甲醇中8组分苯系物溶液标准物质的研制

介绍甲醇中8组分苯系物溶液标准物质的研制过程。采用气相色谱仪(GC-FID)、电感耦合等离子体质谱仪(ICP-MS)和卡尔·费休水分仪(KF)等检测方法,结合质量平衡法对原料纯度进行验证,其纯度验证结果与证书标示值一致,并在不确定度范围内。经F检验和t检验,结果表明,采用重量-容量法制备的甲醇中8组分苯系物溶液标准物质具有良好的均匀性和稳定性,其定值结果为1000μg/mL,相对扩展不确定度为3%(k=2)。该溶液标准物质可用于环境分析中苯系物含量的测定和量值溯源。     

化学需氧量溶液标准物质的定值及不确定度评定

采用重量-容量法,配制了化学需氧量溶液标准物质,利用一级标准物质进行比较定值,并对溶液标准物质进行了均匀性检验和稳定性考察。对定值的不确定度进行了评定。化学需氧量溶液标准物质的定值结果为2000mg/L,扩展不确定度为:Urel=2%,k=2。     

磷溶液标准物质的研制

介绍了磷溶液标准物质的研制。选择磷酸二氢钾为原料,经提纯后,配制成质量浓度为1000μg/mL的磷溶液标准物质。采用准确、可靠并能溯源的磷钼酸喹啉重量法进行定值、均匀性检验及稳定性检验。对影响测量不确定度的因素进行了分析,全面评定了标准物质的不确定度。研制的磷溶液标准物质,均匀性良好,扩展不确定度为0．5％（k=2）,稳定性达2年。     

氯化钾电导率溶液标准物质的研制

介绍了氯化钾电导率溶液标准物质的研制方法,采用与一级标准物质比较定值的方法对该标准物质进行了定值,利用高精度电导率仪对定值结果进行了验证,同时对该标准物质进行了均匀性检验和稳定性考察。氯化钾电导率溶液标准物质的定值结果为1408μS/cm,扩展不确定度为:Urel=0.6%,k=2。其均匀性和稳定性检验结果表明,该标准物质符合国家二级标准物质的技术要求。     

甲醇纯度国家一级标准物质的研制

介绍了甲醇纯度标准物质的研制方法,采用国际基准方法之一的凝固点下降法对该标准物质进行了定值,利用气相色谱法对定值结果进行了验证,同时对该标准物质进行了均匀性检验和稳定性考察.甲醇纯度标准物质定值结果为99.7%,扩展不确定度为0.3%.其均匀性和稳定性检验结果表明,该标准物质符合国家一级标准物质的技术要求.     

一种燃料热沉标准物质候选物的纯度定值及不确定度分析

一种多环烃化合物作为超声速飞行器用燃料热沉标准物质候选物,对于燃料的热沉准确计量具有十分重要的意义.通过采用质量平衡和核磁定量两种不同测量原理的方法,对这种热沉标准物质候选物的纯度进行了定值,并进行了不确定度分析和评定.在此过程中,采用气相色谱法(GC-FID)对候选物的分装样品进行了均匀性检验和稳定性考察.研究结果表...     

水中氟离子溶液标准物质的研制

文章以氟化钠标准物质为原料，超纯水为溶剂，采用重量-容量法制备水中氟离子溶液标准物质，介绍了水中氟离子溶液标准物质的研制方法。研制的水中氟离子溶液标准物质利用离子色谱法进行检测，分别采用F检验和回归曲线法进行均匀性和稳定性检验，方差分析和线性拟合结果表明该标准物质具有良好的均匀性和稳定性。选择国家二级标准物质采用同样的检测方法进行验证，结果表明制备的标准物质的方法准确度满足要求。研制的水中氟离子溶液标准物质的定值结果为1 000 mg/L,相对扩展不确定度U_rel=1%(k=2)。该标准物质量值准确，且具有溯源性，可用于水中氟离子测量过程的质量控制及分析方法的确认和评价。     

维生素K_1冻干标准物质的研制

采用二甲基亚砜(DMSO)作为冻干标准物质的溶剂,以重量法准确配制维生素K_1/DMSO溶液,再进行分装、冷冻干燥,经定性分析、定值分析、均匀性检验、稳定性考察和不确定度评定,研制了维生素K_1冻干标准物质。以维生素K_1纯度标准物质溶液为校准品,对得到的冻干物质进行了高效液相色谱法定值分析,冻干标准物质的准确定值结果为0.96 mg/mL,相对扩展不确定度为7%。建立的维生素K_1冻干标准物质研制方法,对于临床检验中维生素K_1的准确测定和相关疾病的正确诊断治疗以及维生素K_1长期保存具有重要意义。     

GBW(E)100674乙腈中展青霉素溶液标准物质的研制

本课题研制了乙腈中展青霉素的溶液标准物质1种,并已成功申报为国家二级标准物质(GBW(E)100674)。该溶液标准物质以展青霉素纯度国家二级标准物质(GBW(E)100673)为原料,采用重量容量法配制。依据JJF1343-2012《标准物质定值的通用原则及统计学原理》的要求,本研究采用液相色谱法对乙腈中展青霉素溶液标准物质进行均匀性、短期稳定性和长期稳定性的评价。定值不确定度包含原料纯度、溶液配制、均匀性、短期稳定性和长期稳定性五个方面引入的不确定度。最终,该溶液标准物质GBW(E)100674的定值结果为100μg/m L,不确定度为2%。本研究研制展青霉素溶液标准物质的量值具有溯源性和准确性,可以支持国家食品安全检测的需要。     

甲醇水中咖啡因溶液标准物质的研制及不确定度评定

研制了液相色谱-质谱联用仪(LC-MS)校准用甲醇水中咖啡因溶液标准物质并进行不确定度评定。以咖啡因纯品、色谱级甲醇和实验室一级用水为原材料,利用质量平衡法对咖啡因纯品进行纯度核验,利用基准方法重量—容量法配制浓度9.94 mg/L甲醇水中咖啡因溶液标准物质。采用液相色谱法对9.94 mg/L甲醇水中咖啡因标准溶液和国家二级标准物质GBW(E)130453进行量值比对,并对溶液标准物质的均匀性、短期稳定性和长期稳定性进行考察。结果表明研制的9.94 mg/L的甲醇水中咖啡因溶液标准物质的均匀性和稳定性良好,相对扩展不确定度为2%(k=2),有效期为12个月。     

六种多环芳烃溶液标准物质的研制

本文介绍了荧蒽、苯并（b)荧蒽、苯并（k)荧蒽、苯并（a)芘、苯并（ghi)Bai和茚并（1,2,3－cd)芘六种环保用多环芳烃甲醇溶液标准物质的定值测定及均匀性和稳定性考察。定值采用美国国家标准研究院（NIST）的SRM2260和SRM1491作为高一级的标准物质进行量值传递,使用高效液相色谱法（HPLC）,测量不确定度约为3％。     

Certified reference materials of trace elements in water

Measurement of trace elements is playing a vital role in industries and various sectors of science and technology including semiconductors, food, health and environmental sectors. In most of the cases a small error in measurement can vitiate all the measures taken for quality control and management. Many decisions regarding the suitability of material/products are based on the analysis. To reduce or eliminate the rejection rate of the products, accurate and reliable measurements are needed which can be achieved by the use of certified reference materials (CRMs). Their use in calibration of analytical equipments and validation of test methods ensures high quality in measurements and it provides traceability to the measurement data with national/international measurement systems (SI unit) also. In the present scenario of globalization of economy, use of certified reference materials (CRMs) in measurements is essential for global acceptance of products and test reports. Their use fulfil a mandatory requirement of international quality systems (ISO 9000, ISO/IEC standard 17025) including our national accreditation body, National Accreditation Board for Testing and Calibration Laboratories (NABL), World Trade Organization (WTO) etc. International manufacturers of CRMs are meeting most of the requirement of CRMs of the country. To meet the demand of CRMs indigenously, the National Physical Laboratory, India initiated a national programme on preparation and dissemination of certified reference materials.     

高效液相色谱柱后衍生法测定黄曲霉毒素的不确定度评定

本文用过程繁杂的HPLC柱后衍生法测定黄曲霉毒素的不确定度，依据分层建模评定理论进行了评定，对样品的均匀性、检测分散性及提取、净化、食品检测等过程引起的不确定度进行了逐层分析，确定了各分量的分布类型，并进行了分步计算和整体合成，评定过程清晰合理，影响因素不遗漏、不重复，在对其它HPLC法的不确定度进行评定时可借鉴使用。     

Preparation of National CRMs of Active Compounds from Natural Products

According to the standard of GB/T1500.3-2008 and the guidelines of ISO/REMCO, the preparation of National Certified Reference Materials (CRMs) of active compounds was composed of the following two aspects: preparation and certification. This paper presents an example of the preparation of biochanin A to illustrate the preparation of National CRMs of active compounds from natural products. Firstly, the target compound was extracted and purified from crude materials. Then,its chemical structure was identified by UV spectrum, IR spectrum, ESI-MS, and NMR. The purity of the compound was determined by HPLC with the area normalization method. The certified value assessed by comparing the purity values from six independent qualified laboratories and the value of uncertainty were given. Thermal analysis, residual solvent, homogeneity testing and stability testing was tested in the process.     

颗粒计数标准物质定值方法研究

为了探讨颗粒计数标准物质研究中缺乏操作性强、量值溯源可靠的颗粒计数标准物质定值方法等主要技术难点,本文中采用量值可溯源至长度基准的显微图象分析仪,配以血球计数板为球形乳胶颗粒计数标准物质定值,在确定标准值同时对于定值的不确定度进行了分析和研究。研究结果表明:采用这种方法的定值不确定度优于10%(k=2)。     

Multielement trace determination in high purity advanced ceramics and high purity metals

In the field of advanced ceramics two CRMs were developed in the last few years by the Federal Institute for Materials Research and Testing, one for silicon nitride and one for silicon carbide. Besides their application by industry they are appropriate to be used for the validation of special methods used for trace determination in accordance with high purity materials. This is demonstrated, for example, on ultrapure silicon carbide which was analysed by solid sampling electrothermal atomic absorption spectrometry (SS ET AAS). BAM is also certifying primary pure reference materials used as the National Standards for inorganic analysis in Germany. The crucial point of this project is the certification of the total purity of high purity materials, each representing one element of the periodic table. A variety of different analytical methods was necessary to determine the trace contents of metallic and non-metallic impurities from almost the whole periodic table in the high purity materials. The primary CRMs of copper, iron and molybdenum are used as examples to demonstrate the modus operandi, analytical effects observed by using high resolution ICP mass spectrometry (HR ICP-MS) and the results.     

Development of Crude Oil Reference Material Certified for the Concentrations of Sulfur,Iron, Nickel,Vanadium and Magnesium

Crude oil quality and uses are largely affected by the presence of sulfur and some other elements. Controlling the risk associated with these elements in crude oil depends on their accurate determination which is crucially governed by the use of certified reference materials (CRMs). This paper describes the development of a natural-matrix reference material for quantification of sulfur, iron, nickel, vanadium and magnesium in crude oil. The crude oil was homogenized and bottled to prepare the candidate material. Homogeneity and stability of the prepared reference material were investigated and characterization of sulfur content was carried out using wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometry and gravimetric methods. Meanwhile, characterization of iron, nickel, vanadium and magnesium content was carried out using atomic absorption spectrometry (AAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) techniques. Statistical evaluation of the data showed good homogeneity and stability of the candidate reference material. Sufficiently good agreement between methods of characterization was achieved which allowed certification. The certified values and their associated uncertainties were statistically derived using the approach of combining data from two or more independent analytical methods developed by National Institute for Standards and Technology (NIST, Gaithersburg, USA).     

碳黑比表面积标准物质的研制

选择商品化的碳黑作为比表面积标准物质候选材料,利用交叉缩分的方法对碳黑样品进行分装。经均匀性、稳定性(18个月)检验,碳黑标准物质样品具有良好的均匀性和稳定性。按照国际公认的氮气物理吸附BET方法,联合测量能力经确认过的8家实验室对碳黑标准物质样品进行定值(104.6、29.9、8.96 m2/g)。与国内外同类标准物质比较表明:研制的3种碳黑比表面积标准物质的相对不确定度(2.1%、2.3%和3.2%)达到国际同类标准物质的先进水平。     

系列液体和固体水分标准物质的研制

针对水分检测领域对标准物质的需要,研制了系列水分标准物质,包括4种液体水分标准物质,量值覆盖范围为0.139~47.6 mg/g,不确定度范围为0.012~1.1 mg/g;还包括3种含结晶水化合物水分标准物质,量值覆盖范围为50.7~156.3 mg/g,不确定度范围为0.6~1.3 mg/g,以及3种混合物水分标准物质,量值覆盖范围为0.142~9.90 mg/g,不确定度范围为0.013~0.20 mg/g。该系列液体和固体水分标准物质,适用于卡尔·费休库仑法和容量法水分仪的校准和检定,以及水分测量方法的验证,能够保障我国水分检测的量值准确和等效一致。     

粮食中营养成分标准物质制备技术

介绍粮食中营养成分基体标准物质的制备方法和流程,包括总的原则、成分设计、基体选择、物料采集、物料处理、成分初测、粉碎、筛分烘干过程、均匀性初检、分装、辐照灭菌、真空包装及储存。重点讨论和分析制备过程中应注意的细节以及为了保证均匀性和稳定性所采取的措施。