• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to a device for automatic sampling, titration. registration and processing of measurement data, preferably in the process industry. The invention is characterized, inter alia, by a container (3) being filled with an arbitrary volume of samples at a signal from a computer (4), while a second container (6) is filled with a titration solution to an arbitrary level at a signal from the computer, whereby the change in height of the liquid is measured. (7,8) whose measured values of the computer's program are converted to volume. The supply of titration solution is interrupted when the equivalence point of the titration solution and sample is reached, after which the computer's program recalculates consumed volume of titration solution to indicate the sample's quantitative content of searched substance. The results can be sent wirelessly or via landline to other computers.
    公开号:SE1000698A1
    申请号:SE1000698
    申请日:2010-06-29
    公开日:2011-12-30
    发明作者:Torbjoern Thorsell
    申请人:Torbjoern Thorsell；
    IPC主号:
    专利说明:

    The reaction is such that it is possible to detect when a certain molar ratio between the solutions has arisen, for example by the combined solution changing color. Then you stop adding titrant. By adding the titration from a burette, you can subsequently read how large a volume of titration has been added. Using knowledge of the two volumes and the molar ratio to be applied in the titration reaction, the concentration of the unknown solution can be calculated.
    Conductometry is a method of chemical analysis in which the electrical conductivity of a solution is measured. For a solution containing ions of only one salt (eg sodium chloride) the concentration can be determined with a single measurement. Practical applications include control of salinity in aqueous solutions, e.g. in dialysis.
    Conductometry can then under certain conditions give better results than ordinary potentiometric titration.
    Disadvantages of the prior art When, for example, titration of a strong acid against a strong base, the equivalence point should fall at pH 7. A value obtained (5.85) clearly deviates from the theoretical value. The biggest reason for this is in the measurement method used. In reality, the base solution in the acid solution does not drip at a constant rate, but the frequency with which the droplets fall decreases all the time. This causes the titration curve to be deformed to some extent, which means that the equivalence point deviates from the theoretical value pH 7. For a qualitative study, the method used works well, while the method does not work well in a quantitative determination.
    In order to obtain as accurate a titration as possible, extremely so-called pipettes are used, which distribute the solution in a jet or small drops. Due to the small diameter of the pipes, they can be easily clogged by contaminants from the sample. In each case, deposits are obtained inside the tube that interfere with the measurement results.
    The manual handling of all tasks is time consuming, tedious and requires discipline, which means that many eventually forget or do not care about making the necessary notes.
    Lack of connection between analysis results and production can also lead to severe disruptions in production.
    Description of the invention The invention comprises a method for qualitative and quantitative analysis of substances dissolved in liquid. Equipment and procedure are adapted for continuous analysis in the process industry.
    For practicing the invention, apparatus is used which forms an essential part of the invention.
    The invention can also be used for accurate dosing of, for example, liquids in healthcare.
    Figure 1 shows the schematic structure of the invention.
    Sample 1, which is to be tested, is supplied to the measuring equipment via the sampler 2, after which the sample in an arbitrary volume is filled into a vertical standing tube (container) 3. The described operation is controlled by a program built into a computer 4. From a vessel 5 a second vertical standing tube is filled 6 with a titration solution (titrator). Said vertical tubes are in their lower part connected to pressure-sensitive sensors 7 and 8, so-called DP cells. These cells are connected by means of lines 9, 10 to the previously mentioned computer (4).
    A certain volume of the sample (1) is passed from the tube (3) by the valve 11 being ordered by the computer to open. The sample is filled into a titration vessel 12, which may consist of a beaker or a so-called E-flask. The vessel is preferably mounted on a magnetic stirrer 13. In the titration vessel a chemically inert rod (not shown in fi g.) Is placed, which is caused to rotate depending on impulses from the magnetic field which the magnetic stirrer generates. This sequence of the invention is conveyed by the computer program which complements the present invention and which is illustrated by line 14.
    Prior to titration, the sample may be diluted with liquids such as water or glacial acetic acid from the container 15.
    After described measures, titration of the sample can be started. By command of the computer program, the valve 16 is opened to supply the titration solution from the tube (6) to the titration vessel. The volume titrator is registered and processed by the computer's program.
    Characteristic of the invention is that each change in volume in the pipes (3,6) is measured by the change in the hydrostatic pressure which occurs when the volume in the respective pipes decreases or increases. The difference in pressure is measured by the DP cells (7,8), registered and processed by the computer pfOgfâlïl.
    The fact that it is possible to convert registered pressure changes to volume is due to the fact that the connections have been calibrated during tests of the test plant, ie a large number of successively increased volumes have been adjusted to changed pressures.
    Within the scope of the invention, the results can be transmitted wirelessly or via a fixed network to other computers at the same time as the registration. .
    Analysis according to known procedure At Domsjö Fabriker, the so-called base content of the digestion liquid that exposes fibers from the wood binder lignin is determined, among other things. The liquid used is a mixture of sodium hydroxide and sulfur dioxide and the base content is NagO.
    Before each analysis (titration), fill a pipette with 2.0 ml of the sample to be analyzed. Measured volume deviates by in 0.01 ml. The sample is diluted with 100 ml of anhydrous vinegar (glacial acetic acid). 0.1 molar superchloric acid (HClO4) is used as titrator in glacial acetic acid, which is gradually added to the sample from a burette in 0.5 ml portions. Each portion of added to the sample is noted as a change in the conductivity of the sample.
    Since there are great demands that each portion of titrator is really 0.5 ml, the accuracy of the burette is calibrated by adding titrator to a measuring flask with the exact volume of 10 ml portionwise. A correct dosage from the burette means that after 20 servings of 0.5 ml, the volumetric flask should contain exactly 10 ml. In the event of deviations greater than 0.001 ml, the burette or volumetric flask must be checked. This usually means that one of the parts must be discarded.
    Application examples according to the invention In applying the invention, the tube (3) was filled with sample solution. The diameter of the tube was measured to 8 mm, which means that 1 mm in height difference corresponds to a volume of 0.05 ml.
    To fill the titration vessel with exactly 2 ml of the sample, a level change of 40 mm was required.
    This turned out to be true during calibration.
    A tube (6) with a diameter of 4 mm was filled with water. Each level change by 1 mm in this case corresponded to a volume of only 0.01 ml.
    To check that the calculated volume would correspond to level changes in the tube (6), a net flask with a volume of 2 ml was used. Thus, the tube was emptied with the sample solution so that a level change of 200 mm was obtained. Also in this case, a surprisingly good correlation was obtained between calculated and obtained volume.
    For the determination of the base content expressed as NagO in a cooking liquid. an arbitrary volume of sample (1) was taken, which was filled into the tube (3). The tube (6) was filled with an arbitrary volume of superchloric acid.
    The levels in each tube were reset by marking the DP cells' measured values expressed as mA.
    By command from the computer (4), the valve (11) was opened so that the measured value of the DP cell (8) was changed from 0 mA to 20 mA. The volume was 1.8 ml. This fate was transferred to the titration vessel (12). The sample was diluted with glacial acetic acid from the vessel (15).
    Then the valve (16) was opened and closed at a frequency of 2 times per second.
    Each depletion of superchloric acid was recorded by the DP cell (7) as a change in height difference converted to mA. All changes in height differences (pressure changes) were registered by the computer.
    The titration ended when the equivalence point was reached, i.e. when the conductivity (mS / m) after falling began to rise again. By reading in diagram form, a surprisingly clear image (peak) could be read for the equivalence point. The experiments were repeated for two days, with sampling taking place every 3 minutes with lasting surprisingly good reproducibility.
    All measured values were processed using the computer program. Thus, instantaneous values expressed as the content of NagO per liter of liquid were stated.
    Advantages of the invention With an automatic system, precise data can be produced for rapid corrections in the process.
    The automatic system allows settings to be controlled from rooms that are relatively far from the test site.
    A further advantage of the invention is that the process operator does not have to go around and perform manual measurements at each test site. Another advantage is that the results can be gathered in one place and gathered in one place, which facilitates the control of an entire process chain. Full control of the process can more economically and efficiently control the process.
    An automatic system connected to the Internet that simultaneously guides and registers the process makes it easier to present instantly, on the Internet, via e-mail, PDA, as an SMS, or as printed paper.
    A major advantage of the invention is that it is robust and rather insensitive to the external environment but still performs results with surprisingly high precision.
    权利要求:
    Claims (1)
    [1]
    A method for titration and / or dosing of liquid, wherein a container (3) is filled with samples at a signal from a computer (4) while a second container (6) is filled with a titration solution to an arbitrary level at the signal from a computer, characterized in that following signals from the computer, an arbitrary volume of the sample is transferred from the container (3) to a titration vessel (12), the exact volume of the sample being obtained by measuring the change in hydrostatic pressure obtained in the container (3), which pressure change via pressure sensor (8) and computer program is converted to volume, after which the titrator is sequentially fed to the titration vessel, each change of titration solution in height being measured by a further pressure sensor (7), this pressure change via computer program being converted to volume. Method according to Claim 1, characterized in that the fate of liquids is obtained by opening and closing computer-controlled valves (1, 1.16). Method according to claims 1 and 2, characterized in that the fate of the titrator is obtained by opening and closing a valve (16) at a frequency of two occasions per second. Process according to Claims 1 to 3, characterized in that the supply of titration solution is interrupted when the equivalence point of the titration solution and the sample is reached.
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    同族专利:
    公开号 | 公开日
    SE534928C2|2012-02-21|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    CN109856316A|2019-03-26|2019-06-07|上海大学|A kind of water sample real-time quantitative automatic titration device being mounted on hull|
    法律状态:
    2014-02-04| NUG| Patent has lapsed|
    优先权:
    申请号 | 申请日 | 专利标题
    SE1000698A|SE534928C2|2010-06-29|2010-06-29|Automatic titration|SE1000698A| SE534928C2|2010-06-29|2010-06-29|Automatic titration|
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