Device and method for measuring elements in water

Abstract

The invention relates to a spectrum technology, and particularly provides a device and a method for measuring elements in water, the measuring device comprises a paper tape, a driving unit and an element measuring unit, the driving unit is used for driving the paper tape to move; the first applying unit is used for quantifying a water sample and applying the water sample to the paper tape; the first heating unit is used for heating a water sample applying part on the paper tape; and the element measuring unit measures the element content in the sample which is heated by the first heating unit and moved to the measuring unit by the driving unit. The device has the advantages of simple structure, good reliability and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of spectroscopy, in particular to a device and method for measuring elements in water. BACKGROUND

[0002] At present, the detection of elements in water usually adopts the pretreatment technology of water sample atomization, drying and enrichment, and combines with X-ray fluorescence (XRF) technology to realize the rapid detection of inorganic elements in water quality samples such as underground water and river water. The specific scheme is as follows: First, the liquid sample to be measured is introduced into an atomizer, and a certain proportion of dry and clean air is introduced into the atomizer at the same time to realize the atomization of the liquid sample. The atomized sample is then heated in a heating cavity by high-temperature air to eliminate the water in the sample and form aerosol particles. Finally, the above particles are enriched on a paper tape by a gas suction pump, and the concentration of heavy metal elements enriched on the paper tape is detected by XRF technology. The disadvantages of this technical scheme are as follows: 1. Clean air or inert gas needs to be used as the atomization gas source, and a large amount of high-temperature clean air or inert gas needs to be used as the drying gas to completely evaporate the water in the liquid droplets, so that a large flow of gas containing aerosol particles is finally formed, resulting in a large equipment size, high power consumption, large gas consumption, and high requirements for the gas resistance of the filter material due to the large gas flow generated.

[0003] 2. Since the composition of water quality samples such as underground water, surface water and river water is complex, they often contain a large amount of calcium carbonate, sulfate, chloride and other substances, which result in a large amount of aerosol particles. These particles are easily enriched on the paper tape, which can cause paper tape blockage, unstable air flow, and even broken paper tape.

[0004] 3. Since the paper tape is quickly blocked by high-content particles, the total amount of enriched water quality samples is limited, and many low-content heavy metal elements cannot be effectively enriched and detected, resulting in serious distortion of the detection results. SUMMARY

[0005] To solve the above problems in the prior art, the present application provides a device for measuring elements in water.

[0006] The purpose of the present application is achieved by the following technical scheme: The device for measuring elements in water comprises a paper tape and a driving unit, wherein the driving unit is used to drive the movement of the paper tape; the measuring device further comprises: a first application unit, which is used to quantitatively apply water samples to the paper tape; a first heating unit, which is used to heat the part of the paper tape to which the water sample is applied.

[0007] The application also aims to provide a water element measuring method. The water element measuring method comprises the following steps: A1. A first heating unit preheats a sampling area of a paper tape; A water sample is quantitatively applied to the sampling area, the first heating unit heats the sampling area, water is evaporated, and the component to be measured is enriched in the sampling area; A3. The water sample spot enriched with the component to be measured moves with the paper tape to an element measuring unit; A4. The element measuring unit outputs the element content in the water sample according to the detection result of the water sample spot.

[0008] Compared with the prior art, the application has the beneficial effects that: The application directly changes the component to be measured in the water sample into a solid by heating and deposits it on a high-temperature-resistant substrate, without the need for atomization and suction enrichment, has the advantages of simple flow path, no clogging problem, and no need for a large amount of clean air; All elements in the water sample are effectively enriched, significantly improving the detection accuracy. BRIEF DESCRIPTION OF DRAWINGS

[0009] The disclosure of the application will become more apparent with reference to the accompanying drawings. It is easy for those skilled in the art to understand that the drawings are only used to illustrate the technical solutions of the application and are not intended to limit the protection scope of the application. In the drawings: Figure 1 is a structural schematic diagram of a water element measuring device according to an embodiment of the application.

[0010] In the drawings, 11 is a driving unit, 12 is a paper tape, 31 is a first application unit, 310 is a switching module, 311 is a first sample needle, 312 is a water sample tank, 313 is a first pipeline, 314 is a second pipeline, 315 is a filter, 316 is a first pump, 317 is a constant-volume bottle, 318 is a differential pressure sensor, 319 is a second pump, 32 is a second application unit, 321 is a pure water tank, 322 is a syringe pump, 323 is a second sample needle, 33 is a third application unit, 41 is a first heating unit, 42 is a second heating unit, and 51 is an element measuring unit. DETAILED DESCRIPTION

[0011] Figure 1The alternative embodiments of the present application described in the following description and illustrated in the accompanying drawings are presented by way of example only. The novel methods and apparatuses described herein can be implemented in various ways, and the application should not be limited to the embodiments described herein, which are presented as examples. Numerous specific details are described in order to provide a thorough understanding. However, in some instances, well-known or conventional details are not described in order to not unnecessarily obscure the present application. The various novel methods and apparatuses described herein can be implemented in various ways and can be applied to various uses. Embodiment

[0012] The water element measuring device of the embodiment of the present application, as shown in Figure 1 includes: The driving unit 11 is used to drive the paper tape 12 to move.

[0013] The first applying unit 31 is used to quantify the water sample and apply it to the paper tape 12.

[0014] The first heating unit 41 is used to heat the part of the paper tape 12 to which the water sample is applied.

[0015] In order to quantify and apply the water sample, the first applying unit 31 includes: The water sample tank 312 is connected to the constant volume bottle 317 through the first pipeline 313 and the second pipeline 314 respectively.

[0016] The filter 315 is arranged on the second pipeline to retain only the dissolved elements.

[0017] The first sample needle 311 is connected to the constant volume bottle 317.

[0018] The pump, including the first pump 316 and the second pump 319, is used to deliver the water sample in the water sample tank 312 and the constant volume bottle 317.

[0019] In order to obtain the measurement background, the measuring device further includes a second applying unit 32 and a second heating unit 42, the second applying unit 32 is used to quantify pure water and apply it to the paper tape 12; the second heating unit 42 is used to heat the part of the paper tape 12 to which the pure water is applied.

[0020] In order to realize calibration and obtain the spiked recovery rate, the measuring device further includes a third applying unit 33, the third applying unit 33 is used to quantify the standard solution and deliver it to the constant volume bottle 317.

[0021] The water element measuring method of the embodiment, i.e. the working method of the measuring device of the embodiment, includes the following steps: A1. The first heating unit 41 preheats the sampling area of the paper tape 12.

[0022] A quantitative water sample is applied to the sampling area, the first heating unit 41 heats the sampling area, water evaporates, and the component to be measured is enriched in the sampling area. The radius of the water sample spot is a set value.

[0023] A3. The water sample spot enriched with the component to be measured moves to the element measurement unit 51 along the paper tape 12.

[0024] A4. The element measurement unit 51 outputs the element content in the water sample according to the detection result of the water sample spot.

[0025] In order to obtain the measurement background, the measurement method further comprises the steps of: B1. The second heating unit preheats the paper tape; A quantitative pure water is applied to the paper tape, the second heating unit heats the area on the paper tape where the pure water is applied, water evaporates, and the component to be measured is enriched on the paper tape; B2. The spot enriched with the component to be measured moves to the element measurement unit along the paper tape; B3. The element measurement unit outputs the element content in the pure water as the background according to the detection result of the spot.

[0026] The way of applying a quantitative water sample is: the sample in the sample tank is transferred to the constant volume bottle for constant volume, and then applied to the sampling area.

[0027] In order to obtain the spiked recovery rate, the measurement method further comprises a spiked recovery rate test, specifically: In one cycle, the element mass m1 in the sample in the constant volume bottle 317 is obtained; In the next cycle, the standard solution with element mass m0 is added to the constant volume bottle 317 and mixed with the sample, and the element mass m2 in the mixed solution is obtained; The spiked recovery rate (m2-m1) 100% / m0 is obtained.

[0028] Embodiment 2

[0029] Application example of the water element measurement device and method according to Embodiment 1 of the present application.

[0030] In this application example, as shown in Figure 1 The paper tape 12 is made of high-temperature resistant material, such as quartz paper tape, and is wound on the driving wheel and the driven wheel at both ends, so as to be moved.

[0031] The first application unit 31 comprises a water sample tank 312, a first pipeline 313 (a second pipeline 314), a switching module 310, a first pump 316, a constant volume bottle 317, a second pump 319, and a first sample needle 311 connected in sequence. A filter 315 is arranged on the second pipeline for retaining only dissolved elements. The switching module 310 adopts a two-position three-way valve to realize selection of the first pipeline 313 and the second pipeline 314. A differential pressure sensor 318 is connected to the constant volume bottle 317.

[0032] The second applying unit 32 includes a pure water tank 321, a syringe pump 322 and a second adding needle 323 connected in sequence. The pure water is quantitatively provided and applied to the paper tape 12. The second heating unit 42 is used to heat the part of the paper tape 12 to which the pure water is applied.

[0033] The third applying unit 33 is used to quantitatively provide the element standard solution and apply it into the sample constant volume bottle 317.

[0034] The first applying unit 31 and the second applying unit 32 are respectively arranged upstream and downstream of the element measuring unit 51. The element measuring unit 51 adopts an XRF analyzer.

[0035] The water element measuring method of the embodiment, i.e. the working method of the measuring device of the embodiment, includes the following steps: A1. The high-temperature-resistant paper tape 12 is moved so that the paper tape 12 below the second heating unit 42 and the XRF analyzer is clean paper tape, and then the upper and lower parts of the second heating unit 42 are moved and clamp the paper tape.

[0036] The equipment is preheated, and the second heating unit 42 reaches the set temperature.

[0037] The syringe pump 322 draws pure water and deposits it on the high-temperature-resistant paper tape of the second heating unit 42, which is evaporated and dried by vaporization. When the amount of pure water drawn reaches the actual sample test amount, the upper and lower parts of the second heating unit 42 are separated, and then the paper tape with dried pure water is moved to the XRF analyzer for background blank analysis. At this time, the spectrum is used as the background spectrum for subsequent sample measurement.

[0038] The first pump 316 draws the liquid sample in the water sample tank 312, and selects the liquid sample passing through or not passing through the filter 315 through the switching module 310 for subsequent enrichment and analysis. The first pump 316 draws the liquid sample not passing through the filter 315 to measure the element content in the water sample; the first pump 316 draws the liquid sample passing through the filter 315 to measure the dissolved element content in the liquid sample.

[0039] The first pump 316 pumps the liquid sample into the sample constant volume bottle 317. The constant volume bottle 317 can be constant volume by differential pressure principle, such as providing a differential pressure value by a differential pressure sensor 318, of course, it can also be constant volume by a liquid level sensor or other constant volume technology.

[0040] At the same time of the sample into the constant volume bottle 317, the first heating unit 41 clamps the paper tape, preheats in advance, and reaches the set temperature within a specified time.

[0041] A2. After volume adjustment, the second pump 319 draws the sample from the volume adjustment bottle 317 at a certain flow rate, so that the sample is deposited on the high-temperature paper tape at this speed. The high temperature on the paper tape is sufficient to make the deposited liquid sample evaporate and vaporize quickly, so that the deposition spot will not spread and grow larger. After all the liquid sample in the volume adjustment bottle 317 has been deposited, the volume sensor of the volume adjustment bottle 317 shows that the volume is 0. The second pump 319 needs to continue to work for a period of time to ensure that the residual liquid in the pipeline is also pumped into the first heating unit 41 for drying and deposition.

[0042] A3. After the drying and deposition are completed, the first heating unit 41 releases the paper tape, and the driving unit moves the paper tape to the XRF analysis area.

[0043] A4. Perform XRF analysis on the deposited spots to obtain the mass of heavy metal elements, and then combine this with the constant volume to finally obtain the element content in the liquid to be tested.

[0044] When it was time to measure the spiked recovery rate, routine sample testing was performed first. A portion (50 ml) of the sample from water sample container 312 was sent downstream for measurement. The volumetric flask 317 was filled to a final volume of 50 ml. After complete deposition in the sampling area, the enrichment spot area was 1 cm². 2 The measured surface density of Pb was 510.2 ng / cm³. 2 The mass of Pb is 510.2 ng, or 0.51 μg. The corresponding water sample volume is 50 ml, and the corresponding Pb concentration in the water is 10.2 μg / L.

[0045] In the next cycle, another portion (50 ml) of the sample from water sample container 312 is transferred to volumetric flask 317. The syringe in the third application unit 33 draws 1 ml of standard solution and transfers it to volumetric flask 317. The Pb concentration in the standard solution is 10 μg / ml. The standard solution and sample are mixed in volumetric flask 317, and then the 51 ml solution is heated and dried together. The measured Pb surface density is 10435.2 ng / cm³. 2 If the mass of Pb is 10.435 μg, then the spiked recovery rate is (10.435-0.51) / 10 = 99.25%.

[0046] The measuring device in this embodiment has a measurement range of 0-2000 mg / L, and the detection limit for the density of the 12-sided paper tape reaches 0.1-1.0 ng / cm³. 2 Quantity, precision <2%.

Claims

1. A device for measuring elements in water, comprising a paper tape and a driving unit, wherein the driving unit is used to drive the paper tape to move; characterized in that, The measuring device further includes: A first application unit is used to quantify the water sample and apply it onto the paper tape; The first heating unit is used to heat the portion of the paper tape on which the water sample is applied.

2. The measuring device according to claim 1, characterized in that, The first application unit includes: A water sample container and a volumetric bottle, wherein the water sample container is connected to the volumetric bottle via a first pipe and a second pipe, respectively; A filter is provided on the second pipe; A first sampling needle is connected to the volumetric bottle; A pump for conveying water samples from the water sample container and the volumetric bottle.

3. The measuring device according to claim 1, characterized in that, The measuring device further includes: The second application unit is used to quantitatively apply pure water onto the paper tape; The second heating unit is used to heat the portion of the paper tape to which pure water is applied.

4. The measuring device according to claim 2, characterized in that, The measuring device further includes: The third application unit is used to quantitatively measure the standard solution and deliver it to the volumetric bottle.

5. A method for measuring elements in water, characterized in that, The measurement method includes the following steps: A1. The sampling area of ​​the paper tape is preheated by the first heating unit; A quantitative water sample is applied to the sampling area, the first heating unit heats the sampling area, the water evaporates, and the analyte is enriched in the sampling area; A2. The water sample spot enriched with the analyte moves along the paper tape to the elemental measurement unit; A3. The element measurement unit outputs the element content in the water sample based on the detection results of the water sample spots.

6. The measurement method according to claim 5, characterized in that, The measurement method further includes the following steps: B1. The second heating unit preheats the paper tape; A quantitative amount of pure water is applied to the paper tape, and the second heating unit heats the area on the paper tape where the pure water has been applied. The water evaporates, and the component to be measured is enriched on the paper tape. B2. The spots enriched with the analyte move along the paper tape to the elemental measurement unit; B3. The element measurement unit outputs the element content in pure water as background based on the detection results of the spots.

7. The measurement method according to claim 5, characterized in that, The method for quantitative water sampling is as follows: The sample in the sample container is brought to a final volume in a volumetric flask and then applied to the sampling area.

8. The measurement method according to claim 7, characterized in that, The measurement method also includes a spiked recovery test, specifically: Within one cycle, obtain the elemental mass m1 in the sample inside the constant volume bottle; In the next cycle, a standard solution with element mass m0 is added to the volumetric flask and mixed with the sample to obtain element mass m2 in the mixture; The spiked recovery rate was 100% / m0 (m2-m1).

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