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CN-121979009-A - Automatic liquid preparation and conveying control method and system for At-211 separation

CN121979009ACN 121979009 ACN121979009 ACN 121979009ACN-121979009-A

Abstract

The invention relates to the technical field of radioactive separation, and discloses an automatic liquid preparation and conveying control method and system for At-211 separation, comprising the following steps of 1, taking the volume of a column bed, setting the minimum action volume granularity and determining the operation time of a pump; the method comprises the steps of (1) setting a solidifying reagent corresponding to a valve inlet, obtaining background current by buffer solution, obtaining low threshold current, high threshold current, tail threshold current and volume confirmation rule, step 3, generating a loading solution, step 4, conveying low pickling column liquid, buffer solution and preset balance liquid to separate columns, step 5, loading an ionization chamber, enabling output current of the ionization chamber to be tri-stated compared with the low threshold current and the high threshold current, step 6, switching a collecting valve to a product bottle, cutting an organic eluting solvent, and step 7, controlling the collecting valve, and determining the volume of an actual product. The invention realizes the automation and quantitative control of liquid preparation, conveying, elution and collection in the separation process of the At-211.

Inventors

  • GU LONG
  • Su Xingkang
  • WANG GUAN

Assignees

  • 福建睿斯科医疗技术有限公司

Dates

Publication Date
20260505
Application Date
20260403

Claims (10)

  1. 1. The automatic liquid preparation and conveying control method for the At-211 separation is characterized by comprising the following steps of: step 1, acquiring the bed volume of a separation column, setting the minimum action volume granularity, and determining the pump operation time according to the preset target volume; step 2, fixing the dissolved target acid, the low-acid washing column liquid, the buffer liquid and the organic eluting solvent in one-to-one correspondence with the inlets of the multi-inlet selector valve, conveying the buffer liquid to obtain background current through the sampling cavity, determining low threshold current, high threshold current and tail threshold current, and setting a volume confirmation rule; Step 3, determining the adding volume of the dissolved target acid and the buffer volume based on the initial concentration of the dissolved target acid, the target acidity and the preset target volume, and generating a loading solution; Step 4, switching a flow path to a separation column inlet, and sequentially conveying low-acid washing column liquid, buffer liquid and preset balance liquid according to the volume multiple of a preset column bed to generate a separation column with pretreatment and balance completed; step 5, conveying a sample solution at a preset fixed sample loading flow to obtain an ionization chamber output current, comparing the ionization chamber output current with a low threshold current and a high threshold current, and determining a no-product state, a product preparation state or a forced product state by combining a volume confirmation rule; step 6, forming a column washing gradient according to the preset column bed volume multiple after the sample loading is finished, and switching a collecting valve to a product bottle and switching the collecting valve to an organic eluting solvent when the output current of the ionization chamber is higher than a high threshold current and the volume confirmation rule is met; And 7, performing elution according to the volume of the elution chamber at a fixed organic elution flow, obtaining the output current of the ionization chamber, comparing the output current with the low threshold current, the high threshold current and the tail threshold current, controlling the switching of the collecting valve by combining a volume confirmation rule, and determining the actual product volume.
  2. 2. The automated liquid preparation and delivery control method for At-211 separation of claim 1, wherein obtaining a bed volume of the separation column, setting a minimum action volume particle size, and determining a pump run length from a preset target volume comprises: Step 11, obtaining the inner diameter of the separation column, the height of the column bed and the void ratio of the column bed, taking half of the inner diameter of the separation column as a radius, calculating a circular cross-sectional area, multiplying the circular cross-sectional area by the height of the column bed to obtain a column volume, and multiplying the column volume by the void ratio of the column bed to obtain the column bed volume; Step 12, determining the minimum action volume granularity based on the bed volume according to a preset minimum action volume granularity generation rule, dividing the subsequent liquid preparation volume and the conveying volume by the minimum action volume granularity respectively, taking an integer as a regular multiple, and multiplying the regular multiple by the minimum action volume granularity to obtain the regular liquid preparation volume and the regular conveying volume; And 13, acquiring a preset target volume and a preset fixed pump flow, and calculating the ratio of the preset target volume to the preset fixed pump flow to obtain the pump operation duration.
  3. 3. The automated liquid preparation and delivery control method for At-211 separation according to claim 1, wherein fixing the one-to-one correspondence of the dissolution target acid, the low acid wash column liquid, the buffer, the organic eluting solvent, and the multi-inlet selector valve inlet, delivering the buffer to obtain a background current through the sampling chamber, and determining a low threshold current, a high threshold current, and a tail threshold current, and setting a volume confirmation rule, comprising: step 21, acquiring a multi-inlet selector valve inlet number and a preset reagent name list, and fixing the dissolved target acid, the low-acid washing column liquid, the buffer liquid, the organic eluting solvent and the multi-inlet selector valve inlet one by one in a corresponding manner to obtain an inlet map; Step 22, switching to a buffer solution corresponding inlet according to the inlet mapping, conveying the buffer solution through a sampling cavity, acquiring an ionization chamber output current sampling sequence during buffer solution conveying, and determining a minimum sampling value in the ionization chamber output current sampling sequence as background current; Step 23, obtaining a preset threshold generation rule and a volume confirmation rule, adding a background current and a preset low threshold current increment to obtain a low threshold current, adding a background current and a preset high threshold current increment to obtain a high threshold current, adding a background current and a preset tail threshold current increment to obtain a tail threshold current, and taking the accumulated transport volume as an effective condition of the volume confirmation rule when the accumulated transport volume reaches the preset confirmation volume.
  4. 4. The automated liquid preparation and delivery control method for At-211 separation of claim 1, wherein determining the addition volume of the dissolved target acid and the buffer volume based on the initial concentration of the dissolved target acid, the target acidity, and the preset target volume, generating the loading solution comprises: Step 31, obtaining the initial concentration, target acidity and preset target volume of the dissolved target acid, judging that the initial concentration, target acidity and preset target volume of the dissolved target acid are all obtained and are effective values, executing volume granularity consistency verification on the preset target volume, and confirming that the preset target volume meets the integral multiple constraint of the minimum action volume granularity to obtain the preset target volume passing verification; step 32, multiplying the target acidity by a preset target volume passing through verification to obtain a first result, dividing the first result by the initial concentration of the dissolved target acid to obtain a dissolved target acid addition volume, dividing the dissolved target acid addition volume by the minimum action volume granularity and taking an integer as a regular multiple, and multiplying the regular multiple by the minimum action volume granularity to obtain a regular dissolved target acid addition volume; step 33, subtracting the regulated volume of the dissolved target acid from the preset target volume passing the verification to obtain the buffer volume, dividing the buffer volume by the minimum action volume granularity and taking an integer as a regulation multiple, and multiplying the regulation multiple by the minimum action volume granularity to obtain the regulated buffer volume; and step 34, calling an inlet mapping to switch to a corresponding inlet of the dissolved target acid and conveying the dissolved target acid according to the regulated adding volume of the dissolved target acid, calling an inlet mapping to switch to a corresponding inlet of the buffer solution and conveying the dissolved target acid and the buffer solution according to the regulated volume of the buffer solution, conveying the dissolved target acid and the buffer solution to the same target container and mixing the dissolved target acid and the buffer solution to obtain a loading solution.
  5. 5. The automated liquid preparation and delivery control method for At-211 separation of claim 1, wherein switching the flow path to the separation column inlet sequentially delivers a low acid wash column liquid, a buffer liquid, and a preset equilibration liquid At a preset bed volume multiple, creating a separation column that completes pretreatment and equilibration, comprising: Step 41, acquiring a bed volume, a minimum action volume granularity and a preset bed volume multiple sequence, multiplying each preset bed volume multiple in the preset bed volume multiple sequence by the bed volume to obtain a corresponding preset conveying volume, and executing volume granularity consistency check on each preset conveying volume to confirm that each preset conveying volume meets the integral multiple constraint of the minimum action volume granularity; Step 42, switching a flow path to an inlet of a separation column, directing an outlet of the separation column to waste liquid, calling an inlet mapping to sequentially switch to corresponding inlets of low-acid washing column liquid, buffer liquid and balance liquid, and conveying according to corresponding preset conveying volumes respectively; And 43, acquiring a low-acid-washing column liquid conveying completion state, a buffer liquid conveying completion state and a balance liquid conveying completion state, and carrying out consistency judgment on the low-acid-washing column liquid conveying completion state, the buffer liquid conveying completion state and the balance liquid conveying completion state according to a conveying sequence under the condition that an outlet of the separation column points to waste liquid, and generating the separation column which completes pretreatment and balance when the judgment passes.
  6. 6. The automated liquid dispensing and delivery control method for At-211 separation of claim 1, wherein delivering the loading solution At a predetermined fixed loading flow rate, obtaining an ionization chamber output current, and comparing with a low threshold current and a high threshold current, determining a no-product state, a product ready state, or a forced product state in combination with a volume confirmation rule, comprises: step 51, acquiring a preset fixed sample loading flow, a sample loading solution, a separation column for finishing pretreatment and balance, a low threshold current and a high threshold current, conveying the sample loading solution into the separation column for finishing pretreatment and balance at the preset fixed sample loading flow, acquiring an ionization chamber output current sampling sequence, and acquiring a sample loading conveying time length; Step 52, comparing each sampling value in the ionization chamber output current sampling sequence with a low threshold current and a high threshold current respectively to obtain a threshold comparison result sequence, determining the product of a preset fixed loading flow and loading conveying time as an accumulated conveying volume, acquiring a volume confirmation rule and a preset confirmation volume, and determining that the accumulated conveying volume reaches the preset confirmation volume to be a threshold of efficiency; And step 53, when the accumulated conveying volume corresponding to the threshold comparison result sequence reaches the effective threshold, marking the corresponding threshold comparison result as a comparison result sequence after confirmation, and determining no product state, a product ready state or a forced product state according to a preset state mapping rule, wherein the no product state is determined when the comparison result sequence after confirmation is lower than a low threshold current, the product ready state is determined when the comparison result sequence after confirmation is between the low threshold current and a high threshold current, and the forced product state is determined when the comparison result sequence after confirmation is higher than the high threshold current.
  7. 7. The automated liquid preparation and delivery control method for At-211 separation of claim 1, wherein a wash column gradient is formed At a preset column volume multiple after loading is completed, and when the ionization chamber output current is higher than a high threshold current and a volume confirmation rule is satisfied, switching the collection valve to the product bottle and switching to an organic eluting solvent comprises: step 61, obtaining a high threshold current, a preset confirmation volume and an accumulated delivery volume after loading, obtaining an ionization chamber output current, comparing the ionization chamber output current with the high threshold current to obtain a high threshold comparison result, and determining that the accumulated delivery volume reaches the preset confirmation volume as a volume confirmation result; step 62, in the process of washing the column gradient, obtaining a high threshold value comparison result and a volume confirmation result, and determining that the high threshold value comparison result is that the ionization chamber output current is higher than the high threshold value current and the volume confirmation result is established as a linkage switching triggering condition; and 63, switching the collecting valve to the product bottle when the linkage switching triggering condition is met, and calling the inlet mapping to switch to the corresponding inlet of the organic eluting solvent.
  8. 8. The automated liquid dispensing and delivery control method for At-211 separation of claim 1, wherein performing elution At a fixed organic elution flow rate as an elution volume, obtaining an ionization chamber output current and comparing with a low threshold current, a high threshold current, a tail threshold current, controlling a collection valve switch in conjunction with a volume confirmation rule, and determining an actual product volume, comprising: Step 71, obtaining fixed organic elution flow, elution packet volume, low threshold current, high threshold current, tail threshold current, volume confirmation rules and preset confirmation volumes, conveying organic elution solvent according to the elution packet volume at the fixed organic elution flow, and obtaining ionization chamber output current sampling sequences; Step 72, comparing each sampling value in the ionization chamber output current sampling sequence with a low threshold current, a high threshold current and a tail threshold current respectively to obtain a threshold comparison result sequence, obtaining elution conveying time length, determining the product of the fixed organic elution flow and the elution conveying time length as an accumulated conveying volume, and determining that the accumulated conveying volume reaches a preset confirmation volume as a volume confirmation result; And 73, when the volume confirmation result is established, marking the threshold comparison result sequence as a confirmed comparison result sequence, controlling the collection valve to switch between the product bottle and the tail liquid or the waste liquid according to the confirmed comparison result sequence, and determining the actual product volume according to the accumulated conveying volume of the collection valve during the period that the collection valve points to the product bottle.
  9. 9. The automated dispensing and delivery control method for At-211 separation of claim 8, wherein determining the actual product volume from the cumulative delivery volume during which the collection valve is directed to the product bottle comprises: step 81, acquiring the current pointing state of the collecting valve and the accumulated conveying volume, and recording the accumulated conveying volume when the current pointing state of the collecting valve is the product bottle, so as to obtain the accumulated conveying volume of the product bottle; step 82, obtaining a confirmed comparison result sequence, and generating a product section end mark and locking a product section end state when the current pointing state of the collecting valve is the product bottle and the confirmed comparison result sequence is lower than the tail threshold current; and step 83, shielding the switching action of the collection valve in the switching command to the product bottle when the product section end state is locked, and determining the accumulated conveying volume of the product bottle as the actual product volume.
  10. 10. An automated liquid preparation and delivery control system for At-211 separation, characterized in that an automated liquid preparation and delivery control method for At-211 separation as claimed in any one of claims 1-9 is employed, comprising: the bed quantifying module is used for obtaining the bed volume of the separation column, setting the minimum action volume granularity and determining the operation time of the pump according to the preset target volume; The threshold criterion module is used for fixing the dissolved target acid, the low-acid washing column liquid, the buffer solution and the organic eluting solvent in one-to-one correspondence with the inlets of the multi-inlet selector valve, conveying the buffer solution to obtain background current through the sampling cavity, determining low threshold current, high threshold current and tail threshold current, and setting a volume confirmation rule; the sample loading preparation module is used for determining the adding volume of the dissolved target acid and the buffer volume based on the initial concentration of the dissolved target acid, the target acidity and the preset target volume to generate a sample loading solution; the column pretreatment module is used for switching a flow path to a separation column inlet, sequentially conveying low-acid washing column liquid, buffer liquid and preset balance liquid according to the volume multiple of a preset column bed, and generating a separation column with pretreatment and balance completed; the sample loading judging module is used for conveying sample loading solution at a preset fixed sample loading flow, acquiring ionization chamber output current, comparing the ionization chamber output current with low threshold current and high threshold current, and determining a no-product state, a product preparation state or a forced product state by combining a volume confirmation rule; The column washing linkage module is used for forming a column washing gradient according to the volume multiple of a preset column bed after the sample loading is finished, and switching the collecting valve to the product bottle and switching the collecting valve to an organic eluting solvent when the output current of the ionization chamber is higher than a high threshold current and the volume confirmation rule is met; And the elution collection module is used for executing elution according to the volume of the elution bag at a fixed organic elution flow, obtaining the output current of the ionization chamber, comparing the output current with the low threshold current, the high threshold current and the tail threshold current, controlling the switching of the collection valve by combining the volume confirmation rule, and determining the volume of the actual product.

Description

Automatic liquid preparation and conveying control method and system for At-211 separation Technical Field The invention belongs to the technical field of radioactive separation, and particularly relates to an automatic liquid preparation and conveying control method and system for At-211 separation. Background At-211 is an alpha emitting radionuclide with important application value, and the preparation of the alpha emitting radionuclide is usually obtained by bombarding a target material by an accelerator. After the target material is dissolved, a solution system containing At-211 is formed, and then separation and purification of target nuclide, matrix metal and impurity components are realized through a separation column. The process belongs to a wet separation process of radioactive metals, and relates to a plurality of continuous steps of acidity adjustment, pre-column pretreatment, adsorption elution, product collection and the like. The existing At-211 separation process is mostly dependent on manual experience to carry out solution preparation and flow path switching control, a unified quantitative reference is lacking between the volume of a column bed and the conveying volume, the operation consistency among different batches is poor, meanwhile, in the column washing and elution stage, the starting and stopping of a product section are judged usually through manually observing detection signals or a preset time window, quantitative coupling between an online detection signal and the conveying volume is difficult to form, the influence of instantaneous fluctuation or artificial judgment deviation is easy to cause inaccurate volume measurement of the product, and even the mixed collection of the product and tail liquid occurs. In addition, the valve switching and solvent replacement actions often lack coordinated control logic, and the automation degree and repeatability of the separation process need to be improved. Disclosure of Invention The invention provides an automatic liquid preparation and conveying control method and system for At-211 separation, which solve the technical problems that the liquid preparation volume and the conveying volume are difficult to accurately quantify, the reagent switching and the collecting valve switching depend on manual time sequence, an online current criterion is easily influenced by background drift and instantaneous fluctuation, so that the elution interface and the collecting section are unstable in definition, and the batch-to-batch separation and collecting consistency is poor in the related art. The invention provides an automatic liquid preparation and conveying control method for At-211 separation, which comprises the following steps: step 1, acquiring the bed volume of a separation column, setting the minimum action volume granularity, and determining the pump operation time according to the preset target volume; step 2, fixing the dissolved target acid, the low-acid washing column liquid, the buffer liquid and the organic eluting solvent in one-to-one correspondence with the inlets of the multi-inlet selector valve, conveying the buffer liquid to obtain background current through the sampling cavity, determining low threshold current, high threshold current and tail threshold current, and setting a volume confirmation rule; Step 3, determining the adding volume of the dissolved target acid and the buffer volume based on the initial concentration of the dissolved target acid, the target acidity and the preset target volume, and generating a loading solution; Step 4, switching a flow path to a separation column inlet, and sequentially conveying low-acid washing column liquid, buffer liquid and preset balance liquid according to the volume multiple of a preset column bed to generate a separation column with pretreatment and balance completed; step 5, conveying a sample solution at a preset fixed sample loading flow to obtain an ionization chamber output current, comparing the ionization chamber output current with a low threshold current and a high threshold current, and determining a no-product state, a product preparation state or a forced product state by combining a volume confirmation rule; step 6, forming a column washing gradient according to the preset column bed volume multiple after the sample loading is finished, and switching a collecting valve to a product bottle and switching the collecting valve to an organic eluting solvent when the output current of the ionization chamber is higher than a high threshold current and the volume confirmation rule is met; And 7, performing elution according to the volume of the elution chamber at a fixed organic elution flow, obtaining the output current of the ionization chamber, comparing the output current with the low threshold current, the high threshold current and the tail threshold current, controlling the switching of the collecting valve by combining a volume confirmation rule, and determining