Analytical procedure based on slurry sampling for determining selenium in organic vegetable samples by graphite furnace atomic absorption spectrometry

This paper presents a simple, fast and sensitive method to determine selenium in vegetable samples by graphite furnace atomic absorption spectrometry through the direct introduction of slurries of the samples into the spectrometer’s graphite tube. The limits of detection and quantification calculated for 20 readings of the blank of the standard slurries (5 mg mL⁻¹ of microcrystalline cellulose) were 0.33 and 1.10 μg L⁻¹. The proposed method was applied to determine selenium in samples of organically grown vegetables and its results proved compatible with those obtained from samples mineralized by acid digestion in a microwave oven.     

Chromium determination in food by slurry sampling graphite furnace atomic absorption spectrometry using classical and permanent modifiers

A simple method, using permanent modifiers, has been developed for chromium (Cr) determination in food of plant origin by the slurry sampling graphite furnace atomic absorption spectrometry. In particular comparison of the action of Mg(NO₃)₂, iridium (Ir)/niobium (Nb) and iridium (Ir)/tungsten (W) was examined. Finally, for chromium determination in food, the mixture of 2 μg of Ir with 10 μg of Nb was used as permanent modifier. The analytical procedure was optimised carefully on the basis of the data from pyrolysis and atomisation temperature curves studies. The results obtained for four certified reference materials using external calibration with aqueous standards were in good agreement with the certified values. The precision and accuracy of Cr determination by the described method were also acceptable: the RSD were lower than 10% and recoveries for CRMs were in the range of 95-103%. The characteristic mass for chromium was determined to be 3.9 pg and the detection limit for the optimised procedure at the 0.75% (w/v) slurry concentration - 86.6 ng g⁻¹.     

石墨炉原子吸收法测定调味品中痕量铅

采用石墨炉原子吸收光谱法测定不同调味品中铅含量的分析方法.样品采用干法灰化处理,灰化温度为500℃,灰化时间为6h,残渣用1.0％硝酸溶解,然后加入硝酸铵做基体改进剂,优化了仪器条件后进样分析.铅浓度在0μg/L～50μg/L范围内呈良好线性关系,方法最低检出限在0.6μ g/L,回收率为83.80％～87.65％,相对标准偏差RSD为1.82％～3.40％.该方法是一种快速,灵敏,准确的分析方法,可用于调味品中铅的测定.     

石墨炉原子吸收法快速测定血铅的研究

目的 建立一种新的石墨炉原子吸收法测定血铅的快速方法.方法 采用含40 ml/L硝酸与6 ml/L过氧化氢的混合提取液,脱去全血中的蛋白,以硝酸钯(1 g/L)为基体改进剂,石墨炉原子吸收光谱法直接上机测定.结果 线性范围0～ l00μg/L,最低检出限4μg/L,加标回收率88.1％～ 110.3％,相对标准偏差为(RSD) 3.4％ ～9.1％.结论 该方法已成功应用于全血样品的铅测定,结果满意.     

石墨炉原子吸收法测定野菜中的铜和铅

目的为探讨北京地区野菜中重金属的富集特征及人群潜在健康风险。方法选取苦菜和蒲公英为研究对象,采集北京六区县交通道路两旁、山林、农田、公园区域内野菜样品,采用石墨炉原子吸收法测定野菜中Cu、Pb元素含量,并运用目标危害系数(the target hazard quotient,THQ)方法评价人群摄食野菜导致的健康风险。结果六个区县交通道路两旁区域苦菜中铜元素含量在3.90~14.83 mg/kg之间、铅元素含量在0.23~1.82mg/kg之间,蒲公英中铜元素含量在4.26~14.54 mg/kg之间、铅元素含量在0.17~0.61 mg/kg之间;六个区县田地、山上、公园区域苦菜中铜元素含量在3.34~10.40 mg/kg之间、铅元素含量在0.06~0.29 mg/kg之间,蒲公英中铜元素含量在2.91~6.16 mg/kg之间、铅元素含量在0.09~0.25 mg/kg之间。结论交通道路两旁平均10 m区域内野菜中铜和铅元素含量明显高于其他采样区域,多金属复合健康风险评价结果表明,食用非人工种植的北京地区野菜,对人群存在明显的健康风险,野菜引发人群(尤其是儿童)重金属健康风险值得关注,预防食品安全问题发生。     

石墨炉原子吸收分光光度法测定黄豆及腐竹中的硼

目的 建立测定黄豆及腐竹中硼含童的石墨炉原子吸收分光光度法.方法 样品经过HNO_3 + H_2O_2微波消解或加入饱和的Ca(OH)_2助灰化剂干灰化后,选择硝酸钙(10 m/ml)-硝酸铵(20 mg/ml)-柠稼酸(20mg/ml)的混合液作为化学改进剂,采用热解涂层石墨炉原子吸收分光光度法进行测定.结果 硼含量在0～1μg/ml的线性范围内呈线性关系,相关系数r=0.9996,检出限0.017 09μg/ml;方法的精密度(RSD,n=6)为3.56% ～6.45%,回收率为87.20% ～93.70% o结论建立的方法操作简便易行,重现性、灵敏度和准确性能满足分析要求,适用于黄豆及腐竹中硼含量的测定.     

石墨炉法测定食品抗氧化剂TBHQ中铅含量

介绍了国内外食品抗氧化剂TBHQ质量标准中铅限量的规定，认为行标QB2395—1998中铅限量必须修改。同时对TBHQ铅含量采用石墨炉原子吸收光谱法进行了测定，结果表明该法准确性高，数据可靠。     

Evaluation of W-Rh permanent modifier for lead determination in sugar by graphite furnace atomic absorption spectrometry

An alternative procedure that improves the performance of graphite atomizers for the determination of Pb in sugar by electrothermal atomic absorption spectrometry is described. The procedure is based on the injection of 10 μl of an acidified aqueous solution containing 8% w/v sugar and 0.2% v/v HNO₃ into integrated graphite platforms. Either transversely (THGA) as well as longitudinally heated graphite atomizers (LHGA) were evaluated by using conventional co-injection of 0.03% Pd + 0.05% Mg(NO₃)₂ or thermally treated platforms with 250 μg W + 200 μg Rh and co-injection of 5 μg l⁻¹ Rh solution. With W-Rh under the same analytical conditions, the lifetimes of THGA and LHGA reached up to 1110 and 900 firings, respectively. With Pd + Mg the LHGA tube lifetime was limited to approximately 500 firings, but for THGA up to 1020 firings were made with a single tube. Characteristic masses were 11 and 29 pg Pb for LHGA and THGA, respectively. Detection limits (3 s) based on sugar blank solution and on integrated absorbance were 5.0 mg kg⁻¹ with LHGA and 9.3 mg kg⁻¹ Pb for THGA. In general, the coefficients of variation of 20 consecutive measurements of a solution containing 50 μg l⁻¹ Pb were lower than 5%. The obtained detection limits are in consonance with the Codex Alimentarius recommendation for the maximum Pb content in the sugar.     

石墨炉原子吸收光谱法测定豆瓣酱中镉的研究

用经干法处理后的豆瓣酱样品,分别以Mg(NO3)2、La(NO3)3、PdCl2、NH4H2PO4、NH4NO3、酒石酸、柠檬酸、Vc、草酸作为基体改进剂,对石墨炉原子吸收光谱法测定豆瓣酱镉含量过程中,这9种基体改进剂的加入量、灰化温度、原子化温度及作用机理进行了探讨。实验表明,基体改进剂的使用有效降低了背景吸收,提高了信背比,有效消除了食盐的基体干扰。     

石墨炉原子吸收法测定高盐食品中的微量铅

本文研究了吡咯烷二硫代甲酸铵—甲基异丁基甲酮(APDC—MIBK)体系络合萃取高盐食品中微量铅和原子吸收测定的方法。本方法能够将食品中的铅与食盐有效分离，重现性好且易于掌握，结果令人满意。本方法的相对标准偏差为2．8％，回收率为94％。104％，检出限为7．8ng／mL，本方法可用于酱油、蚝油等含盐量高的调味品中铅含量的测定。     

Determination of mercury in fish by cold vapour atomic absorption spectrometry using an automatic mercury analyzer

The concentration of mercury in fish samples from the Atlantic coast of Ghana was determined using a simple, rapid and accurate method. A mixture of HNO₃, HClO₄ and H₂SO₄ was used for complete oxidation of organic tissue. Mercury is detected by the cold vapour atomic absorption spectrometry technique using an automatic mercury analyzer developed at the National Institute for Minamata Disease (NIMD). In total, 56 samples covering 13 species of fish were analysed for total mercury. The concentration of mercury in the edible muscle tissue of these fish ranged from 0.004 to 0.122 μg g⁻¹ wet weight. All fish species sampled had concentrations less than the WHO limit of 0.5 μg g⁻¹ wet weight. The low concentrations of mercury detected in the samples do not constitute any significant mercury exposure to the general population through fish consumption.     

全自动石墨加热消解-石墨炉原子吸收法测定麦苗粉中铅含量的不确定度评定

目的 评定全自动石墨加热消解-石墨炉原子吸收法测定麦苗粉中铅含量的不确定度.方法 麦苗粉样品经全自动石墨加热消解后,石墨炉原子吸收法测定,外标法定量,根据建立的数据模型对每个不确定度分量进行评定,最终得出对合成不确定度的贡献度.结果 置信概率为95％,取包含因子k=2,湿法消解-石墨炉原子吸收法测定麦苗粉中铅含量结果报...     

微波消解-石墨炉原子吸收光谱法检测食品中的铝

目的建立微波消解-石墨炉原子吸收光谱法检测食品中铝的方法。方法以GB 5009.182-2017《食品安全国家标准食品中铝的测定》的石墨炉原子吸收光谱法为基础,以发酵面制品为例,微波消解样品,优化了石墨炉原子吸收光谱法检测条件,建立适合本实验室食品中铝的检测方法。结果在优化实验条件下,铝在0.0~200.0 ug/L范围内呈线性关系,相关系数达到0.9984,加标回收率在95.60%~97.08%之间。选择铝的灵敏线309.3 nm检测,方法检出限达到0.163 mg/kg,相比国家标准提高了1倍。优化了消解罐清洗方式,有效降低了消解罐本底值,提高了检测的准确性。结论本研究优化了微波消解-石墨炉原子吸收光谱法的检测方法,建立的方法能够满足日常检测要求。     

Determination of lead and cadmium in wines by graphite furnace atomic absorption spectrometry.

The lead (Pb) and cadmium (Cd) content of various wines on the Korean market were determined by graphite furnace atomic absorption spectrometry using Zeeman background correction and peak area mode. All wine samples were microwave-digested in concentrated HNO(3). Ammonium dihydrogen phosphate and magnesium nitrate were used as matrix modifiers for both Pb and Cd analyses. The mean Pb content of the wines was about 29 microg l(-1) ranging from 5 to 87 microg l(-1). Also, the means of Cd were about 0.5 microg l(-1) ranging from < 0.1 to 3.0 microg l(-1). The mean recoveries of Pb and Cd were 92.8 and 101.3% and their analytical detection limits were 1.0 and 0.1 microg l(-1), respectively. Sixty brands of wine were classified into red and white, but no statistically significant difference in Pb and Cd content was observed.     

石墨炉原子吸收光谱法测定午餐肉罐头中镉的含量

采用石墨炉原子吸收光谱法测定午餐肉罐头中镉的含量,结果表明,所测样品中镉的含量为4.6μg/kg,该方法简单、快速、准确度高,适用于午餐肉中镉含量的测定.     

石墨炉原子吸收法测定食品接触材料制品中有害重金属迁移量

目的建立一种石墨炉原子吸收法测定聚乙烯制品、聚丙烯制品和三聚氰胺成型品中铅、镉、铬迁移量的检测方法。方法筛选石墨炉原子吸收光谱仪测定铅、镉、铬的最佳灰化温度、原子化温度,采用正交设计仪器参数确定仪器最佳工作条件,测定聚乙烯制品、聚丙烯制品和三聚氰胺成型品中铅、镉、铬迁移量的检出限、重复性、回收率和精密度。结果在最佳试验条件下,铅、镉、铬的线性范围为0~150、0~5、0~100μg/L,检出限为1.04、0.05、0.98μg/L,加标回收率为96.5%~104.0%,样品测定的相对标准偏差均小于5%。结论该方法快速、准确、可靠,可作为食品接触材料制品中铅、镉、铬迁移量的测定方法。     

直接提取进样石墨炉原子吸收法测定大米中的镉含量

建立直接提取进样石墨炉原子吸收仪测定大米中镉含量的分析方法。将粉碎的大米用0.5%硝酸+0.1%曲拉通混合液提取、稀释定容,摇匀待测。以NH_4H_2PO_4+Mg(NO_3)_2为基体改进剂,用塞曼效应扣背景的方式,分别采用一步灰化(氩气)、两步灰化(氩气+空气)标准曲线法和标准加入法测定大米中的镉含量。结果表明三种方法测试样品的RSD(N=6)值分别为1.78%、3.29%、0.62%,加标回收率分别为114.7%、103.9%、102.5%,检出限分别为0.025、0.031、0.035μg/L。经t检验,两两比较,两步灰化和标准加入法无显著性差异,且精密度和准确度都能够满足要求。直接稀释进样测定大米中镉含量的方法操作简便,分析速度快,无污染,灵敏度高且准确性好。     

微波消解-石墨炉原子吸收法测定新鲜樱桃中 铜含量

目的建立基于微波消解的前处理方法,使用石墨炉原子吸收法检测新鲜樱桃中铜含量的方法。方法采用微波消解法对新鲜樱桃样品进行前处理消解,消解好的溶液使用石墨炉原子吸收光谱对其中的铜元素含量进行定量测定。同时进行方法检出限、精密度、回收率的测试。结果本试验确定的最佳消化条件为:樱桃样品的称样质量为2 g,由8 m L HNO_3和2 mL H_2O_2组成的混合酸试剂。测得樱桃中铜含量为0.27 mg/kg~4.32 mg/kg,超过96%的样品含量小于2.0 mg/kg,铜元素含量没有超过标准的要求。实际样品回收率97.7%~103.5%,检出限0.236μg/L,相对标准偏差1.06%。结论该方法测定新鲜樱桃中的铜含量操作简便,准确,方法检出限、精密度、回收率均能满足实际的分析检测要求,测定结果准确可靠,可作为测定樱桃中的铜含量的方法之一。     

石墨炉原子吸收法测定Lanaset染料染色羊绒中铬残留量

 Lanaset是一种由含有活性溴代丙烯酰胺基团的毛用活性染料与金属络合物混合的染料,为了解Lanaset染料对羊绒染色后铬的残留量,采用微波消解进行前处理,以HNO3+H2O2(5+2,V/V)作为消解试剂,采用石墨炉原子吸收（GFAAS）法,建立了一种简便、灵敏、准确的羊绒中痕量铬的GFAAS测定方法。设定样品消化液灰化温度为1100℃,实验原子化温度为2300℃。结果显示,铬的最低检出浓度为0.22 μg/L,相对标准偏差为3.6%～6.3%,回收率为96.0%～102.3%。对15份试验样品进行检测,铬含量在0.126～0.289 mg/kg范围,明显低于生态纺织品标准限量要求。     

Method development for the determination of manganese in wheat flour by slurry sampling flame atomic absorption spectrometry

The wheat is one of the cereals more consumed in the human food in all worlds. In the form of flour it is used for preparation of breads, cookies, pizzas, cakes, and etc. This way, the knowledge of the mineral content this cereal and its flour is very important. Considering it, methods for determination of metals in these matrices are opportune and several papers have been performed.