直读光谱法测定纯金中银铜铁铅锑铋锌钯

研究了直读光谱法直接测定纯金中银、铜、铁、铅、锑、铋、锌、钯等杂质元素的分析条件,探讨了简易的制样技术。方法的检出范围为1×10~(-4)％～1×10~(-2)％,具有操作简便、快速准确、金消耗极少等特点。     

ICP-AES法测定锡铅焊料中铜铁镉锌铝铋

锡铅焊料试样经盐酸、硝酸分解后，加入一定量的硫酸沉淀分离基体铅，以盐酸一氢溴酸排锡后，采用ICP—AES法同时测定铜、铁、镉、锌、铝、铋。方法没有谱线和背景干扰，检出限铜为0．000034％，铁为0．000038％，镉为0．000026％，锌为0．000071％，铝为0．00025％，铋为0．00060％，回收率在91．09／5～99．2％之间。完全满足锡铅焊料中的铜、铁、镉、锌、铝、铋测定的要求。     

光电直读光谱法测定锡青铜中9种杂质元素

利用光电直读光谱仪快速测定了锡青铜中的9种杂质元素,通过调整工作曲线及其它影响测定的因素,最终确定了锡青铜的最佳分析条件,方法的相对标准偏差RSD为0.33%~4.4%,对标准样品的实际测定结果与标准值基本一致,精密度与准确度均能满足日常分析需求。     

直读光谱法测定铸铝115中硅铁镁锌铍

铝合金中化学成分测定常用比色法 [1,2 ]与滴定法 [1] ,这两种方法样品消耗量大 ,且需将样品转化成溶液 ,样品处理工作量大 ,预处理过程繁琐 ,耗时多 ,而且所用化学试剂多 ,化验成本偏高。光谱分析速度快 ,准确度高 ,单个样品从接样到报出结果所需时间不超过 1 0 min,是一种金属化学成分测定的快捷方法。但光谱分析对标准样品要求比较高 ,铸铝 1 1 5材料须分析硅、铁、镁、锌、铍五个元素 ,目前市场上的标样不能覆盖该材料 ,因此需要两套标样 ,本文采用ZLD1 0 1、LC4两套标样 ,用自制的控制试样 ,采取控样法分析铸铝 1 1 5样品 ,消除了因…     

直读光谱法测定铅基合金中铅砷钙铜锑硒锡

叙述了应用直读光谱仪测定蓄电池用铅基合金的方法及效果,其精密度和准确度完全能满足同行业生产和科研需要。     

X-射线荧光光谱法测定锌铝铜合金中的铝、铜、铁、硅、镍、铅和镉

建立了X射线荧光光谱法测定锌铝铜合金ZnAl6Cu1中铝、铜、铁、硅、镍、铅和镉的分析方法。探讨了各元素的分析条件,比较了不同制样方式及不同放置时间对铝强度的影响。在最佳的仪器分析条件下,测定了微量元素的检出限及主、次元素的精密度和准确度。检出限结果表明:各微量元素的检出限均满足标准要求,Cd和Pb元素的定量限稍高。精密度和准确度结果表明,铝、铜、铁元素的测量相对标准偏差在2.1%~5.9%,分析结果与国家标准方法一致。     

光电直读光谱法测定锡青铜中的9个元素

利用光电直读光谱仪快速测定锡青铜中的9个元素,通过实验确定了锡青铜的分析条件,进而利用锡青铜标准样品绘制工作曲线。回测标准样品及已知含量的锡青铜样品,根据标准样品值调整工作曲线参数,使标准样品实际测定值与标准值相一致,精密度与准确度测试均满足日常分析需求。     

直读光谱法测定中低合金钢中氮的含量北大核心CSCD

中低合金钢中的氮是一种有害元素,高氮会导致钢韧性下降[1].冶炼品种钢需要添加钒氮合金,目前氧氮分析仪测定单个样品需要12 min,不能满足在线检验的及时性要求,而直读光谱仪6 min内便可同时测定含氮在内的十几种元素.目前实验室使用的直读光谱仪具备氮的分析通道,能够满足工序快速检验的要求,但低合金钢中氮含量属于mg·kg^(-1)级,外界条件对低合金钢中氮的测定结果影响较大[2],本工作对制样方式、火花台冷却方式、氩气纯度和压力等因素进行探讨,提出了直读光谱法测定中低合金钢中氮含量的方法,并应用到实际生产过程中.     

ICP-AES法测定锌阳极中的铝、镉、铁、铜、铅

通过分析高频功率、雾化压力、辅助气流量和泵速等试验条件，建立了ICP-AES法测定锌阳极中铝、镉、铁、铜、铅的方法。用该方法测定锌阳极中的铝、镉、铁、铜、铅，其RSD分别为0.17%、0.63%、2.7%、5.2%、2.5%，回收率分别为99.3%-101.2%，99.3%-100.3%、97.1%-102.2%、97.8%-102.9%。对锌阳极试样进行测定，该方法的测定结果与GB4951-85方法的测定结果基本一致。     

火花直读光谱法测定铝及铝合金中的钒含量

通过对测定条件的优化,采用高钒系列标准样品建立分析程序,完成类型标准化,校验后再进行测定,建立了火花直读光谱法对铝及铝合金中的钒含量进行测定的方法。选用E2235高钒标准样品进行标准化,所得测定值与标准值基本一致,相对标准偏差为2.9%(n=8)。结果表明,当测定元素含量不超过0.020%时,方法准确、可靠,适合于铝及铝合金中微量钒含量的测定。     

三元硝酸盐预氧化熔融制样-波长色散X射线荧光光谱法测定锌精矿中锌、铜、铅、铁、铝、钙和镁

锌精矿属富锌、高铜、高铅的硫化矿矿物,硫和铜等元素腐蚀铂金坩埚是熔融制样-X射线荧光光谱分析必须解决的问题.在阶梯温度下,以硝酸铵、硝酸钠和硝酸锂的三元硝酸盐混合物为氧化剂,采用半熔法预氧化试料中的硫、铜、锌等元素,以四硼酸锂-偏硼酸锂混合熔剂(m:m=67:33)为熔剂、过饱和溴化锂溶液为脱模剂,于1050℃熔铸成X...     

The determination of cadmium,copper, iron,lead and zinc in aerosols by atomic-absorption spectrometry

The determination of five elements in filter papers loaded with air particulate matter has been investigated. After a wet destruction of about 10 cm² of filter material by a standard procedure, analysis was carried out with a flame atomic absorption method for zinc and a flameless procedure for Cd, Cu, Fe and Pb. Furnace program parameters for each of the elements in different acid solutions are reported. The interferences of some common anions and the most abundant cations in aerosol material are described. For some urban and industrial samples, the results are compared with those obtained by energy-dispersive x-ray fluorescence. Accuracy was checked against standard samples.     

电感耦合等离子体原子发射光谱法测定铅锌选矿流程原尾矿中铅锌铜

用5mL氟化氢铵(50g/L)、10mL盐酸、5mL硝酸、5mL高氯酸分解0.1g样品,盐酸(3%,V/V)为测定介质,定容在250mL容量瓶中,直接用电感耦合等离子体原子发射光谱法测定铅锌选矿流程原尾矿中的铅、锌、铜3种元素。根据分析线的选择原则,结合待测元素的检测范围,选择无干扰、峰形对称、灵敏度适中的谱线Pb 220.353nm、Zn 213.856nm、Cu 324.754nm作为分析线。各元素的质量浓度在一定范围内与其发射强度呈线性,校准曲线的线性相关系数均大于0.999 9,方法中各元素检出限为0.066～0.51ng/mL。方法经国家标准物质分析验证,测定值与认定值相符。按照实验方法测定铅锌选矿流程原尾矿中铅、锌、铜,测试结果与火焰原子吸收光谱法测定结果一致。     

Determination of lead, cadmium, zinc, copper, and iron in foods by atomic absorption spectrometry after microwave digestion: NMKL Collaborative Study

A method for determination of lead, cadmium, zinc, copper, and iron by atomic absorption spectrometry (AAS) after microwave digestion was subjected to a collaborative study in which 16 laboratories participated [including users of inductively coupled plasma (ICP) and ICP-mass spectrometry (MS)]. The types of samples included in the study were minced fish, wheat bran, milk powder, bovine and pig liver, mushroom, 2 simulated diets, and bovine muscle; the last 4 were certified reference materials. These were analyzed as single (4 samples), double blind (1 sample), or split level (2 samples) samples. Before the collaborative study, a pretrial was conducted in which 4 ready-made solutions and one fish tissue sample were analyzed for Pb and Cu. The reproducibility relative standard deviation (RSDR) values, for results above the detection limit, ranged from 59% at 0.155 mg/kg to 16% at 1.62 mg/kg for Pb, from 28% at 0.0124 mg/kg to 11% at 0.482 mg/kg for Cd, from 9.3% at 35.3 mg/kg to 1.7% at 147 mg/kg for Zn, from 39% at 0.241 mg/kg to 3.0% at 63.4 mg/kg for Cu, and from 17% at 7.4 mg/kg to 5.9% at 303 mg/kg for Fe. The RSDR values agreed well with the norms described by the International Union of Pure and Applied Chemistry. As a complement to the AAS determinations, a number of laboratories analyzed the samples either by ICP or by ICP-MS. The results of these analyses agreed well with the AAS results. On the basis of the results of the collaborative study, the method was adopted Official First Action by AOAC INTERNATIONAL.     

Determination of copper, lead, cadmium, zinc, and iron in calcium fluoride and other fluoride-containing samples by means of direct solid sampling GF-AAS

Direct solid sampling graphite furnace AAS (SS-GF-AAS) provides an advantageous alternative to the conventional AAS which requires wet digestion of the samples. This method is suitable for trace element determination in calcium fluoride and other fluoride-containing samples. Matrix effects were studied by using calibration standards, certified reference materials with different matrices and by means of three-dimensional calibration. 3D calibration is suitable for selection of calibration samples for more reliable analyses. Cu, Pb, Cd, Zn, and Fe were determined by means of calibration with variation of sample weight using certified reference materials and suitable fluoride-containing calibration samples. Received: 25 July 1997 / Revised: 15 December 1997 / Accepted: 20 December 1997     

Determination of copper, lead, cadmium, zinc, and iron in calcium fluoride and other fluoride-containing samples by means of direct solid sampling GF-AAS

Direct solid sampling graphite furnace AAS (SS-GF-AAS) provides an advantageous alternative to the conventional AAS which requires wet digestion of the samples. This method is suitable for trace element determination in calcium fluoride and other fluoride-containing samples. Matrix effects were studied by using calibration standards, certified reference materials with different matrices and by means of three-dimensional calibration. 3D calibration is suitable for selection of calibration samples for more reliable analyses. Cu, Pb, Cd, Zn, and Fe were determined by means of calibration with variation of sample weight using certified reference materials and suitable fluoride-containing calibration samples. Received: 25 July 1997 / Revised: 15 December 1997 / Accepted: 20 December 1997     

Determination of iron,cobalt, nickel,manganese, zinc,copper, cadmium and lead in human hair by inductively coupled plasma-atomic emission spectrometry

A method was standardized for the dissolution of hair samples and analysis was carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES). Hair samples were brought into solution by using a mixture of nitric acid and hydrogen peroxide. Various parameters that influence the sample preparation, namely temperature, digestion time and ratio of acid mixture were studied and standardized. The optimized method has been employed to digest standard reference materials and hair samples of residents of India, collected from different age groups and sex, and analyzed for Fe, Co, Ni, Mn, Zn, Cu, Cd and Pb. The values agree for most of the metals with the data reported for human hair samples of residents of India. The NIES CRM Human Hair No. 5 and IAEA Reference Hair HH-1 certified reference materials were used in order to verify the accuracy of the method and the results were in excellent agreement with the certified values.     

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).     

半密闭酸溶-电感耦合等离子体质谱（ICP-MS)）法测定化探样品中的铬镍铜锌镉铅6种重金属

采用半密闭酸溶消解法处理样品,选择离线校正的方式校正了Sn对Cd的同量异位素的干扰,增加积分时间和读数次数提高了Cd的准确度和精密度,建立了电感耦合等离子体质谱仪（ICP-MS）测定化探样品中Cr、Ni、Cu、Zn、Cd、Pb六种重金属元素的方法。对前处理方法和仪器的参数条件进行了优化,结果表明,半密闭体系可达到回流的目的,样品分解完全且无污染现象,在最优的实验条件下,标准曲线的相关系数均不小于0.9997,检出限为0.019~1.65 μg/g ,测定下限为0.057~4.95 μg/g 。按照实验方法对岩石、水系沉积物和土壤国家标准物质中Cr、Ni、Cu、Zn、Cd、Pb平行测定12次,各元素的测定结果与认定值基本一致,相对偏差均不大于3.55%,相对误差均不大于 10.34% 。采用实验方法对土壤样品进行分析,测定结果与四酸溶解-ICP-OES测定Cr、Ni、Cu、Zn、Pb,火焰-石墨炉原子吸收法测定Cd的结果基本吻合。