. 1. 여행목적 : X- 선회절분석장비연수및응용실태조사 2. 동기및배경 ㅇ X-ray spectrometer 장비는하천및호소유역의토양또는저질중에함유된중금속등을 X-ray 투과를통하여측정하는장비로서방사선을이용하므로장비의측정원리나조작방법에대한폭넓은이해가필요함, ㅇ따라서현지제작사를직접방문하여동장비에대한구조, 원리및 S/W 운영에관한지식을습득하고, 또한실제로이장비의운영실태및현장응용현황에대하여사전정보를수집함으로써본장비의효율적인활용을도모할수있을것임. 3. 여행국및방문기관독일 SPECTRO ANALYTICAL INSTRUMENTS GmbH & Co. KG Boschstraβe 10 47533 Kleve Germany Tel: +49-(0)28 21-892-0/ Fax: +49-(0)28 21-892-2200 e-mail: info@spectro-ai.com 4. 여행기간 : 2002. 5. 26 ~ 6. 2 (8일) 5. 출장자 : 한강물환경연구소환경연구관김종민
6. 출장일정 일자 요일 방문기관업무수행내용접촉인물 일 서울출발독일도착 월 SPECTRO 사 회사소개및실험실견학 화 SPECTRO 사 의기본원리설명및응용 수 목 SPECTRO 사 SPECTRO 사 기기운용훈련 작성 검정및보정 등 유지관리및문제해결 재설치 백업 조정 및변환등 금 SPECTRO 사종합토의및질의응답 토 일 귀국
. 1 X-ray Fluorescence technology(xrf) 1. XRF (geology). X- AAS ICP. XRF.,. 1.1? XRF Na U. Na Ce K-lines, Pr U L-lines. Be F X-ray prolene. Table 1 X-lab XEPOS Na U (excitation) Target Target (excited elements) (Voltage) Mo secondary Cr - Y (K), Hf - U 1 (L) 45 2 / 40 3 kv Al 2 O 3 Barkla Zr - Ce (K) 49,5kV HOPG Bragg Na - V (K) 10 4 / 20 5 kv 1 for X-Lab2000 U is done with Al 2 O 3, 2 XEPOS, 3 X_lab2000, 4 solid, 5 liquid
Table 2 XRF Fig. 1 X. 0.02 m grain size
Fig. 2 Fluorine. 1.2 matrix?.. (AAS) XRF. Matrix effect'. matrix.. 3. 1) solvent/matrix. trace analysis ( polymers) 2) matrix 3) matrix effect matrix compton line matrix effect 1 0.5%. XRF, matrix effect.
Fig. 3. X matrix. matrix matrix ( ) X-. Fig. 4. X-.
1.3 (polarization)? spectral background. peak background. X-ray.,,,,. x-ray 90. X- tube target 90. tube x-ray target., detector. x-ray. Fig. 5. XRF : EDXRF, WDXRF EDPXRF
Fig. 6. X- Cartesian 2. 2.1.. (Na Cl ).. 2.2 2.2.1 (pellets) (<100 ) 4g Hoechst Wax 0.9g 15 ton 32mm.
2.2.2 (<100 ) 4g 28mm. 4 prolene foil..
2.2.3 Fusion 100. (<100 ) 1g Lithiumtetraborate 7.0 g 1100 40 mm (bead). 2.3 2.3.1 (Monophased)/ (Polyphased) 32 mm 4 g. 4 prolene film. ( / / ) 6 g 2 g charcoal(merck) 4 g.
2.4 2.4.1 Mill 100. MM200. Ziconium dioxide grinder ( 25ml 10 g ).. 60. TURBOQUANT 100. 2.4.2 Press 15 ton. 2.4.3 Die ( ) Die 15. 2.4.4 Fusion machine. 2.4.5 Hoechst Wax C : pellet Charcoal (Merck) : Spectroflux : Fused beads
Fig. 7. Mill Press 3. calibration method 3.1 TURBOQUANT TURBOQUANT SPECTRO Na U. matrix effect. ( ). 10 20%. Na U (excitation) 3 Target. Na V HOPG target (intense monochromatic non polarized x-rays) (excite). Cr Zr Pr Bi Mo secondary target (intenxe monocromatic non polarized x-rays). Y Ce Barkla Al 2 O 3 target (intenxe polycromatic polarized x-rays).
Table. 3 TURBOQUANT Target Target Type of target Excited elements Mo secondary Cr - Y(K), Pr - Bi (L) Al 2 O 3 Barkla Zr - Ce HOPG Bragg Na - V Fig. 8. Target K L lines (Excitation) TURBOQUANT matrix. 3.1.1. TURBOQUANT for liquids matrix calibration. polyphased liquid. calibration ICP (Merck, Bernd Kraft) oil standards(conostan).
3.1.2. TURBOQUANT for pellets/powder/metals matrix. matrix Compton.. 2 X-lab 2000 1. MCA Calibration ( ) X-lab 2000 MCA pellet 1. pettwt calibration paramter. 1) load. 2) Software load File/ method. 3) MCA calibration (MCA3336) OK. 4) Assigned Standard Samples Box MCA Cal sample ( ). 5) Routine icon 6) Edit icon Measured Spectrum Box Routine Box. 7) Edit Sample Plate Box : Routine for MCA calibration 1 paste. Measure, Evalute, Direct Print. 8) Start. ( 30 operating ) Sample tube film : - 4 m :
- 6 m : Power ( ). Sample 1 10 2. 1) job (file job ) 2) job information box new 3) create new job. 4) sample box new 5) Enter/edit sample date box General Information box @sample name, @comment, @method, @contro; sample. 6) @method select method. (TQL3336 : liquid, air : powder, tablet :, glass : ) 7) Optional entries box OK. 8) Sample Boxso. 9) Routine icon Edit icon. 10) Edit samplr plate box. Routine for sample plate. sample ( 1 ) paste. Measure, Evaluate, Direct print. 11) START. 12) Data job select file OK print
. Dr. Clemens Schaefer, X-ray specialist ( ), Spectro analytical instruments, Boschstra e 10, 47533 Kleve, Germany Tel.: (+49)(0) 28 21 892 4144/ Fax: (+49)(0) 28 21 892 2203 e-mail: CSchaefer@spectro-ai.com Dr. Rainer Schramm, Director sales/ XRF, Spectro analytical instruments, Boschstra e 10, 47533 Kleve, Germany Tel.: (+49)(0) 28 21 892 2144/ Fax: (+49)(0) 28 21 892 4239 e-mail: Rschramm@spectro-ai.com. 1. XRF FUNDAMENTALS, Dr. Rainer Schramm, Spectro analytical instruments, 2002 2. Spectro X-lab Pro software training Manual