便携式X射线荧光光谱法(PXRF)在肥料重金属快速检测中的应用

为了探讨一种简单快捷的肥料重金属含量测定方法,本文采用便携式X射线荧光光谱仪(PXRF)测定了我国典型设施农业生产区肥料中As、Pb、Cu、Zn和Cr的含量,并与常规实验室方法的测定值进行比较,以验证PXRF法测定结果的准确性。结果表明:①PXRF对土壤标准物质中As、Pb、Cu、Zn的测定值与标准值之间的相对标准偏差和相对误差均小于10%,表明该仪器测定As、Pb、Cu、Zn的精密度和准确度较好;②肥料中重金属PXRF法测定的检出限均低于相应的国家或行业标准。当含量超过检出限时,有机肥和无机肥中As、Pb、Cu、Zn和Cr常规实验室方法测定值与PXRF法测定值间均达到了极显著相关,R2在0.70～0.99;③PXRF法的检测成本仅为常规仪器的10%?20%,节省了前处理的时间和费用。因此,PXRF法可用于肥料中重金属含量的快速检测与评价。     

便携式X射线荧光光谱法(PXRF)在矿区农田土壤 重金属快速检测中的应用研究

针对我国普遍存在的土壤重金属污染问题,迫切需要开展土壤重金属的快速检测与评价方法研究。本文采用便携式X射线荧光光谱法(PXRF)和传统实验室方法对云南会泽铅锌矿区农田土壤As、Pb、Cu和Zn进行测定,分析了PXRF法的应用效果。结果表明:1PXRF法测定的精密度与准确度满足我国农田土壤环境质量检测技术规范中规定的仪器检测要求;2土壤As、Pb、Cu和Zn的PXRF法测定值与传统实验室测定值具有良好的一致性,Pb、Cu和Zn的决定性系数均大于0.70;3基于PXRF法原位测定、PXRF法异位测定和传统实验室测定结果的研究区土壤As、Pb、Cu和Zn具有相似的空间分布规律。可见,PXRF法可用于矿区周边农田土壤As、Pb、Cu和Zn的快速检测、污染筛查与评价。     

样品粒径、制样方法对波长色散X射线荧光光谱法测定土壤样品中19种元素的影响

利用波长色散X射线荧光光谱仪建立了压片、熔融土壤样品中As、Co、Cr、Cu、Mn、Ni、P、Pb、S、Ti、V、Zn、Al2O3、CaO、Fe2O3、K2O、MgO、Na2O、SiO₂ 19种元素的分析方法。探讨了样品粒径、制样方法对19种元素检测的影响。方法精密度结果表明,样品中As、Co元素含量在10 mg/kg以上时,0.149 mm(100目)样品压片、0.075 mm(200目)样品压片及样品熔融制样的19种元素的相对标准偏差(RSD)值均小于10 %,As、Co含量在10 mg/kg以下时,200目压片制样的19种元素RSD值小于10%。准确度结果表明,压片制样的标准物质含量在5 mg/kg以上的As、Co、Cu及其他16种元素准确度符合要求;熔融制样的标准物质中高含量的As、Co、Cu、Pb元素及其他15种元素准确度符合要求。不同粒径实验结果显示,元素含量在10 mg/kg以上时,100目、200目压片制样19种元素的RSD值小于10%。不同制样方法的实验结果表明,熔融制样不适用于低含量的As、Co、Cu、Pb元素分析,Cr、P、S、Mn、Ni、V、Zn、Ti、Al2O3、CaO、Fe2O3、K2O、MgO、Na2O、SiO₂ 熔融制样与压片制样RSD值小于10%。压片制样方法操作更简单,成本更低,更适用于大批量土壤样品中As、Co、Cr、Cu、Pb、P、S、Mn、Ni、V、Zn、Ti、Al2O3、CaO、Fe2O3、K2O、MgO、Na2O、SiO₂ 19种元素的分析;对于As、Co元素含量在10 mg/kg以上的样品,利用100目、200目样品压片制样均可获得准确、可靠的结果,对于As、Co含量在10 mg/kg以下的样品,建议使用200目样品压片制样。     

熔融制样—X射线荧光光谱法快速测定复合肥中的磷、钾、钙、镁、锰、铁、铜、钠、锌和铝

为实现复合肥样品中多元素的同时分析,采用熔融片法制样,有效地消除了试样的粒度效应,用X射线荧光光谱法测定复合肥样品中磷、钾、钙、镁、锰、铁、铜、钠、锌和铝10个元素,对仪器工作条件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,以8个合成的样品作为校准样品,采用固定理论α影响系数进行回归及基体效应校正,方法精密度(RSD,n=8)≤1.36%,分析结果与化学法进行对照基本一致。     

Rapid multimineral determination in infant cereal matrices using wavelength dispersive X-ray fluorescence

A rapid and simple method for the determination of a series of macroelements (sodium, magnesium, phosphorus, chlorine, potassium, and calcium) and trace elements (manganese, iron, and zinc) by wavelength dispersive X-ray fluorescence has been developed and validated for infant cereal matrices. Reference values were obtained by inductively coupled plasma optical emission spectroscopy and by potentiometry. The 88 investigated samples were commercially available products. Pellets of 4 g were prepared under 10 tonnes of pressure. For each sample, 3 pellets were prepared and analyzed. Limits of quantification and repeatabilities were evaluated. Calibrations were established with 43 samples, and method validation was made using a second set of 45 samples. An evaluation of this alternative method was done by comparison with data obtained from the reference methods. The results show the good performances of the alternative method to routine infant cereals analysis.     

液相色谱 -原子荧光光谱法测定水溶肥料中无机砷含量

采用液相色谱 -原子荧光光谱法联用技术,建立了水溶肥料中无机砷含量的检测方法。对样品前处理条件进行了优化。在最佳实验条件下,As 3+和 As 5+在线性范围内线性关系良好,线性相关系数( R)分别为0.999 6和 0.9998,检出限分别为 0.8和 2.7ng/mL;对 3个样品平行测定 6次,无机砷测定相对标准偏差(RSD)为 1.90%～ 3.66%,加标回收率为 91.9%～ 107.5%。研究表明,可将本方法应用于不同类型的水溶肥料中无机砷检测。     

Analysis of selected elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry

A rapid method for the determination of 16 elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry has been developed. The method is accurate and precise, and requires only 9 min per sample for quantitation. Sample preparation consists of placing a portion of dried, ground tobacco in a sample cup, and pressing at 25 tons pressure to make a compressed pellet. This pellet is then automatically analyzed by X-ray fluorescence for 16 elements. The results are stored on a computer disk for future recall and report generation.     

Automation of dihydroxyaluminum sodium carbonate analysis in antacid tablets by energy dispersive X-ray fluorescence

A sensitive, specific, automated energy dispersive X-ray fluorescence (EDXRF) method for determination of anhydrous dihydroxyaluminum sodium carbonate in antacid tablets has been developed. The compound was quantitated by impact grinding, pelletizing at 10 tons pressure, and monitoring the aluminum by using a rhodium anode X-ray tube, high resolution thermoelectrically cooled Si(Li) detector with sample spinning, and computer data processing. The assay procedure was validated with spiked laboratory-prepared samples at 100 +/- 20% levels. The average recovery was 100.6% with a relative standard deviation of 1.6% (n = 14). Instrument precision was determined and found to have an average relative standard deviation of 1.0% (n = 16). In addition, analysis precision by the EDXRF method was compared to that for titration and autoanalyzer methodologies and found to be statistically comparable. The sample precision had an averaged relative standard deviation of 2.7% (n = 16) by X-ray methodology. The advantages of this EDXRF method include increased sample throughout with excellent precision and accuracy, no solvent usage, and automated data handling.     

含硝酸盐类水溶肥料的安全性研究

为研究含硝酸盐类水溶肥料的安全性,选取了5种硝酸盐类原料,设置了21种两两混配的硝酸盐样品,从获得农业农村部产品登记证的2 605个国内外硝酸盐水溶肥料中筛选出20种产品,分别采用固体氧化性试验方法对以上样品进行测试。结果表明:肥料行业中常用的六水合硝酸锌与六水合硝酸镁为非氧化性物质,硝酸钾、硝酸钠和硝酸钙分别为Ⅱ类和Ⅲ类氧化性物质,氧化性顺序为硝酸钾硝酸钠硝酸钙;筛选的20种水溶肥料产品中有50%的样品为氧化性物质,表明存在一定的安全风险;建议在今后的产品审批中,对肥料配方中硝酸钾含量超过75%和硝酸钠含量超过85%的水溶肥料产品进行氧化性试验,对达到氧化性物质标准的应在产品备案、包装识别、标签、生产、运输、储存中加大管理力度。     

沼液基含腐植酸水溶性液体肥制取工艺参数优化

为探索沼液开发含腐植酸水溶性液体肥的可行性和工艺方法,促进沼液无害化处理和资源化利用,该文以沼液为基料,以黄瓜配方肥为基肥,螯合剂、稳定剂为辅料,开展了不同工艺参数(沼液添加量、稳定剂添加量、螯合剂添加量,反应温度,反应时间)对含腐植酸水溶性液体肥质量指标影响的单因素和正交试验。结果表明:沼液、螯合剂、稳定剂添加量以及反应温度、时间对液体肥中水不溶物含量有重要影响,沼液制取黄瓜专用型含腐植酸水溶性液体肥的较优工艺参数为:基肥添加量为原料质量的39.6%,沼液添加量为59%,螯合剂添加量为4%,稳定剂添加量为0.4%,反应温度为40℃、反应时间为1.5 h的条件下,所获得的液体肥中总养分质量浓度为220.47 g/L,腐植酸质量浓度为33.25 g/L,水不溶物质量浓度为18.6 g/L,利用该工艺方法生产出来的沼液基含腐植酸水溶性液体肥料产品具有腐植酸、氮磷钾营养元素含量高、水不溶物含量低等特点。该研究为利用沼液开发高品质含腐植酸水溶性液体肥提供技术支撑。     

Multielement analysis of soft drinks by X-ray fluorescence spectrometry

Several commercial soft drinks and respective plastic bottles were analyzed for their multielement contents employing the synchrotron radiation total reflection X-ray fluorescence spectrometry technique (SRTXRF). The SRTXRF method has been developed and validated, and about 20 elements were detected in the investigated samples, including some trace elements, which can be toxic for human beings, such as Ti, Cr, Sb, As, and Pb in soft drinks and Al, Sb, As, and Pb in poly(ethylene terephthalate) (PET) containers. Statistical analysis was performed using chemometric techniques (principal component analysis and cluster analysis), and similarities were verified in the multielement contents of the samples. The results demonstrated that the SRTXRF offers a good multielemental approach for the quality control of food products. Moreover, on the basis of enrichment factors, the possibility of the trace elements in the PET container may be leached to the beverages under normal commercial situations and other results were discussed.     

氢化物发生--原子荧光光谱法同时测定肥料中砷、汞的研究

通过对消化体系的选择及双道原子荧光光度计测试条件的优化,建立了氢化物发生—原子荧光光谱法同时测定肥料中砷、汞的方法。方法线性范围宽(As 0~100μg/L;Hg 0~10μg/L),检出限低(As 0.05μg/L和Hg 0.007μg/L)。无机肥料中As回收率为98.8%~100.4%,Hg回收率为98.9%~102.2%;有机肥料中As回收率为94.4%~105.6%,Hg回收率为97.6%~103.8%。     

氢化物发生——原子荧光光谱法同时测定肥料中砷、汞的研究

通过对消化体系的选择及双道原子荧光光度计测试条件的优化，建立了氢化物发生-原子荧光光谱法同时测定肥料中砷、汞的方法。方法线性范围宽（As0-100μg／L；Hg0-10μg／L），检出限低（As0．05μg／L和Hg0.07μg／L）。无机肥料中As回收率为98．8％-100．4％，Hg回收率为98．9％-102．2％；有机肥料中As回收率为94．4％-105．6％，Hg回收率为97．6％-103．8％。