乳糖及蛋白质中Na,P,K,Ca元素定量分析检测方案(能散型XRF)

XenemetrixThe Power to Change Energy Into InformationeurocontrolITECHNICS GROUP Application Note #XE-2016-3336 Quantitative elemental analysis of lactose ands einpowder using EDXRF Analyser Genius IF Limor Halay， July 2016 器Exectie 仪summ Five laotose and six protemh powders were received for quantitative elemental analysis using EnergyDispersive X-ray fluorescence (EDXRF) technique. Calibration curves were built separately to lactoseand protein according to ICP analysis received for this samples. The requested elements for analysiswere Na， P， kand Ca. The chemical composition of the powders was determined successfully byperforming simple and fast measurements using the Xenemetrix Genius IF Bench-top system. The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 1. Introduction Xenemetrix's Genius IF EDXRF spectrometer provides a non-destructive qualitative and quantitativedetermination from carbon (Z=6) to fermium (Z=100)， providing detection limits from sub-ppm to highweight percent concentrations. The Genius IF has powerful components including： Kfokyintegratedcomputer system， a high resolution Silicon Drift Detector and a powerful X-Ray toberwith variable spotsizes， designed to accommodate samples of various sizes. The Genius IF has a unique patented optical geometry combining eight becomdary targets， with eightcustomizable tube filters allowing for simple software operatedwitch between the techniques ofsecondary target excitation and direct excitation. Direct excitation mode with different filters can bemade very efficient and optimal for any element detectedinXDXRF. The WAG(Wide Angle Geometry)patented secondary target technique provides the best results in partiular for minor and traceelement analysis. The X-ray tube excites the characteristic K lines of a secondary target (a pure metal)which are used to excite the sample "monochrematically"Bysing secondary targets， the detectionlimits for certain elements can be loweredeven further. These cwer detection limits make the GeniusIF suitable for a larger range of applicetionsythat had preyiqusly not been accessible to conventionalEDXRF instruments， and turnthis istrumnent into the most versatile elemental analyser available. 2. Objective Analyse and measure Na， P， K and Ca in powder samples. This reportsymarizes theresults of a quantitative analysis performed on Genius IF EDXRF analyser. 3. Experimental 3.1.Eqdipment All measurements were conducted on a Genius IF system equipped with a Silicon drift detector withan ultra-thin window (SDD-LE version 1). Direct excitation without any filter was used to analyse P. ATi secondary target excitation was used for the analysis of K and Ca. A Si secondary target excitationwas used for the analysis of Na. The measurement parameters are summarized in table 1. The Power to Change Energy Into Information eurocontrol TECHNICS GROUP Instrument Configuration Genius IF， Rh Anode x-ray tube， 50kV，50W Detector Silicon drift detector (SDD-LE version 1) Atmosphere Helium/Air Excitation mode Direct excitation no filter / Si Secondary target excitation /Ti Secondary target excitation. Acquisition time 60 -600 sec Analysis method Regression curves Table 1： measurement parameters 3.2. Sample Preparation No sample preparation is required in this case. 4. Qualitative Analysis 4.1. Lactose powder 网息信器仪限仅 Representative EDXRF spectrum of Lactose powder acquifed fol Na element is shown in Figure 1below. Zoom In NaMg Na Mg Al S Figure 1： XRF spectrum using Si target with 20kV during 600sec acquisition time in helium atmosphere. Xenemetrix The Power to Change Energy Into Information eurocontrol TECHNICS GROUP Representative EDXRF spectrum of Lactose powder acquired for P element is shown in Figure 2 below. Rh 用 使料张 Rh K Ca传 下NgAL XRFspectiym06po filter with 6kV during 300sec acquisition time in air atmosphere. Xenemetrix The Power to Change Energy Into Information eurocontrol TECHNICS GROUP Representative EDXRF spectrum of Lactose powder acquired for K and Ca elements is shown inFigure 3 below. Ti用使料 公 器仪限 有技科成CaK Ti Ca Figere 3： XRF spectrun using Ti target with 25kV during 600sec acquisition time in helium atmosphere. The Power to Change Energy Into Information eurocontrolTECHNICS GROUP 4.2. Protein powder Representative EDXRF spectrum of Protein powder acquired for Na element is shown in Figure4 below. Figture 4： XRF spectrum using Si tareecoth 20kv dymgsoosec acquisition time in helium atmosphere. 器仪限仅 Representative EDXRF spectrum of Protein powderacquired for P，K and Ca elements is shown inFigure 5 below. 人 Figure 5： XRF spectrum using no filter with 6kV during 30sec acquisition time in air atmosphere. The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 5. Quantitative Analysis 5.1. Lactose powder 5.1.1. Na Results CNa=764.64*INa-251.94， R2=0.9651 用使料 传 Figure 6： calibration curve for Na in Lactose powder.公 Sample No. ICP givencncentration LO XRF calculated concentration m mg/kg #1 97 #2 149 #4 248 #6 36 Table 2：Paalvsis vs. EDAAnalysis for Na in Lactose powder. 人 Xenemetrix The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 5.1.2. P Results Cp=2.04*lp+32.93，R2=0.9920 用使料 Figure 7： calibration curve for P in Lactose powder. Sample No.ICP given concentration ER XRF calculated oncentration #1 201 #2 49 '58 #4 319 #6 Table 3： ICP Analysis ts. E oF analysis fo pa Lactose powder Inter-elements effects weyl aseumed between K and Ca. Sample No. ICP given concentration ED_XRF calculated concentration mg/kg mg/kg #1 214 231 #2 155 144 #4 215 214 #6 133 113 Table 4： ICP Analysis vs. ED-XRF analysis for K in Lactose powder The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 5.1.4. Ca Results Inter-elements effects were assumed between K and CaCca=4422.18*lca+4819.44*lk， R2=0.9962 SampleNo.ICP given concentration ED XRF calculated concentration mg/kg mg/kg #1 369 381 #2 193 184 #4 465 463 #6 225 Table 5： ICP Analysis Vs. ED-XRFanalysis for Ca in Lactose powdtr 5.2. Protein powder 公 5.2.1.Na Results CNa=1090.47*INa+536.02，R2=0.8817 Sample No.【ICP given concentration ED_XRF calculated concentration mg/kg mg/kg #1 4535 5028 #2 2192 2273 #3 1375 1658 #4 1746 1761 #5 4428 3488 #6 1683 1749 The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 5.2.2. P Results Inter-elements effects were assumed between K and Ca Cp=1.32*lp+0.29*lk+0.018*lca，R2=0.7670 Sample No. ICP given concentration ED_XRF calculated concentration mg/kg mg/kg #1 3306 3286 #2 2983 3167 #3 1387 2315 #4 2418 #5 4712 #6 3956 Table 7： ICP Analysis VS. ED-XRF analysis for P in Protein powder 5.2.3. KResults Inter-elements effects were assumedbeoveenK and CajCk=14677.85*lk+294.94*lca，R2=0.8484有 Sample No. I ICP given congentratiom EDXRYcalculated concentration mg/kg #1 4803 #2 8007 #3 4887 #4 6094 #5 13351 A6 5740 6510 Table8：CP AnalySis yS. ED-XRF analysis for K in Protein powder The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 5.2.4. Ca Results Inter-elements effects were assumed between Kand Ca Cca=6415.2324*lca+1674.55*lk， R2=0.7712 SampleNo.ICP given concentration ED_XRF calculated concentration mg/kg mg/kg #1 4387 4143 #2 4970 4801 #3 4622 4244 #4 4930 #5 5420 #6 5757 Table 9： ICP Analysis vs. ED-XRF analysis for Ca in Protein powder 6. Homogeny Analysis 8 samples from the same bulk sample were takan ta8 dfferent sample caps. Each time before asample was taken， the bulk sample was shaken to achieve maximum homogeneity. Distributionof ~4% was found in the Lectoge powderang3% in the protein powder. 7. Precision In order to evaluate the precision of the EDXRF in the fabric sample the same spot was measuredfor 10 tineslThedispersionof resuits，i.e. the standard deviation was calculated per element andthe resukts are presentescn Tables 10 and 11. The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 7.1. Lactose powder P[mg/kg] K[mg/kg] Ca[mg/kg] 1 314 201 437 2 319 199 434 3 324 195 429 4 314 195 428 5 311 198 6 315 194 7 313 194 8 313 9 312 427 10 314 428 Average 315 196 429 STD 4 2.1 4.2 Table 10：10 measurements ofactose semlNo.4 in the same spot. 7.2. Protein powder 器仪限仅 Element R[mg/kg] ^K[mg/kg] Ca[mg/kg] 33k 5039 4422 3382 5053 4368 Average 33371 5058 4396 3394 5092 4413 3385 5153 4403 3420 5137 4397 3408 5116 4426 3378 5121 4471 3400 5196 4444 3353 5078 4390 3384 196 429 23.2 2.1 4.2 1% 1.1% 1.0% Table 11： 10 measurements of protein Sample No.1 in the same spot. 8. Conclusions 8.1. Na，P，Kand Ca analysis in protein/lactose powders can be performed using EDXRFspectrometer with ICP certified standard samples. A main difference between differentanalytical methods is the simple and elegant measurement procedure of the XR method， incomparison with other elemental analysis methods； without any samplepreparationrequired. 8.2. Na is a light element and for lactose powder the concertation-is below .the LOQ (Limit ofQuantitation). The LOQ can be improved by using a higher powe system such as EX-6600. 8.3. In order to take into account all inter-elements effects tbat mnight exist in the powder allsamples (with given concentrations) were considerad while creating the calibration curves. _网息信器仪限仅 8.4. The results accuracy can easily be improved by measurig additional calibration standards ofknown concentrations and adding them to the calibration curve which correlate intensity andconcentration. Application Note # XE-2016-3336 The Power to Change Energy Into Information eurocontrol TECHNICS GROUP 9.Summary EDXRF is a fast and non-destructive technique that can quantify any type of sample： solid， powderor liquid， within a few minutes. EDXRF spectrometers can play an important role inassuring thatconsistent quality of samples is retained throughout a manufacturing process EDXtF is an idealmethod for elemental analysis offering the following adharies √Minimal sample preparation √ Fast and automated analysis process √ Limited or no exposure to corrosive reagents used by cther analytical techniques √Ease of use for operation by non-technical or non-swecfalized personel. Xenemetrix The Power to Change Energy Into Informatiog 公限E有mail： info@xenemetrix.com at Gabriel Industrial Zone， 5 Ha shbret st.，rpaylHaemek 2310901， Israel Web： www.xenemetrixcom Tel： +972-4-989131 器仪限仅 www.linkedin.com/company/xenemetrix-ltd. www.facebook.com/Xenemetrix www.youtube.com/user/Xenemetrix Xenemetrix Confidential information pplication Note # XE-enemetrix Confidential information 二次靶技术X射线荧光光谱仪Genius IF利用Genius IF设备对乳糖及蛋白质中Na,P,K,Ca元素做定量分析。Genius IF的二次靶技术能够对这些轻元素进行有效的定性定量分析，相对于传统滤光片荧光光谱仪，分辨率更高，轻元素探测效果更好。