Development of new gallium cells Slovak Institute of Metrology J. Ranostaj S. Ďuriš, Euromet Project 732, WP 4

Objective: To develop a new generation of cells at the Gallium fixed point SMU Pilot Laboratory: SMU FE-LMK, METAS, CMI, Participants: FE-LMK, METAS, CMI, VNIIM Cooperating laboratory: VNIIM Workpackage 4 Gallium melting point

Review of up to date activities Review of WP 4 possibilities Review of WP 4 possibilities Collection of information related to gallium fixed point (literature retrieval) Collection of information related to gallium fixed point (literature retrieval) Realization of cells Realization of cells  selection of supplier and purchase of the gallium  chemical analysis  cell design  cleaning procedure  filling procedure  manufacturing of the cells – under process

WORKING STEP (WS)DESCRIPTIONSKCHSICZ 1. Collecction of the information Participating laboratory will prepare and send to the pilot laboratory all relevant information which concerns the work of this WP (e.g. own literature retrieval, relevant publications, references, …) Pilot laboratory will prepare the list of all collected information. X 2. Design of the call(s)Participating laboratory will prepare they own design of the Ga cell and enclosure. All prepared designs will be discussed in this WP. There is also the possibility to accept two or more designs and to work simultaneously on several designs. X 3. Production of the cell 3.1 Procure the GaSelection of the supplier and buying Ga (investment including). X 3.2 Procure the other materials Selection of the supplier and buying the other materials (investment including). X 3.3 Analysis of Ga sample(s) Providing of chemical / isotopical analyses of the Ga (investment including). X 3.4 Manufacturing of the cell(s) Arrangement of the manufacturing of the cell components (investment including). X 3.5 Filling of the cellFilling of the cell (elaborating of the filling method, corresponding equipment design and realization). X 4. Testing of the cellPreparation of the “testing protocol” for the study the phase transition, parameters of influence …and / or realization of the measurements according to this protocol XXXX Review of WP 4 posibilities

Cells realization  Gallium Supplier: CMK, Ltd. (Slovakia) Supplier: CMK, Ltd. (Slovakia) Charge No.: Charge No.: Purity: 7N Purity: 7N Quantity: 1.1 Kg Quantity: 1.1 Kg (2x0.5 Kg, 4x0.025 Kg) Analyze: Analyze: –GDMS, CMK, Ltd. –GDMS, Shiva Technologies Europe (France) Supplier: CMK, Ltd. (Slovakia) Supplier: CMK, Ltd. (Slovakia) Charge No.: Charge No.: Purity: 7N – MBE Grade Purity: 7N – MBE Grade Quantity: 1.1 Kg Quantity: 1.1 Kg (2x0.5 Kg, 4x0.025 Kg) (2x0.5 Kg, 4x0.025 Kg) Analyze: Analyze: –GDMS, CMK, Ltd. –GDMS, Shiva Technologies Europe (France)

CMK Shiva tech. Europe NRCCMK Shiva tech. Europe NRCCMK Shiva tech. Europe NRCCMK Shiva tech. Europe NRC Li Cr Pd-10.5Er-1- Be Mn Ag50 30Tm-1- B Fe Cd8101Yb-1- C---Co In Lu-1- N---Ni Sn511Hf O---Cu Sb Ta-500- H---Zn1.211Te W150.1 F556GaMatrixI Re-10.2 Na Ge30 10Cs Os-10.2 Mg As510.4Ba310.4Ir-10.3 Al Se1055La Pt-50.3 Si Br101 Ce2010 Au10 5 P0.5 Rb Pr-1-Hg552 S Sr410.1Nd-1-Tl Cl0.412Y110.09Sm-1-Pb K61045Zr Eu-1-Bi Ca855Nb Gd-1-Th Sc Mo Tb-1-U Ti Ru-10.4Dy-1- V Rh-10.1Ho-1  Detection limits of some GDMS analytical laboratories (ppb wt)

CMK Shiva tech. Europe CMK Shiva tech. Europe CMK Shiva tech. Europe CMK Shiva tech. Europe Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. liit LiND0.06ND0.5CrND0.1ND0.5Pd--ND1Er--ND1 BeND0.03ND0.5MnND0.05ND0.5AgND20ND50Tm--ND1 B 0.05ND0.5Fe ND0.5CdND3 10Yb--ND1 C----CoND0.03ND0.5In0.40.1ND1Lu--ND1 N----NiND0.1ND0.5SnND1.2ND1Hf--ND1 O----CuND0.2ND0.5SbND0.3ND1Ta--ND500 H----ZnND0.4ND1TeND0.4ND1W 0.1ND5 F 3 5GaMatrixI--ND1Re--ND1 NaND0.04ND1GeND7 30Cs--ND1Os--ND1 MgND0.04ND0.5AsND0.5ND1BaND1 1Ir--ND1 AlND0.05ND0.5SeND5 5LaND0.2ND1PtND0.3ND5 Si ND0.5BrND4 5Ce--ND10AuND5 10 P ND0.1ND0.5Rb--ND1Pr--ND1HgND1 5 S ND1Sr--ND1Nd--ND1TlND0.1ND1 Cl 20.08ND1Y-- 1Sm--ND1PbND0.21ND1 K 4 10Zr--ND1Eu--ND1BiND0.5ND1 Ca ND4 5Nb--ND1Gd--ND1ThND0.02ND0.5 Sc ND0.01ND0.5MoND0.1ND5Tb--ND1U 0.03ND0.5 Ti ND0.5Ru--ND1Dy--ND1 V 0.02ND0.5Rh--ND1Ho--ND1  GDMS analysis of Ga 7N (ppb wt)

CMK Shiva tech. Europe CMK Shiva tech. Europe CMK Shiva tech. Europe CMK Shiva tech. Europe Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. limit Con. Det. liit LiND0.04ND0.5CrND0.2ND0.5Pd--ND1Er--ND1 BeND0.02ND0.5MnND0.04ND0.5AgND20ND50Tm--ND1 B 0.08ND0.5Fe ND CdND3 10Yb--ND1 C----CoND0.02ND0.5InND0.3ND1Lu--ND1 N----NiND0.1ND0.5SnND1.3ND1HfND0.08ND1 O----CuND0.3ND0.5SbND0.4ND1Ta--ND500 H----ZnND0.4ND1TeND0.3ND1W 0.2ND5 F 3 5GaMatrixIND 0.1 ND1Re--ND1 NaND0.03ND1GeND7 30CsND 0.1 ND1Os--ND1 MgND0.04ND0.5AsND0.5ND1BaND1 1IrND0.2ND1 AlND0.05ND0.5SeND5 5LaND0.2ND1PtND0.2ND5 Si ND0.5BrND4 5Ce--ND10AuND5 10 P ND0.1ND0.5RbND 0.3 ND1Pr--ND1HgND1 5 S ND1SrND0.5ND1Nd--ND1TlND0.1ND1 Cl ND1Y 0.5 ND1Sm--ND1PbND0.2ND1 K 3 10ZrND 0.3 ND1Eu--ND1BiND0.5ND1 Ca ND 3 5NbND 0.05 ND1Gd--ND1ThND0.02ND0.5 Sc ND0.01ND0.5MoND0.1ND5Tb--ND1U 0.02ND0.5 Ti ND 0.01 ND0.5Ru--ND1Dy--ND1 V 0.01ND0.5Rh--ND1Ho--ND1  GDMS analysis of Ga 7N–MBE Grade (ppb wt)

 Design of the cells

 Cleaning of the container and filling of the cells Cleaning procedure for teflon crucible and cap Cleaning procedure for teflon crucible and cap –Washing with detergent –Rinsing and ultrasonic washing with distilled water –Washing with watered-down aqua regia –Rinsing with vapour of redistilled water –Heating in argon atmosphere

Future activities  Finalization of prototype cells  Comparison of prototype cells with SMU primary standard gallium point cell (used in CCT-K3 and Euromet No.: 552)  Study of gallium phase transition realized by prototype cells  pressure effect on the temperature of phase transition  effect of different method and effect of thermodynamic conditions of realization  effect of preceding freezing  effect of moisture ...  Comparison of gallium point realization by different NMIs

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