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Please INSERT ORGANIZATION NAME QUALITY MANAGEMENT SYSTEM insert LOGO Document Code (Number): EG.OP.nn First valid effective date and revision number: Previous revision effective date and revision number This revision effective date and revision number Status: Title: Insert first effective date and revision number as YYYY-MM-DD / Rev. Insert first previous date Nr. and revision number as YYYY-MM-DD / Rev. Insert this date and Nr. effective revision number as select ACTIVE / DRAFT YYYY-MM-DD / Rev. Nr. Electrometers: Instructions for electrical calibration of measurement of charge Prepared by: (Signature) (E.g. Quality Management Supervisor) (Title) (Date) Revised: (Signature) (E.g. Electronics Group Head) (Title) (Date) Approved by: (Signature) (E.g. Director of the Organization) (Title) (Date) EG.CI.01 DATE/REVISION 1 of 11 EG.CI.01 DATE/REVISION 2 of 11 1. Title: ELECTROMETERS: INSTRUCTIONS FOR ELECTRICAL CALIBRATION OF MEASUREMENT OF CHARGE 2. Purpose: To define the set of procedures for the implementation of calibration of electrometers for the measurement of electric charge. 3. Scope: The scope of this instruction extends to the calibration of electrometers using an operational amplifier for the measurement of charge. This instruction is also applicable to the electrical calibration of dosemeters based on the use of an ionization chamber and an electrometer for dose measurement. 4. Definitions: Calibrator: Electronic device generating an electrical signal which main property can be used as a measure of an electrical magnitude. This property is characterized by a reference value whose uncertainty is known. Control measuring instrument: Electronic device allowing to measure the value of the magnitude of a calibrator generated signal (reference value) with uncertainty no greater than that of the reference value. Zero bias: Sudden change in indication at the beginning of the electrometer measuring scale. Zero spread: Continuous changes in the reading indication in the absence of an input signal. Minimal effective value of reading: Minimal value of the reading complying with the electrometer relevant specifications of performance (resolution, repeatability, nonlinearity, variation due to mains power changes). Minimal effective input current: Minimal value of the input current complying with the electrometer relevant specifications of performance (zero bias, zero spread, charge leakage, non-linearity, variation due to temperature, humidity and mains power changes). 5. Symbols and abbreviations: CL The following symbols and abbreviations are adopted in this calibration instruction: - leakage current (CF) CLM - mean leakage current (CFM) di - departure from linearity (i) Dm - zero spread FC - electrometer calibration factor I - electric current Imef - minimal input effective current IR - reference current generated by the calibrator m0,5 - instrument indication when charge q0,5 is applied mevi - minimal effective value of indication EG.CI.01 DATE/REVISION 3 of 11 q0,5 - electric charge leading to an indication value corresponding to half of the maximum of the selected scale for measuring. QE - electrometer indication when charge QR is applied. QEIL (C) - initial electrometer reading indicación in leakage testing. QEFL(C) - final electrometer reading indicación in leakage testing. QR - reference charge generated by the calibrator S - experimental standard deviation of a set of readings Dm - zero drift caused by variation in the conditions of zero adjustment Sza.m - shift in zero indication caused by switching from zero adjustment to measurement mode (Sdz.m) t0,5 - time required to obtain a reading value equal to half of the selected scale when current i is applied. t(s) - time (seconds) tM - measuring time (TM) 6. References: IEC –Medical electrical equipment - Dosimeters with ionization chambers as used in radiotherapy (IEC 60731:1997), Swiss Society of Radiobiology and Medical Physics. Järvinen H., Rantanen E. and Jokela K. “Testing of radiotherapy dosimeters in accordance with IEC specification”. Finnish Centre for Radiation and Nuclear Safety. Helsinki, Finland 1986. ISO GUM: 1995, Guide to the expression of uncertainty in measurement. EA-4/02, Expression of the uncertainty of measurement in calibration, European Co-operation for accreditation, December 1999. 7. Responsibilities: The EG Technical staff members are responsible for the implementation and validation of electrical calibration of measurement of charge. The Head of EG has the responsibility of reviewing and approving any changes or modifications introduced to this calibration instruction. The EG Quality Manager is responsible for addressing the internal quality control measurements, for reviewing the obtained results and keeping documented evidences of the IQC. 7. Procedure: 7.1 General considerations. EG.CI.01 DATE/REVISION 4 of 11 Electrometers are instruments designed to measure very low electric current or charge, very high resistance or electric potential with an instrument of very high impedance. The circuits designed for the measurement of charge and current are commonly based on an operational amplifier in inverting configuration, having either a feedback resistor for the measurement of charge or a feedback capacitor for the measurement of charge. The function of the resistor or the capacitor is to transform the electric current or charge in a voltage signal (accordingly to the Ohm law U=RI or Coulomb law Q=CU, respectively). The operational amplifiers used in the electrometers have a very high input impendance, low output impedance and allow the establishment of a virtual ground level. In some cases the electrometer input circuits are designed to transform the current or charge into a frequency signal, but still acting as an operational amplifier with very high input impedance. The principle of work of some dosemeters is based on the measurement of the electric charge accumulated in an ionization chamber by using an electrometr. In some cases, the electrometer indication is provided in dose units. This instruction can be used for the calibration of such dosemeters, providing that a proportionality factor is established for the conversion from dose to charge units and viceversa. 7.1.1 Fundamentals. Operational amplifiers used in inverting configuration have a very small difference between the inverting and non-inverting (connected to earth) inputs. That is the reason why the non-inverting input is usually called “virtual ground” (see Figure 1). If a tension UR is applied on CR an electric charge qR CRU R will be produced, since the potential difference between the non-inverting and inverting inputs is practically nill. This current or charge is converted into tension by the feedback elements and appears at the output, where the operational amplifier impedance is low (~ 100 Ohm) and can be measured with a conventional voltmeter. The generation of small charge or current by using a voltage source and employing resistors and capacitors serves for the purpose of electrometer calibration. If a suitable capacitor is not available, the generation of charge can be accomplished by integrating continuous current during a priori defined interval of time ( q I t ). EG.CI.01 DATE/REVISION 5 of 11 RR RM (Measurement of current) CM (Measurement of charge) - CR Output + Both inputs are at the same potencial “virtual ground” To voltmeter ELECTROMETER FIGURE 1: Schematic representation of an operational amplifier with inverting configuration. Therefore, the reference charge can be produced by using a calibrator generator for the generation of a reference tension and a reference air capacitor for the charge accumulation. The capacitor CR shall have not only a small uncertainty for the reference value, but also a neglictible variation due to environmental changes (temperature, humidity) Note: This calibration instruction is prepared for the work with electrometers based on operational amplifier and may not be applicable to old electrometers for which the assumption of a “virtual ground” condition is not valid. 7.1.2 Electrometer burden conditions. It must be taken into account that each electrometer model can be used for a limited maximal variation of charge (dQ/dt or current). Some electrometers will indicate false readings when the charge applied to the input, and which is generated by applying tension to a capacitor, exceeds the maximal value of input current at the electrometer input. In such cases, an additional resistor shall be added in serial connection to the capacitor to limit the value of dQ/dt to acceptable level. 7.2 Interconection. Since the type of connectors varies from model to model, it is advisable to have a set of conector adapter cables to allow the use of the available sources of charge and current. 7.3 Electrometer initial verification. This section adressess the main tests than must be performed for the verification of the work performance of the electrometer before its calibration. The provided recommendations are adapted from IEC 60731 and constitute a preliminary step before electrical calibration. EG.CI.01 DATE/REVISION 6 of 11 The concept of minimal effective value of indication (mevi) is defined as the value of the reading complying with the electrometer relevant specifications of performance (resolution, repeatability, non-linearity, variation due to mains power changes). Usually this value is not provided by the instrument manufacturer and can be considered as no less than 200 times the instrument resolution [Järvinen, 1996]. The leakage current values specified by the manufacturer are very low but in practice the effective values depend on environmental conditions, especially on environmental humidity. A survey on the specifications of different models of dosimeters used in radiotherapy revealed a maximal value reported for leakage current of 60 fA. The mevi for current corresponding to this value is therefore of 12 pA (200 x 60 fA). Changes in environmental temperature and humidity affect the electrometer measurements. The calibration must be carried out at a temperature as close as possible to that indicated for the specifications provided (200 C). The limit values for the environmental temperature are 150C and 250C, whereas humidity must be kept around 50 %. 7.3.1 Zero drift evaluation. Electrometer zero drift shall not exceed +1% (+ 0,5% in the case of reference electrometers) of the value indicated when the input minimal effective current is measured. The procedure for zero drift evaluation comprises the following steps: a) Switch on the electrometer and wait for stabilization period. b) If the electrometer has a minimal input current discriminator, it must be adjusted to zero. c) Switch the electrometer to measuring mode, annotate the value of indication and calculate the charge equivalent to this indication Q1(C) d) Maintain the electrometer in measuring mode, and after an interval of time t annotate the value of indication and calculate the charge equivalent to this indication Q2(C). The interval of time t shall be not less than that required for the minimal effective input current to produce the minimal effective value of indication. An interval of 15 min is a practical choice for t. e) Calculate the zero drift Dm in measuring mode as Dm f) Q2 Q1 t Express this zero drift as percentage of the minimal effective input current for the selected scale and compare with accepted limit (1%) (1) 7.3.2 Zero shift evaluation. Electrometer zero shift shall not exceed +1% (+ 0,5% in the case of reference electrometers) of the minimal effective value of indication for any scale whenever the electrometer is switched from zero adjustment or reset to measurement mode. The procedure for zero shift evaluation comprises the following steps: a) If the electrometer has a minimal input current discriminator, it must be adjusted to zero. EG.CI.01 DATE/REVISION 7 of 11 b) After the electrometer has been stabilized and the zero level adjusted, annotate the value of indication and calculate the charge equivalent to this indication as Q1(C). If the electrometer zero adjustment is automatic, assume Q1(C) as zero. c) Swith the electrometer to measuring mode, annotate the value of indication and calculate the charge equivalent to this indication as Q2(C). d) Calculate the shift of the zero resulting from the change in mode of operation as S dz,m Q2 Q1 (2) f) Express this zero shift as percentage of the minimal effective input current for the selected scale and compare with accepted limit (1%). 7.3.2 Leakage test. This test is carried out for electrometers using a charging capacitor for the measurement, and which might present some discharge leakage. The discharge rate (leakage current) shall not exceed 0,5% of the minimal effective input current. The procedure for leakage test comprises the following steps: a) If the electrometer has a minimal input current discriminator, it must be adjusted to zero. For electrometers that have an automatic measuring sequence, the electrometer must be maintaned in the measurement mode. b) The electrometer must be maintained on for the required stabilization period. c) If the electrometer has different measuring scales, select the scale with lowest maximal value. d) Connect the calibrator to the electrometer using a suitable connection cable, make the zero adjustment, switch to measurement mode and apply a charge producing an indication of approximately 50 % of the scale. e) Keeping the electrometer in measurement mode, disconnect the calibrator, the capacitor and any other external connection that might serve as external leakage path for the input connector. Cover the input connector with its metallic cap. Usually a change occurs in the indication when the calibrator is disconnected. f) Further, annotate the indication and observe its variation during the following 15 minutes. g) Calculate the discharge rate in amperes as intial reading minus final, divided by the time and express it as percentage of the minimal effective input current for the selected scale. h) Repeat the steps from d) to g) for each of the measurement scales. 7.3.2 Non-linearity test. The indication variation due to non-linearity in the scale range shall not exceed 0,5 %. This test evaluation is of more impoprtance for EG.CI.01 DATE/REVISION 8 of 11 old electrometer models using a potentiometer associated to a numeric dial for the indication reading. For electrometers with a a selectable scale, the test for non-linearity evaluation must be carried out at 5 equidistant values within each of the scales or if such selection is not possible, at values corresponding to 5%,10%, 20%, 50% and 100% of the scale. For electrometers with a single scale or with automatic scaling the evaluation must be carried out at 5 equidistant values within each decade or if such selection is not possible, at values corresponding to 5%,10%, 20%, 50% and 100% of the decade. The procedure for non-linearity evaluation comprises the following steps: a) If the electrometer has different measuring scales, select the scale with lowest maximal value. b) Connect the calibrator to the electrometer using a suitable connection cable. c) The electrometer must be switch on and maintained on for the required stabilization period. Make zero adjustment. d) Apply a charge q0,5 to produce to an indication value corresponding to half of the maximum of the selected scale. Anottate the value of the reading m0.5 and return the electrometer to the mode of zero adjustment. e) Swith con to measurement mode and apply a charge q1(C) sufficient to produce an indication close to the first value of the series. Annotate the reading as m1 and return the spectrometer to the mode of zero adjustment. f) Calculate and annotate the value of the factor d1 (percentage of deviation from linearity for value q1 as g) h) 7.3 d1 100 m1 1 (3) m 0,5 Repeat the steps e) to f) for each of the values from the measurement sequence to obtain the values d2, d3, d4 and d5. The non-liinearity value is taken from the maximum value from d1, …, d5. Charge measurement calibration. Changes in environmental temperature and humidity affect the electrometer measurements. The calibration must be carried out at a temperature as close as possible to that indicated for the specifications provided (200 C). The limit values for the environmental temperature are 150C and 250C, whereas humidity must be kept around 50 %. The calibration comprises the following steps: a) Connect the calibrator to the electrometer using a suitable connection cable. b) Switch on the electrometer and keep it on for the required stabilization period. c) Follow the manufacturer instructions for zero calibration EG.CI.01 DATE/REVISION 9 of 11 d) e) f) g) .g) Select the measuring scale and switch to measurement mode. Apply a charge q0,5 to produce to an indication value corresponding to half of the maximum of the selected scale. Annotate the reading as m0,5 Repeat the steps d) and e) to obtain 10 replicate readings Calculate the mean ( m ) and standard deviation of the ten replicate readings. The calibration factor for the electrometer is calculated as q CU (4) CF R R R m m where UR is the reference DC voltage supplied by a calibrator, CR is a reference capacitance. The uncertainty of the calibration factor CF is calculated following the specifications provided in the specific procedure EG.OP.004 According to eqn. (4) and the recommendations for uncertainty estimation, the absolute combined uncertainty of the calibration factor can be calculated as u (C F ) qR m u 2 (q R ) q R 2 u 2 (m ) (5) m 2 Several sources contribute to the uncertainties of the reference value qR and the mean of measurements m : u (q R ) u 2 (C R ) U R2 u 2 (U R ) C R2 (6) 2 u (m ) u 2prec (mi ) u res (mi ) (7) 2 u(U R ) u abs (U R ) uch2 (U R ) 2 u(C R ) u abs (C R ) uch2 (C R ) ` (8) (9) The meaning of each the contributions in eqn (6) and (7) are: u abs (U R ) is the absolute absolute uncertainty of the DC voltage reference value reported by the calibrator manufacturer u ch (U R ) is the additional uncertainty of the DC voltage reference value reported by the calibrator manufacturer for the cases when changes in environmental conditions exceed the working interval assumed for operation u abs (C R ) is the absolute uncertainty of the capacitor reference value reported by the manufacturer (it is assumed that additional uncertainty of the reference value due to changes in environmental conditions in reference air capacitors is neglictible). u ch (C R ) is the additional uncertainty of the capacitor reference value reported by the calibrator manufacturer for the cases when changes EG.CI.01 DATE/REVISION 10 of 11 in environmental conditions exceed the working interval assumed for operation u prec (m ) s(m) n n 1 (mi m ) 2 n(n 1) i (9) u res (mi ) is the uncertainty of the electrometer resolution indication, that can be calculated for a rectangular probability distribution as: u res (C R ) 1 12 (resolution ) elect (10) Assuming a normal probability distribution for the calculated calibration factor, a coverage factor k=2 ensures 95 % of coverage probability, and the calibration result is reported from expressions (4) and (5) as CF EG.CI.01 CR 2 u(C R ) m DATE/REVISION (9) 11 of 11