电感耦合等离子体原子发射光谱法测定土壤中有效钼的含量

通过对国家土壤有效态一级标准物质GBW07413、GBW07414中有效钼含量的测试,采用电感耦合等离子体原子发射光谱法,以草酸-草酸铵浸提土壤中的有效钼,在优化实验条件下方法的检出限为0.01mg/kg,测定结果与标准值相吻合,实验结果表明:电感耦合等离子体原子发射光谱法测定土壤有效钼的方法简便、快速、成本低,能够应用于土壤样品中有效钼的分析。     

ICP-AES内标法测定钛铁矿中铜钴镍锰钒铬

采用HCl-HNO3-HF-H2SO4溶矿,利用电感耦合等离子体发射光谱仪内标法（ICP—AES）测定,建立了钛铁矿、钒钛磁铁矿中铜、钴、镍、锰、钒、铬等元素的同时测定方法。对电感耦合等离子体发射光谱仪测定的最佳仪器条件及分析谱线进行了选择,并对钛、铁基体的影响以及采用Y内标元素消除基体的影响进行了研究。实验结果表明：采用内标法能够消除基体对被测元素的影响,改善分析准确度和精密度,与经典分光光度法和原子吸收法相比较,具有检出限低、灵敏度高,操作简便、快速等突出优点。方法经国家一级钒钛磁铁矿标准物质验证,测定值与标准值吻合。     

河南省地矿局制定3个地方标准获批发布

<正>日前,河南省质量技术监督局发布2017年第26号公告,批准发布了河南省地方标准。其中《虎睛石》(DB41/T1427—2017)、《铁矿石赤铁矿、褐铁矿总量的测定滴定法》(DB41/T1438—2017)、《天然碱化学分析方法钠、钾等11种元素量的测定电感耦合等离子体发射光谱法》(DB41/T1439—2017)等3个地方标准由河南省地矿局提出并归口。     

电感耦合等离子体光谱法测定铜矿中砷的含量

采用电感耦合等离子体发射光谱法(简称光谱法)测定铜矿中砷的含量.光谱法用硝酸溶解样品,无须分离铜、铁、硅等元素,直接于全谱直读等离子体发射光谱仪上测定砷含量.克服了传统铜矿中砷分析方法步骤繁琐、耗时长、工作量大,以及需特殊装置的不足.该方法测试准确、可靠,可满足铜矿中砷的分析要求.     

实验用新方法测定含钡硫酸盐中的锶

目前,含钡硫酸盐中锶的分析方法是以火焰原子吸收法等传统的化学分析方法为主,测定过程冗长,操作步骤繁琐,费时费力,且干扰很大。而电感耦合等离子体发射光谱法的分析技术已经特别成熟,这种方法具有稳定、高效、准确度高、精密度好、线性范围广等优点。本文采用ICP-OES法测定含钡硫酸盐中的锶:试料用无水碳酸钠,草酸,硝酸钾混合溶剂分解,水提取,过滤。沉淀用热盐酸溶解后,用ICP-OES测定锶元素的含量,经标准物质准确度验证,获得满意结果。     

ICPAES法同时测定钛铁矿中钾钠钙镁钡锶锌

采用HClHNO3HF HClO4,HClHNO3HF H2SO4敞口和HClHNO3HFHClO4,HClHNO3HF H2SO4微波消解4种方法溶矿,利用电感耦合等离子体发射光谱（ICPAES）测定,建立了钛铁矿中钾、钠、钙、镁、钡、锶、锌等元素的同时测定方法。对电感耦合等离子体发射光谱仪测定的最佳仪器条件及分析谱线进行了选择,并对钛、铁基体的影响、溶矿提取酸度以及溶矿残渣进行了研究。实验结果表明：采用HClHNO3HF HClO4敞口溶矿,具有检出限低、灵敏度高,操作简便、快速等突出优点。该方法测定值与推荐值基本吻合,分析方法的精密度满足《地质矿产实验室测试质量管理规范》的要求。     

电感耦合等离子体发射光谱法测定钛铁矿中主、微量元素

采用氢氟酸-盐酸-硝酸-硫酸四酸溶矿,建立了电感耦合等离子体发射光谱仪法(ICP-AES)同时测定钒钛磁铁矿、钛铁矿中铝、钙、镁、钾、钠、锰、钛、铬、锶、锌和钒11种元素的方法。对最佳仪器条件及分析谱线进行了优化筛选,并探讨了4种消解方法及酸度对测定的影响。实验结果表明:ICP-AES法测定钒钛磁铁矿、钛铁矿中铝、钙、镁、钾、钠等元素,与原子吸收光谱法、分光光度法、滴定法、重量法等单一元素测定方法相比较,具有检出限低、灵敏度高、测量范围宽、操作简便,适合大批量样品测定等突出优点。方法准确度(RE)小于10%,元素精密度(RSD,n=12)为0.68%~5%。采用国家一级标准物质进行了方法验证,取得了令人满意的结果。     

地质样品中稀土元素的分析方法研究进展

对近年来地质样品中稀土元素的分析方法进行了评述,指出了各方法的特点、适应性和存在的问题。特别对电感耦合等离子体质谱法测定稀土元素的干扰及样品处理和引入方法作了介绍,激光烧蚀进样和高分辨电感耦合等离子体质谱联用技术是今后稀土分析的方向。     

ICPAES法测定超基性岩中13元素的方法研究

采用HCl-HNO3-HF-HCl O4,HCl-HNO3-HF-H2SO4敞口,HCl-HNO3-HF-HCl O4密闭和HNO3-HF密闭消解4种方法溶矿,利用电感耦合等离子体发射光谱(ICP-AES)测定,建立了超基性岩石中钾、钠、钙、铝、铁、钛、锰、钴、镍、铬、钒、锶、锌等元素的同时测定方法。对电感耦合等离子体发射光谱仪测定的最佳仪器条件及分析谱线进行了选择,并对镁基体的影响进行了研究,采取标准溶液中加入适量的镁作基体匹配,以消除基体影响。实验结果表明:采用HNO3-HF密闭溶矿,具有检出限低、灵敏度高,操作简便、快速等突出优点。该方法测定值与推荐值基本吻合,分析方法的精密度满足《地质矿产实验室测试质量管理规范》的要求。     

磁铁矿LA-ICP-MS原位微量元素分析方法研究

激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)技术在矿物微量元素分析方面具有原位、高分辨率和高灵敏度等优势，近年来磁铁矿LA-ICP-MS原位微量元素研究进展迅速，并在地质领域得到了广泛应用。利用长安大学成矿作用及其动力学实验室Agilent 7700X四极杆等离子体质谱和Photo Machines Analyte Excite 193 nm激光，建立了LA-ICP-MS测定磁铁矿原位微量元素组成的分析方法。以美国地质调查局(USGS)玻璃标样BIR-1G、BHVO-2G、BCR-2G和GSE-1G为校正标准，采用无内标-多外标法对磁铁矿中微量元素进行了定量计算，并测定了NIST612和自然岩浆磁铁矿BC28的微量元素组成，以评估本实验室建立方法的可靠性。结果表明，NIST612所有微量元素的相对标准偏差(RSD, N=30)变化于1.31%~6.33%之间，多数元素的测定结果与推荐值及前人LA-ICP-MS方法测定值的相对误差小于10%；BC28大部分微量元素的相对标准偏差(RSD, N=30)小于10%，其中11个重要微量元素与前人LA-ICP-MS测定值的相对误差基本小于10%。以上结果表明本实验室建立的方法可以实现对磁铁矿原位微区微量元素的分析测定，分析数据结果准确可靠，具有良好的应用前景。      

菱镁矿、蛇纹岩、碲金矿化学成分标准物质研制

当前我国尚无菱镁矿、蛇纹岩、高品位碲金矿化学成分标准物质,国外相应标准样品存在定值元素少,且主成分含量不成系列,不能满足地质行业对菱镁矿、蛇纹岩、碲金矿标准物质的迫切需求。该文研制了菱镁矿、蛇纹岩、碲金矿化学成分标准物质共12个,将采自典型矿区的样品按照常规球磨方式粉碎混匀,采用电感耦合等离子体发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)进行均匀性和稳定性检验,选择11家有资质的实验室,采取经典分析方法与现代仪器分析方法相结合的方式,选用2种以上不同原理的准确度高的可靠方法对该标准物质联合定值,依照JJF 1343—2012和一级标准物质技术规范,12个化学成分标准物质给出了30项主、微量元素的认定值和不确定度。其中,菱镁矿Mg O的含量范围为43.64%~81.26%,蛇纹岩Mg O的含量范围为23.73%~43.09%,高品位碲金矿Au的含量范围为19.6×10~(-6)~32.1×10~(-6)、Te的含量范围为51×10~(-6)~83×10~(-6),基本涵盖我国菱镁矿、蛇纹岩、高品位碲金矿的矿物类型,能够满足菱镁矿、蛇纹岩、碲金矿勘查、评价和开发的需求。     

Membrane preconcentration of iron in seawater samples and on-site determination in spectrophotometry

A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection. Fe(Ⅱ)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(Ⅱ)-ferrozine-CTAB paired compound, which was collected on a membrane by filtration under vacuum. The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis. Various factors affecting the iron collection and determination were investigated. With different sample preconcentration volumes, the range of determination was broadened to 0.5-120 g/L. The detection limit of this method reached 0.19 g/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45. The relative standard deviation (n = 7) was 1.9% for samples containing 10 g/L Fe. Twelve seawater samples were analyzed on-site using the proposed method, and two were also analyzed in inductively coupled plasma mass spectrometry. No significant difference was shown between the two methods by the Student’s t-test. The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple, accurate and inexpensive.     

The influence of seafloor hydrothermal activity on major and trace elements of the sediments from the South Mid-Atlantic Ridge

Sediment samples obtained from the South Mid-Atlantic Ridge were analyzed for the major and trace elements by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry. Results revealed that the contents of elements (e.g., Fe, Mn, Cu, Zn, V, Co) were high in samples 22V-TVG10 and 26V-TVG05 from the sites near the hydrothermal areas, and low in sample 22V-TVG14, which was collected far from the hydrothermal areas. The contents of Ca, Sr and Ba in the samples showed opposite trends. A positive correlation between the concentrations of metallic elements (Cu, Zn, Co, Ni, Pb, V) and Fe in the samples were observed. These results are consistent with chemical evolution of the dispersing hydrothermal plume.     

Inorganic Elemental Determinations of Marine Traditional Chinese Medicine Meretricis concha from Jiaozhou Bay:The construction of Inorganic Elemental Fingerprint Based on Chemometric Analysis

The goal of this paper is to explore the relationship between the inorganic elemental fingerprint and the geographical origin identification of Meretricis concha,which is a commonly used marine traditional Chinese medicine(TCM) for the treatment of asthma and scald burns.For that,the inorganic elemental contents of Meretricis concha from five sampling points in Jiaozhou Bay have been determined by means of inductively coupled plasma optical emission spectrometry,and the comparative investigations based on the contents of 14 inorganic elements(Al,As,Cd,Co,Cr,Cu,Fe,Hg,Mn,Mo,Ni,Pb,Se and Zn) of the samples from Jiaozhou Bay and the previous reported Rushan Bay were performed.It has been found that the samples from the two bays are approximately classified into two kinds using hierarchical cluster analysis,and a four-factor model based on principle component analysis could explain approximately 75% of the detection data,also linear discriminant analysis can be used to develop a prediction model to distinguish the samples from Jiaozhou Bay and Rushan Bay with accuracy of about 93%.The results of the present investigation suggested that the inorganic elemental fingerprint based on the combination of the measured elemental content and chemometric analysis is a promising approach for verifying the geographical origin of Meretricis concha,and this strategy should be valuable for the authenticity discrimination of some marine TCM.     

电感耦合等离子体原子发射光谱法测定小麦中的微量元素

小麦是中国北方人的主要粮食作物,小麦中含有大量的对人体有益的微量元素,查明这些微量元素的含量对于人体健康具有非常重要的意义。电感耦合等离子体(ICP)测试微量元素具有灵敏度高的特点。该文利用ICP的特点,将小麦硝化分解后,测试小麦中的微量元素,使用美国生产Optima 2100 DV型电感耦合等离子体发射光谱仪,对小麦中人体有益的微量元素硼、铁、钙、镁及重金属污染指标铜、铅、锌进行测试,该方法具有样品的加标回收率和RSD较好,分析速度快、分析结果准确可靠的特点。     

What Depth Should Deep-Sea Water be Pumped up from in the South China Sea for Medicinal Research?

In this study, seawater was pumped up from 150, 200, 300, 500 and 1000 m in the South China Sea and analyzed to make certain what depth should deep-sea water (DSW) be pumped up for medicinal usage. The pumping depth of DSW was determined on the basis of chemical ingredients. The analyses of inorganic elements and dissolved organic matter (DOM) were performed by inductively coupled plasma mass spectrometry (ICP-MS) and ultra performance liquid chromatography-mass spectrometry (UPLC-MS) respectively. The raw data were used for hierarchical cluster analysis (HCA) and principal component analysis (PCA). The results showed that seawater pumped up from 500 m and 1000 m was similar in their chemical ingredients, and was different from the seawater pumped up from other depths. These results indicated that seawater from more than 500 m depth had relatively stable chemical ingredients and could be used as DSW in the South China Sea.