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1.
在对各元素的分析谱线的选择及基体元素镍对相关元素测定的干扰作了系统研究的基础上,提出用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定镍基高温合金中铬、钛、铌、铝、铁及硼6种合金元素的方法。上述6种元素的检出限(3s/k)在0.006 9~0.13 mg.L-1范围内。取GH 33镍基高温标准样品按所提出方法分析,测定值与标准值相互一致,测得相对标准偏差值(n=10)均小于1.5%。在基体镍溶液中加入各被测元素的标准溶液做回收试验,上述6种元素的回收率在98.3%~101.0%之间。为对此方法的准确性作进一步考核,对GH 4145高温镍基合金样品进行分析,各元素的测定值与国家标准方法的测定值相符合。  相似文献   

2.
采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了高纯氧化钇铕中13种杂质稀土元素。取样品1.000 0 g溶于盐酸10 mL中,加水定容至100 mL,供ICP-AES分析,选定了所测定的13种杂质稀土元素的分析谱线。测定中所选用的仪器工作参数为:①冷却气流量12 L.min-1;②护套气流量0.20 L.min-1;③载气流量3.0 L.min-1;④高频发生器频率40.68 MHz,功率1.1 kW;⑤观测高度10~12 mm。用标准加入法对方法的回收率及精密度作了试验,所得回收率在78.5%~99.6%之间;测定值的相对标准偏差(n=11)在0.02%~0.94%之间。  相似文献   

3.
报道了硅铁中锰、钙、铝、铬及铜五元素的电感耦合等离子原子发射光谱法(ICP-AES)同时测定方法.对仪器的工作条件和各元素分析谱线的选择进行了试验和优化.通过对多个硅铁标准样品的分析,证实了方法的可行性,所得测定结果与标准值一致.回收率试验所得结果在99.0%~105.0%之间.  相似文献   

4.
采用电感耦合等离子体原子发射光谱(ICP-AES)法同时测定工业废水中铅、镉、铬和砷。对仪器的工作参数和被测元素的分析谱线进行了优化和选择。方法的检出限依次为0.008,0.002,0.007,0.015 mg.L-1。在质量浓度为0.489 mg.L-1(Pb),0.086 6 mg.L-1(Cd),0.231 mg.L-1(Cr)及0.395 mg.L-1(As)的水平上按试验方法测定8次,作了精密度试验,测得相对标准偏差值依次为1.71%,1.22%,0.95%及1.40%。在两个废水样品的基础上作了加标回收试验,所得结果在95.4%~104.6%之间。  相似文献   

5.
电感耦合等离子体发射光谱法测定低合金钢中痕量硼   总被引:1,自引:0,他引:1  
研究了用标准加入法、电感耦合等离子体发射光谱法(ICP-AES)测定低合金钢中痕量硼的方法,对试样溶样方法、元素分析谱线、共存元素干扰、背景校正、仪器分析最佳条件等因素进行了研究.试验结果表明,在选定的最佳条件下测定,硼的检出限为0.002 mg·L-1,相对标准偏差小于2%,加标回收率为95.0%~108.6%.  相似文献   

6.
采用碱熔再酸化分解样品,电感耦合等离子体原子发射光谱(ICP-AES)法测定高铁土壤中的铝(Al)元素。通过逐级扩大线性范围的方式,选取测定高含量Al的合适谱线;在标准中逐级加入铁基体,考察了铁基体浓度从20μg/mL到80μg/mL时对测定Al的各谱线的干扰情况。用ICP-AES法对国家标准物质GSS-1、GSS-2、GSS-3、GSS-4、GSS-5进行测定,测定值与认定值的相对误差(RE)在-0.37%~0.31%,相对标准偏差(RSD,n=5)为0.26%~0.75%,获得了满意结果。  相似文献   

7.
用硝酸及少量氢氟酸可将试样完全溶解,所得溶液可用于电感耦合等离子体原子发射光谱法(ICP-AES)或钼蓝分光光度法测定镁和镁合金中的硅含量,对ICP-AES测定硅的分析条件作了试验.为避免各共存元素的干扰,方法中选择波长为Si Ⅰ 251.611 nm及Si Ⅰ 212.412 nm的谱线作为分析谱线.在制作工作曲线时加入与待测样品等量的镁以补偿基体组分引起的基体效应,在选用上述两谱线作为分析线时,硅的质量浓度在40.0 mg·L-1以内时与谱线的发射强度均呈线性关系,所得检出限(3S/N)依次为6.2和15μg·L-1.应用此方法分析了3种镁合金标准样品,所得结果与标准值相符.  相似文献   

8.
采用碱熔再酸化分解样品,电感耦合等离子体原子发射光谱(ICP-AES)法测定高铁土壤中的铝(Al)元素。通过逐级扩大线性范围的方式,选取测定高含量Al的合适谱线;在标准中逐级加入铁基体,考察了铁基体浓度从20μg/mL到80μg/mL时对测定Al的各谱线的干扰情况。用ICP-AES法对国家标准物质GSS-1、GSS-2、GSS-3、GSS-4、GSS-5进行测定,测定值与认定值的相对误差(RE)在-0.37%~0.31%,相对标准偏差(RSD,n=5)为0.26%~0.75%,获得了满意结果。  相似文献   

9.
称取镍基单晶高温合金0.100 0g于聚四氟乙烯烧杯中,先令其与盐酸9mL和硝酸1mL加热反应,待反应缓慢时滴加氢氟酸2mL并继续加热使样品完全溶解。加入500g·L^-1酒石酸溶液2mL,冷却至室温,在塑料容量瓶中加水定容至100.0mL。按仪器工作条件采用电感耦合等离子体原子发射光谱法测定其中5种合金元素(Mo、W、Ta、Re、Ru)的含量,选择分析谱线依次为204.598,207.911,240.063,197.312,240.272nm。结果发现:除了Re外,其余4种元素的测定中均受共存元素的光谱干扰,严重影响了测定结果的准确性。为克服其干扰,除了采用基体匹配法消除镍的基体干扰外,试验采用混合校正系数矩阵法对测定结果进行校准。通过一系列试验计算得到混合校准系数矩阵K,并应用于模拟样品的分析。结果表明:经过矩阵K的校准,所测定的5种元素的准确度显著提高,达到了消除共存元素之间光谱干扰的目的。通过精密度试验,测得上述5种元素测定值的相对标准偏差(n=11)均在1.5%以下,并通过标准加入法进行回收试验,测得5种元素的回收率为97.0%~105%。  相似文献   

10.
对电感耦合等离子体原子发射光谱法(ICP-AES)测定储氢合金中8项元素(镍,镧,锰,铝,钴,镨,钕及铈)的分析条件(包括试样溶液的酸度,基体元素的干扰及其消除和分析谱线的选择等)作了研究和优化。在制备校正曲线时采用基体匹配法消除了基体干扰。应用所提出的方法测定了实样中8项元素,测定结果的相对标准偏差值在0.25%~0.71%之间。  相似文献   

11.
用4%醋酸溶液浸泡取自不锈钢食用器皿钢片样品,在室温条件下浸泡24h,将浸泡液按6:1浓缩.通过优化试验确定实验条件,用电感耦合等离子体发射光谱仪准确测定浸泡液中Cr、Ni、Cd的浓度.实验过程操作简单,多种元素同时测定节约试验时间.精密度试验和回收率试验说明该方法检测结果准确可靠.  相似文献   

12.
Cadmium in polyethylene was determined by both inductively coupled plasma atomic emission spectrometry (ICP-AES) and atomic absorption spectrometry (AAS) with continuous-flow gas-phase sample introduction in a reaction medium of ascorbic acid. In the presence of mixture of cobalt and thiourea in the ascorbic acid solution, the sensitivities by both ICP-AES and AAS for cadmium were greatly enhanced. The gaseous cadmium species was phase-separated in a gas–liquid separator and directed via a stream of argon carrier gas to an inductively coupled plasma and an electrically heated quartz tube atomizer (QTA) for atomic spectrometry. Under the optimized experimental conditions, the best attainable detection limits at Cd I 228.802 nm line were 1.3 and 0.017 ng/ml with linear dynamic ranges of 10–500 ng/ml and 0.1–1 ng/ml in concentrations by ICP-AES and QTA-AAS, respectively. The instrumental precisions expressed as the relative standard deviation (R.S.D.) from ten replicate measurements of 50 and 1 ng/ml cadmium by ICP-AES and QTA-AAS were 5.6% and 3.2%, respectively. With the use of ICP-AES and QTA-AAS with gas-phase sample introduction method, six- and 200-fold improvements in detection limits for cadmium were obtained in comparison with their conventional solution nebulization methods, respectively. After the effects of several diverse elements on the determination of cadmium by ICP-AES and QTA-AAS with the present gas-phase sample introduction systems were examined, these methods were applied to the determination of low concentrations of cadmium in polyethylene. The results obtained by the present method were in good agreement with the certified values.  相似文献   

13.
样品用四酸(盐酸+硝酸+高氯酸+氢氟酸)溶解,经阳离子交换树脂分离富集后用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定其中的15种的稀土元素。选用HCl(1.2mol/L)作平衡液和淋洗液,HCl(4.0mol/L)作洗脱液进行实验,测量时选择最佳的分析谱线从而避开杂质峰的干扰。各稀土元素的方法检出限均低于1.5μg/g,相对标准偏差小于11%。经标准物质验证结果可靠,适合地质样品中稀土元素的同时测量。  相似文献   

14.
建立微波消解–电感耦合等离子发射光谱(ICP–AES)测定贵州梵净山特色药用植物中Ni,Cd,As,Co等22种元素含量的方法。以硝酸–过氧化氢(3∶1)为消解体系,样品经微波消解后,用ICP–AES法对厚朴皮与厚朴根、野生艾纳香和人工种植艾纳香中22种元素含量及其差异进行分析。仪器工作条件:RF功率为1.25 k W,等离子体气流量为15.1 L/min,辅助气流量为1.0 L/min,雾化器气体流量为0.6 L/min。各元素在检测范围内有良好的线性,线性相关系数为0.986 7~0.999 6,检出限在0.001 2~0.012 3μg/g之间;加标回收率在95.55%~102.4%之间,测定结果的相对标准偏差为0.8%~3.6%(n=5)。该方法快速、准确、可靠,可用于药用植物样品中的微量元素分析。  相似文献   

15.
提出了电感耦合等离子体原子发射光谱法(ICP-AES)测定钒铁中硅、磷、铝、锰、镍、铬、铜、钛共8个杂质元素含量的方法。钒铁样品(0.5000g),先后加入50%(体积分数)硝酸溶液20mL及50%(体积分数)盐酸溶液10mL,在100℃左右加热溶解,溶解过程中应注意保持溶液体积在25mL左右。将溶液过滤并置于200mL容量瓶中作为母液留用。将滤纸及不溶物一并移入铂坩埚中,置于马弗炉中,先于250℃灰化20min,稍冷后加入无水碳酸钠和硼酸(质量比2∶1)组成的混合熔剂0.3g,升温至950℃融熔15min。冷却,用体积比1∶10的盐酸溶液10mL浸出熔块,将此溶液与上述母液合并并加水定容至200mL。此溶液供ICP-AES在仪器工作条件下进行分析。绘制校准曲线时,加入纯铁和五氧化二钒作为基体,以消除基体干扰,然后加入上述8种元素的标准溶液,并按上述溶液最终稀释体积条件和仪器工作条件制作曲线(R大于0.999)。为验证所提出的分析方法的测定数据的精密度,约请了10个实验室对8个不同含量水平的钒铁样品对方法作协同试验,按GB/T 6379.2-2004所规定的方法求算了重复性标准偏差Sr和重复性限r,以及再现性标准偏差SR和再现性限R,并求得所测定的8种元素在各自的测定范围内的r与w之间和R与w之间的函数关系,说明该方法有较好的稳定性和准确性,而且证明此方法是可行的。  相似文献   

16.
Trace impurities in lead-tin solders were determined using inductively coupled plasma atomic emission spectrometry (ICP-AES) for the forensic discrimination of solder samples from different origins by a comparison of the concentration for each element. After about 10 mg of sample was accurately measured and taken into a glass tube, 1 ml of HNO3 was added. The tube was capped and heated at 80 degrees C for 10 min. After cooling to the room temperature, 1 ml of HCl and 2 ml of purified water were added. It was then agitated until the sample was completely dissolved, followed by dilution to 10 ml. Five elements (Sb, Bi, Cu, As and Ag) in this solution were determined by ICP-AES. The observed values for these elements in the NIST Standard Reference Material 1131 showed good agreement with the certified ones. Eighteen kinds of solder samples could be distinguished from each other, since all of the pairs among these samples provided remarkable difference in the concentration of the trace elements. The copper concentration should have been excluded from the comparison when it increased after melting by a soldering iron made of copper.  相似文献   

17.
A PC-controlled on-line preconcentration system (TRACECON) developed by Knapp et al. [11], was connected to a JY-70 Plus simultaneous ICP spectrometer to preconcentrate on-line seven trace elements (Cu, Fe, Zn, Cr, Ni, Mn, V) in biological and environmental samples. EDTrA-cellulose was used as column material. The elemental concentrations were determined by simultaneous ICP-AES. The effect of pH of the sample solution on the enrichment was studied. It was found that the recoveries of chromium and iron depend strongly on the pH of the sample solution. All the elements mentioned were recovered quantitatively at pH 4.0±0.1. The flow rates of sample solution and element solution were optimized. The enrichment factors for seven elements at 5 ml loading volume range from 3.9 for Cu to 7.9 for Zn. The detection limits of all seven elements were improved. The accuracy of the method was tested by the analysis of a number of CRMs of NIST, BCR and NIES. Most results are in good agreement with the certified values.On leave from Shanghai Institute of Metallurgy, Academia Sinica, Shanghai 200050, People's Republic of China  相似文献   

18.
人参和五灵脂配伍的无机元素含量测定   总被引:1,自引:0,他引:1  
采用电感耦合等离子体发射光谱法(ICP-AES)测定了人参和五灵脂配伍的无机元素含量。结果表明,人参和五灵脂及其合煎液中的铝含量均低于人参单煎液,人参和五灵配伍可减少有害元素铝的溶出;配伍合煎液中钙、硒、钼、钴、镁、铜、锰等有益元素的含量均高于人参单煎液。  相似文献   

19.
Microwave-acid digestion (MW-AD) followed by inductively coupled plasma-atomic emission spectrometry (ICP-AES), graphite furnace atomic absorption spectrometry (GFAAS), and hydride generation atomic absorption spectrometry (HGAAS) were examined for the determination of various elements in coal and coal fly ash (CFA). Eight certified reference materials (four coal samples and four CFA samples) were tested. The 10 elements (As, Be, Cd, Co, Cr, Mn, Ni, Pb, Sb, and Se), which are described in the Clean Air Act Amendments (CAAA), were especially considered. For coal, the HF-free MW-AD followed by ICP-AES was successful in the determination of various elements except for As, Be, Cd, Sb, and Se. These elements (except for Sb) were well-determined by use of GFAAS (Be and Cd) and HGAAS (As and Se). For CFA, the addition of HF in the digestion acid mixture was needed for the determination of elements, except for As, Sb, and Se, for which the HF-free MW-AD was applicable. The use of GFAAS (Be and Cd) or HGAAS (Sb and Se) resulted in the successful determination of the elements for which ICP-AES did not work well. The protocol for the determination of the 10 elements in coal and CFA by MW-AD followed by the joint-use of ICP-AES, GFAAS, and HGAAS was established.  相似文献   

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