火焰原子吸收光谱法测定铬质引流砂中铁镁含量

建立了火焰原子吸收光谱法连续测定铬质引流砂中铁、镁含量的分析方法。试样以碳酸钠-硼酸混合熔剂熔融,以盐酸浸取,在校准溶液中加入重铬酸钾和二氧化硅进行基体匹配,抵消基体影响。对熔剂、熔融温度等进行讨论,确立了最佳分析条件,对样品多次测定,其测定结果与国家标准测定方法测定的结果基本一致,相对标准偏差(RSD,n=11)小于0.3%,加标回收率在98.7%~101%。方法具有操作简便、准确性好、速度快、成本低等特点。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定铬矿砂及再生铬矿砂中二氧化硅

铬矿砂及再生铬矿砂经1 000℃灼烧,研磨,以过氧化钠为熔剂,经高温熔融,热水洗涤,盐酸、硝酸酸化前处理样品,直接用电感耦合等离子体原子发射光谱法测定铬矿砂中的二氧化硅。研究了熔融试样时引入的基体元素钠对被测元素的干扰情况,结果表明,过氧化钠加入为1.5g对检测干扰影响小。采用加基体铬、铁有效克服了基体效应对测定的结果影响。硅的检出限为0.004 9mg/L,二氧化硅测定范围为0.010%~6.0%。对铬矿砂标准物质进行测定,结果与标准值一致,方法相对标准偏差(RSD,n=10)小于1%,克服了常规重量法步骤繁琐、耗时长、工作量大的不足,大大提高了检测效率,满足生产需要。     

电感耦合等离子体原子发射光谱法测定新购及再生铬矿砂中二氧化硅

新及再生铬矿砂经1000℃灼烧,研磨,以过氧化钠为熔剂,经高温熔融,热水洗涤,盐酸、硝酸酸化前处理样品,直接用电感耦合等离子体发射光谱法测定铬矿砂中的二氧化硅。试验了熔融试样时引入的基体元素钠对被测元素的干扰情况,结果表明,过氧化钠加入为1.5克对检测干扰影响小。采用加基体铬、铁有效克服了基体效应对结果影响。硅的检出限为0.0049 mg/L, 二氧化硅测定范围为0.010%～6.0%。对铬矿砂标准物质进行测定,结果与标准值一致,方法精密度(RSD,n=10)小于1%。常规重量方法步骤繁琐、耗时长、工作量大的不足。本检测方法大大提高了检测效率,满足生产需要。     

镁铝铬质耐火材料的X射线荧光光谱分析

将XRFS法应用于Mg-Al-Cr耐火材料中10元素（包括主成分及微量组分）的同时测定。对分解试样的熔剂作了系统研究，发现以1：1混合的四硼酸锂和偏硼酸锂具有最佳熔融效果，所得熔块光滑透明而均匀。选定的熔融温度和时间为1150℃和15min。试样和熔剂的质量比以1：8为好，所得试样在熔剂中的分散度（浓度）适当，可同时适合试样中高、低含量组分的测定，采用熔融法分解试样的方法有效地消除了试样的粒度效应。对仪器工作条件（包括X-光管的电流及电压、分光晶体的选用等）进行了试验并选定最佳条件，使各元素测定所要求的灵敏度和准确度得到满足。此外，采用理论α系数校正法克服了基体吸收及增强效应。用4个标准样品按所提出的方法进行分析，以考核方法的精密度和准确度。10元素的测定结果与其标准值完全相符。     

偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱(ICP-AES)法测定石膏中多组分含量

石膏在我国储量丰富,应用广泛,快速准确分析其成分含量对石膏资源的综合利用具有重要意义。针对酸溶法无法测定SiO2,碱熔法无法测定K2O、Na2O的问题,本文建立一种偏硼酸锂-四硼酸锂熔融-电感耦合等离子体发射光谱法同时测定石膏中CaO、SO3、Al2O3、Fe2O3、MgO、TiO2、K2O、Na2O、SiO2含量。实验优化了熔剂用量、熔融温度,结果表明采用试样与偏硼酸锂-四硼酸锂混合熔剂质量比例1：5,在铂金坩埚中1000 ℃熔融10 min,在超声条件下,于50 mL 10 %盐酸中浸取熔融物,能够有效分解试样而浸取待测组分。向标准溶液系列中加入偏硼酸锂-四硼酸锂-盐酸基体溶液以消除基体对测试结果的影响。各待测组分的校准曲线的相关性系数均大于0.9990,方法检出限在3~292 μg/g范围内;采用实验方法分别对国家一级标准物质GBW03109a、GBW03110和实际样品进行测定,标准物质的5次平行测试的相对标准偏差在0.14 %~8.86 %之间,测定结果的相对误差在0.03~8.75 %之间,测试结果与标准值无显著性差异;实际样品中各成分测定值的RSD（n=5）为0.24~8.80 %。该方法操作简单、准确度高、精密度好、检出限低,可以同时测定石膏中的多组分含量,能够为石膏资源综合利用调查评价提供一定的技术支撑 。     

电感耦合等离子体发射光谱法测定钇铝石榴石中掺杂Yb(Ⅲ)离子

采用碳酸钠-硼砂(质量比1：1)做熔剂分解钇铝石榴石,并确定了熔剂的最优化条件．以电感耦合等离子体光谱法对样品中掺杂Yb(Ⅲ)离子作了定量检测考察了样品和熔剂中单个基体和混合基体对分析结果的影响．发现单个基体Y对Yb的测定有增强效应．基体A1对Yb的测定有一定的抑制作用;基体对Yb测定的干扰可通过基体匹配进行消除元素的俭出限为2μg／L,标准加入回收率为88％～100％实际样品7次检测的RSD为2．1％。本方法可以较好地满足实际样品分析的需要。     

熔融制样-波长色散X射线荧光光谱法测定铁矿石中12种主次成分

采用熔融制样法对铁矿石进行熔融制样;以三氧化二钴(Co2O3)作为铁的内标,并对熔剂、氧化剂、脱模剂、熔融温度和熔融比例进行了讨论。采用理论α系数法、经验系数法校正基体效应和各元素的谱线重叠干扰。建立了波长色散X射线荧光光谱(WDXRF)测定铁矿石中12种组分的分析方法。本法测定铁矿标准物质(GBW07822-GBW07830)各组分的相对标准偏差(RSD)在0.41%~4.2%之间,测定值与标准值相符,且与电感耦合等离子发射光谱的对比测定结果一致。利用本法对实际铁矿样品的全铁含量进行测定,结果与化学分析法的测定结果基本一致。     

熔融制样-X射线荧光测定钨钼锡矿中的主次成分

采用熔融制样-X射线荧光光谱法测定矿物中的Cu、Pb、Zn、Mo、W、Al、Fe、Si、K、Na、Ti、Ca、Sn等13种主次量元素,采用混合均匀的三混熔剂,以硝酸锂为氧化剂、溴化锂为脱膜剂,进行实验条件优化选择。在650℃下对样品进行预氧化,在1100℃下高温熔融,熔融时间为300 s,最后制成均匀透明,表面光滑无气孔的熔片,以部分国家一级标准物质和自制的钨钼锡标准样品,熔融制片进行测定,线性拟合建立标准曲线,并通过测定谱线选择、基体校正,使钨钼锡的测定范围扩宽,从微量到主量均能进行测定,并且适用于多种不同矿石的测定。样品的组成和含量变化会对分析线强度造成吸收、增强以及谱线重叠的影响,采用经验系数和理论α系数结合来校正其产生的基体效应。相同条件下熔融10个标准样品进行测定,其相对标准偏差(RSD)均小于5%,表明方法的准确度、精密度均满足国家相关质量标准的要求。选用一些含量不同的标准样品进行测定,最终的测定结果与标准值相符,表明方法可用于钨钼锡矿的测定。     

熔融制样-X射线荧光光谱法测定白云石中主次量组分

建立了熔融制样-X射线荧光光谱法(XRFS)同时测定白云石中氧化钙、氧化镁、二氧化硅、三氧化二铝、三氧化二铁、二氧化钛、氧化钾、氧化钠、五氧化二磷含量的方法。称取混合熔剂(由质量比67∶33的四硼酸锂和偏硼酸锂混合而成) 6.000 0 g,先将一半熔剂倒入铂-金坩埚中,然后加入碘化铵0.2 g和干燥好的样品0.900 0 g,混匀后,再将剩余的混合熔剂覆盖在表面,在1 000℃熔融12 min,得到的玻璃样片供XRFS分析。以标准物质、光谱纯试剂和基准试剂混合熔融制备校准用标准样品系列,以经验α系数法进行基体校正和谱线重叠效应校正。结果显示:校准曲线的相关系数为0.993 8～1.000,检出限为9.31～129.1μg·g~(-1);对实际样品进行单天内重复测定11次和11天的重复测定,测定值的相对标准偏差(RSD)不大于6.0%和10%;对11个平行制备的样品进行单天和11天连续测定(每天1个样品),测定值的RSD不大于7.0%和8.0%;方法用于分析标准物质和实际样品,测定值和认定值或按GB/T 3286-2012所得测定值的误差均在GB/T 3286-2012的允许差范围内。     

惰气熔融-红外法测定镍钛合金中的氧含量

针对镍钛(NiTi)合金中的氧含量进行研究,建立了惰气熔融-红外吸收法测定NiTi合金中氧含量的新方法。研究了不同助熔剂、称样量、分析功率、分析时间及比较器水平对测定结果的影响。确定采用镍做助熔剂,分析功率为4.0至5.5kW,分析时间为30s,比较水平为2的条件对NiTi合金中氧含量进行测定。惰气熔融-红外法测定NiTi合金氧含量相对标准偏差为1.8%,对标准样品的测定结果与标准值基本相符。方法操作简单,分析速度快,能满足生产要求,对工艺研究和产品质量控制具有积极意义。     

熔融制样X射线荧光光谱法测定碳酸盐岩样品中的主次成分

采用复合熔剂玻璃熔片法制备样片，X射线荧光光谱法测定碳酸盐岩样品中SiO₂、Fe₂O₃、Al₂O₃、TiO₂、CaO、MgO、K₂O、Na₂O、MnO和P₂O₅等主次成分.使用理论α系数校正基体效应，国家一级标准物质验证，方法简单快速.测量结果各元素相对标准偏差（RSD，n=12）低于10%（除含量在检出限附近的元素外），检出限低，能够符合地矿行业的要求.     

The optimization of an ICP injection technique and the application to the direct analysis of small-volume serum samples

The optimization and the analytical properties of an injection technique for the analysis of small-volume samples (50–200 μl) by inductively coupled plasma atomic emission spectroscopy (ICP-AES) are described. Samples are injected into a small funnel connected to a concentric glass nebulizer. A 3 kW argon/nitrogen ICP with power stabilization is used as excitation source. When operating the nebulizer at an argon pressure of 5 bar, relative detection limits for calcium, copper, iron, magnesium and zinc (0.2–50 $\text{ng}\text{ml}$) are a factor of 2 to 10 higher when compared with ICP methods using continuous nebulization. However, the full power of detection of the injection method is obtained at a 50 μl sampling volume. Matrix effects caused by sodium salt concentrations of 5 $\text{g}\text{l}$ are lower than 10%. Relative standard deviations s_r,(I_X) ranged from 0.03 to 0.07. The method was applied to the sequential determination of trace elements (copper, iron and magnesium) in human serum samples after a 1 + 4 dilution with Herrmann solution. The accuracy of the method is illustrated by the analysis results for calcium, copper, iron, magnesium and zinc in a series of test serum samples.     

Flow-injection spectrophotometric determination of chloramben

Abstract

A method for the dechlorination of PCB mixtures (Aroclor formulations) to biphenyl was extended to soils. The contaminated sample was mixed with magnesium flakes, potassium hexachloropalladiate (K₂PdCl₆), propan-2-ol and water then permitted to react for up to six hours. Biphenyl, recovered by extraction into hexane, was quantified by gas chromatography with flame ionization detection. The reaction was very efficient in propan-2-ol / water (～95%), surfactant emulsion or sand mixture and virtually complete in soil provided that excess magnesium (2 g) and the K₂PdCl₆ were added to the sample prior to the addition of water. Higher PCB loadings were readily determined in field contaminated soils either by direct determination within the matrix or by standard additions. However, analyte concentrations were appreciably over-estimated in Soxhlet or sonication extracts of a certified reference material that contained sub-ppm levels of analyte. The over-estimation is considered to result from the conversion in part of natural organic matter to biphenyl.     

Nondestructive 14 MeV neutron activation analysis of magnesium in spheroidal cast iron

The problem of determination of low magnesium concentration (0.02–0.13%) in the presence of a matrix of high activity (nearly 100% of iron) was solved. The²⁴Mg(n, p)²⁴Na(T=15.02 h) reaction was chosen. Since the neutron flux density decreasing with the distance from the target centre (r) slower than 1/r², a facility for simultaneous and long irradiation (1 hour) of six samples was performed. Time of decay t_d=24h. The determination limit corresponding to the 33% relative standard deviation amounted to 0.02% Mg (200 ppm).     

Determination of calcium,magnesium, and phosphate in the presence of iron and each other

Excess EDTA and MgSO₄ solution is added to a mildly acidic solution of the sample containing calcium, magnesium, iron, and phosphate ions. Addition of NH₄OH to this solution results in the precipitation of MgNH₄PO₄·6H₂O and various iron compounds. Calcium ions and a portion of the magnesium ions stay in the solution as the respective EDTA chelates. The mixture is adjusted to a known volume and filtered. The EDTA content of the filtrate with the exception of the EDTA tied up as calcium-EDTA chelate, is titrated with standard CaCl₂ solution at pH 12.5–13.0 in the presence of hydroxy naphthol blue indicator. The calcium content of the sample can be calculated from the result of this titration.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定铸造用硅砂中的Fe2O3、Al2O3、CaO、MgO、TiO2、K2O、Na2O

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铸造用硅砂中Fe_2O_3、Al_2O_3、CaO、MgO、TiO_2、K_2O、Na_2O的方法。研究了溶样方法的选择优化,采用硝酸、氢氟酸溶样,冒高氯酸处理,通过元素分析线的选择,基体和共存元素影响的消除,在最佳的仪器分析条件下得出了方法的线性范围、相关系数及检出限。用硅砂3个梯度含量的标准物质的分析结果评价方法的准确度和精密度。方法的检出限Fe为0.012μg/mL、Al为0.032μg/mL、Ca为0.27μg/mL、Mg为0.003 2μg/mL、Ti为0.002 1μg/mL、K为0.16μg/mL,Na为0.000 44μg/mL。5次数据的相对标准偏差说明方法稳定性较好。方法适用于铸造用硅砂中Fe_2O_3、Al_2O_3、CaO、MgO、TiO_2、K_2O、Na_2O含量的测定。     

Characterization of hot particles in surface soil around the Chernobyl NPP

An ICP-AES method for the analysis of trace amounts of lanthanides and yttrium in sodium or magnesium diuranate samples (yellow cake) and other beneficiation product generated during the uranium extraction process (hydrometallurgy) from its ores is described. Most of the matrix elements are removed by an initial oxalate precipitation of lanthanides using calcium as carrier. A solvent extraction procedure using a mixture of mono 2-ethylhexyl dihydrogen phosphate (H₂MEHP) and bis (2-ethylhexyl) hydrogen phosphate (HDEHP) is used for the removal of calcium, iron and the occluded uranium. A combination of oxalate precipitation and solvent extraction procedure is applied for the selective separation and preconcentration of traces of lanthanides from yellow cake and iron cake samples. The solvent extraction procedure is directly applied for the separation of lanthanides from the uranium leach liquor and lime cake. The accuracy of the method is checked by analyzing synthetic mixture containing known amounts of traces of lanthanides and also by comparing with another standard separation procedure like ion exchange method, and the recovery was better than 95%. The method is rapid, simple, accurate and suitable for the separation of lanthanides from uranium, iron and calcium rich materials. The precision of the method is characterized by an RSD of 2 to 4%.     

东江河砂中微量元素的含量分析及其治疗作用机理

东江河砂外用治疗中医风湿痹证，疗效确切。用原子吸收分光光度法测定了该河砂中铁、锰、钴、锌、铜、钠、镁、钾的含量，并对其在砂疗中的作用进行了探讨。     

Complexometric determination of aluminium in iron ore,sinter, concentrates and agglomerates

A method for the complexometric determination of aluminium in iron ore, sinter, concentrates and agglomerates encountered in international trade is described. The sample is fused in a zirconium crucible with a mixed flux of sodium carbonate and sodium peroxide. The fused mass is completely soluble in hydrochloric acid. The R₂O₃ oxides are then precipitated with ammonia and redissolved in hydrochloric acid. Elements such as iron, titanium and zirconium are separated from aluminium by solvent extraction with cupferron and chloroform. After removal of traces of organic matter from the aqueous phase, the solution is treated with an excess of EDTA, which is then back-titrated with zinc solution (Xylenol Orange as indicator). Addition of ammonium fluoride then releases EDTA equivalent to the aluminium and this is titrated with zinc solution. The method is rapid. The precision and accuracy are excellent, and the results comparable with those obtained by the referee method.     

Trace metal studies of selected white wines: an alternative approach

A number of white wines from vineyards outside the metropolitan region of Melbourne were analyzed for the trace metals copper, iron, potassium, sodium, magnesium and calcium by atomic absorption spectrometry (AAS). The 24 wines analyzed included Chardonnay, Sauvignon Blanc, Riesling, Gewürztraminer and Pinot Gris. In addition, preliminary transmission near infrared (NIR) spectrometric analyses for these metals in the above wines indicated, using both multiple linear regression (MLR) and partial least squares (PLS), that promising results may be obtained for some metals. The squared correlation coefficients (R²) and the ratios of the standard error of cross validation (SECV) and the standard deviation (S.D.) for the calibration models for potassium, sodium, magnesium and calcium were acceptable, however those for iron and copper were not. Although, only a small number of wines were used in this study, the preliminary data indicated that NIR spectrometry may provide a suitable, rapid method for analysis for some metals in white wines, and warrants a further investigation using a larger number of white wines over a wider range of locations.