电感耦合等离子体原子发射光谱(ICP-AES)法测定石灰中二氧化硅和磷含量

以电感耦合等离子体原子发射光谱(ICP-AES)法测定石灰中二氧化硅和磷含量,通过实验对仪器进行优化,确定分析谱线、称样量等分析条件,采用标准溶液绘制校准曲线,通过标准样品验证,加标回收率在101%～113%,相对标准偏差为0.004%～0.006%(n=5)。方法实用,结果满意。     

电感耦合等离子体发射光谱法测定低合金钢中痕量硼

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%.     

电感耦合等离子体原子发射光谱法测定食用菌中微量元素

采用高压消化罐在较低温度下进行缓慢样品消化,减少了消化过程中微量元素的损失.用电感耦合等离子体原子发射光谱法测定了野生元蘑和珍珠菇中钙、钠、钾、镁、锰、钡、铁、钴、锗、铜等微量元素的含量,并比较了湿法消化的结果,两种方法无显著性差异.方法的相对标准偏差在0.28%～2.96%之间,回收率在96.4%～104.0%之间.     

电感耦合等离子体发射光谱法测定铋黄铜合金中微量元素

利用ICP-AES(电感耦合等离子体发射光谱仪)研究了铋黄铜合金中铋、锑、铅、砷、铝、铁元素的测定方法,对仪器参数、分析谱线、干扰情况等因素进行了研究,确定了合适的谱线,并对铋黄铜合金进行精密度和回收实验。结果表明,相对标准偏差小于5%,回收率在94%～106%。     

电感耦合等离子体发射光谱法测定明胶中痕量元素

应用电感耦合等离子体发射光谱技术，建立了定量测定明胶中铁等13种微量元素的方法。采用湿法消解对明胶样品进行了前处理。讨论了ICP-AES同时测定明胶中13种微量元素时，利用功能强大的化学工作站对物理干扰和光谱干扰、背景进行消除。结果表明，此法准确、快速，检出限低，相对标准偏差及回收率均较好。被测元素工作曲线的线性相关系数≥0.9995。     

电感耦合等离子体原子发射光谱法测定玻璃中总硫

应用电感耦合等离子体原子发射光谱法(ICP-AES)测定了玻璃中总硫量。对测定条件,包括试样的溶解方法,分析谱线的选择,共存元素的光谱干扰及仪器的工作参数等作了系统研究。测定中选择了在紫外区的谱线(S 181.972 nm)作分析线可有效地避免了基体中大量钙的干扰。选取5件标准样品或已知样品按所提出方法各进行5次分析,算得方法的RSD值均小于1.5%,进行11次空白试验,算得方法的检出限(3S)为0.01 mg.L-1。通过对两件标准参考物质(NBS 89和GBW 03117)及一件已知样品的分析,验证了方法的准确度,所得测定结果与证书值或已知值相符。     

电感耦合等离子体原子发射光谱法测定8种蔬菜中微量元素

将电感耦合等离子体原子发射光谱法(ICP-AES)应用于 8 种蔬菜中钙、铝、铜、铁、锰、锌、铬、汞、磷、硒、镁、砷、镉、铅、钾、钠等16种微量元素的测定.方法中给出了仪器的工作条件,并叙述了分析谱线的选择,采用微波加热方法对试样进行消解.16 种微量元素的检出限在 0.3～30.0 μg·L-1之间,经试验得出各元素的回收率在 94.3%～104.8%之间.     

水和氯化铵提取-电感耦合等离子体发射光谱(ICP-AES)法测定石灰性土壤中交换性钾钠钙镁

为了提高石灰性土壤中交换性钾钠钙镁的分析效率及分析准确度,本文创新性采用水和氯化铵对石灰性土壤进行处理,并采用振荡交换、离心分离的方式进行石灰盐清洗、钾钠钙镁离子交换提取,提取液直接在电感耦合等离子体发射光谱仪(ICP-AES)上测定。该方法交换性盐基钙、镁、钾、钠的检出限分别为0.01、0.009、0.004、0.012cmol/kg。用国家一级标准物质GBW07498-新疆棕漠土和新疆地区石灰性土壤进行验证,方法精密度均小于5%,回收率在97％~105%。方法适用于石灰性（碱性）土壤（特别是新疆土壤）样品中交换性钾、钠、钙、镁的分析测定。     

电感耦合等离子体原子发射光谱法测定铸造铝合金中磷含量

提出了电感耦合等离子体原子发射光谱法测定铸造铝合金中磷含量的方法。铸造铝合金称样0.500 0g,用硝酸(1+1)溶液12mL和氢氟酸4mL溶解。选择波长为213.618nm谱线作为测定磷的分析线。磷的质量浓度在4.00mg·L-1以内与其发射强度呈线性关系,方法的检出限(3s/k)为0.020mg·L-1。方法用于分析5个铸造铝合金标准物质,测定值与认定值相符,相对标准偏差(n=6)在0.43%～2.2%之间,回收率在94.0%～109%之间。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定H-ZF类光学玻璃中锑含量

采用ICP-AES检测H-ZF类玻璃中锑含量,对共存元素产生的光谱干扰进行校正,并运用离峰扣除背景消除玻璃基体钛铌的干扰。建立简单可靠的测试分析方法,回收率为95-110%,相对标准偏差≤2%,适合日常的快速分析的需要。     

Determination of phosphorus in fertilizers by inductively coupled plasma atomic emission spectrometry

An inductively coupled plasma atomic emission spectrometry (ICP-AES) method was developed for the determination of phosphorus in fertilizers. Total phosphorus, direct extraction available phosphorus (EDTA), and water-soluble phosphorus, reported as phosphorus pentoxide (P205), in 15 Magruder check fertilizers were measured by ICP-AES, and the results were compared with those obtained by the AOAC official method. Five analytical wavelengths of phosphorus, 177.499, 178.287, 213.618, 214.914, and 253.565 nm, were tested for the determination of phosphorus in fertilizers, and their detection limits were obtained. Acid effects of perchloric acid and possible matrix effects of aluminum, calcium, magnesium, potassium, and sodium were negligible for phosphorus determination. Wavelength 213.618 nm was the best analytical wavelength for phosphorus determination by all 3 sample preparation methods for the selected Magruder fertilizers. The results demonstrated that the accuracy and precision of the ICP-AES method were comparable with those of the official methods.     

电感耦合等离子体发射光谱法检测镍基/钴基高温合金中硼磷硅

采用一定比例的混合酸溶解样品,利用基体匹配配制一系列标液消除基体的影响,以及轴向观测喷嘴吹扫技术来提高待测元素的灵敏度,使用电感耦合等离子体发射光谱(ICP-OES)测定镍基/钴基高温合金中硼磷硅。各元素选的分析线依次为B 182.577 nm、P 178.222 nm、Si 185.005 nm。检测范围分别是：B：0.001%-3.0%,P：0.003%-0.20%,Si：0.005%-3.0%,检出限范围是0.00005%-0.0004%,线性相关系数>0.9995。加标回收率为90.0%-105.0%,精密度RSD<2.0%。该方法操作简单快速,结果令人满意。     

电感耦合等离子体发射光谱法测定高纯铝中硅

建立电感耦合等离子体发射光谱(ICP-AES)法测定高纯铝中硅元素的分析方法。样品采用碱溶法进行预处理,以氢氧化钠溶液溶解,再加入盐酸、硝酸酸化。选取了硅251.611 nm分析谱线进行分析。硅的质量分数在0.001%~0.01%范围内与光谱强度具有良好的线性关系,线性相关系数为0.9991。该方法检出限为0.00012%,测定结果的相对标准偏差不大于10.2%(n=8),加标回收率为93.2%~104.2%。该方法操作简便,测定结果准确、可靠,适用于快速检测高纯铝中硅元素,具有推广价值。     

Determination of titanium dioxide in foods using inductively coupled plasma optical emission spectrometry

Titanium dioxide is a common food additive of increasing interest in dietary intake studies and dietary exclusion studies. Food labelling for titanium dioxide is imprecise so a method was developed for its rapid determination in foods using acid digestion and inductively coupled plasma optical emission spectrometry (ICPOES). Twenty-five foods thought to contain titanium dioxide were obtained. Based on preliminary digestion studies, samples (500 mg) were digested in 18 mol l-1 H2SO4 at 250 degrees C for 1 h and then diluted to 5.9 mol l-1 H2SO4 before determination of titanium by ICPOES at 336.121 nm. Emission intensity was suppressed by H2SO4 so standards were matched for acid concentration. Titanium dioxide embedded in gelatine was used to assess accuracy. A standard reference material of known titanium concentration and six foods of known titanium dioxide content were used as external reference materials. Limits of detection were 2-7.5 ppb, depending on spectral integration times, and the signal was linear up to 5 ppm. Results for all control samples were in good agreement with the expected values. Twelve of the foods contained detectable titanium, ranging from 0.001 to 0.782% by weight, but only eight indicated this on their labels, four being exempt under food labelling regulations. Based on food portion sizes, an individual's daily intake of titanium dioxide could exceed 200 mg from just one of these products. This method may facilitate future studies on titanium dioxide intake, given the present limitations of food labelling.     

Determination of total dissolved phosphorus in water samples by axial inductively coupled plasma atomic emission spectrometry

A procedure was developed to determine total dissolved phosphorus in groundwater-like samples using axial ICP-AES. Severe and peculiar matrix effects (strongly positive at lower and leveling off at higher matrix concentrations) in the presence of Na and Ca were observed. To reduce these matrix effects, a double approach was utilized consisting of a so-called minimum matrix in combination with an internal standard (Ga in this case). The ‘minimum matrix’ (small amounts of K, Mg and Na) was only added to the standard solution(s) used for the calibration. The detection limit for the whole procedure was 12 μg/L using the P213 nm line. Residual matrix effects were less than 3% (P213 nm line). Received: 21 February 1997 / Revised: 5 June 1997 / Accepted: 6 June 1997     

Determination of total dissolved phosphorus in water samples by axial inductively coupled plasma atomic emission spectrometry

A procedure was developed to determine total dissolved phosphorus in groundwater-like samples using axial ICP-AES. Severe and peculiar matrix effects (strongly positive at lower and leveling off at higher matrix concentrations) in the presence of Na and Ca were observed. To reduce these matrix effects, a double approach was utilized consisting of a so-called minimum matrix in combination with an internal standard (Ga in this case). The ‘minimum matrix’ (small amounts of K, Mg and Na) was only added to the standard solution(s) used for the calibration. The detection limit for the whole procedure was 12 μg/L using the P213 nm line. Residual matrix effects were less than 3% (P213 nm line). Received: 21 February 1997 / Revised: 5 June 1997 / Accepted: 6 June 1997     

锌精矿中铟的测定

应用电感耦合等离子体发射光谱法测定锌精矿中的铟,确定了最佳工作条件,选择了最佳分析谱线,并利用标准加入法和基体匹配法确定了该方法的准确性。样品用氟化氢铵、盐酸、硝酸、高氯酸溶样,用盐酸浸取。本法与萃取分离盐酸羟胺示波极谱法测定的铟含量结果一致。方法准确,快速,加标回收率为99.6%~101.7%,相对标准偏差为0.97%~2.1%。     

微波消解-电感耦合等离子体发射光谱法测定植物样品中的磷、硫

本方法采用微波消解处理样品,电感耦合等离子体发射光谱法测定植物样品中的磷、硫的含量,选用优化微波消解条件进行消解,磷和硫方法最低检出限分别为0.925mg/kg、1.82 mg/kg。精密度RSD和相对误差RE均小于3%,对新鲜植物样品进行加标回收试验,加标回收率为90.5%~107%,证明本方法既可用于检测干植物样品,又可检测新鲜植物样品。     

电感耦合等离子体发射光谱法同时测定玻璃中的硫和磷

通过对玻璃试样中硫、磷的分解方法、分析线选择、共存元素光谱干扰和仪器最佳分析条件等方面的研究, 建立了ICP-AES 测定玻璃中硫、磷的方法. 选用紫外区谱线S 181.972 nm、 P 177.434 nm, 避免了基体元素对硫、磷的干扰, 该法能够准确、快速地测定玻璃样品中的硫、磷量, 测定结果的相对标准偏差小于2.9%, 方法的检出限分别为 S 0.07 μg/mL, P 0.08 μg/mL, 已用于玻璃样品的分析.