# US 9,751,747 B2 · Process for detecting anomalies during the filling of a liquid metering device and liquid metering device > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,751,747 B2 - Document ID: US9751747B2 - Status: Granted - Kind: B2 - Application number: 14/126,918 - Filed: 2012-06-14 - Published: 2014-05-22 - Granted: 2017-09-05 - Earliest claimed: 2011-06-28 - Assignees: Gilson, Inc. - Applicants: Frédéric Millet - Inventors: Frédéric Millet - Web page: https://patentgrep.com/patent/US9751747B2 ## CPC - B67D 7/16: Arrangements of liquid meters - B01L 3/0227: {Details of motor drive means (B01L3/0231, B01L3/0234 take precedence)} - G01F 11/023: {with provision for varying the stroke of the piston} - G01F 11/029: {provided with electric controlling means (G01F11/022 and G01F11/024 take precedence)} - B01L 2200/146: Employing pressure sensors - B01L 2200/148: Specific details about calibrations - G01N 35/1016: {Control of the volume dispensed or introduced} - B67D: DISPENSING, DELIVERING OR TRANSFERRING LIQUIDS, NOT OTHERWISE PROVIDED FOR (cleaning pipes or tubes or systems of pipes or tubes B08B9/02; emptying or filling of bottles, jars, cans, casks, barrels, or similar containers, not otherwise provided for B67C; water supply E03; pipe systems F17D; domestic hot-water supply systems F24D; measuring volume, volume flow, mass flow or liquid level, metering by volume G01F; coin-freed or like apparatus G07F) - B01L: CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE - G01F: MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME - G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q) ## Abstract Method for detecting anomalies during the filling of a liquid metering device with a liquid to be measured out, said metering device comprising at least one suction member and at least one pressure monitoring means arranged for measuring a pressure in relation to said suction member. The detection method comprises steps consisting of: performing a prior pressure calibration of the filling of the device, calculating for a desired volume a tolerance range having an upper limit and a lower limit on the basis of the prior pressure calibration and checking whether the pressure remains within the tolerance range during the filling of the metering device with the liquid to be measured out. ## Claims ### Claim 1 A method for detecting anomalies during the filling of a liquid metering device with a liquid to be measured out, said metering device comprising: at least one suction member adapted to be in contact with the liquid to be measured out and to contain same during the filling of the metering device, at least one filling means arranged for filling, in an automated manner, the suction member, said filling means comprising at least one zone communicating with the suction member, said zone containing a gas, and at least one pressure monitoring means arranged for measuring the pressure in the at least one zone of the filling means or in a zone of the suction member containing a gas, the detection method comprising steps consisting of: a) performing a prior pressure calibration of the filling of the metering device, said pressure calibration being carried out with at least two reference volumes so as to define a reference filling curve for each of the at least two reference volumes and to determine for each reference volume a maximum vacuum pressure value Pmax_V1, Pmax_V2 corresponding to a maximum vacuum pressure value reached during filling; a maximum vacuum pressure time tmax_V1, tmax_V2 corresponding to a time at which the maximum vacuum pressure value is reached; a residual vacuum pressure Pa_V1, Pa_V2 corresponding to a residual vacuum pressure after filling the metering device; and a characteristic time τ_V1, τ13 V2 representing a rate of decline of the vacuum pressure after the vacuum pressure value Pmax _V1, Pmax_V2 has been reached; b) defining a desired volume of liquid to be measured out; c) calculating for the desired volume a tolerance range having an upper limit and a lower limit, the upper and lower limits of the tolerance range being calculated on the basis of the reference filling curves a calculated filling curve using the following equation P ref ⁡ ( t ) = [ P max - P a ] × ( 1 - t - t max τ ) 2 + P a , wherein Pmax is interpolated from Pmax_V1, Pmax_V2, Pa is interpolated from Pa_V1, Pa_V2, tmax is interpolated from tmax_V1, tmax_V2—, and wherein τ is calculated using the following equation τ = P max - P a V 2 - V 1 ⁢ ( τ V ⁢ ⁢ 2 ⁡ ( V - V 1 ) P max ⁢ _ ⁢ V ⁢ ⁢ 2 - P a ⁢ _ ⁢ V ⁢ ⁢ 2 - τ V 1 ⁡ ( V - V 2 ) P max ⁢ _ ⁢ V ⁢ ⁢ 1 - P a ⁢ _ ⁢ V ⁢ ⁢ 1 ) ; d) filling the suction member with the liquid to be measured out for a time dt; e) measuring the pressure using the pressure monitoring means; f) checking whether the pressure is within the tolerance range and if the pressure is in the tolerance range returning to step d) until a filling time corresponding to the desired volume of liquid to be measured out is attained; and g) if the pressure is outside the tolerance range, reporting that an anomaly has been detected. ### Claim 2 (depends on 1) The method according to claim 1, further comprising; a step h) consisting of calculating, on the basis of the pressures measured during the filling of the metering device, the volume of liquid to be measured out in the suction member; and a step i) consisting of, if the difference between the desired volume and the calculated volume of liquid to be measured out is greater, in absolute terms, than a threshold value, reporting that an anomaly has been detected. ### Claim 3 (depends on 1) The method according to claim 1, wherein step c) further comprises: a step c′) consisting of calculating a filling curve calculated for the desired volume on the basis of the reference filling curves; and a step c″) during which the calculation of the upper and lower limits of the tolerance range comprises a calculation step for the upper limit and the lower limit of respectively adding and subtracting a pressure value ΔP to the calculated filling curve. ### Claim 4 (depends on 1) The method according to claim 1, wherein step c) further comprises: a step c′) consisting of calculating a filling curve calculated for the given volume on the basis of the reference filling curves; and a step c′″) during which the calculation of the upper and lower limits of the tolerance range comprises a calculation step consisting, for the upper limit and the lower limit, of respectively creating a positive and negative time lag by a time value Δt. ### Claim 5 (depends on 1) The method according to claim 1, wherein step a) further comprises: a step a′) consisting of recording pressure values measured using the pressure monitoring means during the filling of the suction member with a reference volume of liquid; and a step a″) consisting of determining the filling curve corresponding to the pressure curve obtained in step a′), said step a″) also optionally consisting of determining the characteristic values corresponding to said pressure curve, steps a′) and a″) being carried out for each of the reference volumes. ### Claim 6 (depends on 1) The method according to claim 1, wherein step c) further comprises; a step c′) consisting of calculating a filling curve calculated for the desired volume on the basis of the reference filling curves; and a step c″) during which the calculation of the upper and lower limits of the tolerance range comprises a calculation step for the upper limit and the lower limit of respectively subtracting and adding a pressure value ΔP to the calculated filling curve, and wherein step c′) further comprises step consisting of linearly interpolating the filling curve and/or characteristic values of the filling curve at the desired volume on the basis of at least two reference volume filling curves and/or characteristic values of the pressure curves of at least two reference volumes. ### Claim 7 (depends on 6) The method according to claim 6, wherein step c) further comprises: a step c′) consisting of calculating a filling curve calculated for the given volume on the basis of the reference filling curves; and a step c′″) during which the calculation of the upper and lower limits of the tolerance range comprises a calculation step consisting, for the upper limit and the lower limit, of respectively creating a positive and negative time lag by a time value Δt, and wherein, during steps c″) and c′″), the upper and lower limits of the tolerance range are calculated on the basis of the calculated filling curve at step c′) using the following formulae: P + ⁡ ( t ) = P ref ⁡ ( t ) + Δ ⁢ ⁢ P +  d ⁢ ⁢ P ⁡ ( t ) d ⁢ ⁢ t  × Δ ⁢ ⁢ t , ⁢ P - ⁡ ( t ) = P ref ⁡ ( t ) - Δ ⁢ ⁢ P -  d ⁢ ⁢ P ⁡ ( t ) d ⁢ ⁢ t  × Δ ⁢ ⁢ t , where P+(t) and P−(t) are the upper and lower limits of the tolerance range at a time t, Pret(t) is the pressure calculated at the time t on the basis of the calculated filling curve and P(t) is the pressure variation measured at the time t. ### Claim 8 (depends on 6) The method according to claim 6, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the pressure variation curves after the corresponding time tmax. ### Claim 9 (depends on 6) The method according to claim 6, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the variation curves of a factor Pcor after the time tmax, the factor Pcor(t) being equal to P ⁡ ( t ) - P a P max - P a . ### Claim 10 (depends on 6) The method according to claim 6, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the variation curves of a factor P′cor after the time tmax as a function of a time variable tcor, the factor P′cor(tcor) being equal to P ⁡ ( t cor ) - P a P max - P a and the time variable tcor being equal to t - t max P max - P a . ### Claim 11 (depends on 6) The method according to claim 6, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the variation curves of a factor P′cor after the time tmax as a function of a time variable tcor, the factor P′cor(tcor) being ,equal to P ⁡ ( t cor ) - P a P max - P a and the time variable tcor being equal to t - t max P max - P a . ### Claim 12 (depends on 1) The method according to claim 1, wherein step c) further comprises a step c′) consisting of calculating a filling curve calculated for the given volume on the basis of the reference filling curves; and a step c′″) during which the calculation of the upper and lower limits of the tolerance range comprises a calculation step consisting, for the upper limit and the lower limit, of respectively creating a positive and negative time lag by a time value Δt, and wherein step c′) further comprises a step consisting of linearly interpolating the filling curve and/or characteristic values of the filling curve at the desired volume on the basis of at least two reference volume filling curves and/or characteristic values of the pressure curves of at least two reference volumes. ### Claim 13 (depends on 12) The method according to claim 12, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the pressure variation curves after the corresponding time tmax. ### Claim 14 (depends on 12) The method according to claim 12, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax, calculated for the desired volume, and wherein the reference and calculated filling curves are the variation curves of a factor Pcor after the time tmax, the factor Pcor(t) being equal to P ⁡ ( t ) - P a P max - P a . ### Claim 15 (depends on 12) The method according to claim 12, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the variation curves of a factor P′cor after the time tmax as a function of a time variable tcor, the factor P′cor(tcor) being equal to P ⁡ ( t cor ) - P a P max - P a and the time variable tcor being equal to t - t max P max - P a . ### Claim 16 (depends on 12) The method according to claim 12, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume, and wherein the reference and calculated filling curves are the variation curves of a factor P″cor after the time tmax as a function of a time variable tcor the factor P″cor(tcor) being equal to P ⁡ ( t cor ) - P a P max - P a and the time variable tcorbeing equal to t - t max P max - P a . ### Claim 17 (depends on 1) The method according to claim 1, wherein the method further comprises, between steps c) and d), a step c*) consisting of operating the filling means for the time tmax calculated for the desired volume. ### Claim 18 (depends on 1) A liquid metering device suitable for implementing a method according to claim 1, the metering device comprising: at least one suction member adapted to be in contact with a liquid to be measured out and to contain same during filling of the metering device; at least one filling means arranged for filling, in an automated manner, the suction member, said filling means comprising at least one zone communicating with the suction member, said zone containing a gas; at least one pressure monitoring means arranged for recording the pressure in the zone of the filling means or in a zone of the suction member containing a gas; warning means suitable for reporting the presence of an anomaly; and control and calculating means arranged for controlling the filling means and at least one pressure monitoring means, the control and calculating means being configured for carrying out a pressure calibration of the filling of the metering device with at least two reference volumes and defining a reference curve for each of the at least two reference volumes, and for determining for each of the at least two reference volumes a maximum vacuum pressure value Pmax _V1, Pmax_V2 corresponding to a maximum vacuum pressure value reached during filling; a maximum vacuum pressure time tmax_V1, tmax_V2 corresponding to a time at which the maximum vacuum pressure value is reached; a residual vacuum pressure Pa_V1, Pa_V2 corresponding to a residual vacuum pressure after filling the metering device; and a characteristic time τ_V1, τ_V2 representing a rate of decline of the vacuum pressure after the vacuum pressure value Pmax_V1, Pmax_V2 has been reached, wherein the control and calculating means is further configured for calculating, for a desired volume of liquid to be measured out, an upper limit and a lower limit of the tolerance range for the desired volume, the upper and lower limits of the tolerance range being calculated by the control and calculating means on the basis of the calculated filling curve using the following equation P ref ⁡ ( t ) = [ P max - P a ] × ( 1 - t - t max τ ) 2 + P a , wherein Pmax is interpolated from Pmax_V1, Pmax_V2, Pa is interpolated from Pa_V1, Pa_V2, tmaxis interpolated from tmax_V1, tmax_V2—, and wherein τ is calculated using the following equation τ = P max - P a V 2 - V 1 ⁢ ( τ V ⁢ ⁢ 2 ⁡ ( V - V 1 ) P max ⁢ _ ⁢ V ⁢ ⁢ 2 - P a ⁢ _ ⁢ V ⁢ ⁢ 2 - τ V 1 ⁡ ( V - V 2 ) P max ⁢ _ ⁢ V ⁢ ⁢ 1 - P a ⁢ _ ⁢ V ⁢ ⁢ 1 ) ; and for checking whether the pressure remains in said tolerance range during filling, said control and calculating means being further arranged for communicating with the warning means. ### Claim 19 (depends on 18) The liquid metering device according to claim 18, wherein the liquid metering device also implements a method for detecting anomalies on the release of the liquid to be measured out. ### Claim 20 A method for detecting anomalies during the release of liquid to be measured out by a liquid metering device, said metering device comprising: at least one suction member adapted to be in contact with the liquid to be measured out and to contain same during the filling of the metering device, at least one filling means arranged for filling, in an automated manner, the suction member, said filling means comprising at least one zone communicating with the suction member, said zone containing a gas, and at least one pressure monitoring means arranged for measuring the pressure in the zone of the filling means or in a zone of the suction member containing a gas, the detection method comprising steps consisting of: Ad) performing a prior pressure calibration of the release of liquid to be measured out by the metering device, said pressure calibration being carried out with at least two reference volumes so as to define a reference releasing curve for each of the at least two reference volumes, and to determine for each reference volume a maximum vacuum pressure value Pmax—1—V1, Pmax—1—V2 corresponding to a minimum vacuum pressure value reached during releasing, a maximum vacuum pressure time tmax_1_V1, tmax_V2 corresponding to a time at which the minimum vacuum pressure is reached, and a characteristic time τ1_V1, τ1_V2 representing a rate of decline of the vacuum pressure after the vacuum pressure value Pmax _1_V1, Pmax_1_V2 has been reached, Bd) defining a desired volume of liquid to be measured out to be released; Cd) calculating for the desired volume a tolerance range having an upper limit and a lower limit, the upper and lower limits of the tolerance range being calculated on the basis of a calculated filling curve using the following equation P ⁡ ( t ) = P max ⁢ _ ⁢ l × ( 1 - t - t max ⁢ _ ⁢ l τ l ) 2 , wherein Pmax_1 is interpolated from Pmax_1_V1, Pmax_1_V2, tmax_1 is interpolated from tmax_1_V1, tmax6_1_V2—, and wherein τ1 is calculated using the following formula τ l = P max V 2 - V 1 ⁢ ( τ l ⁢ _ ⁢ V ⁢ ⁢ 2 ⁡ ( V - V 1 ) P max ⁢ _ ⁢ l ⁢ _ ⁢ V ⁢ ⁢ 2 - τ l ⁢ _ ⁢ V 1 ⁡ ( V - V 2 ) P max ⁢ _ ⁢ l ⁢ _ ⁢ V ⁢ ⁢ 1 ) ; Dd) releasing from the suction member the liquid to be measured out for a time dt; Ed) measuring the pressure using the pressure monitoring means; Fd) checking whether the pressure is within the tolerance range and if the pressure is in the tolerance range returning to step Dd) until a releasing time corresponding to the desired released volume of liquid to be measured out is attained; and Gd) if the pressure is outside the tolerance range, reporting that an anomaly has been detected.