Abstract No. 63. Applications of Borate Fusion for X-Ray Fluorescence Analysis
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1 Abstract No. 63 Applications of Borate Fusion for X-Ray Fluorescence Analysis Author: Dr. Rainer Schramm, FLUXANA GmbH & Co. KG, Borschelstr.3, Bedburg-Hau, Germany Tel , Fax ,, Abstract In steel industry x-ray fluorescence analysis (XRF) is a well established analytical method. Beside the direct measurement of metal samples, other samples will be measured as pressed pellets or fused beads. This presentation will present state of the art fusion technique for different applications in steel industry. A comparision of traditional gas based fusion systems and new modern electric fusion systems will be given. Based on different applications like raw materials, ferro alloys, slags or continuous casting powder all important analytical parameters will be discussed. A new development for the determination of volatile elements like fluorine, chlorine or sulphur from fused beads will be presented.
2 FLUXANA Applications of Borate Fusion for X RAY Fluorescence Analysis Rainer Schramm, 9th International Conference, Düsseldorf Company Portfolio FLUXANA Commercial XRF Analysis DIN EN ISO/IEC Accreditation for XRF from DAkkS (flexibel accreditation) Application development Sample Preparation machines Production and sales of Reference Materials Proficiency tests Service
3 FLUXANA XRF Laboratory: 2 PerformX and 1 QuantX WDRFA / EDRFA Method development based on pressed pellets FLUXANA Method development based on gas fusion systems
4 FLUXANA Method development based on electrical fusion systems Development of new certified reference materials Organisation of proficiency tests XRF contract analysis as service (DIN EN ISO/IEC 17025) FLUXANA
5 Applications related to Steel Industry FLUXANA laboratory: Raw materials Ferro alloys Slags Continuous casting powder Materials: Sand, limestone, clay, gypsum, iron ore, dolomite, alumina, etc. Application Raw Materials XRF Application of raw materials Sample preparation: electrical or gas fusion system XRF: WDXRF Standards: available as CRM glass beads
6 Sample preparation fusion Sample preparation: Preparation as dublicates Dilution 1:8 FX X65 (66% LIT : 34% LIM) Electrical fusion system C XRF instrument: Thermo PerformX WDXRF Calibration: Fundamental parameter Example: Application Raw Oxides Set of standards used for calibration (all CRMs) 1/2 RAW 01b RAW 02 RAW 03a RAW 04a RAW 05a RAW 06 RAW 07 RAW 08 RAW 09a RAW 10 RAW 11 RAW 12 RAW 13 Dolomite Granite Slag Phosphate Bauxite Limestone Limestone Clay Fe2O3 Gypsum Gypsum Sand Iron ore Al2O3 0,20 12,17 6,24 4,96 89,470 3,85 0,212 35,93 0,130 2,57 0,036 12,463 BaO 0,013 0,14 0,006 0,006 0,05 0,003 0,013 CaO 57,46 0,786 31,39 23,72 0,081 77,89 98,02 0,193 41,17 35,66 0,006 4,599 Cr2O3 0,002 0,004 0,018 0,07 Fe2O3 0,86 2,01 0,79 3,76 1,914 1,41 0,080 1,18 99,998 0,060 1,370 0,012 55,737 K2O 0,050 5,03 0,38 3,212 0,020 0,720 0,035 2,54 0,030 0,680 0,005 0,693 MgO 40,71 0,060 19,01 8,70 0,121 1,10 0,265 0,341 0,230 2,19 0,001 1,732 Mn2O3 0,173 0,023 0,873 0,04 0,151 0,019 0,001 0,3663 Na2O 3,38 0,24 0,171 0,020 0,180 0,035 0,387 0,010 0,090 0,003 0,108 P2O5 0,024 7,402 0,222 0,196 0,009 0,081 0,010 0,030 2,368 SiO2 0,51 76,26 39,24 47,39 5,018 14,19 1,24 58,10 0,560 11,00 99,84 20,87 SO3 1,44 0,031 57,810 46,41 0,302 SrO 0,067 0,105 0,034 0,138 0,228 TiO2 0,008 0,091 0,392 0,586 3,133 0,213 0,016 1,23 0,017 0,567 ZnO 0,016 Sum 100,01 99,87 100,14 100,00 100,15 100,01 100,01 100,05 100,00 100,15 100,24 99,92 99,88
7 Example: Application Raw Oxides Set of standards used for calibration (all CRMs) 2/2 RAW 14 RAW 15 RAW 16 RAW 17a RAW 18b RAW 19cRAW 20c RAW 21 RAW 22 RAW 23 RAW 24 RAW 25 Dolomite Bauxite P Cement Cement P Cement Cement Clinker P Cement P Cement Al Cement Al Cement Cement Al2O3 0,63 77,81 4,85 5,55 4,62 5,56 4,84 4,10 6,29 69,74 39,24 4,43 BaO 0,004 CaO 56,56 0, ,48 64,70 61,45 64,94 63,46 61,78 29,39 39,39 65,30 Cr2O3 0,067 0,003 0,008 0,02 0,009 0,006 0,113 Fe2O3 0,52 12,42 0,300 2,62 2,72 3,32 4,15 1,96 2,90 0,08 14,71 3,96 K2O 0,195 0,013 0,11 0,81 0,68 0,95 1,08 0,21 1,12 0,01 0,05 0,50 MgO 39,71 0,017 0,42 1,48 2,11 3,05 1,82 4,10 2,88 0,19 0,51 0,95 Mn2O3 0,034 0,006 0,057 0,065 0,049 0,120 0,003 0,060 0,064 Na2O 0,055 0,100 0,22 0,11 0,15 0,14 1,05 0,49 0,299 0,021 0,084 P2O5 0,008 0,071 0,12 0,163 0,124 0,31 0,003 0,070 0,192 SiO2 2,13 5,41 21,8 20,95 21,53 22,19 22,09 21,27 18,91 0,24 4,02 21,25 SO3 0,21 2,25 2,98 3,07 2,66 0,39 2,88 4,69 2,96 SrO 0,014 0,11 0,285 0,649 0,327 0,019 0,024 0,086 TiO2 3,77 0,04 0,283 0,330 0,335 0,242 0,198 0,270 0,020 1,790 0,243 ZnO 0,001 0,051 0,003 0,068 Sum 99,87 99,83 100,16 99,95 99,88 99,67 99,70 100,06 100,16 100,00 100,00 100,00 Calibration Raw Materials CaO with electrical fusion machine 24 CRMs as duplicates (green) SEE: 0,30% 7 control samples (orange)
8 Control samples for CaO Raw materials Control samples Certificate Results CRM CaO % u(cref) 95% CaO % bias % NIST 1413 sand 0,74 0,04 0,75 0,01 GYP C gypsum 41,04 0,94 41,11 0,07 BAS ironore 7,98 0,11 7,87 0,11 GBW 7108 rock 54,13 0,38 54,23 0,10 BAS 513 limestone 98,58 0,28 98,59 0,01 FX CRM 101 cement 48,24 0,15 48,19 0,05 Sample preparation: Mean value of 3 duplicates Materials: FeSi, FeSiMn, FeSiMnP, FeMo, FeTi, FeV, FeW, FeNb Application Ferro Alloys XRF application of ferro alloys Sample preparation: gas or electrical fusion system XRF: WDXRF Standards: available as CRM + synthetic glass beads
9 Ferro Alloys Sample Preparation Direct method: sample, oxidizer and flux at once in crucible one fusion program with oxidation step 2 step method: sample and oxidizer in crucible fusion program for oxidation only addition of flux main fusion program Internal standard method: addition of an internal standard element Sample preparation: Preparation as duplicates 0.2g sample 1g V 2 O 5, 8g LIT WO 3 int. Standard Gas fusion system VULCAN XRF instrument: WDXRF Calibration: empiric Example FeSi Calibration standards: SARM33, HC 14606, HC 14607, BS 140/1, BS 140/2, BS 140/3, BS 140/4, F3/3 5 synthetic standards to fill gaps
10 2 certified reference materials: Control sample FeSi HC25627 Al Ca Cu Fe Mn P Si Certificate 1,8 0,3 0,172 0,023 76,74 1 1,88 0,31 0,03 21,47 0,175 0,024 76,62 2 1,90 0,28 0,04 20,33 0,172 0,014 76,70 3 1,89 0,32 0,03 20,78 0,180 0,021 76,72 4 1,88 0,29 0,04 20,52 0,184 0,024 76,77 5 1,91 0,30 0,03 20,38 0,168 0,021 76,57 6 1,90 0,29 0,03 20,36 0,178 0,021 76,74 Mean 1,90 0,30 0,03 20,64 0,176 0,021 76,69 STDEV 0,01 0,013 0,003 0,44 0,006 0,003 0,08 bias 0,10 0,02 0,32 0,01 0,001 0,001 0,00 IPT70 Al Ca Cu Fe Mn P Si Certificate 0,21 0,16 0,066 54,1 0,283 0,018 44,7 1 0,23 0,13 0,08 53,67 0,298 0,027 44,82 2 0,23 0,12 0,09 53,78 0,298 0,019 44,85 3 0,23 0,13 0,09 53,38 0,288 0,021 44,83 4 0,22 0,13 0,09 53,78 0,294 0,017 44,71 5 0,24 0,14 0,08 53,64 0,292 0,024 44,74 6 0,20 0,12 0,08 54,19 0,303 0,015 44,62 7 0,22 0,13 0,08 53,98 0,299 0,019 44,63 8 0,22 0,13 0,08 55,05 0,298 0,014 44,82 Mean 0,22 0,13 0,09 53,93 0,296 0,019 44,75 STDEV 0,01 0,006 0,004 0,51 0,005 0,004 0,09 bias 0,01 0,02 0,32 0,01 0,001 0,001 0,00 Special functions for ferro alloys Observation of the oxidation Opening of the furnace on top to let gases going out to avoid long term contamination Use of a lid to avoid spitting in the furnace Electrical fusion system
11 Application Continuous Casting Powders Materials: Products of continuous casting powder (up to 20% carbon) XRF application of continuous casting powders Sample preparation: electrical fusion system XRF: WDXRF Standards: available as CRM glass beads Sample preparation fusion Sample preparation: Preparation as duplicates Dilution 1:8 FX X65 (66% LIT : 34% LIM) Electrical fusion system 1200 C XRF instrument: WDXRF Calibration: Fundamental parameter Calibration standards: DH SX 30 05, DH SX 30 13, DH SX 30 11, DH SX 30 12, NIM G, No , 7212, CRM101, BCS 348, NIST 1883 A, NIST 1882 A 11 synthetic standards to fill gaps
12 Calibration CC Powder and RAW materials F in CaF 2 with electrical fusion machine 8 Standards as duplicates Certified concentration [%] SEE: 0,27% LOC Mg, Fe Control sample Continuous Casting Powder Electrical fusion system: DH SX F Al2O3 CaO Fe2O3 K2O MgO MnO2 Na2O P2O5 SiO2 TiO2 Certificate 6,01 7,19 39,19 0,32 0,256 0,779 0,053 7,09 0,034 41,35 0, ,176 7,204 39,445 0,312 0,251 0,769 0,054 7,006 0,035 41,129 0, ,055 7,189 39,458 0,310 0,260 0,775 0,055 6,967 0,035 41,134 0, ,175 7,151 39,425 0,313 0,262 0,759 0,053 6,999 0,039 41,093 0, ,398 7,189 39,516 0,318 0,255 0,776 0,054 7,032 0,033 41,187 0, ,221 7,248 39,595 0,313 0,255 0,778 0,051 6,993 0,032 41,233 0, ,914 7,224 39,498 0,312 0,252 0,777 0,053 7,067 0,038 41,261 0, ,011 7,178 39,475 0,316 0,261 0,791 0,052 7,052 0,036 41,132 0, ,234 7,207 39,527 0,312 0,250 0,766 0,054 7,026 0,038 41,358 0, ,981 7,231 39,520 0,314 0,253 0,808 0,054 7,182 0,035 40,970 0, ,236 7,243 39,620 0,312 0,258 0,799 0,051 7,234 0,035 41,231 0,039 Mean 6,14 7,20 39,51 0,313 0,255 0,780 0,053 7,05 0,035 41,17 0,038 STDEV 0,147 0,031 0,063 0,002 0,004 0,015 0,001 0,086 0,002 0,106 0,001 bias 0,13 0,02 0,32 0,01 0,001 0,001 0,000 0,034 0,001 0,18 0,010 Comparison with VULCAN gas fusion system: Mean 6,07 7,18 39,03 0,321 0,244 0,782 0,059 7,18 0,032 41,16 0,035 STDEV 0,544 0,084 0,064 0,012 0,005 0,016 0,002 0,150 0,003 0,094 0,001 bias 0,06 0,01 0,16 0,001 0,012 0,003 0,006 0,097 0,002 0,19 0,007
13 Summary Fusion applications related to steel industry in the FLUXANA laboratory Raw materials pressed pellets and fusion Ferro alloys fusion Slags pressed pellets and fusion Continous casting powder fusion Gas and electrical fusion systems complementary Further development of CRMs Organisation of PT Thank you for your attention!
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