导数-原子捕集-火焰原子吸收光谱法测定中草药中的微量铜

研究了在原有基础上对原子捕集装置的改进，并与导数原子吸收光谱法结合，使铜的测定灵敏度有较大提高。在10mV/min灵敏度档下，捕集时间为2min时，方法的检出限和特征浓度分别为0.52和0.85μg/L，分别较常规火焰原子吸收法改善1和2个数量级。利用该法成功测定了甘草、柴胡等10味中药中的微量铜，平均回收率为94.2%－104％。     

开缝石英管原子捕集原子吸收光谱法测定银

试验了空气和乙炔流量、缝管高度、捕集时间、溶液介质等对银灵敏度的影响。结果表明,分别用不同的乙炔流量进行原子捕集与释放可获得最高灵敏度。捕集1min,测得银的特征浓度为8.1×10~(-4)μg·ml~(-1),比常规火焰原子吸收法的灵敏度提高62倍,变异系数2.8％,本法测定了牡蛎中的银。     

悬浮液进样-火焰原子吸收光谱法测定中草药中的微量铜

将悬浮液进样技术应用于火焰原子吸收光谱法,建立了快速测定中草药中微量铜的新方法。将样品磨细,制成悬浮液,喷入空气－乙炔火焰,以空白溶液为参比,用氘灯进行背景和扣除,以标准加入法测定。测定结果与灰化法一致,两种方法的相对误差小于±３．６％,ＲＳＤ小于２．５％,检出限为０．０５７ｍｇ／Ｌ。     

微波溶样-火焰原子吸收光谱法测定人发中锌

锌是人体内主要且必需的微量元素之一。头发作为人体的一部分 ,其发锌含量的多少 ,可以不同程度的反映一个人的营养和健康水平。微波溶样技术是当前世界上最先进的样品预处理技术之一 ,将这一技术应用于发锌含量的测定 ,建立起系统的微波溶样 -火焰原子吸收分析方法 ,获得了满意的结果。该方法的运用对于临床诊断和营养调查有非常重要的作用。1　仪器与试剂AA- 670 1原子吸收分光光度计 (日本岛津公司 )MK- 1型微波溶样炉 (上海新科微波技术应用研究所 )锌标准储备液 :50 0 mg· L-1(中国预防医学会 )锌标准使用液 :取标准储备液 1 .0 0 m…     

萃取-富氧火焰原子吸收光谱法测定中草药中的钼

以水杨基荧光酮为络合剂 ,TritonX 1 0 0为析相剂 ,在pH 3 6的HAc NaAc缓冲溶液中和固体硫酸铵存在下 ,能很好地实现Mo (Ⅵ )与Fe (Ⅲ ) ,Zn (Ⅱ ) ,Cu (Ⅱ ) ,Ni (Ⅱ ) ,Mn (Ⅱ ) ,Cd (Ⅱ )等离子的分离 ,然后利用富氧空气 乙炔火焰原子吸收光谱法对中草药中的钼进行了测定。检出限为 1 0 4× 1 0 - 7g/mL ,线性范围为 5 0 0× 1 0 - 7～ 4 0 0× 1 0 - 5g/mL ,RSD <5 % ,回收率在98 8%～ 1 0 2 0 %之间。     

火焰原子吸收光谱法测定粗锌中的铜

建立火焰原子吸收光谱法测定粗锌中的铜含量。采用硝酸–酒石酸溶解样品,并以其为测定溶液介质,检测波长为324.7 nm,以水为参比,采用空气–乙炔火焰以原子吸收光谱仪进行测定。在优化的实验条件下,铜的质量浓度在0.10~2.50μg/m L范围内与吸光度有良好线性关系,相关系数为0.999 7,方法检出限为0.01μg/m L。测定结果的相对标准偏差为1.0%~3.0%(n=11),样品加标回收率为97%~102%。该方法具有灵敏度高,干扰少,重现性好等优点,适用于铜含量在0.001%~0.50%之间的粗锌中铜的测定。     

火焰原子吸收光谱法测定海水中微量铁和锌

海水中铁和锌为微量金属元素,在海水富营养化研究和赤潮调查的监测中,铁、锌是必测项目,但《海洋监测规范》中未见有关海水中铁的分析方法。     

中草药中铁锌钙的悬浮液进样-火焰原子吸收光谱法测定

将悬浮液进样技术应用于火焰原子吸收光谱法, 建立了中草药中微量元素的快速分析新方法。将样品粉碎、悬浮在琼脂胶体中制成悬浮液; 取适量样品悬浮液配制成试液, 喷入空气－ 乙炔火焰, 用标准加入法测定。 用该法成功地测定了当归、川芎及川乌中的铁、锌、钙, 测定结果与灰化法一致, 方法简便、快速、准确。     

单缝石英管原子捕集原子吸收光谱法测定了水中碲

研究了单缝石英管贫焰捕集－脉冲富焰释放原子捕集原子吸收光谱法测定碲的条件和线性范围;用Ｘ射线衍射分析得碲以Ｔｅ４Ｏ１１形式捕集,探讨了捕集、释放机理。测定质量浓度为２０μｇ／Ｌ的碲（Ⅵ）时,捕集１ｍｉｎ后测得特征质量浓度为１．７６×１０＾－３ｍｇ／Ｌ,比常规ＦＡＡＳ法提高１１３倍,相对标准偏差为２．６％,已用于饮用水样中痕量碲的测定。     

Determination of calcium, magnesium and zinc in lubricating oils by flame atomic absorption spectrometry using a three-component solution

Lubricating oils are used to decrease wear and friction of movable parts of engines and turbines, being in that way essential for the performance and the increase of that equipment lifespan. The presence of some metals shows the addition of specific additives such as detergents, dispersals and antioxidants that improve the performance of these lubricants. In this work, a method for determination of calcium, magnesium and zinc in lubricating oil by flame atomic absorption spectrometry (F AAS) was developed. The samples were diluted with a small quantity of aviation kerosene (AVK), n-propanol and water to form a three-component solution before its introduction in the F AAS. Aqueous inorganic standards diluted in the same way have been used for calibration. To assess the accuracy of the new method, it was compared with ABNT NBR 14066 standard method, which consists in diluting the sample with AVK and in quantification by F AAS. Two other validating methods have also been used: the acid digestion and the certified reference material NIST (SRM 1084a). The proposed method provides the following advantages in relation to the standard method: significant reduction of the use of AVK, higher stability of the analytes in the medium and application of aqueous inorganic standards for calibration. The limits of detection for calcium, magnesium and zinc were 1.3 μg g⁻¹, 0.052 μg g⁻¹ and 0.41 μg g⁻¹, respectively. Concentrations of calcium, magnesium and zinc in six different samples obtained by the developed method did not differ significantly from the results obtained by the reference methods at the 95% confidence level (Student's t-test and ANOVA). Therefore, the proposed method becomes an efficient alternative for determination of metals in lubricating oil.     

原子吸收光谱法测定苦藠中微量元素的含量

苦藠别名小野蒜是食用地下鳞茎及嫩茎叶的野生蔬菜,属药食同源的百合科多年生草本植物.有温中散结,宽胸通阳,祛湿止痢作用~([1,2]).在食疗方面有:(1)降脂作用,且性味辛温,能温阳散结,可用来治疗高胆固醇和高血脂症.(2)降低血压的奇妙作用,常食有通阳气、宽胸的效果.     

浊点萃取-火焰原子吸收光谱法测定水样中痕量铜的研究

提出了浊点萃取火焰原子吸收光谱法测定痕量铜的新方法。详细探讨了溶液pH，试剂浓度等实验条件对浊点萃取及测定灵敏度的影响，在最佳下，富集50mL样品溶液，用火焰原子吸收光谱法测定，铜的检测限为0.35μg/L，铜的富集倍率为71倍。方法用于自来水、河水及海水中痕量铜的测定。     

蒸气发生火焰原子吸收法测定面粉中的铜

用自制的蒸气发生装置,在强还原剂存在下,对铜蒸气的生成进行了详细研究,并通过该装置测定非蒸气发生元素镁和在络合剂掩蔽下测铜两种不同的方法进行了验证。对酸的种类及浓度、NaBH4溶液流速及浓度、反应管道长度的影响等实验参数和干扰情况进行了研究。用该方法测定了面粉中铜的质量分数,检出限为6μg L。     

Determination of cadmium and lead in reference materials by volatile species generation with in situ trapping flame atomic absorption spectrometry

The analytical performance of coupled volatile species generation-integrated atom trap (VSG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Cd and Pb in reference materials. Lead using formation of PbH₄ and Cd⁰ vapors are atomized in air-acetylene flame-heated IAT. A new design of VSG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube or an “integrated trap”) was investigated. A dramatic improvement in detection limit was achieved compared with that obtained using either of the above atom trapping techniques separately. The concentration detection limits, defined as 3 times the blank standard deviation (3σ), were 0.05 and 0.40 ng mL^− 1 for Cd and Pb, respectively. For a 120 s in situ pre-concentration time, sensitivity enhancement compared to flame AAS, was 500 and 575 folds for Cd and Pb, respectively, using volatile species generation-atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 4.4% and 4.1% (n = 6) for Cd and Pb, respectively. The designs studied include slotted tube, single silica tube and integrated atom trap-cooled atom traps. The accuracy of method was verified using certified reference materials (PLANTS 3 and IAEA/W-4) by standard addition calibration technique. The measured Cd and Pb contents in two reference materials were in satisfactory agreement with the certified values.     

Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

The analytical performance of coupled hydride generation — integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H₂Te vapors, is atomized in air–acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube or an “integrated trap”) was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3σ), was 0.9 ng mL^− 1 for Te. For a 2 min in situ pre-concentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation — atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The designs studied include slotted tube, single silica tube and integrated atom trap-cooled atom traps. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.     

火焰原子吸收光谱法测定锌合金中镁

建立火焰原子吸收光谱法测定锌合金中镁含量。选用10 mL盐酸溶液(1+1)溶解样品,加入5 mL质量浓度为100 g/L的LaCl3溶液,以消除铝对镁的化学干扰,在选定的仪器工作条件下进行测定。结果表明,镁的质量浓度在0~1.238 mg/L范围内与与吸光度具有良好的线性关系,相关系数为0.999 4,线性方程为Y=1.086 4X+0.018 5,方法测定下限为0.010 mg/L。样品测定结果的相对标准偏差为1.61%~3.45%(n=6),加标回收率为91.3%~94.7%。该方法准确度高,精密度好,满足锌合金中镁含量的日常检测要求。     

Preconcentration and determination of trace metals by flow injection micelle-mediated extraction using flame atomic absorption spectrometry

Micelle-mediated extraction/preconcentration is incorporated on-line into a flow injection system used to determine low levels of Cd(II), Co(II), Cu(II), Mn(II), Ni(II), Pb(II) and Zn(II) present in various samples. The analyte is complexed with HBDAP (N,N′-bis(2-hydroxy-5-bromo-benzyl)1,2-diaminopropane). Under optimal conditions, a solution of 30% (m/v) NaCl and a sample solution containing 2.5 mL of 1% (m/v) sodium dodecyl sulfate (SDS), 0.5 mL of 1.8 × 10⁻³ M HBDAP and 2.5 mL of pH 8.5 borate buffer solution in 25 mL were pumped through the cotton filled mini-column; onto which the surfactant-rich phase containing the complex is collected. A solution of 0.5 M HNO₃ in 50% acetone is used as the eluent. The limits of detection are (ng mL⁻¹) Cd = 0.39, Cu = 3.2, Co = 7.5, Mn = 3.0, Ni = 3.4, Pb = 17.9 and Zn = 0.89 if the sample is allowed to flow for 30 s, but improved for extended preconcentration periods. Analysis of liquid and solid reference materials showed good agreement with the certified values. Complex formation constants between HBDAP and these metal ions were also determined potentiometrically.     

悬浮液进样-火焰原子吸收光谱法测定百合中的微量元素梁保安

将处理后的百合研磨成粒度小于0.1 mm的粉状物, 加入稳定剂琼脂制成悬浮液, 用LaCl3和CsCl消除相关干扰, 采用标准加入法在同一试液中利用空气-乙炔火焰原子吸收光谱法测定Zn、 Mn、 Fe、 Cu、 Ca、 Mg、 K、 Na 8种元素. 结果表明, 兰州百合中Zn、 Mn、 Fe、 Cu、 Ca、 Mg、 K、 Na的质量分数分别是162.0、 5.0、 30.8、 8.4、 295.9、 574.2、 522.9、 291.6 μg/g. 加标回收率分别为: Zn 99.4%～100.5%、 Mn 98.0%～101.8%、 Fe 92.7%～97.5%、 Cu 99.9%～102.9%、 Ca 96.0%～100.0%、 Mg 93.3%～102.5%、 K 91.7%～103.8%、 Na 99.1%～105.0%. 以传统湿法的测定结果为参考对测定值进行t检验, 发现两者无显著性差异, 说明悬浮液进样法的测定结果准确可靠.     

Determination of cadmium, copper, lead and zinc in water samples by flame atomic absorption spectrometry after cloud point extraction

Cloud point extraction (CPE) has been used for the simultaneous pre-concentration of cadmium, copper, lead and zinc after the formation of a complex with 1-(2-thiazolylazo)-2-naphthol (TAN), and later analysis by flame atomic absorption spectrometry (FAAS) using octylphenoxypolyethoxyethanol (Triton X-114) as surfactant. The chemical variables affecting the separation phase and the viscosity affecting the detection process were optimized. At pH 8.6, pre-concentration of only 50 ml of sample in the presence of 0.05% Triton X-114 and 2×10⁻⁵ mol l⁻¹ TAN permitted the detection of 0.099, 0.27, 1.1 and 0.095 ng ml⁻¹ cadmium, copper, lead and zinc, respectively. The enhancement factors were 57.7, 64.3, 55.6 and 63.7 for cadmium, copper, lead and zinc, respectively. The proposed method has been applied to the determination of cadmium, copper, lead and zinc in water samples and a standard reference material (SRM).