电感耦合等离子体质谱法(ICP-MS)测定废水中有害元素银的含量

为了寻求一种更加适合废水中低含量银的测定方法,本文采用石墨电热板消解-电感耦合等离子体质谱法测定废水中的低含量银离子。通过仪器工作条件最优化、测定线性回归方程、检出限、准确度、精密度、实际样品加标回收率,并与电感耦合等离子体发射光谱法（ICP-AES）的实际样品测定结果进行比对来评价该方法的实用性。石墨电热板消解-电感耦合等离子体质谱法前处理方法简便,分析速度快且该方法检出限较低,为0.03ug/L,标准样品测定的相对误差为-0.7%～1.7%,相对标准偏差为1.1%～2.5%,实际样品加标回收率在97.0%～103%之间,回收率高,能够满足废水中低含量银的测定。     

电感耦合等离子体原子发射光谱(ICP-AES)法和电感耦合等离子体质谱(ICP-MS)法测定大气降尘中的铅、镉、铬、锌、锰、镍、铜、铊

大气中Pb、Cd、Cr、Mn、Ni、Tl等重金属污染物是目前国内外城市大气污染的主要因子之一,研究大气降尘中重金属元素含量具有重大意义。本文采用盐酸-硝酸混合酸为消解体系,在105℃条件下用电热板消解回流大气降尘样品2小时后定容测定,通过电感耦合等离子发射光谱法仪(ICP-AES)和电感耦合等离子体质谱仪(ICP-MS)测定大气降尘中铅、镉、铬、锌、锰、镍、铜和铊等8种重金属元素。测定结果表明： ICP-AES(铅、镉、铬、锌、锰、镍、铜)和ICP-MS(铊)两种方法的曲线线性好,准确度高,测定范围宽,检出限在0.024mg/kg-0.548mg/kg之间,精密度在0.15%-2.38%之间,能准确测定大气降尘中的重金属元素含量。     

微波消解-电感耦合等离子体原子发射光谱法测定两种奶茶粉中微量元素

以微波消解系统对奶茶粉样品进行处理,并采用电感耦合等离子体发射光谱法(ICP-AES)对样品中的微量元素进行测定。优化了仪器工作条件,建立了同时测定奶茶粉中Zn、Fe、Cu、Mn、Cd、As、Ba和Pb 8种元素的微波消解-ICP-AES法。平均回收率为97.1%～103.2%之间,相对标准偏差(RSD)在0.7%～3.6%之间。实验结果表明,方法简便、快速、准确,适用于奶茶粉样品中微量元素的测定。     

微波消解-电感耦合等离子体原子发射光谱（ICP-AES）法测定镍基耐蚀合金中镍

采用微波消解法与电感耦合等离子体原子发射光谱(ICP-AES)法相结合的方式,建立了镍基耐蚀合金中镍元素含量的测定方法。试样在浓硝酸和浓盐酸中微波消解后,用电感耦合等离子体原子发射光谱仪在优化的工作参数下测定,结果表明,稀释的消解液可直接用于镍含量的测定,光谱干扰少。对镍基耐蚀合金中镍含量进行多次平行测定,相对标准偏差(RSD,n=7)为0.29%,且测得值与标准值结果一致。对不同的镍基耐蚀合金样品进行加标回收实验,加标回收率在98.5%~102%。标准物质验证实验表明,测得值与标准值一致。     

微波消解-电感耦合等离子体质谱(ICP-MS)法测定纳米银抗菌产品中多种微量元素

建立了微波消解-电感耦合等离子体质谱(ICP-MS)法测定4种纳米银抗菌产品中多种微量元素的分析方法。比较了湿法消解和微波消解这两种样品前处理方法对样品测定的影响,探讨了消除汞记忆效应的方法,并研究了待测元素的质谱干扰的消除。实验结果表明,采用Au(100μg/L)+HCl(2%)能较好地消除Hg的记忆效应。与湿法消解相比,微波消解可短时间消解样品并获得好的Hg回收率。在优化ICP-MS条件后,各元素线性相关系数均大于0.999。采用微波消解-ICP-MS法对样品进行加标回收,样品加标回收率在84.0%~109%,相对标准偏差在0.97%~13.2%。方法快速、简便,能够满足纳米银抗菌产品中微量元素的定量测定。     

电感耦合等离子体发射光谱法测定植物油中的磷

用电感耦合等离子体发射光谱法(ICP-AES)测定了植物油中的磷.采用多谱线拟合技术(MSF)校正了铜对P213.617 nm和P214.914 nm光谱干扰.比较了活性炭炭化灰化法和微波消解法两种样品前处理方法对分析结果的影响.结果表明这两种前处理方法所得结果都能与国标磷钼蓝分光光度法的分析结果吻合,其中活性炭炭化灰化法的方法检出限(0.053 mg/kg)较微波消解法的方法检出限(0.42 mg/kg)更低,所以对低含量的磷的检测结果其相对误差及精密度更好.该法应用于植物油中磷的测定.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定再生锌中铊

铊是一种典型的危险废物,在选冶过程中,再生锌原料中的铊以氧化物或粉尘的形式排放到环境中,严重污染环境并危害人类健康。再生锌成分复杂,若样品消解不完全,直接影响测定结果的准确性。本文比较了微波消解和电热板常压消解对样品的处理效果。结果表明,微波消解法快速环保,但是对于难消解的再生锌样品,因无高氯酸的加入,其氧化性能降低,无法将样品消解完全,导致铊测定结果偏低。而采用高氯酸-硝酸-盐酸-氢氟酸构成的混合酸并于低温加盖聚四氟乙烯盖,进行电热板常压消解,能够有效地解决再生锌样品前处理难题。本实验采用四酸法消解样品,5%盐酸进行浸取,选择Tl 190.794nm为分析谱线,采用电感耦合等离子体原子发射光谱（ICP-AES）法测定再生锌中铊。在仪器设定的最佳测定条件下,当Tl质量浓度为0.10μg/mL~5.00μg/mL时,与发射强度线性关系良好,线性回归方程为y = 180.77x -0.46,相关系数为0.99998。干扰实验表明,在设定的共存离子干扰上限,Pb、Zn、Cu、Fe、Ca、Bi 、Sb、Sn、As、Al、Cd、Si、Ag等对再生锌中铊的测定基本无影响。按照实验方法,对5个不同铊含量水平的再生锌样品进行11次独立测定,其测定范围为ω(Tl):0.0041%~0.21%,方法检出限为0.004μg/mL,实验相对准偏差（RSD）为2.07%~3.11%,加标回收率为97.3%~107.5%。方法简单,操作性强,能够快速准确测定再生锌中铊。     

电感耦合等离子体质谱法测定香精香料中的硼元素

采用微波消解-电感耦合等离子体质谱法(ICP-MS)测定香精香料中硼元素的含量。对微波消解样品前处理条件和仪器参数进行了优化,该方法硼元素检出限为1.005 ng/mL、平均回收率为106.1%、精密度为6.15%(n=5),并用茶叶国家标准物质(GBW10016)对分析方法进行了校准。该方法适合于香精香料中硼元素的测定。     

电感耦合等离子体发射光谱法测定蚕蛹、蝎子、海肠中20种元素含量

采用电感耦合等离子体发射光谱法(ICP-AES)直接快速测定蚕蛹、蝎子、海肠中20种元素含量,采用微波炉消解样品,试验了微波消解的条件.并对微波消解溶样和常规酸法溶样分别进行了测定和比较.方法的检出限为0.01～0.12 mg·L-1,相对标准偏差为1.4%～4.6%.     

电感耦合等离子体原子发射光谱法同时测定地质样品中的Zr、Hf、Sc、Th

建立了一种用电感耦合等离子体原子发射光谱法,同时测定地质样品中Zr、Hf、Sc、Th的方法。选择了ICP-AES同时测定上述4种元素的最佳工作条件。采用三乙醇胺-氢氧化物沉淀预先除去大量硅、铝、铁等,以消除其在测定时产生的干扰。考察了基体元素Mn的光谱干扰,采用干扰系数校正法扣除背景干扰。Zr、Hf、Sc、Th的检出限分别为3.69、0.45、0.07、0.41μg/g,RSD<10%。     

Pressurized wet digestion in open vessels

The High Pressure Asher (HPA-S) was adapted with a Teflon liner for pressurized wet digestion in open vessels. The autoclave was partly filled with water containing 5% (vol/vol) hydrogen peroxide. The digestion vessels dipped partly into the water or were arranged on top of the water by means of a special rack made of titanium or PTFE-coated stainless steel. The HPA-S was closed and pressurized with nitrogen up to 100 bars. The maximum digestion temperature was 250 °C for PFA vessels and 270 °C for quartz vessels. Digestion vessels made of quartz or PFA-Teflon with volumes between 1.5 mL (auto sampler cups) and 50 mL were tested. The maximum sample amount for quartz vessels was 0.5–1.5 g and for PFA vessels 0.2–0.5 g, depending on the material. Higher sample intake may lead to fast reactions with losses of digestion solution. The samples were digested with 5 mL HNO₃ or with 2 mL HNO₃+6 mL H₂O+2 mL H₂O₂. The total digestion time was 90–120 min and 30 min for cooling down to room temperature. Auto sampler cups made of PFA were used as digestion vessels for GFAAS. Sample material (50 mg) was digested with 0.2 mL HNO₃+0.5 mL H₂O+0.2 mL H₂O₂. The analytical data of nine certified reference materials are also within the confidential intervals for volatile elements like mercury, selenium and arsenic. No cross contamination between the digestion vessels could be observed. Due to the high gas pressure, the diffusion rate of volatile species is low and losses of elements by volatilisation could be observed only with diluted nitric acid and vessels with large cross section. In addition, cocoa, walnuts, nicotinic acid, pumpkin seeds, lubrication oil, straw, polyethylene and coal were digested and the TOC values measured. The residual carbon content came to 0.2–10% depending on the sample matrix and amount.     

ICP-MS法测定聚酯纤维中TiO2含量

采用湿法和微波法对聚酯纤维样品进行消解,利用电感耦合等离子体质谱联用仪(ICP-MS)对样品中TiO2含量进行了测定,得到湿法消解样品测定值2 857.46μg/g(相对标准偏差为1.08%),微波消解样品测定值2599.21μg/g(相对标准偏差为2.76%).分别测定了两种消解方法的检出限,湿法消解检出限为4.0 ...     

一种改进的凝胶分离后蛋白质溶液酶解方法

报道了改进的凝胶电泳分离后蛋白质溶液酶解方法。将凝胶分离后的蛋白转移到PVDF膜上,直接用碳酸氢铵中和从膜上的蛋白洗脱溶液至弱碱性,并在此溶液中直接进行蛋白酶解。方法避免了胶内杂质对质谱鉴定蛋白质的干扰。用标准蛋白进行了验证,并在此基础上鉴定了中国仓鼠卵巢细胞（CHO）细胞系中的16个蛋白点。与已报道的方法比较,本方法蛋白回收率提高到90％左右;与传统的胶内酶解方法比较,本方法具操作简单,实验流程较短;涉及的试剂较胶内酶解少,因此带来的杂质影响小;在蛋白转印以后还可与许多其它实验方法相结合,比如免疫印迹等优点。     

电感耦合等离子体-原子发射光谱测定鱼肉中常见营养元素的样品消解方法

使用干法灰化消解、湿法全消解和湿法半消解三种不同的样品消解方法,结合电感耦合等离子体发射光谱仪测定了淡水鱼和海水鱼两种不同鱼类中的K、Na、Ca、Mg四种常见营养元素的含量。结果表明各元素回收率在91%~109%之间,除Ca外其余元素相对标准偏差小于5%。湿法半消解同其它消解方法相比,缩短了检测时间,提高了分析效率,能够更加有效、快速、准确地测定鱼肉中的K、Na、Ca和Mg元素的含量。     

The Effects of Food on Cannabidiol Bioaccessibility

Cannabidiol (CBD) is a hydrophobic non-psychoactive compound with therapeutic characteristics. Animal and human studies have shown its poor oral bioavailability in vivo, and the impact of consuming lipid-soluble CBD with and without food on gut bioaccessibility has not been explored. The purpose of this research was to study the bioaccessibility of CBD after a three-phase upper digestion experiment with and without food, and to test lipase activity with different substrate concentrations. Our results showed that lipase enzyme activity and fatty acid absorption increased in the presence of bile salts, which may also contribute to an increase in CBD bioaccessibility. The food matrix used was a mixture of olive oil and baby food. Overall, the fed-state digestion revealed significantly higher micellarization efficiency for CBD (14.15 ± 0.6% for 10 mg and 22.67 ± 2.1% for 100 mg CBD ingested) than the fasted state digestion of CBD (0.65 ± 0.7% for 10 mg and 0.14 ± 0.1% for 100 mg CBD ingested). The increase in bioaccessibility of CBD with food could be explained by the fact that micelle formation from hydrolyzed lipids aid in bioaccessibility of hydrophobic molecules. In conclusion, the bioaccessibility of CBD depends on the food matrix and the presence of lipase and bile salts.     

高温法和烘箱法测定水体中总氮的比较

分别采用烘箱法和高压蒸汽消解法对纯水和电解质溶液中的含氮有机化合物进行了消解,并用镉铜还原法测定了溶液中总氮的含量。实验表明,这两种消解方式无显著性差异,可以采用烘箱法代替压力蒸汽消毒器在电解质溶液中对含氮有机化合物进行消解,且烘箱法操作简单。     

Decomposition of organoarsenic compounds for total arsenic determination in marine organisms by the hydride generation technique

The conditions necessary for the complete decomposition of six organic arsenic compounds, namely methylarsonic acid (MMAA), dimethylarsinic acid (DMAA), trimethylarsine oxide, tetramethylarsonium iodide, arsenocholine bromide (AsC) and arsenobetaine (AB), were investigated. The degree of decomposition of the arsenic compounds was monitored using a hydride generation (HYD) technique, because the response from this system depends strongly on the chemical species of arsenic, with inorganic arsenic (the expected product from these decomposition experiments) giving a much more intense HYD signal than the organic arsenic compounds. The arsenic compounds were decomposed by heating them with three types of acid mixture, namely HNO₃? HClO₄, HNO₃? HClO₄? HF, or HNO₃? HClO₄? H₂SO₄. Both MMAA and DMAA were decomposed completely using any of the mixed acids at a decomposition temperature of 200 °C or higher. The HNO₃? HClO₄? H₂SO₄ mixture was the most effective for decomposing AsC and AB, which are the most difficult compounds among all types of organic arsenic compound to decompose and render inorganic. The complete decomposition of AB was only achieved, however, when the temperature was 320 °C or higher, and the sample was evaporated to dryness. When the residue from this treatment was examined by high‐performance liquid chromatography combined with inductively coupled plasma atomic emission spectrometry, all of the arsenic was found to be present as arsenic(V). The optimized conditions (HNO₃? HClO₄? H₂SO₄ at 320 °C) for decomposing AB were then used to determine the total amount of arsenic in marine organisms known to contain AB. Copyright © 2005 John Wiley & Sons, Ltd.     

生物样品快速高压罐消解法研究

本文介绍一种新近研究的生物样品消解法－快速高压罐消解法。它具有消解样品快速的特点，消解速度与微波法相当，此法在消解原理，设备结构等方面具有独自的特点。经过可靠性，适应性，安全性和条件选择等系统试验，证明此法可行。将对快速消解生物类样品提供一种新。     

微波消化光度法测定化学需氧量

研究了微波化制样光度法测定ＣＯＤ的新方法,确定了微波消化的主要因素,要佳消化条件和测定条件,吸光度与ＣＯＤ值在０－１ｇ．Ｌ＾－１范围内呈良好的线性关系。对实际水样测定结果的准确度和精密度都能很好的满意测定要求。     

电感耦合等离子体质谱(ICP-MS)法测定页岩中稀土元素含量

建立了湿法消解和微波消解两种前处理方法处理页岩样品,以铑、铼为内标,采用KED-ICPMS测定页岩样品中15种稀土元素(镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥和铱)。结果表明,各元素在0～100ng/mL范围内线性关系良好,相关系数在0.998以上,方法检出限在0.003～0.034mg/kg,相对标准偏差为1.3%～8.2%(n=6)。由于页岩样品中有机质含量高,湿法消解时应适当提高高氯酸和硫酸的比例。对比湿法消解和微波消解两种前处理方法,微波消解消耗试剂较少,具有更优的检出限、精密度和准确度。