缝式石英管捕集技术的改进

试验了各种条件对Ag、Au、Cu、Pb和Zn灵敏度影响.结果表明,分别用不同火焰条件进行原子捕集与释放可获得最佳灵敏度。捕集1min,测得Ag、Au、Cu、Pb和Zn的特征浓度分别为8.1×10、1.7×10~(-3)、1.8×10~(-3)、2.4×10~(-3)和1.3×10~(-4)μg/ml,比常规火焰原子吸收光谱法的灵敏度分别提高62、106、28、83和77倍。Ag、Au、Cu、Pb和Zn的相对标准偏差依次为2.8％、3.1％、2.6％、2.7％、5.4％。本法测定了牡蛎中Ag和Cu。     

痕量Au Bi和Cd的萃取浮选及原子吸收光谱法测定

浮选法分离痕量金属离子,由于灵敏度高、选择性强已得到广泛应用。本文利用浮选法使Au~(3 )、Bi~(3 )和Cd~(2 )同KBr反应生成的络合阴离子与碱性染料罗丹明B(RB)生成既疏水又疏有机溶剂的三元离子缔合物,后者经甲苯浮选分出,用二甲基甲酰胺(DMF)溶解后,可用原子吸收法测定Au、Bi和Cd的含量。本方法用于海水,锌片和矿样中上述三种元素的微量测定,可提高检测灵敏度,而且K、Na、Ca、Mg等共存离子不生干扰。具体实验方法如下:     

碘化钾-十六烷基三甲基溴化铵体系浮选分离金(Ⅲ)

研究了硫酸铵存在下,碘化钾-十六烷基三甲基溴化铵体系浮选分离Au(Ⅲ)的行为,及其与一些金属离子分离的条件,用火焰原子吸收光谱法测定。当溶液中硫酸铵、碘化钾、十六烷基三甲基溴化铵分别为100 g.L-1,5.0×10-3mol.L-1,2.0×10-3mol.L-1,pH 3.0时,Au(Ⅲ)可与Fe(Ⅱ)、Ni(Ⅱ)、Cu(Ⅱ)、Cr(Ⅲ)、Zn(Ⅱ)、Cd(Ⅱ)定量分离,运用此法对合成水样中Au(Ⅲ)进行了定量分离测定。     

火焰原子吸收光谱法直接测定金锭中银、铜、铁、铅、锑和秘的含量

通过火焰原子吸收光谱法直接测定了金锭中Ag、Cu、Fe、Pb、Bi、Sb的含量.结果表明,该法可极大地缩短分析时间,方法的检出限Ag、Cu、Fe、Pb、Bi、Sb分别为0.008、0.020、0.015、0.032、0.22、0.25 μg/mL;回收率94％～108％;RSD小于1.8％.该法快速、简便、准确.     

铅试金法测定铅精矿及粗铅中的金、银

本试验对铅火试金富集金、银的方法进行研究.该法中的主要干扰元素有Cu、Sb、Bi、As等.结果表明As、Sb、Cu对铅试金法测定Au、Ag基本没有影响,Bi在一定范围内干扰不明显,但当Bi的含量大于5%时对Ag的测定有明显的影响.本次试验与湿法及标准加入法相比较,重现性好、可靠性强、准确度高.本方法的主要目的是解决Ag含量大于1000g/t的铅精矿及粗铅中Au、Ag含量的测定.     

脱脂棉富集-火焰原子吸收测定水中铜、铅、镉

1 引言 本文在pH6.5～7.0范围内,用脱脂棉富集水中痕量Cu、Ph、Cd原子吸收光谱法测定,方法简便快速、灵敏度高,用于水中痕量Cu、Pb、Cd的测定,结果满意。 2 实验部分     

PVC膜AuCl_4~-电极的研究

金电极的报导较多,但由于AuCl_4~-容易以金析出,未找到较好的内参比体系,仍缺乏一种既灵敏度高又性能稳定的电极。Au(CN)_2~-电极虽然灵敏度较高,但对常与Au共存的Ag的选择性较差,且氰化物剧毒。本实验通过比较不同季铵盐和内导体系,研制了全固态PVC膜AuCl_4~-电极。其灵敏度比国内外现有电极稍高,稳定性、重现性好,Ag、Pb干扰小。     

混酸体系中31种金属离子的浮选行为

在总浓度为0.17～3.4N的HCl-HNO_3(〔HCl〕:〔HNO_3〕=2.4:1)体系中,以(18～60)×10~(-5)M的CPC为捕集剂,对(2.755～28.69)×10~(-5)M的31种金属离子进行了浮选,表明Ir(Ⅳ)、Pt(Ⅳ)、Ge(Ⅳ)、Sn(Ⅳ)、Bi(Ⅲ)、Au(Ⅲ)、T1(Ⅱ)、Pd(Ⅱ)、Sn(Ⅱ)可浮选95％以上,而Cr(Ⅵ)、Ti (Ⅳ)、Zr(Ⅳ)、Ga(Ⅲ)、In(Ⅲ)、Fe(Ⅲ)、Sb(Ⅲ)、Al(Ⅲ)、Mn(Ⅱ)、Fe(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)、Cu(Ⅱ)、Zn(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)浮选率低于20％或几乎不浮选,Ru(Ⅱ)、Rh(Ⅱ)、Ir(Ⅱ)、Hg(Ⅱ)、Ag(Ⅰ)、TI(Ⅰ)部分被浮选。与HCl体系的浮选结果进行了比较,发现贵金属的浮选率和选择性在HCl-HNO_3体系中更好。进行了Au(Ⅲ)、Pt(Ⅳ)、Pd(Ⅱ)与Zn(Ⅱ)、Cd(Ⅱ)、Hg(Ⅱ)、Sb (Ⅲ)的分离试验,结果令人满意。     

阳极溶出伏安法同时测定高纯金属锌及试剂中的痕量杂质Cd、Pb、Cu、Bi

阳极溶出伏安法测定高纯金属及高纯试剂中的痕量杂质,正日益得到广泛的应用。我们研究了以酸溶试样后,不用分离主体锌,即可在普通笔录式极谱仪上,用玻碳汞膜电极同时测定其中四种痕量杂质元素Cd、Pb、Cu、Bi的极谱行为和测定条件。实验结果表明:在大量基体Zn存在下,最佳支持电解质体系为:1MHCl～0.2 MNH_4Ac～5×10~(-4)MHgCl_2,只预电解5分钟,Bi、Pb及Cd、Cu的灵敏度分别为4×10~(-10)g/ml、6×10~(-10)g/ml及     

激光剥蚀-电感耦合等离子体质谱对高温合金中17种痕量元素的测定

建立了镍基高温合金中Sc、Cu、Zn、Ga、Ge、As、Ag、Cd、In、Sn、Sb、Te、Ce、Hf、Tl、Pb、Bi17种痕量元素的激光剥蚀-电感耦合等离子体质谱测定方法。对激光剥蚀进样及质谱分析条件进行了优化,通过激光对样品表面的层层剥蚀顺利完成了对低沸点杂质元素的测定。采用格栅扫描采样,严格控制样品的聚焦位置和散焦距离以保证采样的准确性,由高温合金系列标准物质建立了18种痕量元素的校正曲线,其中14种痕量元素的线性相关性较好(r2≥0.99),In、Sn、Sb、Ce、Tl、Pb、Bi等超痕量元素的检出限和气体空白分别低于或接近0.000 005%和0.000 001%。方法对镍基高温合金样品中Cu、Ga、Ag、Cd、In、Sn、Sb、Te、Hf、Tl、Pb和Bi等痕量元素的测定结果与参考值吻合较好,且大部分元素的RSD(n=4)小于或接近30%。     

Catalytic Kinetic Polarographic Determination of Trace Amount of Indium

The method of polarography for determination of trace In(III) had been reported by reference(l-2), However, The method of catalytic kinetic polarography has not been reported. Author discovered that trace indium(III) cold catalyze the discoloring oxidizing reaction of methyl orange by potassium bromate in 0.03mol/L H₂SO₄——0.25mol/L NH₃.H₂O supporting electrolyte, methyl orange exhibits a sensitive polarography wave at -0.45V(vs.SCE), The change in methyl orange concentration is traced by polarography. Hence, a new catalytic kinetic polarography method for determination of trace indium has been established. The method was used to determined trace indium in pure metallic zine with satisfactory results.     

Resonance Rayleigh scattering for the determination of cationic surfactants with Eosin Y

Resonance Rayleigh scattering (RRS) of cationic surfactants–Eosin Y systems and their analytical application have been studied. In aqueous solution at pH 2～3, Eosin Y reacts with a monomer of cationic surfactants (CS), such as Zephiramine (Zeph), tetradecylpyridinium bromide (TPB), cetylpyridinium bromide (CPB), cetylpyridinium chloride (CPC) and cetyltrimethylammonium bromide (CTMAB), to form an ion associate and a new RRS spectrum appears. The spectral characteristics of the five ion associates are similar and their maximum scattering wavelengths (λ_max) are all at 313 nm. The intensity of RRS at λ_max of the ion associate is directly proportional to the concentration of CS in the range of 0～3.0 μg/25 mL. The technique has high sensitivity for the determination of CS; their detection limit is between 5.57 ng/mL and 7.60 ng/mL depending on the CS. In this case, most metal and non-metal ions, NH₄ ⁺ and some anionic surfactants do not interfere, so that the method has a good selectivity. It can be applied to the determination of trace amounts of cationic surfactants in water samples.     

硫氰酸根-吡啰红G荧光光度法测定水及尿样中微量钼

本文利用吡啰红G作为荧光试剂,在强酸性条件下,用丙酮作增溶剂,硫脲作还原剂,Cu~(2+)作催化剂,使Mo(Ⅵ)还原为Mo(Ⅴ)并与SCN~-和试剂形成离于缔合物.该缔合物的荧光强度在测定条件下与钼的浓度成正比,λ_(?)=528/552nm;此法灵敏度高,选择性好,线性范围为0.0～1.4μg/25ml.直接用于自来水和尿样中钼的测定,回收率在97%～105%之间,结果满意.     

Extraction and Spectrophotometric Determination of Diclofenac in Pharmaceuticals

A new simple, rapid and sensitive spectrophotometric method has been developed for the determination of diclofenac sodium (Dicl) in pharmaceutical preparations. This method is based on the reaction of diclofenac sodium with an analytical reagent 1,3,3‐trimethyl‐5‐thiocyanato‐2‐[3‐(1′,3′,3′‐trimethyl‐3′‐H‐indol‐2′‐ylidene)‐propenyl]‐indolium cloride (TIC) at pH 8.0‐11.0 and the extraction of ion associate colored complex. Optimal conditions for the complex formation between Dicl and TIC were studied. This ion associate complex (1:1) was detected and extracted with toluene and an absorption maximum at 566.2 nm against a blank reagent. The calibration graph was linear from 0.9‐11.0 μg/mL of diclofenac and the detection limit was 0.86 μg/mL.     

离子色谱法测定饮用水中痕量溴酸盐

建立一种检测饮用水中痕量溴酸盐的离子色谱方法。利用On GuardⅡAg柱过滤去除水中氯离子,直接进样,电导检测器检测。该方法避免了氯离子对溴酸盐的干扰,测定水质溴酸盐的灵敏度和准确度均有很大提高。溴酸盐的检出限为0.005 mg/L,测定结果的相对标准偏差为7.56%(n=7),加标回收率为92.0%~110.0%。该方法操作简便快速、准确度高,适合于饮用水中痕量溴酸盐的测定。     

Resonance Rayleigh scattering for the determination of cationic surfactants with Eosin Y

Resonance Rayleigh scattering (RRS) of cationic surfactants–Eosin Y systems and their analytical application have been studied. In aqueous solution at pH 2∼3, Eosin Y reacts with a monomer of cationic surfactants (CS), such as Zephiramine (Zeph), tetradecylpyridinium bromide (TPB), cetylpyridinium bromide (CPB), cetylpyridinium chloride (CPC) and cetyltrimethylammonium bromide (CTMAB), to form an ion associate and a new RRS spectrum appears. The spectral characteristics of the five ion associates are similar and their maximum scattering wavelengths (λ_max) are all at 313 nm. The intensity of RRS at λ_max of the ion associate is directly proportional to the concentration of CS in the range of 0∼3.0 μg/25 mL. The technique has high sensitivity for the determination of CS; their detection limit is between 5.57 ng/mL and 7.60 ng/mL depending on the CS. In this case, most metal and non-metal ions, NH₄ ⁺ and some anionic surfactants do not interfere, so that the method has a good selectivity. It can be applied to the determination of trace amounts of cationic surfactants in water samples. Received: 9 September 1998 / Revised: 17 November 1998 / Accepted: 18 November 1998     

流动注射化学发光测定甲基对硫磷

首次研究了农药甲基对硫磷在碱性介质中（ｐＨ：１１．５～１２．０）与鲁米诺和过氧化氢产生化学发光的行为及反应机理,并发现水溶性高分子聚乙二醇对该反应具有显著的增效作用,据此建立了流动注射化学发光测定甲基对硫磷的新方法。甲基对硫磷的浓度在 ５×１０－８～１．０ ×１０－５ｇ／ｍＬ范围内与化学发光强度呈良好的线性关系;检出限为 ２×１０－８ｇ／ｍＬ;对 １．０×１０－６ｇ／ｍＬ甲基对硫磷进行了１１次平行测定,相对标准偏差小于４％;标准加入回收率为８３％～９４％。该法应用于谷物中农药残余量的测定,结果满意。     

Spectrophotometric determination of trace ionic and non-ionic surfactants based on a collection on a membrane filter as the ion associate of the surfactant with Erythrosine B

The spectrophotometric method for the determination of trace surfactants with Erythrosine B (EB) based on the aqueous reaction and the collection on a membrane filter by filtration was studied. Cationic surfactants (CS⁺), such as a quaternary ammonium ion, and polyoxyethylene non-ionic surfactants (NS) in the presence of potassium ion, containing a long-chain alkyl group associate with EB buffered at pH 5.5. CS⁺ associates with anionic surfactants (AS⁻). For the determination of CS⁺, four methods were employed: the collection of the ion associate of CS⁺ with EB on a mixed cellulose ester (MCE) or PTFE membrane filter, the collection of the ion associate of CS⁺ with AS⁻ on a PTFE membrane filter followed by the ion exchange of AS⁻ with EB, and the first collection of CS⁺ followed by the second collection of EB on a PTFE membrane filter. For the determination of AS⁻, the collection of the ion associate of AS⁻ with CS⁺ on a PTFE membrane filter followed by the ion exchange of AS⁻ with EB was done. For the determination of NS, the ion associate of NS with EB was collected on a MCE membrane filter. The MCE membrane filter with the analyte was dissolved in methyl cellosolve. The analyte on the PTFE membrane filter was eluted with ethanol. The CS⁺ up to 5×10⁻⁷ M can be determined by the absorbance at 542 nm of the methyl cellosolve solution or the absorbance at 535 nm of the ethanol solution. The AS⁻ up to 5×10⁻⁷ M can be determined by the absorbance at 536 nm of the ethanol solution. The NS up to 2.53×10⁻⁶ M can be determined by the absorbance at 537 nm of the methyl cellosolve solution. This is the sensitive method for the determination of 10⁻⁸ to 10⁻⁷ M order of ionic surfactants and 10⁻⁷ to 10⁻⁶ M order of NS without toxic organic solvents.     

甲基绿选择性电极催化电位法测定茶叶中锰

根据在氨三乙酸存在下,Mn2+催化高碘酸根(IO-4)氧化甲基绿的反应,对用甲基绿选择性电极催化电位法测定痕量锰进行了研究.实验表明,该方法灵敏度高,测定锰的线性范围为3.0～100ng/25mL,选择性好,操作简单,温度控制方便.测定了几种茶叶样品中的锰,与原子吸收法比较,结果满意.     

钒(Ⅴ)催化氧化甲基紫的反应动力学及其应用

在 H2 SO4 介质中 ,以抗坏血酸为活化剂 ,痕量的钒 ( )可强烈地催化溴酸钾氧化甲基紫的反应 ,研究了反应的最佳条件及动力学参数 ,探讨了反应机理 ,建立了测定超痕量钒的高灵敏方法 ,方法的线性范围 0 .0～ 2 50 pg/m L ,检出限为 6.5×1 0 - 13g/m L。方法用于井水、蔬菜及血清中痕量钒的测定 ,获得令人满意的结果