CN115436585A - Online intelligent labeling method for water quality monitoring - Google Patents
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Abstract
The invention provides an online intelligent labeling method for water quality monitoring, which comprises the following steps: (1) Detection volume is V 1 Original concentration C of the analyte in the water sample 1 According to the original concentration C 1 Determining the volume V of the spiked liquid 2 ＝(nC 1 ×V 1 )/C 2 Wherein, C 2 The concentration of the standard solution is shown, and n is the standard addition multiple; (2) Determination of the theoretical Standard concentration C s ＝(C 1 ×V 1 +C 2 ×V 2 )/(V 1 +V 2 ) Judgment of C s Whether the concentration is within the maximum concentration detection range R of the monitor or not; and according to different theoretical concentration values of the added standard sample, obtaining the added standard recovery rate. The water quality monitoring online intelligent labeling method selects different volumes of the labeling liquid according to different sample concentrations, so that the labeling amount is close to the sample content, the deviation is in a proper range, and the accuracy of the labeling recovery rate is improved; meanwhile, according to the determined theoretical standard sample concentration, selecting corresponding standard sample, measuring the standard sample concentration, obtaining the standard recovery rate, and further improvingThe accuracy of the standard recovery rate is high, and the measurement accuracy of a reaction instrument is better.
Description
Technical Field
The invention belongs to the technical field of environmental monitoring, and particularly relates to an online intelligent labeling method for water quality monitoring.
Background
The quality control mode of the existing water quality on-line monitor mainly comprises quality control sample examination, actual water sample comparison, water sample labeling recovery test and the like. The quality control sample examination can reflect the accuracy of the instrument in a simple sample matrix, the accuracy of the instrument facing the actual sample matrix cannot be investigated, and automatic quality control sample examination is easy to realize; the actual water sample comparison mode requires detection personnel to determine the water sample in a laboratory according to a standard method, and the method has the disadvantages of complicated steps, long time consumption and high cost. Is not suitable for long-term and daily accuracy verification.
The water sample labeling recovery test is a good accuracy verification method, can greatly reduce the workload of operation and management personnel, improve the verification density of the monitor, and can truly reflect the measurement accuracy of the instrument on actual samples. In the prior art, most of water quality on-line monitors realize sample labeling recovery testing through an external labeling recovery module, or a fixed labeling mode adds a standard sample with fixed volume and concentration into a sample, and the fixed labeling mode cannot adapt to the sample measured each time well because the variation range of the actual sample concentration is uncertain, so that the labeling recovery rate is unsatisfactory. The invention patent CN201410856135.8 provides a dynamic standard adding method for water quality monitoring, but the method can only ensure that the concentration after standard adding does not exceed the measuring range of an analyzer, and cannot control the adding quantity within a certain reasonable interval range of sample content.
Therefore, the invention provides an intelligent online labeling method for water quality monitoring, and the obtained labeled recovery rate can more accurately reflect the measurement accuracy of the actual sample of the instrument.
Disclosure of Invention
The invention aims to provide an online intelligent labeling method for water quality monitoring, and solves the technical problem that the existing labeling method cannot accurately reflect the measurement accuracy of an instrument.
The purpose of the invention is realized by the following technical scheme:
an online intelligent labeling method for water quality monitoring comprises the following steps:
(1) Detection volume is V 1 Original concentration C of the analyte in the water sample 1 According to the original concentration C 1 Determining the volume V of the spiked liquid 2 ＝(nC 1 ×V 1 )/C 2 Wherein, C 2 The concentration of the standard solution is shown, and n is the standard addition multiple;
(2) Determination of the theoretical Standard concentration C s ＝(C 1 ×V 1 +C 2 ×V 2 )/(V 1 +V 2 ) Judgment of C s Whether the concentration is within the maximum concentration detection range R of the monitor or not;
if C s Within the maximum concentration detection range R of the monitor, the volumes are respectively V 1 、V 2 Mixing the water sample with the standard solution to obtain a standard sample, and measuring to obtain the standard sample concentration C 3 (ii) a Obtaining the recovery rate of adding standard P = [ C = 3 ×(V 1 +V 2 )-C 1 ×V 1 ]/C 2 ×V 2 ；
If C s If the concentration is larger than the maximum concentration detection range R of the monitor, determining the dilution factor k, and re-determining the volume V of the water sample 1 ’＝V 1 K, volume of spiked liquid V 2 ’＝V 2 K, and volume of diluent V 3 ’＝V 1 X (1-1/k); the volume is V 1 ' Water sample, V 2 ' the addition of a labeling solution and a volume of V 3 ' mixing the diluents and determining the concentration of the added standard sample C 3 '; obtaining the recovery rate P' = [ C ] of the added standard 3 ’×(V 1 ’+V 2 ’+V 3 ’)-C 1 ×V 1 ’]/C 2 ×V 2 ’。
The invention can be improved as follows, the concentration C of the marking liquid 2 Is 10-20 times of the measuring range of the monitor. By setting in this way, V can be set 2 Is small.
In the invention, the value of the adding standard multiple n is in the range of 0.5-2. Too low or too high addition amount can cause large deviation of the addition amount recovery rate, and the accuracy of the instrument cannot be truly reflected. Under the condition that the standard addition needs to meet the appropriate standard addition concentration range, the adding amount of the sample is 0.5-2 times, and the accuracy of the reaction instrument can be better.
In the present invention, the dilution multiple k is determined by the theoretical standard concentration C s And determining the ratio of the maximum concentration detection range R of the monitor.
Further, when 1 < C s When the/R is less than or equal to 2, the dilution multiple k is 2; when 2 < C s the/R is less than or equal to 3, and the dilution multiple is 3; when 3 is more than C s When the/R is less than or equal to 4, the dilution multiple k is 4.
Compared with the prior art, the invention has the following beneficial effects:
the water quality monitoring online intelligent labeling method selects different volumes of the labeling liquid according to different sample concentrations, so that the labeling amount is close to the sample content, the deviation is in a proper range, and the accuracy of the labeling recovery rate is improved; meanwhile, according to the determined theoretical standard sample adding concentration, the corresponding standard sample is selected, the standard sample adding concentration is measured, the standard sample adding recovery rate is obtained, the accuracy of the standard sample adding recovery rate is further improved, and the measurement accuracy of a reaction instrument is better.
Detailed Description
The present invention is further described below in conjunction with specific examples so that those skilled in the art can better understand and implement the technical solutions of the present invention.
Example 1
The intelligent standard adding method is executed by adopting a water quality ammonia nitrogen online monitoring instrument, the low-concentration water sample is measured, the range R of the online ammonia nitrogen monitoring instrument is 20mg/L, and the concentration of the standard adding liquid is 200mg/L.
An online intelligent labeling method for water quality monitoring comprises the following steps: (1) Detecting the original concentration C1 of an object to be detected in a water sample with the volume of V1, and determining the volume V2= (nC 1 multiplied by V1)/C2 of the standard solution according to the original concentration C1, wherein C2 is the concentration of the standard solution, and n is the standard addition multiple;
the specific operation process is as follows: a water sample is conveyed to an overflow cup through a peristaltic pump, 10mL of the water sample is conveyed to a colorimetric pool through an injection pump and is measured by a spectrophotometry method, and the measured sample concentration C1 is 1.6 mg/L; the scaling factor n was set to 1, and the volume V2 of the scaled solution was 0.08mL by concentration calculation.
(2) Adding standard sample concentration C according to theory s ＝(C 1 ×V 1 +C 2 ×V 2 )/(V 1 +V 2 ) And calculating to obtain the theoretical standard concentration Cs of 3.17mg/L, which is smaller than the detection range R of the instrument.
Mixing the water samples with the volumes of 10mL and 0.08mL respectively with the standard solution to obtain a standard sample, and determining to obtain the concentration C of the standard sample 3 3.05mg/L; according to P = [ C = 3 ×(V 1 +V 2 )-C 1 ×V 1 ]/C 2 ×V 2 And the normalized recovery rate P =92.15% is obtained.
Example 2
The intelligent standard adding method is implemented by adopting a water quality ammonia nitrogen online monitoring instrument, a high-concentration water sample is measured, the range R of the online ammonia nitrogen monitoring instrument is 20mg/L, and the concentration of a standard adding liquid is 200mg/L.
An online intelligent labeling method for water quality monitoring comprises the following steps:
(1) Detecting the original concentration C1 of an object to be detected in a water sample with the volume of V1, and determining the volume V2= (nC 1 multiplied by V1)/C2 of the standard solution according to the original concentration C1, wherein C2 is the concentration of the standard solution, and n is the standard addition multiple;
the specific operation process is as follows: a water sample is conveyed to an overflow cup through a peristaltic pump, 10mL of the water sample is conveyed to a colorimetric pool through an injection pump and is measured by a spectrophotometry method, and the measured sample concentration C1 is 15.2mg/L; the standard addition multiple n is set to be 1, and the volume V2 of the standard addition solution is 0.76mL according to the concentration calculation.
(2) From the theoretical spiked concentration Cs = (C1 × V1+ C2 × V2)/(V1 + V2), the theoretical spiked concentration Cs was calculated to be 28.25mg/L, which is higher than the range R =20mg/L of the monitor.
Calculating to obtain a ratio of the theoretical normalized concentration Cs to the measuring range R to be 1.4, determining the dilution multiple to be 2 according to the relation between the ratio and the dilution multiple, and obtaining the adjusted water sample volume V1'=5mL, V2' =0.38mL and V3'=5mL according to the water sample volume V1' = V1/k, the normalized liquid volume V2'= V2/k and the diluent volume V3' = V1X (1-1/k);
TABLE 1C s Concentration to range R ratio and corresponding dilution factor k
| C s /R | Dilution factor k |
| 1＜C s /R≤2 | 2 |
| 2＜C s /R≤3 | 3 |
| 3＜C s /R≤4 | 4 |
Mixing a water sample with the volume of 5mL, a standard solution with the volume of 0.38mL and a diluent with the volume of 5mL respectively to obtain a standard sample, and determining to obtain the standard sample with the concentration C3' of 14.41mg/L; according to the recovery rate of the added standard P' = [ C 3 ’×(V 1 ’ +V 2 ’+V 3 ’)-C 1 ×V 1 ’]/C 2 ×V 2 ', a normalized recovery P' =96.8% is obtained.
Example 3
The intelligent standard adding method is executed by adopting a water quality ammonia nitrogen online monitoring instrument, the low-concentration water sample is measured, the range R of the online ammonia nitrogen monitoring instrument is 20mg/L, and the concentration of the standard adding liquid is 200mg/L.
An online intelligent labeling method for water quality monitoring comprises the following steps: (1) Detecting the original concentration C1 of an object to be detected in a water sample with the volume of V1, and determining the volume V2= (nC 1 multiplied by V1)/C2 of the standard solution according to the original concentration C1, wherein C2 is the concentration of the standard solution, and n is the standard addition multiple;
the specific operation process is as follows: a water sample is conveyed to an overflow cup through a peristaltic pump, 10mL of the water sample is conveyed to a colorimetric pool through an injection pump and is measured by a spectrophotometry method, and the measured sample concentration C1 is 0.25 mg/L; the standard adding multiple n is set to be 2, and the volume V2 of the standard adding liquid is 0.025mL according to the concentration calculation.
(2) Adding standard sample concentration C according to theory s ＝(C 1 ×V 1 +C 2 ×V 2 )/(V 1 +V 2 ) And calculating to obtain the theoretical standard concentration Cs of 0.748mg/L, which is smaller than the detection range R of the instrument.
Mixing the water samples with the volumes of 10mL and 0.025mL respectively with the standard solution to obtain standard sample, and determining to obtain standard sample concentration C 3 0.773mg/L; according to P = [ C = 3 ×(V 1 +V 2 )-C 1 ×V 1 ]/C 2 ×V 2 And the normalized recovery rate P =104.99% is obtained.
Example 4
The intelligent standard adding method is implemented by adopting a water quality ammonia nitrogen online monitoring instrument, the high-concentration water sample is measured, the range R of the online ammonia nitrogen monitoring instrument is 20mg/L, and the concentration of the standard adding liquid is 200mg/L.
An online intelligent labeling method for water quality monitoring comprises the following steps:
(1) Detecting the original concentration C1 of an object to be detected in a water sample with the volume of V1, and determining the volume V2= (nC 1 multiplied by V1)/C2 of the standard solution according to the original concentration C1, wherein C2 is the concentration of the standard solution, and n is the standard addition multiple;
the specific operation process is as follows: a water sample is conveyed to an overflow cup through a peristaltic pump, 10mL of the water sample is conveyed to a colorimetric pool through an injection pump and is measured by a spectrophotometry method, and the measured sample concentration C1 is 16.3mg/L; the standard addition multiple n is set to be 0.5, and the volume V2 of the standard addition solution is 0.4075mL according to concentration calculation.
(2) From the theoretical spiked concentration Cs = (C1 × V1+ C2 × V2)/(V1 + V2), a theoretical spiked concentration Cs of 23.49mg/L was calculated, which is higher than the range R =20mg/L of the monitor.
Calculating to obtain a ratio of the theoretical standard adding concentration Cs to the measuring range R to be 1.17, determining the dilution multiple to be 2 according to the relation between the ratio and the dilution multiple, and obtaining the adjusted water sample volume V1'=5mL, V2' =0.20375mL and V3'=5mL according to the water sample volume V1' = V1/k, the standard adding liquid volume V2'= V2/k and the diluent volume V3' = V1X (1-1/k);
TABLE 2C s Concentration to range R ratio and corresponding dilution factor k
| C s /R | Dilution factor k |
| 1＜C s /R≤2 | 2 |
| 2＜C s /R≤3 | 3 |
| 3＜C s /R≤4 | 4 |
Mixing a water sample with the volume of 5mL, a standard solution with the volume of 0.20mL and a diluent with the volume of 5mL respectively to obtain a standard sample, and determining to obtain the standard sample with the concentration C3' of 11.60mg/L; according to the standard addition recovery rate P' = [ C 3 ’×(V 1 ’ +V 2 ’+V 3 ’)-C 1 ×V 1 ’]/C 2 ×V 2 ', a normalized recovery P' =90.46% is obtained.
The above embodiments are described in detail for different implementations of the present invention, but the implementation manner of the present invention is not limited thereto, and those skilled in the art can achieve the object of the present invention based on the disclosure of the present invention, and any modifications and variations based on the concept of the present invention fall within the protection scope of the present invention, and the specific protection scope is subject to the claims.
Claims (5)
1. An online intelligent labeling method for water quality monitoring is characterized by comprising the following steps:
(1) Detection volume is V 1 Original concentration C of the analyte in the water sample 1 According to the original concentration C 1 Determining the volume V of the spiked liquid 2 ＝(nC 1 ×V 1 )/C 2 Wherein, C 2 The concentration of the standard solution is shown, and n is the standard addition multiple;
(2) Determination of the theoretical Standard concentration C s ＝(C 1 ×V 1 +C 2 ×V 2 )/(V 1 +V 2 ) Judgment of C s Whether the concentration is within the maximum concentration detection range R of the monitor or not;
if C s Within the maximum concentration detection range R of the monitor, the volumes are respectively V 1 、V 2 Mixing the water sample with the standard solution to obtain a standard sample, and measuring to obtain the standard sample concentration C 3 (ii) a Obtaining the standard addition recovery rate P = [ C = 3 ×(V 1 +V 2 )-C 1 ×V 1 ]/C 2 ×V 2 ；
If C s If the concentration is larger than the maximum concentration detection range R of the monitor, determining the dilution factor k, and re-determining the volume V of the water sample 1 ’＝V 1 K, volume of spiked liquid V 2 ’＝V 2 K, and volume of diluent V 3 ’＝V 1 X (1-1/k); the volume is V 1 ' Water sample, V 2 ' the addition of a labeling solution and a volume of V 3 ' mixing the diluents and determining the concentration of the added standard sample C 3 '; obtaining the recovery rate P' = [ C ] of the added standard 3 ’×(V 1 ’+V 2 ’+V 3 ’)-C 1 ×V 1 ’]/C 2 ×V 2 ’。
2. The water quality on-line intelligent standard adding method for monitoring according to claim 1, characterized in that the value of the standard adding multiple n is in the range of 0.5-2.
3. The water quality monitoring online intelligent labeling method according to claim 1, characterized in that the concentration C of the labeling liquid 2 Is 10-20 times of the measuring range of the monitor.
4. The water quality monitoring online intelligent labeling method according to claim 3, characterized in that the dilution multiple k passes through the theoretical standard sample concentration C s And determining the ratio of the maximum concentration detection range R of the monitor.
5. The water quality on-line intelligent labeling method for water quality monitoring according to claim 4, wherein when C is more than 1 s When the/R is less than or equal to 2, the dilution multiple k is 2; when 2 < C s the/R is less than or equal to 3, and the dilution multiple is 3; when 3 < C s When the/R is less than or equal to 4, the dilution multiple k is 4.
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| CN103091152A (en) * | 2013-02-21 | 2013-05-08 | 广州伊创仪器有限公司 | Intelligent dilution system and intelligent dilution method for on-line analyzer |
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