NMISA NEW GAS FLOW CALIBRATION FACILITY. Deona Jonker 7 October 2013

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1 NMISA NEW GAS FLOW CALIBRATION FACILITY Deona Jonker 7 October 2013

2 Introduction Flow the total volume of a fluid that flows past a fixed point in a given time Flow measurements used in industry as a means of process or quality control Environmental monitoring Industrial hygiene Manufacturing process control Research and development NMISA to provide South African industry with traceable measurements Califlow replaced by new primary standard

3 Overview of the NMISA Flow Laboratory Part of Flow section (Pressure, Viscosity, Gas Flow laboratories) One metrologist Only gas flow calibration services offered Flow range 0,5 ml/min to ml/min Flow medium - nitrogen gas Typical instruments received for calibration Mass flow controllers Mass flow meters Bubble flow meters Rotameters

4 Overview of the NMISA Flow Laboratory (cont.) Laboratory equipment Bios Met Lab ML-800 primary flow standard with three flow cells Bios Integrator 110 Met Lab Command & Control Module (awaiting delivery) Bios Gas Flow Bench (awaiting delivery) Vane anemometer (currently out of service) Bubble flow meter Environmental monitoring equipment barometers temperature- and humidity loggers

5 Overview of the NMISA Flow Laboratory (cont.) NMISA Gas Flow laboratory not yet SANAS accredited Measurements traceable to international standards (NIST) SANAS accreditation by 2014

6 Standard flow rate versus volumetric flow rate Volumetric flow rate the actual volume flow of the gas exiting a flow meter Typically the flow rate measured by primary standard flow meters (piston provers; bubble flow meters) Mass flow meters measure the mass of the medium flowing past a point in a given time Standard flow rate the equivalent flow rate of the gas if the temperature and pressure were at standard conditions Most useful measure of gas flow it defines the mass flow; number of molecules; heat carrying capacity of the gas

7 Standard flow rate versus volumetric flow rate (cont.) Term STP Standard Temperature and Pressure Refer to a customer specific set of reference conditions Not specified usually refers to a temperature of 273,15 K (0 C) and a pressure of 101,325 kpa (760 mmhg) Volumetric flow rate converted to Standard flow rate: T Volumetric flow = Q T Q - Standard flow rate T m - Measured temperature of the gas in the flow tube T std - Standard temperature P m - Gas pressure measured in the flow tube P std - Standard pressure m std P P std m

8 Standard flow rate versus volumetric flow rate (cont.) Reporting flow rates Standard flow rate values sccm standard cubic centimetres per minute slpm standard litres per minute Volumetric flow rates ccm cubic centimetres per minute lpm litres per minute

9 NMISA Primary Standard for Gas Flow Calibrations

10 NMISA Primary Standard for Gas Flow Calibrations (cont.) Bios Met Lab ML-800 new primary standard A positive displacement primary piston prover Can be used for gas flow measurements in either pressure or vacuum applications Complies with requirements necessary for a primary standard Flow measurements are made in terms of volume per unit time A piston moving in a cylinder of known cross-sectional area over a measured distance in a measured time

11 NMISA Primary Standard for Gas Flow Calibrations (cont.) Volumetric or standardized flow readings can be selected/obtained Standardised values calculated from Pressure measured by built in barometer Temperature entered by metrologist Measurements performed manually or automatically Up to 100 measurements performed in an averaging sequence Measures gas flow rates at measured atmospheric pressure ± 7 mmhg

12 NMISA Primary Standard for Gas Flow Calibrations (cont.) ML-800 consists of two primary components A common base Selectable flow cells Housed in the base component The main computer Timing crystal Precision barometer Flow cells plug into the base to create a functional system two components cannot operate independently

13 NMISA Primary Standard for Gas Flow Calibrations (cont.) Flow cells Consist of a borosilicate glass tube with a precision-machined piston Contain an integrated temperature sensor and barometric pressure transducer in the gas flow stream - instant conversion of volumetric readings into standardised flow

14 NMISA Primary Standard for Gas Flow Calibrations (cont.) FLOW CELLS MODELS ML-800 Ultra low flow cell: ML (in use at NMISA) Flow range: 0,5 50 sccm (ml/min) Accuracy: ± 0,25% ML-800 Low flow cell: ML (future purchase being considered) Flow range: sccm (ml/min) Accuracy: ± 0,15% ML-800 Medium flow cell: ML (in use at NMISA) Flow range: sccm (ml/min) Accuracy: ± 0,15% ML-800 High flow cell: ML (in use at NMISA) Flow range: sccm (ml/min) Accuracy: ± 0,15%

15 NMISA Primary Standard for Gas Flow Calibrations (cont.) Measurements performed with ML-800 traceable to international standards Before dispatch standard was calibrated at supplier s calibration laboratory (NVLAP accredited - USA) Base unit clock period of timing crystal and barometer calibrated Ultra-low flow cell gravimetrically calibrated together with its temperature and pressure sensors Medium and high flow cells dimensionally calibrated together with their temperature and pressure sensors

16 NMISA Primary Standard for Gas Flow Calibrations (cont.) For each flow cell Temperature and pressure corrections applied To obtain standardised flow readings

17 Validation of the Bios Met Lab ML-800 Primary Flow Standard Purpose of the validation To ensure flow standard was not damaged during shipping from the United States of America to South Africa To demonstrate the competence of the new flow metrologist in the operation of the ML-800 and the calibration of flow instrumentation

18 Validation of the Bios Met Lab ML-800 Primary Flow Standard (cont.) Validation method Use the ML-800 to calibrate two mass flow controllers of a Dynamic Dilution Calibrator Mass flow controllers previously calibrated against MKS Califlow primary gas flow standard Used nitrogen gas as flow medium Inlet port of mass flow controller connected to nitrogen gas cylinder Outlet port of mass flow controller connected to inlet port of appropriate ML-800 flow cell Connections directly to inlet and outlet ports of mass flow controller To ensure there was no gas diffusion/leakage possible via any other gas paths Full gas stream passed through the mass flow controller being calibrated

19 Validation of the Bios Met Lab ML-800 Primary Flow Standard (cont.) Validation method (cont.) Before performing measurements gas path was investigated for leaks Each mass flow controller calibrated at twenty points At each calibration point ten measurements performed and averaged Measurements recorded manually on worksheet Ambient conditions recorded

20 Measurement Results Calibration Point Ref Val (L/min) Lab Val (L/min) Lab Val Ref Val (L/min) Ref Val Unc (%) Lab Val Unc (%) Calculated E n value 1 0,805 0,815 0,010 0,64 1,27 0,01 2 1,870 1,910 0,040 0,64 0,19 0,06 3 2,932 2,985 0,053 0,64 0,18 0,08 4 3,995 4,058 0,063 0,64 0,18 0,09 5 5,077 5,136 0,059 0,64 0,16 0,09 6 6,156 6,223 0,067 0,64 0,16 0,10 7 7,248 7,304 0,056 0,64 0,16 0,08 8 8,336 8,396 0,060 0,64 0,16 0,09 9 9,433 9,489 0,056 0,64 0,16 0, ,52 10,58 0,06 0,64 0,16 0, ,62 11,68 0,06 0,64 0,16 0, ,74 12,78 0,04 0,64 0,16 0, ,85 13,89 0,04 0,64 0,16 0, ,95 15,01 0,06 0,64 0,16 0, ,07 16,12 0,05 0,64 0,16 0, ,19 17,25 0,06 0,64 0,15 0, ,30 18,37 0,07 0,64 0,15 0, ,41 19,52 0,11 0,64 0,15 0, ,47 20,65 0,18 0,64 0,16 0, ,51 21,80 0,29 0,64 0,16 0,44

21 Measurement Results (cont.) Bios ML-800 Validation Measurements Ambient temperature: 20 C ± 2 C UUT: Dynamic Dilution Calibrator Ambient humidity: 50 %rh ± 20 %rh Manufacturer: API Ambient pressure: 850 mbar ± 100 mbar Model: 700 Standard pressure = Pa = mbar = 760 mmhg Serial Number: 777 Standard temperature = 25 C MFC -S/N: (MFC1) Volumetric flow = standardised flow *(std pressure/meas pressure) *(meas temp/std temp) Date: 2013/01/30 Standardised flow = volumetric flow *(meas pressure/std pressure) *(std temp/meas temp) std temp (K) = C = K Readout: Bios ML-800 Primary Flow Standard Std Pres temp (K) = C Serial Number: Std Temp 25 Bios ML-800 readings = standardised flow Bios Flow Cell: ML (S/N: ) Uncertainty of reference values (%) = ) Dil Driv 250 Nominal Flow Rate (l/min) AVE STDEV ESDM ESDM % Lab Val - Ref Val Mass Flow Controller Reading (ml/min)@ 0 C (l/min) Temperature ( C) Pressure (mbar) Mass Flow Controller Reading (ml/min)@ 25 C Time 9h10 9h25 Unc (%) = En= ) Dil Driv 500 Nominal Flow Rate (l/min) AVE Mass Flow Controller Reading (ml/min)@ 0 C Temperature ( C) Pressure (mbar) Mass Flow Controller Reading (ml/min)@ 25 C Time 9h30 9h38 Unc (%) = En= ) Dil Driv 750 Nominal Flow Rate (l/min) AVE Mass Flow Controller Reading (ml/min)@ 0 C Temperature ( C) Pressure (mbar) Mass Flow Controller Reading (ml/min)@ 25 C Time 9h40 9h50 Unc (%) = En=

22 Measurement Results (cont.) Nominal Flow Rate (l/min) (highlighted in yellow) Mass flow controller reading as previously calibrated (760 mmhg and 25 C) reference value Uncertainty of reference values (%) = 0,64 (highlighted in orange) Uncertainty associated with all the reference values Mass Flow Controller Reading 0 C ML-800 flow reading standardised to 760 mmhg and 0 C Temperature ( C) Temperature reading from the ML a measure of the temperature of the gas stream in the flow cell Pressure (mbar) Pressure reading from the ML a measure of the pressure of the gas stream in the flow cell

23 Measurement Results (cont.) Mass Flow Controller Reading 25 C Calculated value. Flow values of the Mass Flow Controller, controlled by the API Calibrator and ML-800, differed significantly Reason - flow rates displayed by the API calibrator were standardised to 760 mmhg and 25 C; ML-800 displayed readings were s tandardised to 760 mmhg and 0 C Difference in the standardised temperatures caused the difference in the standardised flow readings For direct comparison purposes - a calculation was necessary to convert the ML-800 readings (ST: 0 C) to ML-800 readings (ST: 2 5 C) according to the following formula: ( 273,15 25) + ML 800( ST : 25 C) = ML 800( ST : 0 C) 273,15

24 Measurement Results (cont.) Mass Flow Controller Reading 25 C (con t.) Green highlighted values - the calculated averages of the ten calculated measurements (760 mmhg and 25 C) for each point - the l aboratory values Blue highlighted values - Unc % x.xxx - the measurement uncertainty calculated for each point Column Lab Val Ref Val (l/min) - indicates that there is good agreement between the values of the two calibrations of the instruments

25 Measurement Results (cont.) Time Time period over which the ten measurements were performed Calculated Normalised Error (E n ) values E n value is calculated for each point Method used for the evaluation of the measurement results was to calculate the error, E n, normalised with respect to the UoM using the following formula: E n = ( Lab value Re ference value ) 2 2 ( U + U ) Lab value - Mass Flow Controller Reading 25 C Reference value - Nominal Flow Rate (l/min) LAB REF U lab - value highlighted in blue at the bottom of each measurement block Unc % x.xxx U ref - Uncertainty of reference values (%) = 0,64 (highlighted in orange)

26 Measurement Results (cont.) Calculated Normalised Error (E n ) values (cont.) To ensure that the error is within the laboratory s uncertainty of measurement (UoM), the E n value should be between the limits of ±1 Therefore values of En < 1 - the measurement results obtained during calibration of the mass flow controller using the ML-800 were equivalent to those previously obtained during the calibration against the MKS Califlow Validated ML-800 travelled well after calibration from USA Flow Laboratory metrologist competent

27 Uncertainty Budget Calibration of a MFC (Calibrator) Manufacturer: API Model: 700 Serial number: 777 & (MFC1) Certificate number: Validation Calibration medium: Nitrogen gas MFC Flow Range L/min L/min Bios flow cell ML ML Value U(Xi) Unit Probability Distr Divisor Factor Sensitivity coeff Ci ui(k=1) (%) Reliability % D.o.f. (D.o.f)eff Value U(Xi) Unit Probability Distr Divisor Factor Sensitivity coeff Ci ui(k=1) (%) Reliability % D.o.f. (D.o.f)eff REF STD: Bios ML-800 flow cell % Normal k = E % Normal k = E-08 Temperature Normal k = E Normal k = E+00 Pressure Normal k = E Normal k = E+00 ESDM % Normal k = E % Normal k = E-06 Resolution % Rectangular E % Rectangular E-14 UUT: ESDM Normal k = E+00 Normal k = E+00 Resolution % Rectangular E % Rectangular E E E+00 uc(k=1) (%): Eff deg of freedom E E-06 t(eff d.o.f.): U(k=2) (%):

28 Uncertainty Budget (cont.) Sources of uncertainty considered Flow cell accuracy calibration certificates for the flow cells provided evidence that their accuracy was well within the manufacturer s accuracy specification manufacturer s accuracy specification was accepted as the uncertainty estimate Temperature no uncertainty contribution for temperature was considered - the ML-800 sensitivity to temperature was unknown ML-800 was used in a laboratory environment specified by manufacturer effect of temperature was assumed to be negligible

29 Uncertainty Budget (cont.) Sources of uncertainty considered (cont.) Pressure No uncertainty contribution for pressure was considered The ML-800 sensitivity to pressure was unknown ML-800 compensated for atmospheric pressure Repeatability of measurements (ESDM) The Experimental Standard Deviation of the Mean was used as the uncertainty estimate for the variation of repeated measurements Measurements were performed under repeatability conditions (conditions remained the same) and the calculated mean value of ten independent flow measurements were reported Degrees of freedom were the number of measurements minus one, which for ten measurements was nine.

30 Uncertainty Budget (cont.) Sources of uncertainty considered (cont.) Resolution of standard (Bios ML-800) Displayed resolution of the ML-800 was dependent on which flow rate was being measured Uncertainty estimate was accepted as one least significant digit of the displayed flow Resolution of the API Calibrator Displayed resolution of the API Calibrator was dependent on which mass flow controller was being calibrated Uncertainty estimate was accepted as one least significant digit of the displayed flow

31 Uncertainty Budget (cont.) Uncertainty estimates converted into relative values in percentage Measurement uncertainties calculated for each measurement point Uncertainty calculations show that apart from the flow cell s uncertainty, the repeatability uncertainty contributor proved to be the most significant.

32 The Way Forward First priority - to achieve SANAS accreditation for gas flow calibrations in 2014 Second priority - to decrease current client calibration turnaround times Equip laboratory with the necessary instrumentation, tools, tubing and fittings necessary for the calibration of the wide variety of flow instrumentation being received for calibration

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