SCOHIA)\, NOLAN NOISNTAVMOWIAL 40 JOOSGNV]] Y waosouzypoy wag fq LOUVZZ WLS LAK WALAGZE A ON ee A aw ral (AVE . vy Ce aeNotice ‘CEM Corporation has repared this handbook for use by users of EM equipment andor cf _ does rot represert.a commiment onthe part of CEM Corperation. “The microwave equipnent used it the preparation of procedures described in this manual is covered by US Patents. CAUTION Appropriate safety precautions must be observed when working with hot molten reagents and high temperature furnaces. These precautions include, but ae not limited to these of insulated eves for hundling al ofthe cricbes and tongs fer grasping the metal crucibles. A Handbook of Microwave Fusion Pepaation Methods” as writes by Eva Ratenerva, Institue of Metalurgy and Materials ical University Kosice, loka whilem lave at “The Department of Chemisty Ledere Sraduate Research Center, University of Mischusets ‘Amst Masset USA [MAS 7000™sa traderark, and CEM sa mgstered rademark of CEM Crporation Moos mi Table of Contents Flow Diagram of Fusion Decompe ‘Table of Flux Materials ard Matrices ‘Table of Flux Materials ard Melting Point ‘Table of Flux Ratios for Sdected Inorganic ‘Table of Matrix to Flux Retios for Lithium ‘Metaborate Stock Solutons for AS .. 1B, Ekments Analyzedin Peruvian Soil. 38 2B. ICP Results for Per-viah $0 nsw 3B. Detection Limits in Blank Flux Soluticns... 4B, Analytical Detection Limits in Fused Flux 5B, Analytical Detectior Limits in Fused Flux Blanks in G2 (6B, Recommended Levels of Maor Analytes in Pt and . Platinum Crucible Fusion Blanks Graphs nenWSN MISS AN SEA Q WEN SEAN is WSCEZAM INTRODUCTION ‘The most important and most time-consuming step in an analysis is often ‘the sample pretreatment. Unfortunately, the majoriy of modem inorganic ele- ‘mental analytical techniques like Graphite Fumace Atornic Azsorption ‘Spectrometry (GFA), Inductively Coupled Plasrra-AtomicEmission Spectrometr, (ICP-AIS), or Anodic Stripping Voltanmetry (ASV) require the sample in sdution. Thus, dissolution is ofen the lnitin factor when using high efficiency analytial equiprent. ‘Many organic materials dissolve inacids at thir boiling temperature in ‘open vessels The lst becomes longer when high pessure disotutions in closed vessels with thermal er microwave heating are inclded. However, there are stil a number of mateials lke bumt refractory; cenentalurrinates;sibcates; Th and Zr ores slags; Be,Si and Almixed ors, Cr Si and Fe oxides; W, Si and Al rived oxides, and SiC that ether completely resist attack by acids, or dissolve very slowly or only patially in acids. The best wayto dissolve or to speed up the dissolution ofthese material isby Fusion, A fuson can beused also for ‘decompositin of insoluble residues left by acid digestion. Fusion é a heterogeneous action between a fix, usually an inorganic sak, and sanple matefal that ismade to cur at high temperature. Asa result, the original mineral or refractory phases are brokendown and converted to dif- ferent solid forms thatare more readily dissolved by acids bases, or water. ‘Decomyosition ofmany resstant phases may cxcur at temperatures lower ‘than the furxreagent’smelting point. This prooedur: is know as sintering, Sintering desomposiins are empirical particular onditions frequently apply only toa cerain type of material and may not be applicable to other materials {1}. Generally the following procedure could be reccmmendet: the sample and the flux shotld be very finely pulverized and thoroughly med. An advantage ofthis procedure is tt platinum (Pt) crudles could be usedin combination with sodium peroxide(Na.O) at temperatures below 480 °C. Analytical prac- tice has mairly emploved sintering with alkali carbonates ané peroxides either alone or mixed with oxides, mostly those of divalert cations [I].‘Aheavy duty heat source is newssary for performing fusions. Simple and retro Sach furaces opie camdrtably over the range from om tere ture to 1200°C. This handbook i a cllection of microwave fusion methods for the prepa- ration of difficult-to-disolve samp material for which the metal content ‘must be analyzed. These matrices have proven dificultto decompose by tadi- ae , 7 niques, and micowave-heated dosed vessd (Na) in Ni, Zs, and GC crucibles for the determination of metals by spectroscopic methods. Themujorcorstituentis TiO: EQUIPMENT: MAS-7000 Microwave Mufe Furnace CRUCIBLES: Ni, 30 0150 mL, Feher Scertiic 24,35 oF 55 ml, Fisher Scientific GC, 30m, Sigracur EMC Industries REAGENTS: Sodium Peroxide, 779%, ACS, Aldrich Hydrochloric Aci 37%, A.CS, Fisher Scientific Hydrofluoric Add 48%, A.CS, E. Merck ‘TIME: The total decompesition time of Rutile Ore by this ‘method i 20-30 ninutes. PROCEDURE: 1. Weigh 20 g of Nas into crucble. 2 Weigh 0.2 of Rutile Ore and mixit with NeOsin the ‘rucible using Por glas rod. 3. Put the crucible into the humace ard punge te cavity with nitrogen Progam the marowave unit as follows 4. Take the crucible out ofthe cavity and cool for3-5 minutes. 5. Leach the melttwice with 10 ml- deionized water, pour the slurry into a 10) mL beaker, rinse the crucible twice wih 10 mL of 5% Hcland once with 5 mL5% HCL Add al slurrss to the beaker. 6. Heatthe solution modentely until dear a Incase of fusion in Ni crucible, the black NiO has tobe disolved. be ncase of fio in Zr cle, tis neces to Final lution tori apronimately 0.2g/50 mL.EQUIPMENT: CRUCIBLES: REAGENTS: TIME: PROCEDURE: DECONPOSITICN OF cx Al:Os BY FUSION WITH SODIUM PEROXIDE + This method providesfor the decomposition of a - ALOs by fuson with sxdium peroxide (N03) in N, Zr, and SC crucites forthe detemuination of metals by spectroscopic mechods. The ‘mar constitient is AIOs- usually betwen 90 to 10% MAS-7000 MicrowaveMutffle Ferace Ni,30 or 50 nL, Fisher Scientific Zs, 35 0r 55 nl, FisherScientific GC 30 mL, Sigradur EMC Industries The total decomposition time of «= ALOs by this method 4s 35-45 minutes, 1. Weigh 3( g of Na: into crucible. 2. Weigh 0. g of a ALOs and mix it with NasOs inthe crucible ting a platinum or glass rod. 3. Put the cucibe ino the furnace and parge the civity with nitrogen. Program the microwave unitas follows: 7 ne 4. Take the aucible ott of the cavity and cool for 3.5 minutes. 5. Leach themelt twice with 10 mL of debnized water, pour 6. Heat the solution rroderately until lea: «In caseof fusionin Ni crucible, the Hack NiO hs tote dso Final diluion factoris 02g/50 mL. DECOMPOSITION OF o: - Al:Os BY FUSION WITH LITHIUM METABORATE OR LITHIUM TETRABORATE SCOPE This method provides for te decomposition ofc - alumina by tually Between 90 t0 1003. EQUPMENT MAS-7000 Microwave Mutfle Fumace CRUCIBLES Pt 30 ml, Fisher cientiic Graphite 85 ml, Spex REAGENTS. Lithium Metabonte or Littium Tetraborate, 9.997%, Johnson Matthey Nitric Acid, 67%,A.CS, Fisher Scientific TIME: The total decomposition tine of a - ALOsby this method is 45-50 minutes PROCEDURE: 1. Weigh 05 g o/LiBO: orLiBO; into crucible. 2. Weigh 0.1 g of e.- ALOsand mix t with LiEO: or LisEO: in the crucble using a Ft or glass tod. 3, Put he crucibie into the furnace and purge the cavity with nitrogen. Program the microwave unit as follows:DECOMPOSITION OF CANMET ROCK MRG - 1 BY FUSION WITH SODIUM PEROXIDE ‘SCOPE: This methodprovides{or the decomposition of Carmet Rock ‘MKG-1 by fusion withsodium peroxide (Na:O:) in Ni, Zs, and ‘GC cruciblesfor the determination of mets by spextroscopic ‘methods. The major canstituents are 39326 SiOs 17.85% FeOs 850% AlOs; 369% TiO. EQUIPMENT: MAS-7000 MaowaveMuffle Fumace CRUCIBLES: Ni, 30 0r 50 ml, FisherScientific Zs, 35.0r 56 nL, Fisher Scientific GG, 30 mL, Sigradur EMC Industries REAGENTS: Sodium Peroxide, 97.9%, ACS, Aldrich Hydrochloric Acid, 375, A.CS, Fisher Scientific HydrofluoricA cid, 489, A.CS, E. Merck TIME: The total decompositio time of Canmet Rock MRG1 by this, ‘method is 20-30 minues. PROCEDURE: 1. Weigh 20g of NaiGsinto a cucble. vith 10 mc of HCl and once with SL 9% Hand add all sles tothe beaker. 6. Heat the lution moderately until deat 2. Incase of fusion in Ni crucbl, the back NiO has to be dissolved. ». Incase fusion in Zr crucble itis mcessary © add 1 nl. HF to dear the solution. DECOMPOSITION OF CANMET ROCK MRG -1 BY FUSION WITH ‘SODIUM PEROXIDE AND LITHIUM METABORATE MIXTURE ‘SCOPE This method provdes for the decomposition of Canmet fock ‘MRG- by fusion with sodium peroxide (Na.O;) + lithiura ‘metaborate LiBO: mixture iz GC crucibles for the determination ‘of metals by spectoscopic methods, The major constituerts are 39.32% SOx 17 85% FeO; 850% ALO; 36% TOs. EQUIPMENT: MAS-7000 Microwave Mute Furnace ‘CRUCIBLES: GC, 30 mL, Sigracur EMC Industries REAGENTS:Sodium Peroxide, 95% purisp.a, Fluka Lithium Metaborae, 99.9975, Johnson Matthey ‘Hydrochloric Acid 30%, Suprapur, EM Science NOTE: The total decompesition time of Canmet Rock MRG-1 by this, ‘method is 20 minutes, ‘Weigh 10 g olNaO» ard 05 g LiBO: into the crucible. ‘Weigh 0.1 g ol Canmet Rock MRG-1 and mix it with NasO: + LiBOs mixture in the cucble using Ptor glass rod. 3, Put the crucibie into thefurnace at 700°C and purge the cavity with nitrogen Program the micrwave unitas follows: PROCEDURE: 1. 2 fl z a i é ° i a 3 2 i z a LE i | E Final dilution actor is 01 g/50 mL.DECOMPOSITON OF CANMET ROCK MFG-1 BY FUSION WITH LITHIUM METABORATE OF LITHIUM TETRA3ORATE ‘SCOPE: EQUIPMENT: CRUCTBLES: REAGENTS: PROCEDURE: ‘This method provides ior the decomposition of Carmet Rock are 39.32% SiD17 A5%6FeOy 8.50% ALOs3.69% Tis. ‘MAS-7000 Merowave Mule Furnace 4,30 mL, Fither Scentfic Graphite, 85m, Spex Lithium Metiborate orLithium Tetraborat,99.997%, Johnson Matthey Nitric Acid, %, A.CS, Fisher Scientific ‘The total decemnposition time of Canmet Rock MRGI by this method is 45. 50 minus. 1. Weigh 05g of LiBC. of LiBO into a cucble. 2. Weigh 0.1 of Carmet Rock MRG-1 ard mix it with |iBO: oF LEBO> in the crucible using P-or glass 1d. 3. Pathe cre inthe famace and purge he city with DESOMPOSITION OF PERUVIAN SOIL SRM 4355, BY FUSION WITH SODIUM PEROXIDE ‘SCOPE: This method provides for the decomposition of Peruviar Soil ‘SRM 4355 by fusin with sedium peroxide (NaO)) in Ni Zr, and (GCerudbles for he deterrination of metals by spectrossopic ‘methods. The maor constituents are 70.6% SiO 15.50% ALOs 64% FeOy 3.18% Ca. EQUPMENT: MAS-7(00 Microwave Muse Furnace CRUCIBLES : Ni, 30 0°50 ml, Fisher Scientific 1,35 0155 ml, Fsher Scientific GC, 30 ml, Sigradur EMCIndustries REAGENTS: Sodium Peroxide, 97.9%, ACS, Aldrich Hydrochloric Adi, 37%, ACS, Fisher Scientific Hydrofhuoric Ac, 48%, ALS, E. Merck ‘TIME: The total decompxsition tine of Peruvian Soll by this methodis 25-35 minutes. PROCEDURE: 1. Weigh2.0 ofNa.Or nb crucible. 2. Weigh 02g ofSoil and mix it with NasOs in the cructle using Ptor glass rod. 3. Pat the crucibe into thefumace and purge the cavity with nitrogen. Progam the microwave unit as fllows: 10 ml. of 5% HCl and once with Sm 5% HCI and acd all lures to the beaker. 6, Heal the soluton moderately unt ear. a. Incase of fusion in N crucible, the black NiO has b be dissolved. 1b. Incase of fision in Z: crucible, its necessary toDECOMPOSITION OF PERUVIAN SOIL SRM 4355 BY FUSION WITH LITHIUM METABORATE SCOPE: This method providesfor the dezompositin of Perwvian Soil ‘SRM 4355 by fusion with lithium metabonte (L:BO) in platirum. or graphite cucibles fer the determination of metals by spect— 15.50% ALOs; 64% FeO 3.18% CaO. EQUIPMENT: MAS-7000 MicrowaveMuffle Fumace CRUCIBLES: Pt, 30 ml, Fisher Scienific Graphite, 85m, Spex REAGENTS: Lithium Metborate, 997%, Johnson Matthey Nitric Acid, 0%, A.CS, Fisher Scientific ‘TIME: The total decomposition time of Peruvian ilby this smehod is 45 5b nutes 2 PROCEDURE: 1. Weigh 0: of LiBO. intoa crucible, nitrogen. Program fhe microwave unitas follows ‘Main Menu: Quick Test Dwell Time: 25 ninutes 4. Take the cucble ott ofthe cavity and ool for 3-5 minutss 5. Take the melt out othe crucble (in graphite, themeltforns Final diluion: ol [NOTE Table 28 in Appendix Bshows lens that wee determin in the Sl SRM by IC-AES analysis alter fusion with bof the pero and metaborate fixe inal ve cucble ype. Only the 2or 3 mast inteee elemental ines were investigated. | Le t jt (yi 1 il Et 1 | DECOMPOSITION OF PERUVIAN SOIL SRM 4355 BY FUSION WITH SODIUM PEROXIDE AND LITHUM METABORATE MIXTURE SCOPE: This method provides for te decomposition of Peruvian Soil ‘of metals by specroscopic methods. The major constituents are 393296 SiO 17.88% FesOr 850% ALOs; 369% TiO EQUPMENT: MAS-7(00 Microvave Mufle Furnace CRUCIBLES: GC, 30 mL, Sigratur EMCIndustries REAGENTS: Sodium Peroxide >95% purispa, Fluka Lithium Metabonte, 9.997%, Johnson Matthey Hydrochloric Acid, 30%, Suprapu, EM Science ‘TIME : The total decomposition time of Peruvian Soil SRM 4355by this, method is 25 minstes. PROCEDURE: 1. Weigh]0golNOv ard 05 g 90 int the ruc Final dilution actor is 01 g/SOmL.DECOMPOSITION OF CHROMIUM OXIDE (CrO:) BY FUSION WITH SODIUM PEROXIt SCOPE: This method providesfor the desompositon of mum trioxide (chromic acid by fusion with sodium peroside (Na) in ior Zr cucibles fer the determination of metalsby spect scopic metheds. The najor constituent is Crs EQUIPMENT: MAS-7000 Microwave Muffle Fumace CRUCIBLES: Ni,30 0r 50 mL, Fishes Scientific 235 or 55 nL, FisherScientiic GC, 30 mL, Sigradur EMC Industries REAGENTS: Sodium Perexde, 9796, ACS, Aldrich Hydrochlork Acid, 37%, A.CS, Fisher Sciific Hydrofluoric Acid, 48%, A.C, © Merck ‘TIME: The total decompositian time of CrOs by this method {is 0-50 minutes. PROCEDURE: 1. Weigh 2((g of Na into a crucible. 2. Weigh 02 8 of C1O and mixit with NuOs in the crucible using Ptor glass rod. 3. utthe cucibe int the furnace and purge the avity with nitrogen. Program ‘he microwave untas follows: Main Menu: Quick Test ‘Temperature: 80 °C Dwell Time: 30 minutes 4. Take the aucble out ofthe cavity and 20 for3-5 minus. 5. Leach themelt twice with 10 mL deionized wate, pour the slurry into a 100 ml-beake, rinse the cucible wee with 10mL of 3% HCl aad once with 5 mL 5% HCl aad add all >. Incaseof fusionin Zr crucible, itis necessary 0 add 1 nL HF to lear the solution. DECOMPOSITION OF EURNT REFRACTORY SRM 78a BY FUSION WITH SODIUM PEROXIDE SCOPE: This method provides for the decomposition of Bumt Refractory ‘methods. The maor constituents are 71.7% ALOy 19.4%0:; 3.2% TOs, EQUPMENT: MAS-700 Microwave Mufle Furnace CRUCTBLES: Ni, 30 or 50 mL, Fisher Scientific Zs, 35.0155 ml, Fsher Scientific GC, 30 mL, Sigratur EMC Industries REAGENTS: Sodium Peroxide 979%, ACS, Aldrch Hydrochloric Add 37%, A.SS, Fisher Scientiic Hiydrofluoric Adi, 48%, A.CS, E. Merck ‘TIME: The total decomposition tine of Burnt Refractory SRM 7a by this method is 40-50 minutes, PROCEDURE: 1. Weigh 20 ofNa:Os inb a crucible, 2. Weigh 0.2 g ofBumt Reractory SRM 78a ard mix it with Nas in the crucible using Pt or glass rod, 3. Put the crucible into thefurnace and purge the cavitywith nitrogen. Progam the microwave unit as follows: 6. Heatthe solution modentely until lear 2. Incase of fusion in Nicrucible, the black NiO has b be dissolved. '. Incase of fision in Zrcrucible itis necessary to Final dilution actor is 02g /50 ml.DECOMPOSITION OF BURNT REFRACTORY SRM 7Ba BY FUSION WITH SODIUM PEROXIDE AND LITHIUM TETRATABORATE MIXTURE SCOPE: This method provides ior the decomposition of Burt Refractory SEM 78a by fusion with sodium peroxide (Na:O)) lithium metaborate (Li3O) mixture in GCcrucbles ir the de'er- ‘miration of netals by spectroscopic methcds. The raj con- stituents are 71.7% ALO 194%S(0: 32% iO. EQUIPMENT: MAS7000 Mcrowave Muffle Fumace CRUCIBLES: GC, 30 mL., Sgradur EMC Industries REAGENTS: Sodium Peroxide, >95% purrispa, Fluka Lithium Metzborate, 997%, Johnson Mathey Hydrochloric Acid, 30%, Suprapr, EM Scence ‘TIME: Thetotal decomposition time of Burt Refmctory SRM Baby this method is 55 minutes, PROCEDURE: 1. Weigh 10g ofNaand 05 LiBO-hio he 2 ‘igh 1g of Burt Refactry SRM 7h and cit with Na; + LiBG mixturein the creible using Pt or glass ed, 3. Put the crucible int the furnace a 700'C and purge the cavity with nitregen. Program the microwave unit as folows: Fal luton factors O1 g/m. DECOMPOSITION OF BURNT REFRACTORY SRM 78a BY FUSION WITHLITHIUM TETRABORATE ‘SCOPE: This method provdes for dtcomposition of Bumt Refracory 71% AbOy 194% SiOz 32% TIO. EQUIPMENT: MAS-7000 Microwave Mufile Fumace ‘CRUCIBLES: Pt, 30 ml, Fisher Scientific Graphite, 85 mL, Spex REAGENTS: Lithium Tetraborae, 99.9975, Johnson Matthey Nitric Add, 67%, ACS, Fisher Scientific TIME: The total decompesition time for Burnt Refractory SRM 7Ba by this method is 5-75 minutes. PROCEDURE: 1. Weigh 05 g of LiBO- ino a cructle. 4. Tate cate out ie cavity and cool 63 - Sites 5. Take the melt cut of the cucble (in graphite. the meltforms Final dation fori 0/50.BY FUSIONWITH SODIUM PEROXIDE 3Y FUSION WITHLITHIUN METABORATE SCOPE: Thi method ovis br he decmposin of Pate Cay SEM t DECOMPOSITION OF PLASTIC CLAY SRM 98b (| DECOMPOSITION O PLASTIC CLAY SRM 98b { I ‘SCOPE: This method provides forthe decomposition of Plastic Chy | { graphite crucibles ir the deermination of metals by specro- scopic methods The mipr consttuents ac 37% Si 27% Al; scopic methods, The major onstituen’s are 57% SiOs 27% 17% FeO, 1 ‘ALOs; 17% FeO. EQUIPMENT: MAS-7000 Mcrowave Mute Furnace | EQUIPMENT: MAS-70W0 Microwave Muffe Fumace CRUCIBIES: Ni, 30or 50 nl, Fisher Scientific Af CRUCTBLES: P%, 30 ml, Fisher Stientific 25,35 0F 35 ml, Fisher Scientific Graphite. 85 mL, Spex GC.30mL, Sgradur EMC Industries REAGENTS: Lithium Metaborae, 99.9975, Johnson Matthey REAGENTS: Sod.um Peroxide, 9799, ACS, Aldrich Nitric Add, 67%, 4.CS, Fisher Scentiic HycrochloricAcid, 37%, A.CS, Fisher Scientific Hyérofluoric Add, 48% A.CS, E. Merck , ‘TIME: The total decompasition time of Plastic Clay SRM 98b by his | ‘method i 60-70 minutes. TIME: The total dectmposition time of Plastic Clay SRM 985 by this method is 20-30 minut. \ PROCEDURE: 1. Weigh 05 g of BOs inte a crucible. 2. Weigh 0g of last Czy and mix it with LiBOs in the PROCEDURE: 1. Weigh 20g of NaC: into a crucible. crucible using Pt or glassrod. 2. Weigh 02g of Plastic Clay and mix it with 3. Put he crucible into the tumace ard purge te cavity vith 'Na.Orin te crucible using Ptor glass red. nitrogen. Progam the merowave unit as follows. 3. Put the crucible intothe furnace and purge the cavity with Main Mem Quick Tist nitrogen. Program the microwave units follows “Temperatur: 950°C Main Menu: Quick Test ‘Dwell Time 40 minutes ‘Tempeaature: 750°C 1 4. Take the cructe out of ie cavity and cool for 3-5 minutes. Dwell Time: 10 minutes, 5. Take the melt aut ofthe eucble (in graphite the melt 4. Take the cucible ou: ofthe cavity and ool for 3-5 minute. I forms a bead) and put it into a100 mL beaker: 5. Leach the melt twice with 10 mL-deionized water pour the | 6. Discalve the melt in 25 ml. 10% HNOs+ 10 aL deionized slurry intoa 100 ml beaker riase the crucible twine with =) water by modaate heating and sticring. 10 mL of % HC and once with 5 ml. 5% HC and u! 7. ‘Transfer the soltion to a50 ml. volumetric lask «dd all slurries to the beaker. ' 8. Dilute solutionto volume. 6. Heat the solution moderately until dear | Final dilution fctoris0.1g/50 mL. 2 Incase fusion ia Ni crucible, the beck NiO fas to be dissolved In case of fusion in Zr crucible, itis necessary te "inal dluton factors 02 /S0mL.t DECOMPOSITION OF PLASTIC CLAY SRM 98b BY FUSION WITH SODIUM | PEROXIDE AND LITHIUM METABORATE MICTURE SCOPE: EQUIPMENT: CRUCTBLES: REAGENTS: TIME: PROCEDURE: ‘This method provides ir the decomposition of Plasic (Clay SRM 9% by fusien with sodium peroxide (Na) + lithixm ‘metaborate (iBO:) misture in GC crucibles for deteminationof ‘metals by spectroscopic methods. The majsr constituents are £7% SiQy 27% Aly 17% FeO. MAS-7000 Mecrowave Mutfle Furnace GC, 30 ml, Sgmdur EMC Industries Sodium Perocide, >95% purrispa, Fluka Lithium Metsborate, 9.997%, Johnson Matthey ‘Hydrochloric Acid, 30%, Suprapur, EM Scence The total decomposition time of Plastic Clzy SRM 98 by this method is 30minutes. 1. Weigh 1.0 of Nai: and 05 g LiBOs into the crucible. 2. Weigh 0.1 of Plaste Clay arei mix with Na.O: + LBO: mixture in he crucbie using Pt or glass od. Ce Put he cacibent the fue at 700'C purge cavity : DECOMPOSITION OF BORON CARBIDE BY FUSION WITH SODIUM CARBONATE ‘SCOPE: This method provits for the decomposition ofboroncattide by EQUIPMENT: MAS70X0 Microwave Mulfe Furnace CRUCIBLES: Pt, 30 ml, Fisher Sientific REAGENTS: Sodium Carbonate anhydrass; A.CS, Fisher Scientific Hydrochioric Acid30%, Suprapur, EM Science TIME: The total decomposition time of Boron Carbide by this ‘method i 50 minutes, PROC:DURE: 1. Weigh25 g of NaxCO> into a crucible 2. Weigh 01 g of Soron Casbide and mix it with NaxCOv.n the crucitle using Peor plassrod. 3. Putthe crucible into the fimace. Program the microwave Final lution ctor is 01/50 mL.' DECOMPOSITION OF BORON CARBICE i | DECOMPOSITION OF ALUMINUM NITRIDE BY FUSION WITH BY FUSION WITH SODIUM PEROXID: \ SODIUM PEROXIDE AND LITHIUM METABORATE MIXTURE SCOPE: This methodprovidesfor the decomposition of Boron Carbide fl SCOPE: Thismetod proses forthe decomposton ofauminan tide by fusion wih sodium peroxide (Na:O) ia GC crucbles for EQUIPMENT: MAS-7000 MicrowaveMuffle Fumace EQUPMENT: MAS-7(00 Microvave Mufle Famace CRUCIBLES: GC, 30 mL, Sigradur EMC Industries CRUCIBLES : GC, 30 mL, Sigradur EMC industries REAGENTS: Sodium Peroxide, 979%, ACS, Aldrich ‘Hydrochloric Acid, 30%, Suprapur, EM Science REAGENTS: Soxtium Peroxide,>95% purisp.a, Fuka { Lithium Metaborate, 99 997%, Johutson Matthey TIME: The total deompositn time for Boron Carbide by his method Hydrochloric Aci, 30%, Suorapur, EM Science is 3-40 minutes NOTE: Ts foal decompstion tine of aluminum iid by this PROCEDURE: 1. Weigh 20g of Nass into a cucble. | 120-14) minutes 2. Weigh 011g of Boren Carbide and mixit with NeOs in the rucible wing Pt orglass rod. PROCEDURE: 1. Weigh 1.0 g of NaiO: and 05g LiBO: into the crucible 3, Put the crucible into the furncce and purge the cavity with nitrogen. rogram the microwave unitas follows: ‘Main Menu: Quick Test 3, Pat the crucible into the iumace at200 °C ‘Temperature: 75)°C. and purge the cavity wit nitroger. Program the micmwave unites follows ‘Main Ment: Quick Tat 5 ee ere i earls tear ‘Temperature: 750 °C _ Dwell Time 60 minuées - The tme to reach 750 °Cis 6 minutes that means the complete fusion time is about 2 hous. 4. Take the crucitle out of te cavity and cool for 3-5 minutes. Final dilution factor is 0.1 g/SOmL.el DECOMPOSITION OF SILICON CARBIDE (NORTON F400) BY FUSION WITH =| | ‘Appendix A ‘SODIUM PEROXIDE AND LITHUM METABORATE MIXTURE \ “able 1A. Spplors dt ax Matas and rues ‘SCOPE: This method provides ior the decomposition of Notion silicon carbide F400>y Fusionwith sodium peroxde(Na.O)+lthiun | {og ‘epee rte patate ‘metaborate (LiBO:) mitture in GC crucibles for deternination i e ‘of metals by spectroscopic methods. The major ae Alfa Acsar 800-3130 Fluxes ans constituents te 70% Siand 20.9% C. Jotyco MatheyCalog Company 1-230 cnucbies EQUIPMENT: MAS-7000 Microwave Muffle Furnace : ‘Ward Hill, MA 01535 - 8099 UCIBLES: Sigradur EMC industries ' ‘Aldsich 00589160 hows and a ey eae oe : : 1001 Vest Saint Paul Avenue 414-73.4979 crucibles REAGENTS: Sodium Peroxide, >95%, purris.pa,, Fluka PO, Box 2060. Lithium Metzborate, 9.997%, Johnson Matthey 1 Milwaskee, W1S5I233 Hydrochloric Acid, 30%, Suprapur, BM Scence Fluka Chemika Bio Chemika sn58-5087 uses ane ee Fa Gute orp. Seo TIME: Approximate 120 mis. oe pera Ronkorkoma, NVI1779-7238 PROCEDURE: 1. Weigh 10g of NaxCsand 0.5 g LiBOs ino the cruible. Fisher Scientie 30076-7000 Aioesand 2 Weigh 0.18 of silico carbide and mix with NaDs+ 711 Fobes Avene TH ED crucbies LiBO: misture in the crucible using Pt cr glass rod. Pittsburgh, PA 15319-9919 3. Patthe crcl into the furnace at 200°C | Thomas Scents: wos. Funes and and purge the cavity with nitogen. Program the nicrowave 99 ig ul Ro at 1-235, ova7-00 cxucbles unit as follows: PO. Bax 99 ‘Main Menu: Quick Test ‘Swedesboro, NY #8085 -0099 ‘Temperature: 754°C Janssen Chimica « wees Fluxes ‘Dwell Time: 60 riinutes -The time to reach 754°C is 60 Boy ane OP a minutes that mans te complete fsiontimeis approx Now Boncwride J 06901 rately hours. EM Scence soo-220342 Funes 4. Take the cucible ou-of the vty and ool for 3-5 minutes S Dison of EM nds ne. apace 5. Leach the melt twice with 10 mL deionized water pour th Po.Ba7 sturry intoa 100 mL beaker rinse the crcble twice 480 Denocrat oud with 3 mLof 30% Hl, and cambine shurries. Gibbstuwn, NJ 08127 6 Heat the solution moderately until clear and dilute solution JTBaker ‘800-JI BAKER Fluxes for volume 50ml in volumetric flask. | I ‘22 Red School Lane 906-859-2151 7. Wundscved ede our tr the xidue at sinseit | Prisburg NBs three times with deionized distilled watr. This is solution 4. : ‘Stewrn Chemdeala Ine. 7 Mallken Way. 508-523191 9. Weigh theignited residue andadd 5 tines the rexdue Frit qupment Diin SEBS Soe Woghtof 100. Foroampe the reves | SP Cott gad 0.0500gL1DOs and fe» S00 °C fr Hen om minutes, EMC Industries 6igradur) 908-896-4472 Crucibles 10. After the cucible coxls down, dissolve he melt ir the { 8 Readng Road, Suite 110 aucible wth 1 mL cf 30% HC + 5 mL deionized | ‘Flemington, NJ 04822 11. Transfer sclutions Aand B to z 50 mL volumetric Jask. 12 Dilute soltion to vdume. | | 1 ( i jinGC ‘Mn, Cu, Ti >10 i é ZnMg. >a 7 Feceal 2 \ N “ao i a. sank # es 3