CN110907371B - On-site detection reagent tube for ferric ions in water and detection method - Google Patents
On-site detection reagent tube for ferric ions in water and detection method Download PDFInfo
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- CN110907371B CN110907371B CN201911177862.0A CN201911177862A CN110907371B CN 110907371 B CN110907371 B CN 110907371B CN 201911177862 A CN201911177862 A CN 201911177862A CN 110907371 B CN110907371 B CN 110907371B
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Abstract
The invention relates to a field detection reagent tube for ferric ions in water and a detection method, belongs to the technical field of water quality detection and monitoring, and solves the problems of complex operation, low accuracy, high cost and low efficiency in the detection process of the ferric ions in water in the prior art. The invention discloses a field detection reagent tube for ferric ions in water, which comprises a colorimetric tube, a colorimetric tube cock and a color-developing agent cock, wherein the colorimetric tube cock is connected with the colorimetric tube. According to the on-site detection reagent tube for ferric ions in water, the sleeve is arranged in the color comparison tube cock, the sealing film is used for sealing the sleeve, the screw rod of the color development reagent cock is matched with the sleeve, the solid color development reagent is preassembled in the groove at the end part of the screw rod, and the sealing film is pushed open by screwing the screw rod to release the solid color development reagent when a water sample to be detected is detected.
Description
Technical Field
The invention relates to the technical field of water quality detection and monitoring, in particular to a reagent tube for on-site detection of ferric ions in water and a detection method.
Background
Iron is a trace element necessary for human body, and iron is one of essential elements constituting human body, and has various physiological functions in human body. In daily life, iron element accounts for a corresponding proportion of trace elements absorbed by human bodies through drinking water, and the detection of iron ion content is a detection item specified by national drinking water standards. Ferric ion is a common iron ion, and is mainly present in iron salts and solutions thereof. Ferric ions are highly oxidative, and the solution is brownish yellow, but the color of the ferric ions is not the color of the ferric ions themselves, but the complex formed by the reaction of the lewis acid and water. The ferric ion has stronger oxidability and easy hydrolysis, and can catalyze various reactions. Ferric ions are extremely toxic and have strong oxidizing action in human bodies to cause organ failure of human bodies. Therefore, the detection and analysis of ferric ions in the environmental water body are particularly important.
The existing national and industrial standard methods mainly measure ferric ions in water in a laboratory, and the ferric ions in water are measured in the laboratory, so that a water sample to be measured needs to be transported back to the laboratory, and a liquid color developing agent is prepared, and is not easy to store. However, after the water sample to be detected contacts air in the sampling process, ferrous ions in the water are easily oxidized into ferric ions; iron is easy to generate valence state change in the storage and transportation processes of the water sample to be detected, namely, ferrous ions are converted into ferric ions; when the pH is more than 3.5, the trivalent iron ions are easily hydrolyzed and precipitated, and thus, it is difficult to accurately measure the trivalent iron ions in water.
In summary, the method for measuring ferric ions in water in laboratory has the following disadvantages: (1) The water sample to be detected needs to be transported back to a laboratory for analysis, and valence state change easily occurs between ferrous ions and ferric ions in the water in the storage and transportation processes of the water sample to be detected, so that the ferric ions are difficult to accurately determine; (2) The liquid color developing agent prepared in a laboratory and used for detecting ferric ions in water is not easy to store and needs to be prepared regularly; a large-scale analytical instrument is needed during laboratory test, the sampling amount is large, and correspondingly, more reagents are consumed; the sample storage and transportation need corresponding expenses, resulting in higher comprehensive cost; (3) After the water sample to be tested is collected, the water sample needs to be transported back to a laboratory for waiting analysis, the test period is long, and the efficiency is low.
Disclosure of Invention
In view of the foregoing analysis, embodiments of the present invention are directed to provide a reagent tube for on-site detection of ferric ions in water and a detection method thereof, so as to solve the problems of complex operation, low accuracy, high cost and low efficiency in the existing detection process of ferric ions in water.
The embodiment of the invention provides a field detection reagent tube for ferric ions in water, which comprises a colorimetric tube, a colorimetric tube cock and a color developing agent cock, wherein the colorimetric tube cock is connected with the colorimetric tube.
Further, a sleeve is arranged in the color comparison tube cock, and the sleeve is cylindrical and is provided with an internal thread.
Further, a sealing film is arranged at the bottom of the sleeve.
Further, the color developing agent cock comprises a screw cap and a screw rod, and the screw rod is connected with the sleeve.
The embodiment of the invention provides an on-site detection method for ferric ions in water, which uses a detection reagent tube as claimed in any one of claims 1 to 4;
the method comprises the following steps:
step 1: preparing a prefilled liquid medicament;
and 2, step: establishing a detection standard curve;
and step 3: judging whether a detection standard curve needs to be reestablished; if yes, executing step 2, otherwise, executing step 4;
and 4, step 4: and (5) detecting the water sample to be detected on site.
Further, in the step 1, the prefilled liquid medicament is 0.5ml of a PH adjusting and stabilizing solution, and the PH adjusting and stabilizing solution is prepared from 0.1ml of a sulfuric acid solution with a mass percentage of 8% and 0.4ml of a hydrochloric acid solution with a mass percentage of 10%; the pre-filled liquid medicament is arranged in the colorimetric tube.
Further, in step 2, the establishing of the detection standard curve includes:
step 2.1: preparing a standard solution;
diluting the ferric ion standard solution into a series of standard solutions of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0 mg/L;
step 2.2: sampling a standard solution;
respectively transferring 2.5ml of series standard solutions of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L into a 6-branch colorimetric tube, and screwing a cock of the colorimetric tube;
step 2.3: carrying out color reaction on the standard solution;
screwing the color developing agent cock into the sleeve, pushing the sealing film open by the screw rod, releasing the solid color developing agent, shaking uniformly, and waiting for 5min;
step 2.4: testing a standard solution;
and (3) performing instrument zeroing by taking 0.0mg/L standard solution as a reference solution, sequentially placing colorimetric tubes filled with 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L series of standard solutions in colorimetric wells of a photometer for absorbance determination, and storing the test program.
Further, in step 4, the field detection of the water sample to be detected comprises the following steps:
step 4.1: sampling a water sample to be detected;
using a syringe or a pipette to transfer 2.5ml of water sample to be detected into the colorimetric tube, and screwing down the cock of the colorimetric tube;
step 4.2: performing color reaction on a water sample to be detected;
screwing the color developing agent cock into the sleeve, pushing the sealing film open by the screw rod, releasing the solid color developing agent, shaking uniformly, and waiting for 5min;
step 4.3: testing a water sample to be tested;
and (3) zero setting of the instrument is carried out by taking 0.0mg/L standard solution as a reference, the colorimetric tube of the water sample to be tested is placed in a colorimetric hole of a photometer, the concentration of ferric ions in the water sample to be tested is read, and the field test is completed.
Further, the solid color developing agent is a superior pure potassium thiocyanate crystal.
Furthermore, the solid color developing agent is preloaded in the groove, and the preloading mass is 0.05g.
Compared with the prior art, the invention can realize at least one of the following beneficial effects:
(1) The sleeve is arranged in the color comparison tube cock, the sealing film is arranged at the bottom of the sleeve, the reinforcing strips are arranged on the outer circumferential surface of the sleeve and connected with the sealing film, so that when the solid color developing agent is released, the sealing film at the bottom of the sleeve is ensured to be opened, the opened sealing film is prevented from falling off, the structure is simple and convenient, and the operation is easy;
(2) The groove is formed in the bottom of the screw, the solid color developing agent is preassembled in the groove, the screw is screwed in to push the sealing film at the bottom of the sleeve open, and then the solid color developing agent can be released, so that the structure is simple, and the operation is convenient and fast;
(3) The solid color developing agent is a superior pure potassium thiocyanate crystal, the pre-loading mass is 0.05g, the purchased solid color developing agent is directly pre-loaded in the reagent tank, secondary preparation is not needed, and the pre-loading amount is only 0.05g, so that the detection cost is reduced compared with a liquid color developing agent which needs secondary preparation, has a larger preparation volume and uses more solid medicaments;
(4) The method comprises the following steps of pre-filling a liquid medicament in a colorimetric tube to be 0.5ml of PH regulating and stabilizing solution, and preparing the PH regulating and stabilizing solution by 0.1ml of sulfuric acid solution with the mass percent of 8% and 0.4ml of hydrochloric acid solution with the mass percent of 10%, so that ferric iron and a solid color developing agent in water generate a stable red complex, and the accuracy of a test result is ensured;
(5) Transferring 2.5ml of water sample to be detected into a colorimetric tube, screwing in a screw rod to push open a sealing film, releasing a solid color developing agent, and shaking up; compared with the sequence of releasing the solid color developing agent and adding the water sample to be detected, the color developing agent can exist for a long time, and the accuracy of detecting the content of ferric ions in water is ensured;
(6) Compared with a laboratory detection method, the method can be used for carrying out on-site detection on the water sample to be detected, the storage and transportation of the water sample to be detected are not required, the valence state conversion of iron ions in the water sample to be detected is avoided, and the detection accuracy is ensured; the field detection can be completed within 5-10 min, and the water sample to be detected is transported to a laboratory for detection, so that the detection period is more than 24 hours, and the detection efficiency is improved.
In the invention, the technical schemes can be combined with each other to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.
FIG. 1 is a schematic view of the overall structure of a detection reagent tube;
FIG. 2 is a schematic diagram of a cuvette structure of a detection reagent tube;
FIG. 3 is a cross-sectional view of a cock of a cuvette that detects a reagent tube;
FIG. 4 is a bottom view of the cuvette cock of the detection reagent tube;
FIG. 5 is a schematic diagram showing the overall structure of a color reagent cock of the detection reagent tube;
FIG. 6 is a cross-sectional view of a plug of a color reagent of the detection reagent tube;
FIG. 7 is a bottom view of a color reagent cock of the detection reagent tube;
FIG. 8 is a flow chart of a detection method.
Reference numerals:
1-a colorimetric cylinder; 2-a color comparison tube cock; 21-a sleeve; 22-sealing film; 23-a reinforcing strip; 3-color reagent cock; 31-a nut; 32-screw rod; 321-grooves.
Detailed Description
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate preferred embodiments of the invention and together with the description, serve to explain the principles of the invention and not to limit the scope of the invention.
Example 1
A specific embodiment of the present invention, as shown in fig. 1 to 7, discloses a field test reagent tube for ferric ions in water, which comprises a colorimetric tube 1, a colorimetric tube cock 2 and a color reagent cock 3, wherein the colorimetric tube cock 2 is in threaded connection with the colorimetric tube 1, a sleeve 21 is arranged in the colorimetric tube cock 2, and the sleeve 21 has a cylindrical structure and is provided with an internal thread; the bottom of the sleeve 21 is provided with a sealing film 22, illustratively, the sealing film 22 is a PVC film, and is adhered to the bottom of the sleeve 21 by adhesive; the outer circular surface of the sleeve 21 is provided with a reinforcing strip 23, illustratively, the reinforcing strip 23 is made of PVC, the reinforcing strip 23 is adhered to the outer circular surface of the sleeve 21, and the reinforcing strip 23 is connected with the sealing film 22; the color developing agent cock 3 comprises a screw cap 31 and a screw rod 32, the screw rod 32 is connected with the sleeve 21, and the bottom of the screw rod 32 is provided with a groove 321. It should be noted that, in this embodiment, the bottom of the sleeve 21 is a PVC film, a PVC reinforcing strip is arranged outside the PVC film, the PVC reinforcing strip is of an L-shape, one side of the PVC reinforcing strip is connected with the PVC film at the bottom of the sleeve 21, the other side of the PVC reinforcing strip is connected with the outer wall of the sleeve 21, and the PVC reinforcing strip has the following functions: after the color developing agent cock 3 props against the PVC film at the bottom of the barrel 21, the color developing agent cock 3 continues to be screwed in forcibly, the PVC film can be pushed open and does not fall off, the PVC reinforcing strip keeps connection and is not pushed away, and finally the purpose that the PVC film does not fall off when the solid color developing agent is released is achieved.
Compared with the prior art, in the embodiment, the sleeve is arranged in the color comparison tube cock, the sealing film is arranged at the bottom of the sleeve, the reinforcing strips are arranged on the outer circumferential surface of the sleeve and connected with the sealing film, and when the solid color developing agent is released, the sealing film at the bottom of the sleeve can be ensured to be opened, and the opened sealing film can not fall off; through being provided with the recess bottom the screw rod, solid developer is preloaded to the recess, and the precession screw rod is opened the seal membrane of sleeve bottom and can be released solid developer, and the simple structure of detect reagent pipe releases solid developer's simple operation.
In order to facilitate the colorimetric operation of the developed water sample to be detected in the detection process, the colorimetric tube 1 is made of transparent hard glass; in the embodiment, a portable spectrophotometer needs to be carried to detect a water sample to be detected, in order to match with a cuvette groove of the portable spectrophotometer, when the cuvette groove of the portable spectrometer is circular, a colorimetric tube 1 is circular, the diameter of the colorimetric tube 1 is slightly smaller than that of a colorimetric hole of the portable spectrophotometer, and the diameter of the colorimetric tube 1 is 12-15 mm; when the cuvette groove of the portable spectrophotometer is a square or rectangular strip, the colorimetric tube 1 is square, and the side length of the colorimetric tube 1 is 12-15 mm; the wall thickness of the cuvette 1 cannot be too thin, which is easy to break, nor too thick, which affects absorbance, and exemplarily, the wall thickness of the cuvette 1 is 1mm; the height of the colorimetric tube 1 is set according to the colorimetric hole structure of the portable spectrophotometer, not only about two thirds of the tube body of the colorimetric tube 1 is ensured to be inserted into the colorimetric hole of the portable spectrophotometer, but also the colorimetric tube 1 with a certain distance is ensured to be exposed outside the colorimetric hole, so that the colorimetric tube 1 is conveniently inserted into and taken out of the colorimetric hole, and exemplarily, in order to be suitable for the American Hash DR2800 portable spectrophotometer, the height of the colorimetric tube 1 is designed to be 60 mm-85 mm; the upper end of the colorimetric tube 1 is a spiral opening, the height of the spiral opening is 7mm, the diameter of the colorimetric tube is 11mm, the height of the spiral opening is moderate, the manufacturing cost is high if the height is too long, and the colorimetric tube cock 2 is insecure if the height is too short.
In the embodiment, the colorimetric cylinder plug cock 2 is made of plastic and has a cylindrical structure; in order to facilitate the exertion of force by hand, the colorimetric tube cock 2 is screwed down or unscrewed, and the height of the colorimetric tube cock 2 is 10mm; the diameter of the colorimetric tube cock 2 is equal to the diameter or side length of the colorimetric tube 1; in order to fix the sleeve 21 in the colorimetric tube cock 2 and prevent the sleeve 21 from shaking randomly, the upper end of the colorimetric tube cock 2 is a 3mm thick solid plastic layer, a hole is formed in the center of the solid plastic layer, the outer diameter of the sleeve 21 is in interference fit with the hole of the solid plastic layer, and the sleeve 21 can be fixed without other connection modes; the sleeve 21 is provided with an internal thread matched with the screw 32, and has an internal diameter of 5mm and a height of 8mm.
The color developing agent cock 3 is made of plastic, the height of the nut 31 is required to be smooth when the color developing agent cock 3 is pinched by fingers to be screwed in and out, illustratively, the height of the nut 31 is 5mm, and the diameter of the nut 31 is equal to that of the colorimetric tube cock 2; the diameter of the screw 32 is 5mm, and in order to ensure that the screw 32 can burst the sealing film 22 at the bottom of the sleeve 21, the length of the screw 32 must be greater than the height of the sleeve 21, and exemplarily, the length of the screw 32 is set to be 13mm. It should be noted that, the inner diameter of the sleeve 21 is set to be half of the outer diameter of the color comparison tube cock 2, which not only ensures the normal screwing and opening operation of the color comparison tube cock 2 and the color comparison tube 1, but also ensures the normal screwing operation of the screw rod 32 of the sleeve 21 and the color developing agent cock 3, the height 8mm of the sleeve 21 is smaller than the length 13mm of the screw rod 32, mainly ensuring that the screw rod 32 can smoothly burst the sealing film 22 at the bottom of the sleeve 21, and after the color developing agent cock 3 is screwed down, the top of the screw rod 32 has 5mm to expose the sleeve 21, and ensuring that the solid color developing agent in the groove 321 can be fully dissolved in a water sample or fully dissolved in a standard curve preparation solution.
Furthermore, the top end of the screw 32 is provided with a groove 321 with the diameter of 2.5mm and the depth of 2mm, and the groove is used for containing the solid color developing agent; a red line is marked 8mm away from the top of the screw rod 32, and when the groove 321 is preloaded with the solid color developing agent, the screw rod 32 is just screwed into the sleeve 21 by 8mm, so that the top of the screw rod 32 is tightly attached to the PVC film at the bottom of the sleeve 21.
Example 2
The embodiment provides an in-situ detection method for ferric ions in water, and is shown in fig. 8. The method is implemented by using an on-site detection reagent tube, and comprises the following steps: step 1: preparing a prefilled liquid medicament; step 2: establishing a detection standard curve; and step 3: judging whether a detection standard curve needs to be reestablished; if necessary, executing the step 2, and if not, executing the step 4; and 4, step 4: and (5) detecting the water sample to be detected on site.
In the on-site detection method in the embodiment, the detection standard curve is established to carry out on-site test on the water sample to be detected, and compared with a laboratory detection method, the storage and transportation of the water sample to be detected are not required, so that the valence state conversion of iron ions in the water sample to be detected is avoided, and the detection accuracy is ensured; the field detection can be completed within 5-10 min, and the water sample to be detected is transported to a laboratory for testing, and the general test period is more than 24 hours, so that the detection efficiency is improved.
In the embodiment, in the step 1, the prefilled liquid medicament is 0.5ml of a PH adjusting and stabilizing solution, and the PH adjusting and stabilizing solution is prepared from 0.1ml of a sulfuric acid solution with a mass percentage of 8% and 0.4ml of a hydrochloric acid solution with a mass percentage of 10%; it should be noted that the pre-filled liquid medicament is filled into the colorimetric tube 1 in advance, and both takes part in the reaction in the process of testing the water sample to be tested and preparing the standard curve, that is, the pre-filled liquid medicament is present in the colorimetric tube 1 in the processes of testing the water sample to be tested and preparing the standard curve. The concentration and volume ratio of sulfuric acid and hydrochloric acid determine the stability of a red complex generated by ferric ions and a solid color developing agent (potassium thiocyanate) in a water sample to be tested, the accuracy of a test result is directly influenced, and a pre-filled liquid medicament prepared by 0.1ml of sulfuric acid solution with the mass percent of 8% and 0.4ml of hydrochloric acid solution with the mass percent of 10% is pre-filled in a colorimetric tube 1, so that the ferric ions and the solid color developing agent in the water generate the stable red complex, and the accuracy of the test result is ensured. In this embodiment, the prepared pre-filled liquid medicament enables the complex formed by the solid color developing agent and the complex formed by the liquid color developing agent used in the standard laboratory detection method to have the same stability, and the accuracy of the detection result is not affected, as shown in table 1.
TABLE 1 comparison of the detection method of the present invention with the laboratory Standard method for detecting the concentration of ferric ions in water
As can be seen from Table 1, the detection results of the field detection method in this example are consistent with those of the laboratory standard method (DZ/T0064.24-93), and there is no significant difference through T-test. The sample addition recovery rate of the on-site detection method in the implementation is 95.07-106.17% (see table 2). It should be noted that the sample standard adding recovery rate is mainly used for explaining the accuracy of the method, a certain amount of ferric ions are added into the sample, then the detection method of the embodiment is used for detecting whether the content of the added ferric ions can be accurately detected, and the standard adding recovery rate of 95.07% -106.17% meets the test quality management specification part 6 of the DZ/T0130.6-2006 geological mineral laboratory: water sample analysis "requirement for accuracy control of detection method in standard. The standard DZ/T0130.6-2006 requires that when the concentration of the index to be detected in water is 1-100 mg/L, the recovery rate is allowed to be 90-110%, the recovery rate of the detection method in the embodiment is 95.07-106.17%, the standard requirement is met, and the detection method in the embodiment has accurate field detection result.
TABLE 2 test standard for recovery rate of sample added with standard by the detection method of the present invention
In this embodiment, in step 2, a detection standard curve is established, and the steps include:
step 2.1: preparing a standard solution; purchasing ferric ion standard substance solution with a national standard substance certificate, and diluting the ferric ion standard solution into series standard solutions of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0 mg/L;
step 2.2: sampling a standard solution; respectively transferring 2.5ml of series standard solutions of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L into a 6-branch colorimetric tube 1 by using a syringe or a pipette, and screwing a cock 2 of the colorimetric tube;
step 2.3: carrying out color reaction on the standard solution; screwing the color developing agent cock 3 into the sleeve 21, screwing the color developing agent cock 3 by force, tightly attaching the nut 31 of the color developing agent cock 3 to the colorimetric tube cock 2, ejecting the sealing film 22 at the bottom of the inner sleeve 21 of the colorimetric tube cock 2 by the screw 32 of the color developing agent cock 3, connecting the sealing film 22 with the outer wall of the sleeve 21 by the reinforcing strip 23, ejecting the sealing film 22, but not dropping, hanging the sealing film 22 on the outer wall of the sleeve 21 without influencing sample analysis, releasing the solid color developing agent, shaking the color developing agent uniformly, fully mixing and dissolving the water sample to be measured in the colorimetric tube 1 and the solid color developing agent, waiting for 5 minutes, and finishing color developing reaction.
It should be noted that, when the solid color developing agent is released, in the first case, the solid color developing agent smoothly falls into the colorimetric tube 1 and is mixed with the water sample to be measured; in the second case, even if some solid color developing agent remains in the groove 321, since the screw 32 of the color developing agent cock 3 has been screwed out of the sleeve by 5mm, when the sample is sufficiently shaken up, the groove 321 can be sufficiently cleaned by the sample to be measured in the colorimetric tube 1, so that the solid color developing agent is completely dissolved in the sample to be measured.
Step 2.4: testing a standard solution; a user program is newly established in a portable spectrophotometer, the mode is single wavelength, the analysis wavelength is 480nm, the standard measurement (or reading) step is carried out after the setting is finished, the instrument zero setting is carried out by taking 0.0mg/L standard solution as reference solution, colorimetric tubes filled with series of standard solutions of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L are respectively and sequentially placed in a colorimetric holes of the spectrophotometer for absorbance measurement, the concentration value of the standard solution is required to be input into the program when each standard solution sample is placed, the portable spectrophotometer can automatically draw a standard curve after the absorbance measurement is finished, a linear equation is calculated, and finally the test program is stored. After the test program is saved, the built in-water ferric ion on-site detection method is added to a user program of the portable spectrophotometer, the method comprises a standard curve, a linear equation calculated according to data of the standard curve and an analysis wavelength, and the method is directly called from an instrument when a water sample to be detected is detected subsequently. As shown in table 3, the testing apparatus uses standard curve data of the on-site detection method for ferric ions in water established by the usa hash DR2800 portable spectrophotometer.
TABLE 3 Standard Curve data of the on-site detection method of ferric ions in water established by the invention
It should be noted that, when the water sample to be detected is detected in a short time, only the 'in-water ferric iron on-site detection method' stored in the portable spectrophotometer needs to be taken, and the detection standard establishment step does not need to be carried out again, namely, the detection standard can be established for one day when one detection standard is prepared, the detection standard establishment is carried out for one time without detecting one water sample to be detected, then, after the blank zeroing is carried out by using a reagent, the step 4 is directly carried out, the detection of one water sample to be detected is completed, the step 4 is still repeated for the next water sample to be detected, and when the water sample to be detected is continuously detected, the 'zeroing' can be carried out once. After the on-site detection is completed on the same day, if the interval time is longer, the detection standard curve should be reestablished generally for more than two days, and when the on-site detection method for ferric ions in water is used again, the series of standard solutions need to be reconfigured, and the standard curve is updated to complete the calibration of the standard curve, so that the sample test can be continued.
In the field detection method of this embodiment, before the field detection of the water sample to be detected in step 4, it is determined whether a detection standard curve needs to be reestablished; if yes, step 2 is executed, if no, step 4 is executed, and the judgment basis is whether the detection standard established last time exceeds 24 hours.
Further, in step 4, the field detection of the water sample to be detected comprises the following steps:
step 4.1: sampling a water sample to be detected; using a syringe or a pipette to transfer 2.5ml of water sample to be detected into the colorimetric tube 1, and screwing down the colorimetric tube cock 2;
it should be noted that, if the water sample to be tested is turbid, the water sample to be tested should be filtered through a 0.45 μm filter membrane, and then 2.5ml of the water sample to be tested should be removed into the colorimetric tube 1.
Step 4.2: performing color reaction on a water sample to be detected; screwing the color developing agent cock 3 into the sleeve 21, screwing by force, tightly attaching the nut 31 of the color developing agent cock 3 to the colorimetric tube cock 2, ejecting the sealing film 22 at the bottom of the inner sleeve 21 of the colorimetric tube cock 2 by the screw 32 of the color developing agent cock 3, connecting the outer wall of the sleeve 21 with the sealing film 22 by the reinforcing strip 23, ejecting the sealing film 22, but not dropping, suspending the sealing film 22 on the outer wall of the sleeve 21 without influencing sample analysis, releasing the solid color developing agent, shaking uniformly, fully mixing and dissolving the water sample to be tested in the colorimetric tube 1 and the solid color developing agent, waiting for 5 minutes, and finishing color developing reaction.
It should be noted that 2.5ml of the water sample to be measured is transferred into the colorimetric tube, and then the screw 32 is screwed in to push open the sealing film 22, release the solid color developing agent, and shake uniformly; compared with the sequence of releasing the solid color developing agent and adding the water sample to be detected, the color developing agent can be stored for a long time, and the accuracy of detecting the content of ferric ions in water is ensured.
Step 4.3: testing a water sample to be tested; the newly established (or newly calibrated) in-water ferric iron field detection method is called out from a user program of a portable spectrophotometer, the zero setting of the instrument is carried out by taking 0.0mg/L standard solution as reference, a colorimetric tube 1 of a water sample to be tested is placed in a color comparison hole of the portable spectrophotometer, the concentration of ferric iron ions in the water sample to be tested is read, and the field test is completed.
It should be noted that the in-situ detection method for ferric ions in water stored by the portable spectrophotometer includes a standard curve and a linear equation, so that the portable spectrophotometer can automatically calculate the concentration of ferric ions in a water sample to be detected according to the measured absorbance when detecting the water sample to be detected, and display the concentration value of ferric ions on a screen.
In the field detection method of this embodiment, the solid developer is a high-grade pure potassium thiocyanate crystal, and the solid developer is preloaded in the groove 321, where the preloaded mass is 0.05g. The purchased solid color developing agent is directly pre-installed in the groove 321, secondary preparation is not needed, and the pre-installation amount is only 0.05g, so that the detection cost is reduced compared with a liquid color developing agent which needs secondary preparation, has a larger preparation volume and uses more solid medicaments; the liquid color developing agent used in the ferric ion detection method in the laboratory refers to a solution-state color developing agent, and specifically refers to a liquid reagent prepared by dissolving a solid color developing agent (potassium thiocyanate, sulfosalicylic acid or other color developing agents) in a solvent (pure water, acid-base or other chemical solutions) according to a certain proportion, wherein the liquid reagent is used for a ferric ion complexing color developing reaction, and the liquid color developing agent is obtained. The liquid color developing agent is not easy to store, and in the embodiment, the solid color developing agent is a high-purity medicine, and the shelf life is generally more than one year. The liquid color developing agent is prepared from a high-purity solid medicine and a solvent, the concentration is low, the solvent contains water or an acid-base reagent, chemical components of the color developing agent are easy to change, the color developing agent loses efficacy and cannot normally perform color developing reaction, the effective period of the general liquid reagent is within three months, even the shelf life of some liquid reagents is only about one week, and individual liquid reagents need to be stored in a dark place, so that the liquid color developing agent is difficult to store, needs to be prepared frequently, and is high in cost. The on-site assay of the invention is shown in Table 4 in comparison to the standard laboratory assay.
TABLE 4 comparison of the amounts of reagents used in the test method of the present invention and the laboratory Standard test method
According to the reagent tube for on-site detection of ferric ions in water, the sleeve is arranged in the color comparison tube cock, the sealing film is arranged at the bottom of the sleeve, the reinforcing strips are arranged on the outer circumferential surface of the sleeve and connected with the sealing film, and when the solid color developing agent is released, the sealing film at the bottom of the sleeve is ensured to be opened, and the opened sealing film is prevented from falling; through being provided with the recess bottom the screw rod, solid developer is preloaded to the recess, and the precession screw rod is opened the seal membrane of sleeve bottom and can be released solid developer, and the simple structure of detect reagent pipe releases solid developer's simple operation. According to the method for detecting the ferric ions in the water on site, the water sample to be detected is subjected to on-site test by establishing the detection standard curve, and compared with a laboratory detection method, the storage and transportation of the water sample to be detected are not required, so that the valence state conversion of the ferric ions in the water sample to be detected is avoided, and the detection accuracy is ensured; the field detection can be completed within 5-10 min, and the water sample to be detected is transported to a laboratory for testing, the testing period is generally more than 24 hours, and the detection efficiency is improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (3)
1. A field detection method for ferric ions in water is characterized in that,
the reagent tube used in the on-site detection method consists of a colorimetric tube, a colorimetric tube cock, a color reagent cock, a sealing film and a reinforcing strip, wherein the colorimetric tube cock is connected with the colorimetric tube; a sleeve is arranged in the color comparison tube cock, is of a cylindrical structure and is provided with an internal thread; the upper end of the color comparison tube cock is a solid plastic layer, a hole is arranged in the center of the solid plastic layer, and the outer diameter of the sleeve is in interference fit with the hole of the solid plastic layer; the inner diameter of the sleeve is half of the outer diameter of the plug of the colorimetric tube; the sealing film is arranged at the bottom of the sleeve;
the color developing agent cock comprises a screw cap and a screw rod, and the screw rod is connected with the sleeve; the colorimetric tube is a straight tube, the upper end of the colorimetric tube is a threaded opening connected with the colorimetric tube cock, one end of the reinforcing strip is connected with the outer wall of the sleeve, the other end of the reinforcing strip is connected with the sealing film, the bottom of the screw is provided with a groove for placing the solid color developing agent, and the length of the screw is greater than that of the sleeve; a marking line is arranged at a position which is away from the top of the screw rod by a length of the sleeve, and when the groove is pre-filled with the solid color developing agent, the screw rod is screwed into the sleeve, so that the top of the screw rod is ensured to be tightly attached to a sealing film at the bottom of the sleeve;
the detection step comprises:
step 1: preparing a prefilled liquid medicament, wherein the prefilled liquid medicament is 0.5ml of pH adjusting and stabilizing solution, and the pH adjusting and stabilizing solution is prepared from 0.1ml of sulfuric acid solution with the mass percent of 8% and 0.4ml of hydrochloric acid solution with the mass percent of 10%; the pre-filled liquid medicament is arranged in the colorimetric tube;
and 2, step: establishing a detection standard curve;
in the step 2, the detection standard curve is established, and the steps include:
step 2.1: preparing a standard solution;
diluting the ferric ion standard solution into 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L series standard solutions;
step 2.2: sampling a standard solution;
respectively transferring 2.5ml of series standard solutions of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L into a 6-branch colorimetric tube, and screwing down a stopcock of the colorimetric tube;
step 2.3: carrying out color reaction on the standard solution;
screwing the color developing agent cock into the sleeve, pushing the sealing film open by the screw rod, releasing the solid color developing agent, shaking uniformly, and waiting for 5min;
step 2.4: testing a standard solution;
performing instrument zeroing by taking 0.0mg/L standard solution as a reference solution, sequentially placing colorimetric tubes filled with 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L and 2.0mg/L series of standard solutions in a colorimetric hole of a photometer for absorbance determination, and storing a test program;
and step 3: judging whether a detection standard curve needs to be reestablished; executing step 2 when the detection standard curve established last time exceeds 24 hours, and executing step 4 when the detection standard curve established last time does not exceed 24 hours;
and 4, step 4: detecting a water sample to be detected on site;
in the step 4, the field detection of the water sample to be detected comprises the following steps:
step 4.1: sampling a water sample to be detected;
using a syringe or a pipette to transfer 2.5ml of water sample to be detected into the colorimetric tube, and screwing down the cock of the colorimetric tube; when the water sample to be detected is turbid, filtering the water sample to be detected through a 0.45 mu m filter membrane and then transferring the water sample to be detected;
step 4.2: performing color reaction on a water sample to be detected;
screwing the color developing agent cock into the sleeve, pushing the sealing film open by the screw rod, releasing the solid color developing agent, shaking uniformly, and waiting for 5min;
step 4.3: testing a water sample to be tested;
and (3) zero setting of the instrument is carried out by taking 0.0mg/L standard solution as a reference, the colorimetric tube of the water sample to be tested is placed in a colorimetric hole of a photometer, the concentration of ferric ions in the water sample to be tested is read, and the field test is completed.
2. The in-situ detection method according to claim 1, wherein the solid color developing agent is superior pure potassium thiocyanate crystal.
3. The in-situ test method according to claim 2, wherein the solid developer is pre-loaded into the grooves with a pre-loading mass of 0.05g.
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| CN2806353Y (en) * | 2005-04-19 | 2006-08-16 | 汕头市粤东机械厂有限公司 | Improved pouring and drinking device and container employing the same |
| CN207036703U (en) * | 2017-07-30 | 2018-02-23 | 北京蓝木科技有限公司 | Protein content detection means in a kind of liquid milk of scene |
| CN207667679U (en) * | 2017-12-14 | 2018-07-31 | 广东健安检测科技有限公司 | A kind of closed integrated detection reagent pipe |
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| CA2078648A1 (en) * | 1991-09-30 | 1993-03-31 | David C. Yeaw | Test kit and method for the determination of metal ion concentration in solution |
| CN2277510Y (en) * | 1996-11-14 | 1998-04-01 | 陈立宏 | Refrigerating tube |
| CN2577278Y (en) * | 2002-11-12 | 2003-10-01 | 吉林大学化学学院 | Disposable colorimetric quick test package of methanal in air |
| CN103760330B (en) * | 2013-12-31 | 2016-03-30 | 杭州迪图科技有限公司 | A kind ofly to collect and the device of analyte in test fluid sample |
| CN105466858B (en) * | 2015-11-20 | 2017-04-26 | 广东伟创科技开发有限公司 | Integrated digestion colorimetric pool |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2806353Y (en) * | 2005-04-19 | 2006-08-16 | 汕头市粤东机械厂有限公司 | Improved pouring and drinking device and container employing the same |
| CN207036703U (en) * | 2017-07-30 | 2018-02-23 | 北京蓝木科技有限公司 | Protein content detection means in a kind of liquid milk of scene |
| CN207667679U (en) * | 2017-12-14 | 2018-07-31 | 广东健安检测科技有限公司 | A kind of closed integrated detection reagent pipe |
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