岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2014年
6期
844-848
,共5页
于兆水%张勤%李小莉%樊守忠%潘晏山%李国会
于兆水%張勤%李小莉%樊守忠%潘晏山%李國會
우조수%장근%리소리%번수충%반안산%리국회
生物样品%主次量元素%高压粉末制样%波长色散X射线荧光光谱法%基体效应
生物樣品%主次量元素%高壓粉末製樣%波長色散X射線熒光光譜法%基體效應
생물양품%주차량원소%고압분말제양%파장색산X사선형광광보법%기체효응
biological sample%major and minor elements%high pressure powder pelleting preparation%Wavelength Dispersion X-ray Fluorescence Spectrometry%matrix effect
应用X射线荧光光谱法（XRF）分析生物样品时，采用传统低压粉末制样方法（压强220～440 MPa）难以将样品压制成符合测定需要的样片，样片表面粗糙，粉末容易脱落，污染XRF仪器样品室，影响仪器的长期稳定性。本文采用高压粉末制样方法在1760 MPa下压制则完全克服了低压制样的弊端，制备的样片表面光滑、致密，大幅改善了制样重现性，5次制样重现性为0．1％～2．6％，且降低了仪器的维护成本。在此基础上，建立了波长色散X射线荧光光谱法直接测定生物样品中23种主次量元素（Al、Ca、Cl、K、Mg、Na、P、S、Si、Ba、Br、Co、Cr、Cu、Fe、Mn、Ni、Pb、Rb、Sr、Ti、V、Zn）的分析方法，采用经验系数法、散射线内标法和峰背景作内标校正基体效应，大部分元素的方法精密度提高至0．4％～11．3％，检出限为0．08～140．96μg／g。经国家一级生物标准物质验证，表明方法准确可靠，能满足日常分析要求。
應用X射線熒光光譜法（XRF）分析生物樣品時，採用傳統低壓粉末製樣方法（壓彊220～440 MPa）難以將樣品壓製成符閤測定需要的樣片，樣片錶麵粗糙，粉末容易脫落，汙染XRF儀器樣品室，影響儀器的長期穩定性。本文採用高壓粉末製樣方法在1760 MPa下壓製則完全剋服瞭低壓製樣的弊耑，製備的樣片錶麵光滑、緻密，大幅改善瞭製樣重現性，5次製樣重現性為0．1％～2．6％，且降低瞭儀器的維護成本。在此基礎上，建立瞭波長色散X射線熒光光譜法直接測定生物樣品中23種主次量元素（Al、Ca、Cl、K、Mg、Na、P、S、Si、Ba、Br、Co、Cr、Cu、Fe、Mn、Ni、Pb、Rb、Sr、Ti、V、Zn）的分析方法，採用經驗繫數法、散射線內標法和峰揹景作內標校正基體效應，大部分元素的方法精密度提高至0．4％～11．3％，檢齣限為0．08～140．96μg／g。經國傢一級生物標準物質驗證，錶明方法準確可靠，能滿足日常分析要求。
응용X사선형광광보법（XRF）분석생물양품시，채용전통저압분말제양방법（압강220～440 MPa）난이장양품압제성부합측정수요적양편，양편표면조조，분말용역탈락，오염XRF의기양품실，영향의기적장기은정성。본문채용고압분말제양방법재1760 MPa하압제칙완전극복료저압제양적폐단，제비적양편표면광활、치밀，대폭개선료제양중현성，5차제양중현성위0．1％～2．6％，차강저료의기적유호성본。재차기출상，건립료파장색산X사선형광광보법직접측정생물양품중23충주차량원소（Al、Ca、Cl、K、Mg、Na、P、S、Si、Ba、Br、Co、Cr、Cu、Fe、Mn、Ni、Pb、Rb、Sr、Ti、V、Zn）적분석방법，채용경험계수법、산사선내표법화봉배경작내표교정기체효응，대부분원소적방법정밀도제고지0．4％～11．3％，검출한위0．08～140．96μg／g。경국가일급생물표준물질험증，표명방법준학가고，능만족일상분석요구。
In the determination of biological samples by X-ray Fluorescence Spectrometry (XRF),sample powder pellets pressed by traditional sample preparation technique at 220-440 MPa are not compact and smooth,so the sample room of XRF instrument becomes contaminated by dropped sample powder,which can then influence long-term stability.Biological sample powder can be pressed into smooth and compact pellets using high pressure of 1 760 MPa,therefore the sample preparation reproducibility is improved to 0.1% -2.6% (RSD,n=5 ). A method for direct determination of 23 major and minor elements (Al,Ca,Cl,K,Mg,Na,P,S,Si,Ba,Br, Co,Cr,Cu,Fe,Mn,Ni,Pb,Rb,Sr,Ti,V and Zn)in biological samples by Wavelength Dispersion X-ray Fluorescence Spectrometry was established on this sample preparation basis.The matrix effects can be corrected by using Rh-Kα(from the X-ray tube target)Compton-scattered radiation and by using the background as the internal standard.The precision of the method is 0.4%-1 1 .3%(RSD)for most elements and the detection limits is 0.08-1 40.96 μg/g.The feasibility of the proposed method was tested by analyzing several national biological standard materials;the results obtained were consistent with the certified values.
