extraction process of ternary ion-association complexes of molybdenum (VI) with some polyphenols (4-nitrocatechol, 2,3-dihydroxy naphthalene) and thiazolyl blue has been investigated by using an extraction-spectrophotometric method. The optimum conditions for their quantitative preparation in aqueous medium and subsequent extraction into an organic solvent have been found. The extraction, distribution and association constants, and the recovery factors have been calculated. The composition of the complexes has been determined. A precise, sensitive and simple extraction-spectrophotometric method for determination of molybdenum in products from ferrous metallurgy has been developed.     

Spectrophotometry Determination of Molybdenum with N-Cyanoacylacetaldehyde Hydrazone

N-cyanoacylacetaldehyde hydrazone (CAAH), which is a laboratory synthetic reagent, is proposed as a new reagent for spectrophotometry determination of microamounts of molybdenum at λ_max 790 nm. The reagent forms 1:1 blue coloured complex with molybdenum (VI) in phosphoric acid solution. The stable blue colour is obtained finally after changing from yellow to green. The colour development depends on temperature, time and concentration of phosphoric acid. This reagent is applied for the determination of molybdenum in steel alloys and the results are satisfactory.     

铈量法快速测定镍钼矿硫酸介质加压浸出液中的钼

镍钼浸出液中的大量Fe^2＋和Fe^3＋,采用氢氧化钠沉淀分离,以消除铈量法在测定钼时产生的干扰。通过在钼标准中加入Ni试验证明,测定体系中存在大量Ni^2＋时,不干扰钼的测定。用草酸一硫酸联氨将Mo^6＋还原至Mo^5＋,用次甲基蓝作氧化促进剂,加快了滴定时的反应速度,终点突跃明显。拟定方法的样品加标回收率为95．0％～103．5％,相对标准偏差均〈1％。在实际测定中,方法快速准确,值得推荐。     

Filtration through nylon membranes negatively affects analysis of arsenic and phosphate by the molybdenum blue method

Filtering synthetic arsenic- or phosphate-containing solutions (1.5-47.6 μmol/L) with nylon syringe filters significantly reduced absorbances (by 6-74%) when analyzed with the colorimetric molybdenum blue method. Filtering the same solutions with cellulose acetate syringe filters yielded no significant differences as compared to unfiltered controls. The detrimental effect of nylon membranes was also observed when pure Milli-Q water was filtered and subsequently spiked with arsenic(III) or phosphate suggesting that some compound(s) eluting from the filter membranes interfere with the color formation in the assay. Consequently, we caution against using nylon filters when filtering water samples for the determination of arsenic or phosphate with the molybdenum blue method.     

分光光度法测定水样中的硫离子

A new simple spectrophotometric method was proposed for the determination sulphur ion in water samples.In the medium of 0.05 mol/L HCl,sulphur anion turns mixed acid of the silicon and molybdenum into molybdenum blue.Its absorption maxima was found at the wavelength of 700 nm,with a molar absorptivity of 2.48×104L·mol-1·cm-1.Influencing factors such as the amount of reagent and reaction time were optimized,and the interferences from common aions were also investigated.This method was successfully used for t...