共查询到19条相似文献,搜索用时 140 毫秒
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利用高效液相色谱法测定奶粉中黄曲霉毒素M1含量,对测定结果的不确定度进行评定。通过实验步骤和定量方法建立数学模型,分析不确定度来源,计算合成不确定度和扩展不确定度。结果表明,标准溶液配制、重复性测量、样品处理对测定结果的不确定度贡献较大。在实际工作中,可以通过选择A级标准玻璃器具、优化样品处理方法、重复测定样品来减小结果的不确定度,提高检测结果的准确性。当样品中黄曲霉毒素M1的质量分数为0.522 μg/kg时,其扩展不确定度为0.027 μg/kg(k=2)。 相似文献
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胡新华 《分析测试技术与仪器》2020,26(2):143-150
对微波消解火焰原子吸收法测定火龙果中铁含量的不确定度进行评估.建立相应的不确定度数学模型,根据测试过程分析不确定度来源有7个方面,计算各不确定度分量,得到火龙果中铁含量测定结果是X=(1.308±0.281)mg/100 g(k=2).测量过程不确定度的主要来源是样品溶液测量、样品空白及样品溶液定容等3个方面,其中,标准曲线制作和工作曲线拟合引起的不确定度最大.不确定度评定结果可为水果等营养元素检测方面提供参考,避免或减少一些不必要检测误差,使测试结果更加准确. 相似文献
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建立了电感耦合等离子体发射光谱(ICP-AES)测定糖果中铅的相应数学模型, 对数学模型中各个参数进行不确定度来源分析, 分别对A类不确定度或B类不确定度进行评定. 对各不确定度分量合成和扩展, 得到铅质量分数的不确定度. 结果表明: 标准溶液的配制、标准曲线拟合线性方程及样品溶液的定容是不确定度的主要来源. 相似文献
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建立对微波消解-石墨炉原子吸收法测定化妆品中微量砷的不确定度评定方法.建立有效的数学模型,对影响因素进行全面分析,并评定各因素的不确定度.扩展不确定度为0.25mg/kg,测量结果表示为2.00±0.25 mg/kg(k=2).测量不确定度的来源主要为样品检测的回收率产生的不确定度和重复性引起的不确定度. 相似文献
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研制乳粉中硝酸盐、亚硝酸盐分析标准样品。获得原料并确认后,对原料添加目标物,混匀,喷雾干燥,分装,包装制成标准样品。对样品进行均匀性、稳定性检验,通过多家实验室联合定值的方式对样品进行定值,从而获得标准值及其不确定度。样品中硝酸盐、亚硝酸盐均匀性检测数据经F检验在95%置信水平时单元件不具有统计显著性,表明样品是均匀的;样品稳定性检测数据经t检验,表明样品在-20℃保存条件下18个月内量值稳定;对8家有能力的实验室联合定值数据统计分析得到样品中硝酸盐标准值为22.4 mg/kg,不确定度为0.95 mg/kg(k=2);亚硝酸盐标准值为23.0 mg/kg,不确定度为0.93 mg/kg(k=2)。样品均匀性、稳定性、赋值和不确定度评估等均符合有证标准样品的要求,能够满足预期用途。 相似文献
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电感耦合等离子体发射光谱法测定镍钴锰氢氧化物中硫酸根含量的不确定度评定 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-OES)测定镍钴锰氢氧化物(三元正极材料NCM前驱体)中硫酸根含量.确定了适宜的测试条件,依据不确定度评定的方法,分析了不确定度来源、量化不确定度分量、计算检测结果的合成标准不确定度和扩展不确定度.结果表明,NCM前驱体中硫酸根的质量分数为2 709±88 mg/kg,样品加标回收率为97.5%~99.7%,相对标准偏差(RSD)为2.02%.方法简单、快速. 相似文献
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分析与讨论了汽油中锰含量测定过程中的不确定度来源,并对各个不确定度分量进行量化与合成,计算出火焰原子吸收光谱法测定汽油中锰含量的相对合成不确定度为0.083(锰含量约为10 mg/L),扩展不确定度U为1.8 mg/L(置信水平为95%,k=2). 比较各个不确定度分量可知,测定结果的不确定度主要源自标准工作溶液的最小二乘法拟合. 相似文献
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Turner AD Hatfield RG Rapkova-Dhanji M Norton DM Algoet M Lees DN 《Journal of AOAC International》2010,93(5):1482-1493
In 2009, a refined HPLC method based on AOAC Official Method 2005.06 was developed and validated for the determination of paralytic shellfish poisoning (PSP) in mussels. A single-laboratory validation study of this method was undertaken here for the analysis of PSP toxins in oysters, cockles, clams, and razor clams. The method was characterized for selectivity, sensitivity, linearity, precision, repeatability, recovery, ruggedness, and uncertainty of measurement. Validation data were utilized to determine method performance characteristics for non-mussel bivalves for all commercially available certified reference toxins, extending the method to dcNEO and dcGTX2,3, where available. A period of parallel testing of oysters, cockles, and clams enabled a comparison of sample toxicities obtained using mouse bioassay (MBA) and HPLC methodologies, although only a very low number of PSP-positive samples were obtained through the United Kingdom official control monitoring program. Results from the MBA and HPLC methods were well-correlated for PSP-negative samples, but the low number of naturally contaminated PSP-positive samples has prevented any comparative statistical assessment of method performance for non-mussels between the two official methods. However, some evidence for potentially significant differences in total saxitoxin equivalents obtained by the two methods in some species has highlighted the need for further comparative testing in non-mussel samples to be conducted prior to implementation of the HPLC method in routine official control monitoring programs. 相似文献
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A protocol has been developed illustrating the link between validation experiments, such as precision, trueness and ruggedness
testing, and measurement uncertainty evaluation. By planning validation experiments with uncertainty estimation in mind, uncertainty
budgets can be obtained from validation data with little additional effort. The main stages in the uncertainty estimation
process are described, and the use of trueness and ruggedness studies is discussed in detail. The practical application of
the protocol will be illustrated in Part 2, with reference to a method for the determination of three markers (CI solvent
red 24, quinizarin and CI solvent yellow 124) in fuel oil samples.
Received: 10 April 1999 / Accepted: 24 September 1999 相似文献
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分光光度计测铁矿石中钛的测量不确定度评定 总被引:1,自引:0,他引:1
紫外-可见分光光度计在化学分析中应用较为广泛。对于借助其进行化学分析测量不确定度的评定,目前较多见于溶液测定。实际应用中,测试样品多为固体,涉及到称样、溶解、稀释、定容等步骤。此文试从随机效应和系统效应的角度考虑,对紫外-可见分光光度计应用ISO4691:1985铁矿石中钛含量的测定——二安替比林甲烷分光光度法对铁矿石中钛的测量过程中的不确定度来源进行了较为全面的分析,并最终给出评定结果。 相似文献
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电感耦合等离子体发射光谱(ICP-OES)法同时测定活性炭中铝、钴、镉、铜、铁、镁、锰、钠、磷、硫10种元素 总被引:2,自引:0,他引:2
提出了使用ICP-OES同时测定活性炭中Al、Co、Cr、Cu、Fe、Mg、Mn、Na、P和S的分析方法。采用高氯酸和硝酸处理样品,以硝酸作为测定介质,在选定的仪器工作条件下直接测定。各元素的测定检出限为0.002~0.012μg/mL,相对标准偏差(RSD,n=6)为0.32%~1.83%。对样品进行加标回收试验,回收率在92.1%~108.4%之间。实验表明:方法不仅具有较高的灵敏度和较低的检出限,而且快速、准确,能够满足活性炭和以活性炭为载体的催化剂杂质元素分析的要求。 相似文献
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A stir rod sorptive extraction (SRSE) with monolithic polymer as coating was proposed to avoid the friction loss of coating during the stirring process. In our study, poly(2-acrylamide-2-methylpropanesulfonic acid-co-octadecyl methacrylate-co-ethylene glycol dimethacrylate) [poly(AMPS-co-OCMA-co-EDMA)] monolithic polymer was used as a coating of SRSE. The effect of concentration of porogen on SRSE performance was studied. Four fluoroquinolones (FQs) were selected as testing analytes to evaluate the extraction efficiency of SRSE. To achieve the optimum extraction conditions of SRSE towards FQs, several parameters, including extraction time, extraction temperature, stirring rate, sample solution pH and contents of inorganic salt in the sample solution were investigated. Under the optimized conditions of SRSE, a method for the determination of FQs in honey sample was proposed based on the combination of SRSE with liquid chromatography and electrospray ionization mass spectrometry (SRSE/LC/ESI-MS). The detection limits (LODs) of the proposed method for four FQs ranged from 0.06 to 0.14 ng/g and the recoveries were in the range of 70.3–122.6% at different concentrations for honey samples. Good method reproducibility was found as intra- and inter-day precisions, yielding the relative standard deviations less than 11.9% and 12.4%, respectively. The results show that SRSE with poly(AMPS-co-OCMA-co-EDMA) monolithic polymer as coating possessed good extraction capacity towards FQs in honey samples. Finally, the monolithic polymer coated stir rod was demonstrated to be reused at least 60 times. 相似文献
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J.C. Burridge 《Analytica chimica acta》1978,99(2):401-404
A study of the dissolution rate of magnetite electrodes required a reasonably precise method for the determination of iron in aqueous solutions containing 1 mol kg-1 sodium perchlorate. Atomic absorption spectrometry with electrothermal atomization in the wavelength range 248–392 nm with ashing at 1600°C proved to be the most satisfactory method. Iron concentrations in the range 0.1–100 μg ml-1 were determined with 1-μl samples. The addition of low flow rates of acetylene to the nitrogen purge gas improved the reproducibility and increased the carbon rod lifetime. 相似文献