CN102565433B - High dilution factor water sample analysis method and device thereof - Google Patents

High dilution factor water sample analysis method and device thereof Download PDF

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CN102565433B
CN102565433B CN201110461717.2A CN201110461717A CN102565433B CN 102565433 B CN102565433 B CN 102565433B CN 201110461717 A CN201110461717 A CN 201110461717A CN 102565433 B CN102565433 B CN 102565433B
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dilution
sample
grade
mixing chamber
level
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CN102565433A (en
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唐小燕
项光宏
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HANGZHOU JUGUANG ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
Focused Photonics Hangzhou Inc
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HANGZHOU JUGUANG ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
Focused Photonics Hangzhou Inc
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Abstract

The invention relates to a high dilution factor water sample analysis method, which includes the following steps: A, confirming input parameters: the volumes of n-1 grade dilution sample and a diluent adopted during nth grade dillution can be obtained as per the dilution factor gn of the n grade, wherein the dilution grade is m, and n belongs to the interval from 1 to m (including 1 and m), the product of dilution factors of all grades is the total dilution factor, and the dilution sample of 0 grade is a to-be-diluted sample; B, performing m grade dilution for the sample until the m grade dilution sample is formed: an injection pump is controlled through a control unit to respectively inject an n-1 grade dilution sample and the diluent both with the volumes corresponding to those of the n grade dilution in an nth mixing chamber through multi-channel direction selecting valves, so as to form the n grade dilution sample; and C, detecting the concentration of an m grade dilution sample, so as to finish the measurement. The invention further provides a high dilution factor water sample analysis device. The high dilution factor water sample analysis method and the high dilution factor water sample analysis device have the advantages of convenience for operation and accuracy in dilution.

Description

A kind of highly diluted factor water sample analysis method and apparatus
Technical field
The present invention relates to a kind of water sample dilution analysis method and apparatus, especially a kind of water sample analysis method and apparatus that is applicable to the highly diluted factor.
Background technology
While adopting water quality online analyzer to carry out polluted-water on-line monitoring, analytical instrument can be designed to analyze accordingly range conventionally.If water pollution degree is too high, can make the concentration of the corresponding monitoring level of factor of water body too high, exceed analyser range; Or some colourity serious interference while disturbing the too large and spectrophotomelric assay of matrix concentration, can impact analysis result.When there is above-mentioned situation, often need water body to dilute accurately, and then carry out analyzing and testing.
The existing water sample automatic dilution system that can be applicable to water quality online analyzer is mainly by controlling water sample and controls dilution gfactor with flow rate ratio or the volume ratio of thinning agent.
Figure 1 shows that water sample automatic dilution system, is by regulating the flow rate of water sample pump and dilution pumps than controlling dilution gfactor, now, and dilution gfactor=(dilution pumps flow velocity+water sample flow rate pump)/water sample flow rate pump.Water sample pump and dilution pumps are all used peristaltic pump to keep accurate flow velocity and then to guarantee accurately to dilute water sample conventionally.But also there is following problem in this water sample automatic dilution system:
1), peristaltic pump is aging makes to detect error change greatly
With the peristaltic pump growth of service time, peristaltic pump tube can be aging, and flow velocity also drift in various degree can occur simultaneously, and these all can cause accurately controlling dilution gfactor, makes the detection signal error of analytical instrument become large.
2), residual water sample pollutes next time and measures sample, causes detecting inaccurate
Peristaltic pump tube can touch water sample and be polluted by water sample, and sometimes pollute and also can damage pump line, and then accurate Quality control flow velocity; The pump line having been polluted by water sample brings pollution can to follow-up measurement sample, makes analysis result inaccurate.
3), peristaltic pump flow rate range is limited, cannot realize the demand of dilution highly diluted factor water sample analysis.
The automatic dilution of water sample shown in Fig. 2 system, is by regulating the volume ratio of water sample quantity tube and thinning agent quantity tube to control dilution gfactor, now, and dilution gfactor=(thinning agent quantity tube volume+water sample quantity tube volume)/water sample quantity tube volume.Also there are some problems in this water sample automatic dilution system:
1), residual water sample contaminate subsequent measures sample, causes detecting inaccurate
Water sample quantity tube meeting residual fraction water sample, the water sample that residual water sample meeting contaminate subsequent is analyzed, makes analysis result inaccurate;
2), troublesome poeration
When needs change dilution gfactor, need the manual corresponding quantity tube of changing, operate cumbersome;
3), cannot meet the demand of highly diluted factor water sample analysis.
Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides a kind of easy and simple to handle, dilute the water sample analysis of the highly diluted factor accurately method and apparatus.
For achieving the above object, the present invention adopts following technical scheme:
A highly diluted factor water sample analysis method, comprises the following steps:
A, determine input parameter
According to n level dilution gfactor g nshow that n level dilutes corresponding n-1 level dilute sample and the volume of thinning agent; Wherein, dilution progression is m, n ∈ [1, m], and the amassing as total dilution gfactor of dilution gfactors at different levels, 0 grade of dilute sample is undiluted sample;
B, sample is carried out to the dilution of m level until form m level dilute sample
Control module is controlled syringe pump and in n mixing chamber, is injected respectively n-1 level dilute sample and the thinning agent that n level is diluted corresponding volume by multi-channel direction selecting valve, forms n level dilute sample;
Until form m level dilute sample;
C, detection m level dilute sample concentration, measure and finish.
Further, in step B, control module control syringe pump by multi-channel direction selecting valve by the n-1 level dilute sample unloading in n-1 mixing chamber to temporary room;
From extracting n-1 level dilute sample in temporary room, inject n mixing chamber, and with the mixing diluents of injecting in n mixing chamber, form n level dilute sample.
As preferably, all mixing chambers are same mixing chamber.
Further, in steps A, according to surveying maximum sample concentration C in instrument range L and standard method 0draw dilution progression m and dilution gfactor at different levels, wherein, total dilution gfactor g=L/C 0.
Further, described instrument range is User Defined range or the current range of instrument.
Further, in step C: detect m level dilute sample and show that its concentration is C 1;
If N≤C 1/ L≤1, measures and finishes, wherein: N makes measured value drop on the default lower limit of reliable interval in range;
Otherwise adjusting apparatus tolerance journey, makes L=yC 1, wherein
Figure GSB0000119524760000031
return to steps A.
As preferably, dilution gfactors at different levels are identical.
Further, according to M value, control dilution sum of series dilution gfactors at different levels, wherein, M value is dilution gfactor maximum critical value.
As preferably, dilution gfactors at different levels are and meet
As preferably, in mixing chamber, pass into measuring the gas without impact, make sample and mixing diluents even.
The present invention also provides a kind of highly diluted factor water sample analysis device, comprising:
Sample injection unit, described sample injection unit comprises syringe pump, liquid storage ring and multi-channel direction selecting valve, described multi-channel direction selecting valve is connected with sample, thinning agent, mixing chamber, control module and detecting unit respectively;
Control module, described control module is also connected with described syringe pump, and described control module is controlled syringe pump and in n mixing chamber, is injected n-1 level dilute sample and the thinning agent that n level is diluted corresponding volume respectively by multi-channel direction selecting valve, forms n level dilute sample; Until form m level dilute sample; Wherein, dilution progression is m, n ∈ [1, m], and the amassing as total dilution gfactor of dilution gfactors at different levels, 0 grade of dilute sample is undiluted sample;
Detecting unit, described detecting unit detects the concentration of m level dilute sample.
Further, control module is according to surveying maximum sample concentration C in instrument range L and standard method 0draw dilution progression m and dilution gfactor at different levels.
As preferably, described detecting unit is also connected with described control module, and described detecting unit passes to described control module using testing result and adjusts the foundation of instrument range as control module.
Further, described analytical equipment also comprises temporary room, and described temporary room is connected with described multi-channel direction selecting valve, for temporary dilute sample.
As preferably, each mixing chamber is same mixing chamber.
The present invention compared with prior art has following beneficial effect:
1, realize intellectuality, the automatic multi-step dilution of water sample
Control module is based on dilution gfactor maximum critical value, in conjunction with current measurement data, automatic decision single-stage extension rate and dilution progression, and control by stream, the realization high monitoring factor or matrix, colourity are disturbed automatic dilution, the detection of king-sized sewage, remove the trouble of manpower intervention from, realize automatic, the accurate analysis of variable concentrations scope water sample.
2, realize automatic adjusting and the switching of instrument range
By control module, realize the interlock between range value-dilution gfactor-dilution progression-measured value, its range ability no longer adopts traditional fixing shelves mode, but by water sample measured value, determined the range value of analyser, make range ability without any restriction, and can carry out full automatic range switching, and then avoid measured value higher than the immesurable problem of analyser maximum amount journey.
3, dilution accuracy is high
By increase, dilute the method for progression, dilution gfactor is reduced, effectively increased the volume of the required quantitative sample of each dilution and thinning agent, it is quantitatively more accurate to make.
By design atmospheric equilibrium hole, introduce anti-suck device, prevent that syringe pump is when process dilute sample is quantitative, what because of the impact of liquid level gravity in pipeline, cause is quantitatively inaccurate, and can effectively prevent the waste liquid suck-back during from temporary room resorption at dilute sample, has avoided stream pollution.
4, mix
In automatic dilution process, dilute solution mixes completely at mixing chamber, has solved the mixing problem of non-uniform that conventional automatic dilution method district band diffusion-stay is brought.
Accompanying drawing explanation
Fig. 1 recently controls the schematic diagram of dilution gfactor by controlling the flow rate of water sample and thinning agent in background technology;
Fig. 2 is by regulating the volume ratio of water sample quantity tube and thinning agent quantity tube to control the structural representation of dilution gfactor in background technology;
Fig. 3 is highly diluted factor water sample analysis apparatus structure schematic diagram in embodiment 1;
Fig. 4 is highly diluted factor water sample analysis apparatus structure schematic diagram in embodiment 2;
Fig. 5 is anti-suck device architecture schematic diagram in embodiment 2.
Embodiment
Embodiment 1
Refer to Fig. 3, a kind of highly diluted factor water sample analysis device, comprising: sample injection unit, control module 200 and detecting unit 301.
Described sample injection unit is connected with sample, thinning agent, mixing chamber, control module 200 and detecting unit 301.
In the present embodiment, thinning agent is clear water, and described thinning agent also can be used for cleaning each device and the pipeline of described analytical equipment simultaneously.
In the present embodiment, sample injection unit comprises syringe pump 201, multi-channel direction selecting valve 202, liquid storage ring 203 and each pipeline.
Described syringe pump 201 one end are connected with thinning agent, and one end is connected with multi-channel direction selecting valve 202 by liquid storage ring 203, and the material pumping into is carried out to accurate quantification.
Liquid storage ring 203, for the temporary transient sample being pumped into by syringe pump 201 that stores, effectively avoids the sample being pumped into by syringe pump 201 directly to contact the syringe in syringe pump 201, protects high-accuracy syringe to avoid wearing and tearing or corrosion.
Highway o, sample channel a, dilution tunnel and waste fluid channel c are set on multi-channel direction selecting valve 202; Mixing chamber is connected with multi-channel direction selecting valve 202 by dilution tunnel; Described highway o connects liquid storage ring 203.
Realizing the m level dilution of sample, is by 1 grade of dilute sample of sample and mixing diluents formation, then extract 1 grade of dilute sample of part again with mixing diluents, form 2 grades of dilute samples ..., finally form m utmost point dilute sample.
Wherein, according to n level dilution gfactor g nthe n-1 level dilute sample adopting while drawing the dilution of n level and the volume of thinning agent, and the n-1 level dilute sample of respective volume and thinning agent are mixed to get to n level dilute sample in n mixing chamber, wherein, n ∈ [1, m].
Now, each mixing chamber is different mixing chamber or same mixing chamber.When wherein each mixing chamber is same mixing chamber, need to be by the unloading of process dilute sample to temporary room, from extraction process dilute sample in temporary room to mixing chamber and mixing diluents.
In the present embodiment, every grade of dilution is all to carry out in different mixing chambers, and different mixing chambers is to be all connected with multi-channel direction selecting valve by different dilution tunnels; That is, n level is diluted in n mixing chamber mixes, and n mixing chamber 100n is connected with multi-channel direction selecting valve 202 by dilution tunnel bn; As the 1st mixing chamber 1001 is connected with multi-channel direction selecting valve 202 by dilution tunnel b1; The 2nd mixing chamber 1002 is connected with multi-channel direction selecting valve 202 by dilution tunnel b2 ... in n mixing chamber 100n, inject respectively n-1 level dilute sample and thinning agent, forms n level dilute sample.Other dilute sample outside m level dilute sample is process dilute sample.
Waste liquid is connected with multi-channel direction selecting valve 202 by waste fluid channel d.
Multi-channel direction selecting valve 202 is controlled switching and the location of stream between each passages, is combined with syringe pump 201, realizes the dilution of water sample, can guarantee simultaneously stream switch location precisely with without dead volume, and simplify flow path designs, reduce the fault point.
Described control module 200 is connected with syringe pump 201 with multi-channel direction selecting valve 202, controls multi-channel direction selecting valve 202 and selects respectively the passage of sample or thinning agent, and control syringe pump 201 undiluted sample or thinning agent or process dilute sample are injected to corresponding mixing chamber.
Described control module 200 draws input parameter according to dilution gfactor and dilution progression, i.e. the volume of sample and thinning agent; Described control module 200 is controlled described sample injection unit according to input parameter and inject undiluted sample/process dilute sample in corresponding mixing chamber;
Obtain described dilution gfactor and dilution progression has various ways, as user knows in advance and inputed to control module; Or by control module according to surveying maximum sample concentration C in instrument range L and standard method 0draw dilution progression m and dilution gfactor at different levels, wherein, total dilution gfactor is g=L/C 0, the amassing as total dilution gfactor of dilution gfactors at different levels.
Described instrument range is User Defined range or the current range of instrument.
In described standard method, can survey maximum sample concentration C 0for the highest sample concentration of surveying in corresponding measuring method; Wherein, corresponding measuring method can be national standard method, or industry standard, or iso standard method or other measuring method.
When total dilution gfactor is less than dilution gfactor maximum critical value, according to dilution gfactor, sample is carried out to 1 grade of dilution; When total dilution gfactor is greater than dilution gfactor maximum critical value, dilution gfactors at different levels are and meet
Figure GSB0000119524760000072
wherein: m ∈ Z, M is dilution gfactor maximum critical value, calculates corresponding dilution gfactor at different levels and dilution progression m, control module 200 generates corresponding input parameter according to dilution gfactors at different levels and dilution progression.User can self-defined dilution gfactor maximum critical value, by software interface, arranges.User-defined dilution gfactor maximum critical value M=20 in the present embodiment.
According to dilution gfactors at different levels and dilution progression, can generate input parameter: the population of samples of setting after each dilution amasss as V always, the volume of each draw samples is: V sample=V always/ g n, the volume that at every turn extracts thinning agent is V dilution=V always-V sample.Owing to diluting the volume of rear sample, be V alwaysso the volume of mixing chamber is greater than V always, in the present embodiment, the volume of mixing chamber is the V of 1.5 times always.
The present embodiment also provides a kind of highly diluted factor water sample analysis method, comprises the following steps:
A, determine input parameter
In the present embodiment, total dilution gfactor g=25, dilution gfactor critical value M=20,, m=2; Sample is carried out to 2 grades of dilutions, every grade of dilution gfactor g 1=g 2=5;
Therefore, user is by dilution gfactor g at different levels 1=g 2=5 and dilution progression m=2 input to control module 200, by control module 200 according to the dilution gfactor g at different levels of input 1=g 2=5 draw input parameter with dilution progression m=2: the population of samples of setting after each dilution amasss as V alwaysbe 6000 μ L, the volume of each draw samples is: V sample=1200 μ L, the volume that at every turn extracts thinning agent is V dilution=V always-V sample=4800 μ L; The volume of mixing chamber is 1.5 times of V alwaysbe 9000 μ L.
B, sample is carried out to 2 grades of dilutions i.e. the 1st grade of dilution and the 2nd grade of dilution, until form 2 grades of dilute samples; Wherein, the 1st grade of dilution comprises that pre-suction sample and mixing chamber 1001 mix; The 2nd grade of dilution comprises that 1 grade of dilute sample of pre-suction and mixing chamber 1002 mix; Concrete steps are as follows:
The 1st grade of dilution of B1
1) inhale in advance sample
Syringe pump 201 is drawn sample from sample channel a, preliminary filling sample hose, and unnecessary sample pushes away useless, by waste fluid channel c, discharges;
Syringe pump 201 is drawn thinning agent and is cleaned liquid storage ring 203, then the liquid after cleaning is pushed away useless;
2) mixing chamber 1001 mixes
Mixing chamber 1001 cleanings, emptying;
Syringe pump 201 is drawn the thinning agent of the 1st grade of dilution requirement in syringe, and now diluent volume is 4800 μ L;
Syringe pump 201 is drawn 100 μ L air to liquid storage ring 203 from air duct;
The sample that syringe pump 201 is drawn the 1st grade of dilution requirement from sample channel a is to liquid storage ring 203, and now sample volume is 1200 μ L;
Syringe pump 201 is pushed into the 1st mixed chamber 1001 by the thinning agent in liquid storage ring 203, sample by dilution tunnel b1 to be mixed, and obtains 1 grade of biased sample;
As preferably, in mixing chamber, pass into measuring the gas without impact, make sample and mixing diluents even.In the present embodiment, be to pass into air, after soon sample and thinning agent are injected into mixing chamber, further comprising the steps of:
Syringe pump 201 is drawn air to liquid storage ring 203 from air duct;
Syringe pump 201 is shifted the air in liquid storage ring 203 in mixing chamber 1001 onto by dilution tunnel b1, and thinning agent and sample are fully mixed;
The 1 grade of dilute sample that obtains mixing;
B2, the 2nd grade of dilution
1) inhale in advance 1 grade of dilute sample
Syringe pump 201 is drawn 1 grade of dilute sample from dilution tunnel b1, preliminary filling sample hose, and unnecessary 1 grade of dilute sample pushes away useless;
Syringe pump 201 is drawn thinning agent and is cleaned liquid storage ring 203, then the liquid after cleaning is pushed away useless;
2) mixing chamber 1002 mixes
Mixing chamber 1002 cleanings, emptying;
Syringe pump 201 is drawn the thinning agent of the 2nd grade of dilution requirement in syringe, and now diluent volume is 4800 μ L;
Syringe pump 201 is drawn 100 μ L air to liquid storage ring 203 from air duct;
1 grade of dilute sample that syringe pump 201 is drawn the 2nd grade of dilution requirement from dilution tunnel b1 is to liquid storage ring 203, and 1 grade of dilute sample volume now drawing is 1200 μ L;
Syringe pump 201 is pushed into the thinning agent in liquid storage ring 203,1 grade of dilute sample the 2nd mixed chamber 1002 by dilution tunnel b2 and mixes, and obtains 2 grades of biased samples;
As preferably, by process dilute sample, be after 1 grade of dilute sample in the present embodiment and thinning agent are injected into mixing chamber, further comprising the steps of:
Syringe pump 201 is drawn air to liquid storage ring 203 from air duct;
Syringe pump 201 is shifted the air in liquid storage ring 203 in mixing chamber 1002 onto by dilution tunnel b2, and thinning agent and 1 grade of dilute sample are fully mixed;
2 grades of dilute samples that finally obtain mixing;
C, detect 2 grades of dilute sample concentration, measure and finish;
After measurement finishes, carry out the cleaning of whole each device of water sample analysis device and pipeline, emptying, reset.
User inputs to control module by known dilution gfactor and dilution progression, control module can be determined input parameter, by stream, control, the realization high monitoring factor or matrix, colourity are disturbed automatic dilution, the detection of king-sized sewage, remove the trouble of manpower intervention from, realize automatic, the accurate analysis of variable concentrations scope water sample.
In automatic dilution process, dilute solution mixes in mixing chamber, has solved the inhomogeneous problem of mixing that conventional automatic dilution method district band diffusion-stay is brought.
By increase, dilute the method for progression, dilution gfactor is reduced, effectively increased the volume of the required quantitative sample of each dilution and thinning agent, it is quantitatively more accurate to make.
Embodiment 2
Refer to Fig. 4, a kind of highly diluted factor water sample analysis device, different from the analytical equipment described in embodiment 1:
Described analytical equipment also comprises temporary room 204, and described temporary room 204 is connected with multi-channel direction selecting valve 202 by temporary passage d, for temporary process dilute sample.
In the present embodiment, temporary room is one section of pipeline, need not certain container be set in addition again and keep in process dilute sample, installs and arranges conveniently.
The volume of needed n-1 level dilute sample when wherein, unloading to the volume of the n-1 level dilute sample in temporary room should be greater than and carry out the dilution of n level.
In the present embodiment, the volume of needed 1 grade of dilute sample when unloading to the volume of 1 grade of dilute sample in temporary room 204 should be greater than and carry out 2 grades of dilutions; As preferably, the volume of temporary room is the V of 1.5 times sample.
All mixing chambers are all a mixing chamber 1001, and described mixing chamber 1001 is connected with hyperchannel option valve 202 by dilution tunnel b1.
The interior temporary process dilute sample of temporary room 204, in order to make mutually not pollute between sample, needs often to clean temporary room 204; While cleaning temporary room 204, syringe pump 201 is evacuated to the liquid in temporary room 204 in liquid storage ring 203 by temporary passage d, then the liquid in liquid storage ring 203 is discharged by waste fluid channel c.In this process, with the cleaning fluid of residual sample, still can remain on liquid storage endless tube wall, cause secondary pollution;
In order more fully to clean temporary room 204, liquid storage ring, as preferably, temporary room 204 is also connected with waste liquid, so that unidirectional emptying temporary room 204, the liquid being about in temporary room 204 drains into waste liquid, makes the cleaning of temporary room 204 more thorough;
In order to prevent that liquid backflow in waste liquid is to temporary room 204, meanwhile, for when the suction process dilute sample, quantitatively more accurate, as preferably, temporary room 204 is connected with waste liquid by anti-suck device 205; Refer to Fig. 5;
On described anti-suck device 205, atmospheric pressure equalizing port 51 is set, for the inside and outside atm difference of balance anti-suck device 205; Described anti-suck device 205 for preventing when from temporary room 204 extracting liquid, waste liquid suck-back is to temporary room 204, and when suction process dilute sample, avoids quantitatively inaccurate because liquid level difference causes in pipeline.
The present embodiment also provides a kind of highly diluted factor water sample analysis method, different from the analytical approach in embodiment 1:
Step B2 comprises the following steps: first by temporary room 204 clean-drains, then by 1 grade of dilute sample unloading in mixing chamber 1001 to temporary room 204; Mixing chamber 1001 clean-drains; 1 grade of dilute sample of pre-suction; Mixing chamber 1001 mixes, and obtains 2 grades of dilute samples; Concrete steps are as follows:
1), temporary room 204 clean-drains
Syringe pump 201 is drawn air 5000 μ L to liquid storage ring 203 from air duct;
Syringe pump 201 is pushed into temporary room 204, unidirectional emptying temporary room 204 by the air in liquid storage ring 203 by temporary passage d;
Syringe pump 201 is drawn thinning agent 5000 μ L to syringe;
Syringe pump 201 is pushed into temporary room 204 by the thinning agent in liquid storage ring 203, unidirectional cleaning temporary room 204;
Syringe pump 201 is drawn air 5000 μ L to liquid storage ring 203 from air duct;
Syringe pump 201 is pushed into temporary room 204 by the air in liquid storage ring 203, unidirectional emptying temporary room 204;
2), 1 grade of dilute sample unloading in mixing chamber 1001 is to temporary room 204
Syringe pump 201 is drawn 100 μ L air to liquid storage ring 203 from air duct;
Syringe pump 201 is drawn 2000 μ L1 level dilute samples to liquid storage ring 203 from dilution tunnel b1;
Syringe pump 201 is pushed into 1 grade of dilute sample in liquid storage ring 203 in temporary room 204 by temporary passage d;
3), mixing chamber 1001 clean-drains
By the interior remaining 1 grade of dilute sample waste discharge of mixing chamber 1001, and clean the pipelines such as mixing chamber 1001 and dilution tunnel b1;
Wherein, waste discharge and cleaning step and describe before similarly, do not repeat them here;
Now cleaning mixing chamber 1001 is for fear of the cross pollution between dilute samples at different levels;
4), inhale in advance 1 grade of dilute sample
Syringe pump 201 is drawn thinning agent 1000 μ L to syringe;
Syringe pump 201 is drawn 100 μ L air to liquid storage ring 203 from air duct;
Syringe pump 201 is drawn 100 μ L1 level dilute samples to liquid storage ring 203 by temporary passage d from temporary room 204;
Syringe pump 201 pushes away useless by the thinning agent in liquid storage ring 203, air, 1 grade of dilute sample;
5), mixing chamber 1001 mixes
Syringe pump 201 is drawn the thinning agent of the 2nd grade of dilution requirement in syringe, and now diluent volume is 4800 μ L;
Syringe pump 201 is drawn 100 μ L air to liquid storage ring 203 from air duct;
1 grade of dilute sample that syringe pump 201 is drawn 2 grades of dilution requirements by temporary passage d from temporary room 204 is to liquid storage ring 203, and 1 grade of dilute sample volume now drawing is 1200 μ L;
Syringe pump 201 is pushed into mixed chamber 1001 by the thinning agent in liquid storage ring 203, air, 1 grade of dilute sample by dilution tunnel b1;
Syringe pump 201 is drawn air to liquid storage ring 203 from air duct;
Syringe pump 201 is pushed into the air in liquid storage ring 203 in mixing chamber 1001 by dilution tunnel b1, and thinning agent and 1 grade of dilute sample are fully mixed, and forms 2 grades of dilute samples.
The present embodiment, by temporary room is set, has greatly reduced the quantity of the mixing chamber that carries out the required outfit of multistage dilution, has improved the utilization factor of mixing chamber, makes instrument setting compacter.
Embodiment 3
A highly diluted factor water sample analysis device, different from the analytical equipment described in embodiment 2:
Described control module 200 is according to the maximum sample the surveyed concentration C in instrument range L and GB national standard method 0draw dilution progression m and dilution gfactor at different levels, wherein, total dilution gfactor is g=L/C 0, the amassing as total dilution gfactor of dilution gfactors at different levels.So just remove user from and inputted the trouble of diluting progression and dilution gfactors at different levels.
In the present embodiment, described instrument range is User Defined range.
While analyzing, user only need to be by the input of instrument range, and all the other operations complete by control module control instrument, realize the dilution of sample.
The present embodiment also provides a kind of highly diluted factor water sample analysis method, different from the analytical approach described in embodiment 2:
In steps A, user inputs to control module 200 by instrument range L=63mg/L, by control module 200, according to instrument range L and national standard method (GB), can survey maximum sample concentration C 0=1mg/L draws dilution progression m and dilution gfactor at different levels; In the present embodiment, the total dilution gfactor g=63 drawing, dilution gfactor critical value M=30, m=2; Sample is carried out to 2 grades of dilutions, and wherein, 1 grade of dilution gfactor is that 7,2 grades of dilution gfactors are 9;
Control module 200 draws input parameter according to dilution gfactors at different levels and dilution progression: the population of samples of setting after each dilution amasss as V alwaysbe 6300 μ L, the sample volume of 1 grade of dilution requirement is 900 μ L, and the volume of thinning agent is 5400 μ L; The 1 grade of dilute sample volume that carries out 2 grades of dilution requirements is 700 μ L, and the volume of thinning agent is 5600 μ L.
Embodiment 4
A highly diluted factor water sample analysis device, different from the analytical equipment described in embodiment 3:
The detecting unit 301 of the present embodiment is connected with control module 200, and testing result is passed to control module 200, and control module 200 is adjusted current range according to testing result.
When control module 200 is adjusted instrument range according to testing result, the sample concentration that detecting unit 200 detects after being diluted is C 1if, N≤C 1/ L≤1, measures and finishes, wherein: N makes measured value drop on the default lower limit of reliable interval in range; Can determine N value according to the detection limit of GB analytical approach itself, N=detection limit/detection range.
Otherwise adjusting apparatus tolerance journey, makes L=yC 1, wherein,
Figure GSB0000119524760000141
sample after dilution is diluted again, until final dilute sample concentration reaches measurement termination condition.
The present embodiment also provides a kind of highly diluted factor water sample analysis method, different from the analytical approach described in embodiment 3:
In step C, detect 2 grades of dilute samples and show that its concentration is C 1;
If N≤C 1/ L≤1, measures and finishes, wherein: N makes measured value drop on the default lower limit of reliable interval in range;
Otherwise adjusting apparatus tolerance journey, makes L=yC 1, wherein,
Figure GSB0000119524760000142
return to steps A.
In the present embodiment, N is set as 0.1, y and is set as 2.
By control module, realize the interlock between range value-dilution gfactor-dilution progression-measured value, its range ability no longer adopts traditional fixing shelves mode, but by water sample measured value, determined the range value of analyser, make range ability without any restriction, and can carry out full automatic range switching, and then avoid measured value higher than the immesurable problem of analyser maximum amount journey.
Embodiment 5
A highly diluted factor water sample analysis device is identical with the analytical equipment in embodiment 4.
The present embodiment also provides a kind of highly diluted factor water sample analysis method, different from the analytical approach in embodiment 4:
In steps A, the current range that instrument range is analytical instrument.
When carrying out Sample Dilution, adopt the current range of instrument as initial range like this, the dirigibility of analytical instrument is higher; Meanwhile, follow-up dilution is adjusted according to the concentration of sample after dilution by system completely, without user, participates in completely, thereby realizes full-automatic.
Above-mentioned embodiment should not be construed as limiting the scope of the invention.Key of the present invention is: control module is based on dilution gfactor maximum critical value, in conjunction with current measurement data, automatic decision extension rate and dilution progression, and control by stream, the realization high monitoring factor or matrix, colourity are disturbed automatic dilution, the detection of king-sized sewage, remove the trouble of manpower intervention from, realize automatic, the accurate analysis of variable concentrations scope water sample.In the situation that not departing from spirit of the present invention, within any type of change that the present invention is made all should fall into protection scope of the present invention.

Claims (12)

1. a highly diluted factor water sample analysis method, comprises the following steps:
A, determine input parameter
According to n level dilution gfactor g nshow that n level dilutes corresponding n-1 level dilute sample and the volume of thinning agent; Wherein, dilution progression is m, n ∈ [1, m], and the amassing as total dilution gfactor of dilution gfactors at different levels, 0 grade of dilute sample is undiluted sample;
B, sample is carried out to the dilution of m level until form m level dilute sample
Control module control syringe pump by multi-channel direction selecting valve by the n-1 level dilute sample unloading in n-1 mixing chamber to temporary room; From extracting n-1 level dilute sample in temporary room, inject n mixing chamber, and with the mixing diluents of injecting in n mixing chamber, form n level dilute sample;
Until form m level dilute sample;
C, detection m level dilute sample concentration, measure and finish.
2. analytical approach according to claim 1, is characterized in that: all mixing chambers are same mixing chamber.
3. analytical approach according to claim 1, is characterized in that: in steps A, according to surveying maximum sample concentration C in instrument range L and standard method 0draw dilution progression m and dilution gfactor at different levels, wherein, total dilution gfactor g=L/C 0.
4. analytical approach according to claim 3, is characterized in that: described instrument range is User Defined range or the current range of instrument.
5. analytical approach according to claim 3, is characterized in that: in step C:
Detect m level dilute sample and show that its concentration is C 1;
If N≤C 1/ L≤1, measures and finishes, wherein: N makes measured value drop on the default lower limit of reliable interval in range;
Otherwise adjusting apparatus tolerance journey, makes L=yC 1, wherein
Figure FSB0000118927120000011
return to steps A.
6. according to the arbitrary described analytical approach of claim 1~5, it is characterized in that: dilution gfactors at different levels are identical.
7. analytical approach according to claim 6, is characterized in that: according to M value, control dilution sum of series dilution gfactors at different levels, wherein, M value is dilution gfactor maximum critical value.
8. analytical approach according to claim 7, is characterized in that: dilution gfactors at different levels are
Figure FSB0000118927120000022
and meet g 2 - m ≤ M , g 2 - ( m - 1 ) > M .
9. a highly diluted factor water sample analysis device, comprising:
Sample injection unit, described sample injection unit comprises syringe pump, liquid storage ring and multi-channel direction selecting valve, described multi-channel direction selecting valve is connected with sample, thinning agent, mixing chamber, control module and detecting unit respectively;
Temporary room, described temporary room is connected with described multi-channel direction selecting valve, for temporary dilute sample;
Control module, described control module is also connected with described syringe pump, described control module control syringe pump by multi-channel direction selecting valve by the n-1 level dilute sample unloading in n-1 mixing chamber to temporary room; From extracting n-1 level dilute sample in temporary room, inject n mixing chamber, and with the mixing diluents of injecting in n mixing chamber, form n level dilute sample; Until form m level dilute sample; Wherein, dilution progression is m, n ∈ [1, m], and the amassing as total dilution gfactor of dilution gfactors at different levels, 0 grade of dilute sample is undiluted sample; Detecting unit, described detecting unit detects the concentration of m level dilute sample.
10. analytical equipment according to claim 9, is characterized in that: control module is according to surveying maximum sample concentration C in instrument range L and standard method 0draw dilution progression m and dilution gfactor at different levels.
11. analytical equipments according to claim 10, is characterized in that: described detecting unit is also connected with described control module, and described detecting unit passes to described control module as the foundation of control module adjustment instrument range using testing result.
12. analytical equipments according to claim 9, is characterized in that: each mixing chamber is same mixing chamber.
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