CN101943695B - Water quality analyzing device and method for realizing recovery rate of water quality analyzing apparatus - Google Patents
Water quality analyzing device and method for realizing recovery rate of water quality analyzing apparatus Download PDFInfo
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- CN101943695B CN101943695B CN2010102596497A CN201010259649A CN101943695B CN 101943695 B CN101943695 B CN 101943695B CN 2010102596497 A CN2010102596497 A CN 2010102596497A CN 201010259649 A CN201010259649 A CN 201010259649A CN 101943695 B CN101943695 B CN 101943695B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000011084 recovery Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002372 labelling Methods 0.000 claims abstract description 90
- 239000007788 liquid Substances 0.000 claims abstract description 83
- 238000005070 sampling Methods 0.000 claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 238000004458 analytical method Methods 0.000 claims description 32
- 238000005259 measurement Methods 0.000 claims description 21
- 230000002572 peristaltic effect Effects 0.000 claims description 7
- 238000007599 discharging Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 6
- 238000012421 spiking Methods 0.000 description 5
- 239000012086 standard solution Substances 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The invention discloses a water quality analyzing device and a method for realizing a recovery rate of the water quality analyzing apparatus, aiming at solving the problem of not convenient for judging the reliability of testing data of the water quality analyzing apparatus under various occasions in the prior art. The water quality analyzing device of the invention comprises a labeling pool and a labeling device, wherein the labeling pool is provided with a sample inlet, an upper end overflow port, a lower end overflow port, a sampling port and a sample discharging port; the labeling device comprises a labeling operation element and a labeling liquid storing device. The labeling operation element is used for adding the labeling liquid in the labeling liquid storing device in the labeling pool.
Description
Technical Field
The invention relates to the technical field of water quality monitoring, in particular to a water quality analysis device and a method for realizing the standard recovery rate of a water quality analysis instrument.
Background
According to the specification of the national environmental protection agency 'water and wastewater monitoring and analyzing method', the measurement of the standard recovery rate can reflect the accuracy of the test result. The recovery rate of the added standard is obtained by adding a certain amount of standard substance to a subsample of the same sample for measurement while measuring the sample, and subtracting the measurement value of the sample from the measurement result.
The calculation formula of the standard recovery rate is shown as the formula (0), wherein P represents the standard recovery rate.
P ═ (spiked sample measurement-sample measurement)/spiked quantity × 100% >,. (0)
When the recovery rate is measured according to the parallel standard addition, the obtained result can reflect the accuracy of the test result and can also judge the precision of the test result. The recovery rate of the added standard is a main method for controlling the laboratory quality specified by the national environmental protection agency. The size of the standard recovery rate reflects the technical level of analysis operation, more importantly, whether the analysis method is suitable for the detected water body or not is reflected, so that the analysis personnel can be helped to find out the problems existing in the analysis in time, and the accuracy and the reliability of the analysis data are ensured.
The measurement value of the spiked sample and the measurement value of the sample in the formula (0) may be concentration values, and the theoretical formula for calculating the spiked recovery rate from the concentration values may be expressed as the formula (1):
P＝(c2-c 1)/c3×100％...................(1)
in the formula:
p is the recovery rate of the added standard;
c1 is the sample concentration, i.e. the sample measurement;
c2 represents the concentration of the spiked sample, i.e. the measured value of the spiked sample;
c3 is a calibration amount, c3 is c0 × V0/V2, and m is c0 × V0;
m1 is the content of the substance in the sample; m2 is the content of the substance in the standard sample; m is the content of the substance in the added standard volume;
v1 is sample volume; v2 is the spiked sample volume, V2 ═ V1+ V0; v0 is the spiked volume; c0 is the standard solution concentration for labeling.
In the case where the spiked volume does not affect the analytical results, i.e. V2 ═ V1, when
When c3 is c0 × V0/V1, the recovery rate P from spiking can be calculated by the formula (2).
P＝[(c2-c1)×V1]/(c0×V 0)×100％..................(2)
In the case where the normalized volume affects the analytical result, i.e., V2 ═ V1+ V0, when
When c3 is (c0 × V0)/(V1 decav 0), the recovery rate P for spiking can be calculated according to formula (3).
P＝[(c2-c1)×(V1+V0)]/(c0×V0)×100％...................(3)
The measurement value of the spiked sample and the measurement value of the sample in the formula (0) may be the amount of the substance, and the spiked recovery rate calculated from the amount of the substance contained in the sample may be calculated according to the formula (4) or the formula (5):
P＝(m2-m1)/m×100％..................(4)
P＝(c2×V2-c 1×V1)/c0×V0×100％..................(5)
according to the existing method, the reliability of the test data of the instrument is judged according to the consistency of the test results of the manual test and the instrument by testing the water sample in the manual test and the instrument test. However, when the instrument is tested on site, manual testing is often not performed to judge the reliability of the instrument data, so that according to the existing method, the reliability of the test data of the water quality analyzer in various occasions is not convenient to judge.
Disclosure of Invention
The invention mainly aims to provide a water quality analysis device and a method for realizing the standard recovery rate of a water quality analysis instrument, so as to solve the problem that the reliability of test data of the water quality analysis instrument in various occasions is not convenient to judge in the prior art.
In order to solve the above problems, according to an aspect of the present invention, there is provided a water quality analyzing apparatus.
The water quality analyzing apparatus of the present invention comprises: a labeling pool; a labeling device; the labeling pool is provided with a sample inlet, an upper end overflow port, a lower end overflow port, a sampling port and a sample discharge port; the mark adding device comprises a mark adding operating element and a mark liquid storage device, and the mark adding operating element is used for adding the mark liquid in the mark liquid storage device into the mark adding pool.
Furthermore, the labeling operation element is a micro sample injection pump, and the micro sample injection pump is connected with the labeling pool and the labeling liquid storage device and is used for extracting the labeling liquid from the labeling liquid storage device and then adding the labeling liquid into the labeling pool.
Further, the marking operation element is a photoelectric liquid level metering device, and the photoelectric liquid level metering device is connected with the marking pool and the marking liquid storage device and is used for extracting quantitative marking liquid from the marking liquid storage device and then adding the marking liquid into the marking pool.
Further, the marking operation element is a peristaltic pump metering device, and the peristaltic pump metering device is connected with the marking pool and the marking liquid storage device and is used for extracting marking liquid from the marking liquid storage device and then adding the marking liquid into the marking pool.
Furthermore, the adding mark operation element is an overflow constant volume device, and the overflow constant volume device is connected with the adding mark pool and the mark liquid storage device and is used for measuring a fixed amount of the mark liquid from the mark liquid storage device and then adding the mark liquid into the adding mark pool.
In order to solve the problems, according to another aspect of the invention, a method for realizing the spiking recovery rate of a water quality analyzer is provided.
The method for realizing the standard adding recovery rate of the water quality analyzer applies the water quality analyzer and comprises the following steps: collecting a sample from a sample inlet into a labeling pool, and stopping collecting the sample after the liquid level in the labeling pool reaches an upper end overflow port; sampling from a sampling port by a water quality analysis instrument and testing to obtain a sample measured value; after the sampling is finished, enabling the sample in the labeling pool to overflow through the lower end overflow port, and adding a preset amount of labeling liquid into the labeling pool by using a labeling operation element after the liquid level in the labeling pool reaches the lower end overflow port; sampling from a sampling port by a water quality analyzer for testing to obtain a measured value of a standard sample; calculating the standard recovery rate of the water quality analyzer according to the following formula: the recovery rate of spiked sample (spiked sample measurement value-sample measurement value)/spiked amount × 100%.
In order to solve the problems, according to another aspect of the invention, another method for realizing the spiking recovery rate of the water quality analysis instrument is provided.
The method for realizing the standard adding recovery rate of the water quality analyzer applies the water quality analyzer and comprises the following steps: collecting a sample from a sample inlet into a labeling pool, and stopping collecting the sample after the liquid level in the labeling pool reaches an upper end overflow port; a water quality analysis instrument takes a predetermined amount of samples from a sampling port to test to obtain a sample measured value; after the predetermined amount of sample is taken, adding a preset amount of standard liquid into the standard adding pool by using a standard adding operation element; the water quality analysis instrument takes out all the standard adding samples in the standard adding pool from the sampling port and then tests to obtain the measured value of the standard adding samples; calculating the standard recovery rate of the water quality analyzer according to the following formula: the recovery rate of spiked sample (spiked sample measurement value-sample measurement value)/spiked amount × 100%.
According to the technical scheme of the invention, the standard adding liquid is added into the standard adding pool from the standard adding device, so that the standard adding recovery rate of the water quality analyzer can be conveniently measured, and the reliability of the test data of the water quality analyzer in various occasions can be judged.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
fig. 1 is a schematic diagram of a basic structure of a water quality analyzing apparatus according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Fig. 1 is a schematic diagram of a basic structure of a water quality analyzing apparatus according to an embodiment of the present invention. As shown in fig. 1, the water quality analyzer according to the embodiment of the present invention mainly includes a labeling tank 1 and a labeling device 2.
The labeling pool is provided with a sample inlet 11, an upper end overflow port 12, a lower end overflow port 13, a sampling port 14 and a sample discharge port 15; the marking device 2 comprises a marking operation element 21 and a marking liquid storage device 22, as shown in fig. 1, the marking operation element 21 is used for adding the marking liquid in the marking liquid storage device 22 into the marking pool 1.
The labeling operation element 21 can adopt a micro-sample pump, the micro-sample pump is connected with the labeling pool 1 and the labeling liquid storage device 22, and the labeling liquid is extracted from the labeling liquid storage device 22 and then added into the labeling pool 1. The precision of the micro sample injection pump can be 5 mu L, so that the standard adding requirement of a small-volume sample can be met.
The marking operation element 21 may also be an electro-optical level gauge. Since the photoelectric liquid level measuring device can accurately measure liquid in a photoelectric mode, the photoelectric liquid level measuring device can be connected with the standard liquid storage device 22 of the standard liquid adding pool 1, and is used for extracting quantitative standard liquid from the standard liquid storage device 22 and then adding the quantitative standard liquid into the standard liquid adding pool 1.
The labeling operation element 21 can also adopt a peristaltic pump metering device, and compared with a micro sample injection pump, the peristaltic pump can extract liquid and simultaneously ensure higher precision of the extraction amount. A peristaltic pump metering device may be connected to the beaconing tank 1 and the beaconing liquid storage device 22 for drawing the beaconing liquid from the beaconing liquid storage device 22 and then adding the beaconing liquid to the beaconing tank 1.
The indexing operation element 21 may also be an overflow volumetric device. The main principle of the overflow constant volume device is to ensure that a preset volume of liquid is measured by means of overflow. The overflow constant volume device is connected with the labeling pool 1 and the labeling liquid storage device 22, and is used for measuring a certain amount of labeling liquid from the labeling liquid storage device 22 and then adding the labeling liquid into the labeling pool 1.
The minimum accurate volume of the photoelectric liquid level metering device, the peristaltic pump metering device and the overflow constant volume device can be about 0.1-0.5 mL, so that the requirement of large volume adding can be met.
The water quality analyzing apparatus according to the embodiment of the present invention may be provided with a water outlet and a water inlet (not shown) as a whole, wherein the water outlet is communicated with the upper end overflow port 12, the lower end overflow port 13 and the sample discharge port 15, and the water inlet is communicated with the sample inlet 11. An electromagnetic valve may be attached to a pipe from the lower overflow port 13 to the drain port, and an electromagnetic valve may be attached to a pipe from the sample discharge port 15 to the drain port. Thus, overflow and stock discharge of the labeling tank can be controlled by the relevant control device.
For the calibration cell 1, the volume V1 defined by the overflow port 12 at the upper end and the volume V2 defined by the overflow port 13 at the lower end are both constant values, so that the calibration cell can be used for making a sample or a calibration sample constant values so as to measure the calibration recovery rate of the water quality analysis instrument. The sampling port 14 may be connected to a sampling port of a water quality analyzer during measurement.
When the water quality analysis device provided by the embodiment of the invention is used for realizing the standard adding recovery rate of the water quality analysis instrument, various modes can be flexibly adopted according to needs, and two examples are shown below.
One mode is to fix the volume of a standard sample and fix the volume of a sample, and the specific steps are as follows:
collecting a sample from a sample inlet 11 into the labeling pool 1, and stopping collecting the sample after the liquid level in the labeling pool 1 reaches an upper end overflow port 12;
the water quality analyzer samples from the sampling port 14 to perform testing to obtain a sample measured value;
after sampling is finished, enabling a sample in the labeling pool 1 to overflow through the lower end overflow port 13, and adding a preset amount of labeling liquid into the labeling pool 1 by using a labeling operation element 21 after the liquid level in the labeling pool 1 reaches the lower end overflow port 13;
the water quality analyzer samples from the sampling port 14 and tests to obtain a measured value of a standard sample;
and (4) calculating the standard recovery rate of the water quality analyzer according to the formula (0).
The amount of standard solution added should be small, typically not exceeding 3% of the sample volume. As can be seen from the above steps, the sample in the labeling pool 1 overflows through the lower overflow port 13, so that the volume of the labeled sample is constant.
Another way of using the water quality analyzing apparatus according to the embodiment of the present invention is to perform a constant volume process on the sample, because the volume V1 defined by the overflow port at the upper end is a constant value, the volume of the added standard sample is also constant. The method comprises the following specific steps:
collecting a sample from a sample inlet 11 into the labeling pool 1, and stopping collecting the sample after the liquid level in the labeling pool 1 reaches an upper end overflow port 12;
the water quality analysis instrument takes a predetermined amount of sample from the sampling port 14 to perform a test to obtain a sample measurement value;
after the sampling of a predetermined amount of sample is completed, a preset amount of standard solution is added into the standard adding pool 1 by using the standard adding operation element 21;
the water quality analyzer takes out all the standard adding samples in the standard adding pool 1 from the sampling port 14 and then tests to obtain the measured value of the standard adding samples;
and (4) calculating the standard recovery rate of the water quality analyzer according to the formula (0).
In the above steps, the water quality analyzer takes a predetermined amount of sample from the sampling port 14, that is, the constant volume of the sample is realized, and then the sample is directly marked without overflowing from the lower overflow port 13. The volume of the spiked sample is now the difference between V1 and the volume of the sample taken by the water quality analyzer from the sampling port 14.
From the two using modes, the principle of adding the standard and the yield is the same as that of manual measurement by using the water quality analysis device provided by the embodiment of the invention, but the operation is very convenient. The water quality analysis device provided by the embodiment of the invention can be integrated with various existing water quality analysis instruments. According to the use method of the water quality analysis device provided by the embodiment of the invention, a corresponding control program can be easily written, and the program can be operated by the control device in the water quality analysis instrument, so that the actions of all components in the water quality analysis device provided by the embodiment of the invention can be controlled. The device of the embodiment of the invention can also be used as a single device, when in use, the sampling tube of the water quality analysis instrument is inserted into the labeling pool 1 through the sampling port for sampling, and the electromagnetic valve can also be a manual valve.
In an implementation, the volume of spiking cell 1 may be 20mL to 1000mL, V1 may be 10mL to 500mL, and V2 may be 5mL to 250 mL. The volume of the standard solution storage means 22 may be 5mL to 500mL, and the standard solution is filled therein before use. The overall size of the water quality analysis device provided by the embodiment of the invention can be approximately 5cm to 100cm in length, 5cm to 100cm in width and 5cm to 100cm in height, and the volume is convenient to carry and use on line.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by 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 (7)
1. A water quality analyzing apparatus, comprising:
a labeling pool;
a labeling device; wherein,
the labeling pool is provided with a sample inlet, an upper end overflow port, a lower end overflow port, a sampling port and a sample discharge port;
the mark adding device comprises a mark adding operating element and a mark liquid storage device, and the mark adding operating element is used for adding the mark liquid in the mark liquid storage device into the mark adding pool.
2. The water quality analyzer according to claim 1, wherein the labeling operation element is a micro-sample pump connected to the labeling tank and the labeling liquid storage device, for extracting the labeling liquid from the labeling liquid storage device and then adding the labeling liquid to the labeling tank.
3. The water quality analyzer according to claim 1, wherein the labeling operation unit is an electro-optical level gauge connected to the labeling tank and the labeling liquid storage unit for extracting a predetermined amount of the labeling liquid from the labeling liquid storage unit and then adding the same to the labeling tank.
4. The water quality analyzing apparatus according to claim 1, wherein the labeling operation member is a peristaltic pump metering device connected to the labeling tank and the labeling liquid storage device for drawing the labeling liquid from the labeling liquid storage device and then adding the labeling liquid to the labeling tank.
5. The water quality analysis device according to claim 1, wherein the standard adding operation element is an overflow constant volume device, and the overflow constant volume device is connected with the standard adding pool and the standard liquid storage device and is used for measuring a certain amount of standard liquid from the standard liquid storage device and then adding the standard liquid into the standard adding pool.
6. A method for realizing the standard recovery rate of a water quality analyzer, which is characterized by applying the water quality analyzer of any one of claims 1 to 5 and comprising the following steps:
collecting a sample from a sample inlet into a labeling pool, and stopping collecting the sample after the liquid level in the labeling pool reaches an upper end overflow port;
sampling from a sampling port by a water quality analysis instrument and testing to obtain a sample measured value;
after the sampling is finished, enabling the sample in the labeling pool to overflow through the lower end overflow port, and adding a preset amount of labeling liquid into the labeling pool by using a labeling operation element after the liquid level in the labeling pool reaches the lower end overflow port;
sampling from a sampling port by a water quality analyzer for testing to obtain a measured value of a standard sample;
calculating the standard recovery rate of the water quality analyzer according to the following formula:
the recovery rate of spiked sample (spiked sample measurement value-sample measurement value)/spiked amount × 100%.
7. A method for realizing the standard recovery rate of a water quality analyzer, which is characterized by applying the water quality analyzer of any one of claims 1 to 5 and comprising the following steps:
collecting a sample from a sample inlet into a labeling pool, and stopping collecting the sample after the liquid level in the labeling pool reaches an upper end overflow port;
a water quality analysis instrument takes a predetermined amount of samples from a sampling port to test to obtain a sample measured value;
after the predetermined amount of sample is taken, adding a preset amount of standard liquid into the standard adding pool by using a standard adding operation element;
the water quality analysis instrument takes out all the standard adding samples in the standard adding pool from the sampling port and then tests to obtain the measured value of the standard adding samples;
calculating the standard recovery rate of the water quality analyzer according to the following formula:
the recovery rate of spiked sample (spiked sample measurement value-sample measurement value)/spiked amount × 100%.
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| CN103728891B (en) * | 2013-12-25 | 2017-02-15 | 力合科技（湖南）股份有限公司 | Method and device for controlling water quality on-line monitoring data |
| CN104569332B (en) * | 2014-12-31 | 2017-02-22 | 聚光科技(杭州)股份有限公司 | Dynamic standard liquid adding method and device for water quality monitoring |
| CN107966411A (en) * | 2017-12-27 | 2018-04-27 | 北京东方园林环境股份有限公司 | A kind of miniature automatic water quality monitoring quality control system and mark-on reclaims method |
| CN109633117B (en) * | 2019-01-10 | 2019-11-26 | 杭州绿洁环境科技股份有限公司 | A kind of dynamic quality control system of monitoring water quality on line equipment |
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