CN115656076A - Method for detecting anion synthetic detergent based on microextraction technology - Google Patents
Method for detecting anion synthetic detergent based on microextraction technology Download PDFInfo
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Abstract
The invention relates to the technical field of detergent detection, in particular to a method for detecting an anion synthetic detergent based on a microextraction technology, which comprises the following steps of S1, adjusting the temperature and the PH value of a sample solution; step S2, adding a methylene blue solution and stirring; s3, controlling a micro-extraction device to discharge chloroform droplets to extract the sample solution; and S4, collecting the gray scale change rate of the real-time image of the chloroform droplet to judge the extraction state, selecting a standard content range according to the real-time gray scale, calculating the real-time content of the sample according to the absorbance difference value of the chloroform droplet and the blank chloroform droplet, and checking the real-time content of the sample with the standard content range. The invention adopts the micro-extraction device to discharge the chloroform liquid drops for extraction, and checks the content of the calculated sample in real time, thereby overcoming the problems of limited contrast range and inaccurate detection result caused by a small amount of chloroform, ensuring accurate result, reducing the use of chloroform and improving the detection efficiency of the anion synthetic detergent.
Description
Technical Field
The invention relates to the technical field of detergent detection, in particular to a method for detecting an anion synthetic detergent based on a microextraction technology.
Background
The main component of anionic synthetic detergent, i.e. detergent powder, detergent, laundry detergent liquid, soap, etc. which are frequently used in daily life, is sodium dodecyl sulfate, which is a low-toxic substance, and because of its advantages of convenient use, easy dissolution, good stability, low cost, etc., it is widely used in disinfection enterprises, but if the flow of cleaning and disinfection is improperly controlled, the residual of anionic synthetic detergent on the surface of the cleaned object can be caused, which has adverse effect on human health, therefore, the residual anionic synthetic detergent on the surface of the cleaned object in disinfection enterprises is usually required to be detected.
Chinese patent publication No.: CN101776582B discloses a flow injection colorimetric measurement method for measuring the content of an anionic synthetic detergent in water and a measurement instrument thereof, and therefore, the detection of the residual quantity of the anionic synthetic detergent in the prior art needs repeated manual extraction of a large amount of chloroform, and not only has long analysis period with tedious operation and unsatisfactory reproducibility and accuracy, but also needs a large amount of toxic reagents and causes pollution to the environment.
Disclosure of Invention
Therefore, the invention provides a method for detecting an anion synthetic detergent based on a microextraction technology, which is used for solving the problems of large dosage and low detection efficiency of chloroform used for detecting the anion synthetic detergent in the prior art.
In order to achieve the above objects, the present invention provides a method for detecting an anionic synthetic detergent based on microextraction technology, comprising,
step S1, washing the surface of an object to be detected to obtain a sample solution, putting the sample solution into a treatment pool, detecting the real-time solution temperature of the sample solution in real time through a temperature detector, adjusting a temperature control device according to the real-time solution temperature of the sample solution, adjusting the temperature of the sample solution, and controlling the amount of an acidic regulator and an alkaline regulator to adjust the real-time PH value of the sample solution;
s2, adding a methylene blue solution into the sample solution with the temperature and PH value adjusted, and stirring the sample solution by controlling a stirrer at the bottom of the treatment pool;
step S3, preheating the chloroform in the micro-extraction device, controlling the micro-extraction device to discharge chloroform droplets downwards after the chloroform is preheated, moving the micro-extraction device with the chloroform droplets suspended at the lower part into a treatment pool, enabling the suspended chloroform droplets to be below the liquid level of the sample solution, and stirring the sample solution by controlling the stirring speed of a stirrer so as to enable the chloroform droplets to extract the sample solution;
and S4, carrying out real-time image acquisition on the chloroform droplets, carrying out gray processing on the chloroform droplet real-time images through a central control unit, calculating the image gray change rate in unit detection time to judge whether extraction is finished or not, comparing the real-time gray of the extracted chloroform droplet real-time images with a chloroform gray matrix arranged in the central control unit, selecting a standard content range from a content range matrix arranged in the central control unit, moving the extracted chloroform droplets and unextracted blank chloroform droplets into a detection pool, respectively detecting blank absorbance of the blank chloroform droplets and sample absorbance of the extracted chloroform droplets through a photometer, calculating the sample real-time content according to the blank absorbance and the sample absorbance through the central control unit, comparing the sample real-time content with the selected standard content range, and outputting the sample real-time content as a detection result when the sample real-time content is in the standard content range.
Further, in the step S1, a first preset temperature T1 and a second preset temperature T2 are provided in the temperature control device, wherein T1 is less than T2, the sample solution in the processing pool is heated at an initial heating temperature Tc by the temperature control device, wherein Tc is greater than T2, a real-time solution temperature Ts of the sample solution is detected in real time by a temperature detector, the real-time temperature Ts is compared with the first preset temperature T1 and the second preset temperature T2 by the central control unit,
when Ts is less than T1, the central control unit judges that the real-time solution temperature does not reach a first preset temperature, and the central control unit does not adjust the initial heating temperature Tc of the temperature control device;
when T1 is more than or equal to Ts and less than T2, the central control unit judges that the real-time solution temperature reaches a first preset temperature and does not reach a second preset temperature, and the central control unit adjusts the initial heating temperature Tc of the temperature control device to be Tc ', tc' = T2;
and when Ts is more than or equal to T2, the central control unit judges that the real-time solution temperature reaches a second preset temperature, and the central control unit judges the real-time PH value of the sample solution.
Further, a standard pH value Kb and a standard pH difference value Delta Kb are arranged in the central control unit, when the central control unit judges that the real-time solution temperature reaches a second preset temperature, the real-time solution pH value Ks of the sample solution is detected through a pH meter arranged in the processing pool, the central control unit calculates the real-time solution pH difference value Delta Ks according to the real-time solution pH value Ks and the standard pH value Kb of the sample solution, the Delta Ks = | Kb-Ks |, the central control unit compares the real-time solution pH difference value Delta Ks with the standard pH difference value Delta Kb,
when the delta Ks is less than or equal to the delta Kb, the central control unit judges that the real-time solution pH difference value of the sample solution does not exceed the standard pH difference value, adds a methylene blue solution into the sample solution in the treatment pool, and stirs the sample solution by controlling a stirrer at the bottom of the treatment pool;
and when the delta Ks is larger than the delta Kb, the central control unit judges that the real-time solution pH difference value of the sample solution exceeds the standard pH difference value, and compares the real-time solution pH value Ks of the sample solution with the standard pH value Kb to adjust the pH value of the sample solution.
Further, when the central control unit judges that the real-time solution pH difference value of the sample solution exceeds the standard pH difference value, the central control unit compares the real-time solution pH value Ks of the sample solution with the standard pH value Kb,
when Ks is less than Kb, the central control unit judges that the real-time solution pH value of the sample solution is lower than the standard pH value, calculates the input amount M1 of an alkaline regulator, wherein M1= (Kb-Ks). Times.a, a is the input coefficient of the alkaline regulator, inputs the alkaline regulator into the treatment tank, and detects the real-time solution pH value in the treatment tank through the pH meter, and repeats the calculation and judgment operation of the real-time solution pH difference value until the calculated real-time solution pH difference value does not exceed the standard pH difference value, adds a methylene blue solution into the sample solution in the treatment tank, and stirs the sample solution through a stirrer at the bottom of the control treatment tank;
when Ks is larger than Kb, the central control unit judges that the real-time solution pH value of the sample solution is higher than the standard pH value, calculates the adding amount M2 of the acidic regulator, wherein M2= (Ks-Kb). Times.b, b is the adding coefficient of the acidic regulator, adds the acidic regulator into the treatment tank, detects the real-time solution pH value in the treatment tank through the pH meter, and repeats the calculation and judgment operation of the real-time solution pH difference value until the calculated real-time solution pH difference value does not exceed the standard pH difference value, adds the methylene blue solution into the sample solution in the treatment tank, and stirs the sample solution through a stirrer at the bottom of the treatment tank.
Further, in the step S3, an initial stirring speed Vc of the stirrer is set in the central control unit, the chloroform in the micro-extraction device is preheated to a chloroform real-time temperature Tf, wherein T1 is greater than Tf and less than T2, the micro-extraction device is controlled to discharge chloroform droplets downwards, the chloroform droplets are suspended at the lower part of the micro-extraction device, the micro-extraction device suspended with the chloroform droplets at the lower part is moved into the processing tank, the suspended chloroform droplets are below the liquid level of the sample solution, and the stirrer is controlled by the central control unit to stir the sample solution in the processing tank at the initial stirring speed Vc.
Further, a unit detection time length t is arranged in the central control unit, when the stirrer stirs the sample solution in the treatment tank at an initial stirring speed Vc, the real-time image acquisition is carried out on the chloroform liquid drops below the liquid level of the sample solution, the central control unit carries out gray level processing on the real-time images of the chloroform liquid drops, the average gray level of the chloroform liquid drop area in the real-time images is obtained as the real-time gray level Gs of the real-time images, and the central control unit calculates the real-time gray level change rate Gs, gs = (Gs-Gs ')/t in any unit detection time length t, wherein Gs is the real-time gray level of the current real-time images of the chloroform liquid drops, and Gs' is the real-time gray level of the real-time images of the chloroform liquid drops before the unit detection time length t.
Further, a standard gray scale change rate Gb and an extraction gray scale change completion rate Gw are arranged in the central control unit, wherein Gb is larger than Gw, the central control unit compares the calculated real-time gray scale change rate Gs with the standard gray scale change rate Gb and the extraction gray scale change completion rate Gw,
when Gs is larger than or equal to Gb, the central control unit judges that the real-time gray scale change rate Gs is not lower than the standard gray scale change rate Gb, the central control unit judges that the extraction of the chloroform liquid drop is in a standard state, and the initial stirring speed of the stirrer is not adjusted;
when Gb is larger than Gs and larger than Gw, the central control unit judges that the real-time gray scale change rate Gs is between the standard gray scale change rate Gb and the extraction completion gray scale change rate Gw, and adjusts the initial stirring speed Vc of the stirrer to Vc ', vc' = Vc- [ Vc x (Gw/Gs) ];
and when Gs is less than or equal to Gw, the central control unit judges that the real-time gray change rate Gs reaches the extraction completion gray change rate Gw, the central control unit judges that the chloroform droplet is extracted, the stirrer is controlled to stop stirring, the real-time gray ga of the chloroform droplet real-time image is obtained, and the micro-extraction device and the extracted chloroform droplet suspended below the micro-extraction device are moved into the detection pool.
Further, a chloroform gray matrix L (g 1, g2, g3, … gn) and a content range matrix Ce (Ce 1, ce2, ce3, … Cen) are arranged in the central control unit, the central control unit compares the real-time gray ga of the real-time image of the chloroform droplet with each standard contrast gray in the chloroform gray matrix L, selects a corresponding standard contrast gray gi, enables g (i-1) < ga ≤ gi, and selects a corresponding standard content range Cei, i =1, 2, 3, … n from the content range matrix Ce (Ce 1, ce2, ce3, … Cen);
wherein g1 is the 1 st standard contrast gray scale, g2 is the 2 nd standard contrast gray scale, g3 is the 3 rd standard contrast gray scale … gn is the nth standard contrast gray scale, and g1 is more than g2 and more than g3 and more than … and more than gn; ce1 is the 1 st content range, ce2 is the 2 nd content range, ce3 is the 3 rd content range, … Cen is the nth content range, any of the content ranges Cev includes Cevmin and Cevmax, and Cevmin = Ce (v-1) max, cevmax = Ce (v + 1) min, where v =1, 2, 3, … n, cevmin is the minimum content value of the vth content range, and Cevmax is the maximum content value of the vth content range.
Further, the micro-extraction device and the extracted chloroform droplet suspended below the micro-extraction device are moved into the detection cell, the sample absorbance Ay of the extracted chloroform droplet is detected by a photometer, the micro-extraction device is controlled to discharge the unextracted blank chloroform droplet into the detection cell, the blank absorbance Ak of the blank chloroform droplet is detected by the photometer, the sample absorbance difference Δ Ay, Δ Ay = Ay-Ak is calculated by a central control unit, and the real-time sample content Cy, cy = Δ Ay × Q, is calculated, wherein the Q blue complex content absorbance is converted into a parameter.
Further, the central control unit compares the calculated real-time sample content Cy with the selected corresponding standard content range Cei,
if the real-time content Cy of the sample is in the standard content range Cei, the central control unit judges that the detection of the anionic synthetic detergent in the sample solution is finished, and outputs the real-time content Cy of the sample as a result;
and if the real-time content Cy of the sample is not in the standard content range Cei, the central control unit judges that the detection of the sample solution is invalid, and the sample solution is prepared again for detection.
Compared with the prior art, the method has the advantages that the sample solution containing the anion synthetic detergent is obtained by washing the surface of the object to be detected, the temperature and the PH value of the sample solution are accurately controlled, the methylene blue solution is added to react with sodium dodecyl benzene sulfonate in the anion synthetic detergent to form a blue complex, the reaction is ensured to be sufficient, the chloroform liquid drops are discharged by adopting a micro-extraction device to extract the blue complex in the sample solution, the using amount of chloroform is greatly reduced, meanwhile, the quick extraction can be realized due to the extremely small using amount of chloroform needing to be extracted, the detection efficiency of the anion synthetic detergent is improved, whether the extraction is finished or not is judged according to the image gray scale change rate of the chloroform liquid drops after the extraction is finished by adopting a central control unit, the extraction degree can be accurately judged in the quick extraction, the content range is determined by adopting gray scale contrast, the real-time content of the sample is calculated by detecting the absorbance of the chloroform liquid drops, the traditional colorimetric detection is replaced, the problems that the contrast range is limited and the detection result is not accurate, the anion synthetic detergent is effectively improved on the basis of the detection result, and the effective detection of the anion synthetic detergent is improved.
Especially, the temperature control device is provided with the initial heating temperature higher than the second preset temperature to heat the sample solution, so that the sample solution can be rapidly heated, the second preset temperature is used as the standard of the temperature of the sample solution, the first preset temperature is used as the limit value for heating the sample solution, the phenomenon that the temperature of the sample solution is too high to influence the reaction effect of the methylene blue solution and sodium dodecyl benzene sulfonate in the anion synthetic detergent is avoided, and the accuracy of detection of the anion synthetic detergent is guaranteed.
Further, the pH value of the sample solution after temperature control is detected, whether the pH value is within a set standard range or not is judged according to the real-time pH value of the sample solution, when the real-time pH value of the sample solution is not within the standard range, the adding amount of the acidic regulator or the alkaline regulator is calculated according to the real-time pH value of the sample solution and the standard pH value to accurately regulate the pH value, repeated regulation caused by excessive adding of the acidic regulator or the alkaline regulator is avoided, and the detection efficiency of the anion synthesis detergent is improved on the basis of ensuring the stable reaction of the methylene blue solution and the sodium dodecyl benzene sulfonate.
Especially, the temperature difference between the discharged chloroform liquid drops and the sample solution is reduced by preheating the chloroform in the micro-extraction device, so that not only can the stable extraction effect be ensured, but also the adsorption force of the micro-extraction device on the chloroform liquid drops can be improved, the phenomenon that the chloroform liquid drops drop under the stirring state is avoided, meanwhile, the sample solution is stirred by the stirrer, the extraction speed of the chloroform liquid drops is accelerated, and the detection efficiency of the anion synthetic detergent is improved.
Furthermore, real-time image acquisition is carried out on the chloroform liquid drops, gray processing is carried out on the real-time images, real-time color change of the chloroform liquid drops is reflected conveniently through image gray, real-time gray change rate of the chloroform liquid drops is calculated by setting unit detection duration, the extraction speed is extremely high due to the fact that the volume of the chloroform liquid drops is small, the real-time gray change rate of the chloroform liquid drops is calculated to judge the extraction degree of the chloroform liquid drops, and accurate control over the chloroform liquid drop extraction process can be achieved.
Particularly, the extraction state of the chloroform droplets is judged by setting a standard gray scale change rate and an extraction completion gray scale change rate, when the real-time gray scale change rate is not lower than the standard gray scale change rate, the chloroform extraction efficiency is high, therefore, the stirring speed is not adjusted, when the real-time gray scale change rate is between the standard gray scale change rate and the extraction completion gray scale change rate, the chloroform droplets are close to the extraction completion state, and because the extraction amount of the chloroform droplets is large, the stirring speed is gradually reduced, the separation of the chloroform droplets is avoided, and when the gray scale change rate reaches the extraction completion gray scale change rate, the chloroform droplets are extracted and completed, and are transferred into a detection pool for detection.
Furthermore, a corresponding gray scale interval is selected in the chloroform gray scale matrix according to the real-time gray scale of the chloroform liquid drop real-time image, a corresponding standard content range is selected in the content range matrix, the image is combined to replace the traditional colorimetric detection, the detection precision is improved, the content range of the detected anion synthetic detergent is determined, and the detection accuracy is guaranteed.
Furthermore, the sample absorbance of the extracted chloroform droplets and the blank absorbance of the blank chloroform droplets are detected through distribution of a photometer, the difference value between the sample absorbance and the blank absorbance is calculated, the real-time content of the sample is accurately calculated through a central control unit, the calculated real-time content of the sample is checked and compared with a standard content range selected according to the gray level, the result is output, and the accuracy of the detection result is improved.
Drawings
FIG. 1 is a flow chart of the method for detecting synthetic anionic detergent based on microextraction technology in this example.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and do not delimit the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Referring to fig. 1, which is a flow chart illustrating a method for detecting an anionic synthetic detergent based on a microextraction technique according to the present embodiment, the present embodiment discloses a method for detecting an anionic synthetic detergent based on a microextraction technique, comprising,
step S1, washing the surface of an object to be detected to obtain a sample solution, putting the sample solution into a treatment pool, detecting the real-time solution temperature of the sample solution in real time through a temperature detector, adjusting a temperature control device according to the real-time solution temperature of the sample solution, adjusting the temperature of the sample solution, and controlling the amount of an acidic regulator and an alkaline regulator to adjust the real-time PH value of the sample solution;
s2, adding a methylene blue solution into the sample solution with the temperature and PH value adjusted, and stirring the sample solution by controlling a stirrer at the bottom of the treatment pool;
step S3, preheating the chloroform in the micro-extraction device, controlling the micro-extraction device to discharge chloroform droplets downwards after the chloroform is preheated, moving the micro-extraction device with the chloroform droplets suspended at the lower part into a treatment pool, enabling the suspended chloroform droplets to be below the liquid level of the sample solution, and stirring the sample solution by controlling the stirring speed of a stirrer so as to enable the chloroform droplets to extract the sample solution;
and S4, carrying out real-time image acquisition on the chloroform droplets, carrying out gray processing on the chloroform droplet real-time images through a central control unit, calculating the image gray change rate in unit detection time to judge whether extraction is finished or not, comparing the real-time gray of the extracted chloroform droplet real-time images with a chloroform gray matrix arranged in the central control unit, selecting a standard content range from a content range matrix arranged in the central control unit, moving the extracted chloroform droplets and unextracted blank chloroform droplets into a detection pool, respectively detecting blank absorbance of the blank chloroform droplets and sample absorbance of the extracted chloroform droplets through a photometer, calculating the sample real-time content according to the blank absorbance and the sample absorbance through the central control unit, comparing the sample real-time content with the selected standard content range, and outputting the sample real-time content as a detection result when the sample real-time content is in the standard content range.
The method comprises the steps of washing the surface of an object to be detected to obtain a sample solution containing an anion synthetic detergent, accurately controlling the temperature and the PH value of the sample solution, adding a methylene blue solution, enabling the methylene blue solution to react with sodium dodecyl benzene sulfonate in the anion synthetic detergent to form a blue complex, ensuring full reaction, extracting the blue complex in the sample solution by discharging chloroform droplets through a micro-extraction device, greatly reducing the using amount of chloroform, achieving rapid extraction due to the fact that the using amount of the chloroform required to be extracted is extremely small, improving the detection efficiency of the anion synthetic detergent, judging whether extraction is completed or not according to the image gray scale change rate of the chloroform droplets after extraction is completed through a central control unit, accurately judging the extraction degree in rapid extraction, determining the content range by gray scale comparison, calculating the real-time content of the sample by detecting the absorbance of the chloroform droplets, replacing the traditional colorimetric detection, effectively overcoming the problems that the contrast range is limited and the detection result is not accurate due to the use of a small amount of chloroform droplets, and greatly improving the detection efficiency of the anion synthetic detergent on the basis of ensuring the accurate detection result of the anion synthetic detergent.
Specifically, in the step S1, a first preset temperature T1 and a second preset temperature T2 are provided in the temperature control device, wherein T1 is less than T2, the sample solution in the treatment tank is heated at an initial heating temperature Tc by the temperature control device, wherein Tc is greater than T2, a real-time solution temperature Ts of the sample solution is detected in real time by the temperature detector, the real-time temperature Ts is compared with the first preset temperature T1 and the second preset temperature T2 by the central control unit,
when Ts is less than T1, the central control unit judges that the real-time solution temperature does not reach a first preset temperature, and the central control unit does not adjust the initial heating temperature Tc of the temperature control device;
when T1 is more than or equal to Ts and less than T2, the central control unit judges that the real-time solution temperature reaches a first preset temperature and does not reach a second preset temperature, and the central control unit adjusts the initial heating temperature Tc of the temperature control device to be Tc ', tc' = T2;
and when Ts is more than or equal to T2, the central control unit judges that the real-time solution temperature reaches a second preset temperature, and the central control unit judges the real-time PH value of the sample solution.
Through temperature control device sets up the initial heating temperature who is higher than the second and predetermines the temperature and heats sample solution, can make sample solution rapid heating up, predetermines the temperature with the second as the standard of sample solution's temperature to through setting up the first restriction value of predetermineeing the temperature as heating sample solution, avoided sample solution temperature too high, influence the reaction effect of the sodium dodecyl benzene sulfonate in methylene blue solution and the anion synthetic detergent, ensured anion synthetic detergent detection's accuracy.
Specifically, a standard pH value Kb and a standard pH difference value Delta Kb are arranged in the central control unit, when the central control unit judges that the real-time solution temperature reaches a second preset temperature, the real-time solution pH value Ks of the sample solution is detected through a pH meter arranged in the treatment pool, the central control unit calculates the real-time solution pH difference value Delta Ks according to the real-time solution pH value Ks and the standard pH value Kb of the sample solution, the Delta Ks = | Kb-Ks |, and the central control unit compares the real-time solution pH difference value Delta Ks with the standard pH difference value Delta Kb,
when the delta Ks is less than or equal to the delta Kb, the central control unit judges that the real-time solution pH difference value of the sample solution does not exceed the standard pH difference value, adds a methylene blue solution into the sample solution in the treatment pool, and stirs the sample solution by controlling a stirrer at the bottom of the treatment pool;
and when the delta Ks is larger than the delta Kb, the central control unit judges that the real-time solution pH difference value of the sample solution exceeds the standard pH difference value, and compares the real-time solution pH value Ks of the sample solution with the standard pH value Kb to adjust the pH value of the sample solution.
Specifically, when the central control unit judges that the real-time solution pH difference of the sample solution exceeds the standard pH difference, the central control unit compares the real-time solution pH value Ks of the sample solution with the standard pH value Kb,
when Ks is less than Kb, the central control unit judges that the real-time solution pH value of the sample solution is lower than the standard pH value, the central control unit calculates the input amount M1, M1= (Kb-Ks). Times.a of an alkaline regulator, wherein a is the input coefficient of the alkaline regulator, the alkaline regulator is input into the treatment tank, the real-time solution pH value in the treatment tank is detected through the pH meter, the central control unit repeats the calculation and judgment operation of the real-time solution pH difference value until the calculated real-time solution pH difference value does not exceed the standard pH difference value, the methylene blue solution is added into the sample solution in the treatment tank, and the sample solution is stirred through a stirrer at the bottom of the control treatment tank;
when Ks is larger than Kb, the central control unit judges that the real-time solution pH value of the sample solution is higher than the standard pH value, calculates the adding amount M2 of the acidic regulator, wherein M2= (Ks-Kb). Times.b, b is the adding coefficient of the acidic regulator, adds the acidic regulator into the treatment tank, detects the real-time solution pH value in the treatment tank through the pH meter, and repeats the calculation and judgment operation of the real-time solution pH difference value until the calculated real-time solution pH difference value does not exceed the standard pH difference value, adds the methylene blue solution into the sample solution in the treatment tank, and stirs the sample solution through a stirrer at the bottom of the treatment tank.
The pH value of the sample solution is detected by controlling the temperature, whether the pH value is within a set standard range or not is judged according to the real-time pH value of the sample solution, when the real-time pH value of the sample solution is not within the standard range, the input amount of an acidic regulator or an alkaline regulator is calculated according to the real-time pH value of the sample solution and the standard pH value to accurately regulate the pH value, repeated regulation caused by excessive input of the acidic regulator or the alkaline regulator is avoided, and the detection efficiency of the anion synthetic detergent is improved on the basis of ensuring the stable reaction of the methylene blue solution and sodium dodecyl benzene sulfonate.
Specifically, in the step S3, an initial stirring speed Vc of the stirrer is set in the central control unit, chloroform in the micro-extraction device is preheated to a chloroform real-time temperature Tf, where T1 is greater than Tf and less than T2, the micro-extraction device is controlled to discharge chloroform droplets downwards, the chloroform droplets are suspended at the lower part of the micro-extraction device, the micro-extraction device suspended with the chloroform droplets at the lower part is moved into the processing tank, the suspended chloroform droplets are below the liquid level of the sample solution, and the stirrer is controlled by the central control unit to stir the sample solution in the processing tank at the initial stirring speed Vc.
The chloroform in the micro-extraction device is preheated, so that the temperature difference between the discharged chloroform liquid drops and the sample solution is reduced, the stable extraction effect can be ensured, the adsorption force of the micro-extraction device on the chloroform liquid drops can be improved, the phenomenon that the chloroform liquid drops drop off under the stirring state is avoided, the sample solution is stirred by the stirrer, the extraction speed of the chloroform liquid drops is accelerated, and the detection efficiency of the anion synthetic detergent is improved.
Specifically, a unit detection time period t is arranged in the central control unit, when the stirrer stirs the sample solution in the treatment tank at an initial stirring speed Vc, the chloroform liquid drops below the liquid level of the sample solution are subjected to real-time image acquisition, the real-time images of the chloroform liquid drops are subjected to gray scale processing through the central control unit, the average gray scale value of the chloroform liquid drop area in the real-time images is obtained and is used as the real-time gray scale Gs of the real-time images, and the central control unit calculates the real-time gray scale change rate Gs and Gs = (Gs-Gs ')/t in any unit detection time period t, wherein Gs is the real-time gray scale of the current real-time images of the chloroform liquid drops, and Gs' is the real-time gray scale of the real-time images of the chloroform liquid drops before the unit detection time period t.
The real-time image acquisition is carried out on the chloroform liquid drops, the gray processing is carried out on the real-time image, the real-time color change of the chloroform liquid drops is reflected conveniently through the image gray, the real-time gray change rate of the chloroform liquid drops is calculated through setting the unit detection duration, the extraction speed is extremely high due to the fact that the volume of the chloroform liquid drops is small, the real-time gray change rate of the chloroform liquid drops is calculated to judge the extraction degree of the chloroform liquid drops, and the accurate control of the chloroform liquid drop extraction process can be achieved.
Specifically, a standard gray scale change rate Gb and an extraction completion gray scale change rate Gw are arranged in the central control unit, wherein Gb is larger than Gw, the central control unit compares the calculated real-time gray scale change rate Gs with the standard gray scale change rate Gb and the extraction completion gray scale change rate Gw,
when Gs is larger than or equal to Gb, the central control unit judges that the real-time gray scale change rate Gs is not lower than the standard gray scale change rate Gb, the central control unit judges that the extraction of the chloroform liquid drop is in a standard state, and the initial stirring speed of the stirrer is not adjusted;
when Gb is larger than Gs and larger than Gw, the central control unit judges that the real-time gray scale change rate Gs is between the standard gray scale change rate Gb and the extraction completion gray scale change rate Gw, and the central control unit adjusts the initial stirring speed Vc of the stirrer to Vc ', vc' = Vc- [ Vc x (Gw/Gs) ];
and when Gs is less than or equal to Gw, the central control unit judges that the real-time gray change rate Gs reaches the extraction completion gray change rate Gw, the central control unit judges that the chloroform droplet is extracted, the stirrer is controlled to stop stirring, the real-time gray ga of the chloroform droplet real-time image is obtained, and the micro-extraction device and the extracted chloroform droplet suspended below the micro-extraction device are moved into the detection pool.
The extraction state of the chloroform liquid drops is judged by setting a standard gray scale change rate and an extraction completion gray scale change rate, when the real-time gray scale change rate is not lower than the standard gray scale change rate, the chloroform extraction efficiency is high, therefore, the stirring speed is not adjusted, when the real-time gray scale change rate is between the standard gray scale change rate and the extraction completion gray scale change rate, the chloroform liquid drops approach to the extraction completion state, at the moment, the extraction amount of the chloroform liquid drops is large, the stirring speed is gradually reduced, the separation of the chloroform liquid drops is avoided, when the gray scale change rate reaches the extraction completion gray scale change rate, the chloroform liquid drops are extracted and completed, and the chloroform liquid drops are moved into a detection pool for detection.
Specifically, a chloroform gray matrix L (g 1, g2, g3, … gn) and a content range matrix Ce (Ce 1, ce2, ce3, … Cen) are arranged in the central control unit, the central control unit compares the real-time gray ga of the real-time image of the chloroform droplet with each standard contrast gray in the chloroform gray matrix L, selects a corresponding standard contrast gray gi, enables g (i-1) < ga to be not more than gi, and selects a corresponding standard content range Cei, i =1, 2, 3, … n from the content range matrix Ce (Ce 1, ce2, ce3, … Cen);
wherein g1 is the 1 st standard contrast gray scale, g2 is the 2 nd standard contrast gray scale, g3 is the 3 rd standard contrast gray scale … gn is the nth standard contrast gray scale, and g1 is more than g2 and more than g3 and more than … and more than gn; ce1 is the 1 st content range, ce2 is the 2 nd content range, ce3 is the 3 rd content range, … Cen is the nth content range, any content range Cev includes Cevmin and Cevmax, and Cevmin = Ce (v-1) max, cevmax = Ce (v + 1) min, where v =1, 2, 3, … n, cevmin is the minimum content value of the vth content range, and Cevmax is the maximum content value of the vth content range.
The method comprises the steps of selecting a corresponding gray scale interval in a chloroform gray scale matrix according to the real-time gray scale of a chloroform liquid drop real-time image, selecting a corresponding standard content range in a content range matrix, replacing traditional colorimetric detection with the combined image, improving detection precision, determining the content range of the detected anion synthetic detergent, and guaranteeing detection accuracy.
Specifically, the microextraction device and the extracted chloroform liquid drop hung below the microextraction device are moved into the detection pool, the sample absorbance Ay of the extracted chloroform liquid drop is detected through a photometer, the microextraction device is controlled to discharge the unextracted blank chloroform liquid drop into the detection pool, the blank absorbance Ak of the blank chloroform liquid drop is detected through the photometer, the sample absorbance difference delta Ay, delta Ay = Ay-Ak is calculated through a central control unit, and the real-time sample content Cy, cy = delta Ay multiplied by Q is calculated, wherein the Q blue complex content absorbance conversion parameter is calculated.
Specifically, the central control unit compares the calculated real-time sample content Cy with the selected corresponding standard content range Cei,
if the real-time content Cy of the sample is within the standard content range Cei, the central control unit judges that the detection of the anion synthetic detergent in the sample solution is finished, and outputs the real-time content Cy of the sample as a result;
and if the real-time content Cy of the sample is not in the standard content range Cei, the central control unit judges that the detection of the sample solution is invalid, and the sample solution is prepared again for detection.
The method comprises the steps of detecting the sample absorbance of extracted chloroform droplets and the blank absorbance of blank chloroform droplets through distribution of a photometer, calculating the difference value between the sample absorbance and the blank absorbance, and accurately calculating the real-time content of a sample through a central control unit, wherein the content absorbance conversion parameter of a blue complex is set in real time according to the volume of a used methylene blue solution, chloroform and chloroform droplets generated by a micro-extraction device, the calculated real-time content of the sample is checked and compared with a standard content range selected according to the gray level, the result is output, and the accuracy of the detection result is improved.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for detecting an anion synthetic detergent based on a microextraction technology is characterized by comprising the following steps,
step S1, washing the surface of an object to be detected to obtain a sample solution, putting the sample solution into a treatment pool, detecting the real-time solution temperature of the sample solution in real time through a temperature detector, adjusting a temperature control device according to the real-time solution temperature of the sample solution, adjusting the temperature of the sample solution, and controlling the amount of an acidic regulator and an alkaline regulator to adjust the real-time PH value of the sample solution;
s2, adding a methylene blue solution into the sample solution with the temperature and PH value adjusted, and stirring the sample solution by controlling a stirrer at the bottom of the treatment pool;
step S3, preheating the chloroform in the micro-extraction device, controlling the micro-extraction device to discharge chloroform droplets downwards after the chloroform is preheated, moving the micro-extraction device with the chloroform droplets suspended at the lower part into a treatment pool, enabling the suspended chloroform droplets to be below the liquid level of the sample solution, and stirring the sample solution by controlling the stirring speed of a stirrer so as to enable the chloroform droplets to extract the sample solution;
and S4, carrying out real-time image acquisition on the chloroform droplets, carrying out gray processing on the chloroform droplet real-time images through a central control unit, calculating the image gray change rate in unit detection time to judge whether extraction is finished or not, comparing the real-time gray of the extracted chloroform droplet real-time images with a chloroform gray matrix arranged in the central control unit, selecting a standard content range from a content range matrix arranged in the central control unit, moving the extracted chloroform droplets and unextracted blank chloroform droplets into a detection pool, respectively detecting blank absorbance of the blank chloroform droplets and sample absorbance of the extracted chloroform droplets through a photometer, calculating the sample real-time content according to the blank absorbance and the sample absorbance through the central control unit, comparing the sample real-time content with the selected standard content range, and outputting the sample real-time content as a detection result when the sample real-time content is in the standard content range.
2. The method for detecting anion synthetic detergent based on micro-extraction technology as claimed in claim 1, wherein in the step S1, a first preset temperature T1 and a second preset temperature T2 are provided in the temperature control device, wherein T1 < T2, the sample solution in the processing pool is heated by the temperature control device at an initial heating temperature Tc, wherein Tc > T2, the real-time solution temperature Ts of the sample solution is detected by the temperature detector in real time, the real-time temperature Ts is compared with the first preset temperature T1 and the second preset temperature T2 by the central control unit,
when Ts is less than T1, the central control unit judges that the real-time solution temperature does not reach a first preset temperature, and the central control unit does not adjust the initial heating temperature Tc of the temperature control device;
when T1 is more than or equal to Ts and less than T2, the central control unit judges that the real-time solution temperature reaches a first preset temperature and does not reach a second preset temperature, and the central control unit adjusts the initial heating temperature Tc of the temperature control device to be Tc ', tc' = T2;
and when Ts is more than or equal to T2, the central control unit judges that the real-time solution temperature reaches a second preset temperature, and the central control unit judges the real-time PH value of the sample solution.
3. The method of claim 2, wherein the central control unit has a standard pH Kb and a standard pH difference Δ Kb, when the central control unit determines that the real-time solution temperature reaches a second predetermined temperature, the central control unit detects the real-time solution pH Ks of the sample solution through a pH meter disposed in the processing tank, the central control unit calculates the real-time solution pH difference Δ Ks, Δ Ks = | Kb-Ks | according to the real-time solution pH Ks of the sample solution and the standard pH Kb, and the central control unit compares the real-time solution pH difference Δ Ks with the standard pH difference Δ Kb,
when the delta Ks is less than or equal to the delta Kb, the central control unit judges that the real-time solution pH difference value of the sample solution does not exceed the standard pH difference value, adds a methylene blue solution into the sample solution in the treatment pool, and stirs the sample solution by controlling a stirrer at the bottom of the treatment pool;
and when the delta Ks is larger than the delta Kb, the central control unit judges that the real-time solution pH difference value of the sample solution exceeds the standard pH difference value, and compares the real-time solution pH value Ks of the sample solution with the standard pH value Kb to adjust the pH value of the sample solution.
4. The method for detecting anionic synthetic detergent based on microextraction technology as claimed in claim 3, wherein when said central control unit determines that the real-time solution pH difference of the sample solution exceeds the standard pH difference, the central control unit compares the real-time solution pH Ks of the sample solution with the standard pH Kb,
when Ks is less than Kb, the central control unit judges that the real-time solution pH value of the sample solution is lower than the standard pH value, the central control unit calculates the input amount M1, M1= (Kb-Ks). Times.a of an alkaline regulator, wherein a is the input coefficient of the alkaline regulator, the alkaline regulator is input into the treatment tank, the real-time solution pH value in the treatment tank is detected through the pH meter, the central control unit repeats the calculation and judgment operation of the real-time solution pH difference value until the calculated real-time solution pH difference value does not exceed the standard pH difference value, the methylene blue solution is added into the sample solution in the treatment tank, and the sample solution is stirred through a stirrer at the bottom of the control treatment tank;
when Ks is larger than Kb, the central control unit judges that the real-time solution pH value of the sample solution is higher than the standard pH value, calculates the adding amount M2 of the acidic regulator, wherein M2= (Ks-Kb). Times.b, b is the adding coefficient of the acidic regulator, adds the acidic regulator into the treatment tank, detects the real-time solution pH value in the treatment tank through the pH meter, and repeats the calculation and judgment operation of the real-time solution pH difference value until the calculated real-time solution pH difference value does not exceed the standard pH difference value, adds the methylene blue solution into the sample solution in the treatment tank, and stirs the sample solution through a stirrer at the bottom of the treatment tank.
5. The method for detecting the anionic synthetic detergent based on the microextraction technology according to claim 4, wherein in the step S3, an initial stirring speed Vc of the stirrer is arranged in the central control unit, the chloroform in the microextraction device is preheated to a chloroform real-time temperature Tf, wherein T1 < Tf < T2, the microextraction device is controlled to discharge chloroform droplets downwards, the chloroform droplets are suspended at the lower part of the microextraction device, the microextraction device suspended with the chloroform droplets at the lower part is moved into the treatment tank, the suspended chloroform droplets are below the liquid level of the sample solution, and the stirrer is controlled by the central control unit to stir the sample solution in the treatment tank at the initial stirring speed Vc.
6. The method for detecting the anionic synthetic detergent based on the microextraction technology as claimed in claim 5, wherein a unit detection time length t is set in the central control unit, when the sample solution in the treatment tank is stirred by the stirrer at an initial stirring speed Vc, real-time image acquisition is performed on chloroform droplets below the liquid level of the sample solution, gray processing is performed on real-time images of the chloroform droplets by the central control unit, an average gray value of a chloroform droplet region in the real-time images is obtained as a real-time gray Gs of the real-time images, and the central control unit calculates a real-time gray change rate Gs, gs = (Gs-Gs ')/t within any unit detection time length t, wherein Gs is the real-time gray of the current real-time image of the chloroform droplets, and Gs' is the real-time gray of the real-time image of the chloroform droplets before the unit detection time length t.
7. The method for detecting anion synthetic detergent based on micro-extraction technology as claimed in claim 6, wherein the central control unit has a standard gray scale change rate Gb and a complete extraction gray scale change rate Gw, wherein Gb > Gw, the central control unit compares the calculated real-time gray scale change rate Gs with the standard gray scale change rate Gb and the complete extraction gray scale change rate Gw,
when Gs is larger than or equal to Gb, the central control unit judges that the real-time gray level change rate Gs is not lower than the standard gray level change rate Gb, the central control unit judges that the extraction of the chloroform liquid drops is in a standard state, and the initial stirring speed of the stirrer is not adjusted;
when Gb is larger than Gs and larger than Gw, the central control unit judges that the real-time gray scale change rate Gs is between the standard gray scale change rate Gb and the extraction completion gray scale change rate Gw, and adjusts the initial stirring speed Vc of the stirrer to Vc ', vc' = Vc- [ Vc x (Gw/Gs) ];
and when Gs is less than or equal to Gw, the central control unit judges that the real-time gray change rate Gs reaches the extraction completion gray change rate Gw, the central control unit judges that the chloroform droplet is extracted, the stirrer is controlled to stop stirring, the real-time gray ga of the chloroform droplet real-time image is obtained, and the micro-extraction device and the extracted chloroform droplet suspended below the micro-extraction device are moved into the detection pool.
8. The method for detecting the anion synthetic detergent based on the micro-extraction technology as claimed in claim 7, wherein a chloroform gray matrix L (g 1, g2, g3, … gn) and a content range matrix Ce (Ce 1, ce2, ce3, … Cen) are arranged in the central control unit, the central control unit compares a real-time gray ga of a real-time image of the chloroform droplet with each standard contrast gray in the chloroform gray matrix L, selects a corresponding standard contrast gray gi, makes g (i-1) < ga ≤ gi, and selects a corresponding standard content range Cei, i =1, 2, 3, … n from the content range matrix Ce (Ce 1, ce2, ce3, … Cen);
wherein g1 is the 1 st standard contrast gray scale, g2 is the 2 nd standard contrast gray scale, g3 is the 3 rd standard contrast gray scale … gn is the nth standard contrast gray scale, and g1 is more than g2 and more than g3 and more than … and more than gn; ce1 is the 1 st content range, ce2 is the 2 nd content range, ce3 is the 3 rd content range, … Cen is the nth content range, any content range Cev includes Cevmin and Cevmax, and Cevmin = Ce (v-1) max, cevmax = Ce (v + 1) min, where v =1, 2, 3, … n, cevmin is the minimum content value of the vth content range, and Cevmax is the maximum content value of the vth content range.
9. The method as claimed in claim 8, wherein the micro-extraction device and the extracted chloroform droplet suspended therebelow are moved into the detection cell, the sample absorbance Ay of the extracted chloroform droplet is detected by a photometer, and the micro-extraction device is controlled to discharge the unextracted blank chloroform droplet into the detection cell, and the blank absorbance Ak of the blank chloroform droplet is detected by the photometer, the sample absorbance difference Δ Ay, Δ Ay = Ay-Ak is calculated by a central control unit, and the real-time sample content Cy, cy = Δ Ay × Q, is calculated, wherein Q blue complex content absorbance is converted into a parameter.
10. The method for detecting anionic synthetic detergent based on microextraction technology according to claim 9, wherein the real-time content Cy of the calculated sample is compared with the corresponding standard content range Cei selected by the central control unit,
if the real-time content Cy of the sample is within the standard content range Cei, the central control unit judges that the detection of the anion synthetic detergent in the sample solution is finished, and outputs the real-time content Cy of the sample as a result;
if the real-time content Cy of the sample is not in the standard content range Cei, the central control unit judges that the detection of the sample solution is invalid, and the sample solution is prepared again for detection.
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