CN107957398A - A kind of assay method and analyzer of the CODMn of continuous sample introduction - Google Patents
A kind of assay method and analyzer of the CODMn of continuous sample introduction Download PDFInfo
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- 238000003556 assay Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 70
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 62
- 238000004458 analytical method Methods 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 238000001514 detection method Methods 0.000 claims abstract description 47
- 230000008569 process Effects 0.000 claims abstract description 40
- 230000029087 digestion Effects 0.000 claims description 99
- 239000007788 liquid Substances 0.000 claims description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000002699 waste material Substances 0.000 claims description 34
- 238000004140 cleaning Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 16
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 230000001079 digestive effect Effects 0.000 claims description 12
- 238000006479 redox reaction Methods 0.000 claims description 10
- 238000004847 absorption spectroscopy Methods 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 230000002457 bidirectional effect Effects 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 238000002835 absorbance Methods 0.000 claims description 3
- 238000000862 absorption spectrum Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000007259 addition reaction Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 229940124597 therapeutic agent Drugs 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 18
- 238000004611 spectroscopical analysis Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 22
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 22
- 235000010288 sodium nitrite Nutrition 0.000 description 11
- 238000005070 sampling Methods 0.000 description 10
- 239000012286 potassium permanganate Substances 0.000 description 7
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 150000002191 fatty alcohols Chemical class 0.000 description 5
- 230000006870 function Effects 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical group CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 2
- 229940039790 sodium oxalate Drugs 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- -1 constant volume Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- IPGOVDXOBDFUBM-UHFFFAOYSA-N oxalic acid;sodium Chemical compound [Na].OC(=O)C(O)=O IPGOVDXOBDFUBM-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000002133 sample digestion Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3125—Measuring the absorption by excited molecules
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of assay method of the permanganate index of continuous sample introduction, it is characterised in that：Including the sample introduction process, chemical reaction process, analysis detection process performed successively；Wherein, the sample introduction process is that continuous continual sample introduction or the continuous sample introduction by the appointed interval time, form sample and line up；The chemical reaction process is, with specified time beat, each sample in lining up for sample, the reagent of the various resolution reactions of addition automated one by one with the mode of operation of assembly line, carries out resolution reaction；The analysis detection process is that the measure of permanganate index is carried out for the sample for completing resolution reaction.And brand-new permanganate index analyzer is designed and developed according to the method.The release of this method and instrument will solve sample turbidity and colourity interference problem in permanganate index test, improve the efficiency and quality of test.Gas molecule in space spectroscopic analysis methods widely using in permanganate index test is promoted at the same time.
Description
Technical field
The present invention provides a kind of chemical analysis method and instrument, and in particular, to a kind of survey of the CODMn of continuous sample introduction
Determine method and analyzer.
Background technology
Permanganate index is referred to for surface water body by the synthesis of organic pollution and reducing inorganic contaminants degree
Mark, the oxygen consumed when referring in acid or alkalescence medium using permanganate by oxidizer treatment water sample, with the mg/L of oxygen
To represent.Permanganate index often by as surface water body by organic pollution and the synthesis of reducing inorganic Substances Pollution degree
Index.
Existing national standard method mainly with oxalic acid sodium reduction residue potassium permanganate and adds excess, then with potassium permanganate residual titration mistake
Sodium oxalate is measured, manually observes solution colour change to judge reaction end.(see《GB11892-89 water quality permanganate indexs
Measure》With《Water and effluent monitoring analysis method (fourth edition)》), existing method mainly mainly has following ask in practical applications
Topic：
(1) it need to judge that reaction end and reagent consume, and are not suitable for measure higher turbidity and containing colored by color change
Sample；
(2) judge in test process there are the manually-operated titration of many places needs, aberration and etc., it is easily introduced operation and misses
Difference is high to operator's skill set requirements；
(3) it is difficult to realize high-precision automation mechanized operation, it is difficult to meet high-volume testing requirement.
Although in existing technology, the sodium oxalate in GB11892-89 methods is replaced to lead to as reducing agent using nitrite
Cross using gas-phase molecular absorption spectrometry method (Gas-Phase Molecular Absorption Spectrometry, hereinafter referred to as
GPMAS) the mode of indirect determination nitrite, establishes the literature method of the fast quantitative analysis of permanganate index in water.
This method can solve the problems, such as that turbidity influences aberration judgement in GB11892-89 methods, but still remain problems with：
(1) this method can only be interrupted sample introduction analysis, it is impossible to which continuous sample introduction is analyzed.Permanganate digestion process it is generally time-consuming compared with
Length is, it is necessary to 30 minutes.Therefore, sample can only be interrupted sample introduction and wait to analyze again after the completion of clearing up, it is impossible to which continuous sample introduction is simultaneously analyzed.It is if single
GPMAS analyses are carried out after a sample digestion, then efficiency is too low.
(2) if sample is cleared up in batch, the GPMAS analyses link to follow-up nitrous acid solution causes progress to block.It is tighter
Weight, since nitrite solution cannot preserve for a long time under sour environment, can constantly decompose.So when using in batch
The mode of resolution, the progress of its analysis link produced block, and can cause the rotten of subsequent sample, and then experimental result can be made
Into seriously affecting：The repeatability variation not only tested, experimental result are also inaccurate.
(3) this method is a kind of semiautomation operation method, in addition to GPMAS analyzes link, in Specimen eliminating and nitrous acid
Other link steps such as reduction of sodium are all to use manual process.Also, the design based on its chemical processes is not suitable for
Automation mechanized operation, can not instruct actual instrumentation to develop.
(4) since this method is in sample introduction, add the processes such as various reagents, constant volume, liquid relief still can only manual operation, cause
Both precision is insufficient for this method, also inefficiency.It is also not suitable for the high-volume testing requirement of permanganic acid index.
To sum up, although gas-phase molecular absorption spectrometry method solves water in permanganate index test compared to national standard method
Sample turbidity and colourity interference problem.But still remain and be unable to continuous sample introduction, it is impossible to the problem of automating, so that cause efficiency low,
Precision cannot be guaranteed, and also seriously hinder popularization and application of the GPMAS methods in the test of actual permanganate index.Limit
Gas molecule in space spectroscopic methodology is not used for testing permanganate index on a large scale in real work, is not based on Vehicles Collected from Market yet
The instrument of this method produces and sells.
The content of the invention
The present invention provides a kind of test method of gas-phase molecular absorption spectrometry method test permanganate index, and according to this side
Method has designed and developed brand-new achievable continuous sample introduction, the permanganate index analyzer of detection, has filled up in this field
Domestic and international blank.The release of this method and instrument will solve sample turbidity and colourity interference problem in permanganate index test,
The efficiency and quality of test are improved, while promotes gas molecule in space spectroscopic analysis methods to make extensively in permanganate index test
With.
The present invention provides a kind of assay method of the permanganate index of continuous sample introduction, it is characterised in that：With assembly line
Mode perform following process successively in digestion tube queue:Sample introduction process, reaction process, analysis detection process；
Wherein, above-mentioned sample introduction process is continuous continual sample introduction or the continuous sample introduction by the appointed interval time and resolution
Reagent, forms sample queue；
The sample introduction is to digestion tube sample introduction, and then realizes the reaction process such as follow-up resolution reaction.Above-mentioned interval time can
To carry out any setting, generally 5 minutes according to the property of sample.
Above-mentioned reaction process is, with specified time beat, each sample in the sample queue reacted for completion resolution,
The addition reaction reagent of automation is (such as：Sodium nitrite etc.), carry out redox reaction；
The time beat refers to the order of addition and interlude of every kind of reagent, such as：While each sample feeding
Addition acid and permanganate, clear up 30 minutes；And in the wait digestion time of 30 minutes, to other digestion tubes carry out sample and
Loading device, when reaching the stand-by period of 30 minutes, is switched to initial digestion tube by the addition work of acid and permanganate
Carry out the addition of sodium nitrite reagent.And so on, when also needing to add other reagents, all in accordance with every kind of reagent characteristic and stop
The time is stayed to be waited.User can be set and be adjusted to the time beat according to the needs of various sample tests.
Above-mentioned analysis detection process is to carry out gas-phase molecular absorption spectrometry analysis for the sample for completing redox reaction
And the calculating of permanganate index.
Further, the assay method of the permanganate index of a kind of continuous sample introduction provided by the invention, also has so
The characteristics of：I.e., cleaning process is further included；
After the analysis for completing a sample or one group of sample detects process and/or sample introduction process, cleaning is automatically switched to
Process；
Above-mentioned cleaning process is that cleaning solution is set to what the sample for completing analysis detection process and/or sample introduction process was flowed through
The process that standby and/or pipeline is cleaned.
Further, the assay method of the permanganate index of a kind of continuous sample introduction provided by the invention, also has so
The characteristics of：I.e., concrete technology step is as follows：
Step 1: nitrite standard specimen successively sample introduction to each digestion tube is formed into sample queue, in 80-100 DEG C of temperature
After lower insulation 5-10 minutes, analysis detection is carried out one by one to it, and make absorbance standard curve；
Step 2: keeping temperature, sample to be tested and digestive reagent are added into digestion tube N, waits interval time to be specified,
The digestive reagent is acid and permanganate；
Step 3: digestion tube N+1, N+2, N+3......N+n into queue successively, the action of repeat step two, until
All digestion tubes complete sample to be tested and the addition of digestive reagent or total time-consuming reaches the digestion time of setting, and N and n are certainly
So number；
Step 4: when the stand-by period of digestion tube N having reached the digestion time of setting, nitrous is added into digestion tube N
Hydrochlorate, carries out redox reaction；
Step 5: after redox reaction is completed, after partly or entirely the extracting of liquid in digestion tube N, with acid,
Fatty alcohol is reacted, and the analysis result of the gas phase analysis absorption spectrum of the gas obtained according to reaction, calculates corresponding Gao Meng
Recorded after hydrochlorate index；
Step 6: the pipeline and/or equipment that are flowed through to digestion tube N and sample, are cleaned automatically with pure water；
Step 7: keeping temperature, sample to be tested and digestive reagent are added into digestion tube N, waits interval time to be specified；
The process is after the liquid in a digestion tube in queue is drawn into the link of analysis, continues to complete to the cleaning
Digestion tube in the follow-up sample to be tested of addition, it is achieved thereby that continuously, the effect analyzed in sample introduction
Step 8: next digestion tube is turned to, (such as：N=N+1), repeat step four to seven, until all samples to be tested are completed
Chemical analysis；
Wherein, in step 1, after each digestion tube completes standard specimen sample introduction, the pipeline and equipment that are flowed through to the standard specimen,
Cleaned automatically with pure water, at the same each standard specimen complete analysis after, the pipeline and equipment that are flowed through to the standard specimen, with pure water into
The automatic cleaning of row；
It is to be measured to this after each digestion tube completes the addition of sample to be tested and digestive reagent in step 3 and seven
The pipeline that sample flows through, is cleaned automatically with pure water；
In step 6, when there is liquid residual in digestion tube N, then after first discharging the remaining waste in digestion tube N, then offset
The pipeline and/or equipment that solution pipe N and sample flow through, are cleaned automatically with pure water.
A kind of in addition, permanganate index analyzer present invention also offers continuous sample introduction, it is characterised in that：Including into
Egf block, chemical reaction module, analysis detection module；
Above-mentioned sample introduction module includes sample sets, sample introduction equipment；
The sample introduction module is used to pass through the reagent in sample sets in the sample introduction equipment such as pump input chemical reaction module；
The sample introduction module can realize at least two functions, first, when sample is standard sample or sample to be tested, by into
Sample equipment is inputted in resolution apparatus and carries out resolution reaction；Second, when sample for cleaning solution (such as：Pure water) when, can by into
Sample equipment is pumped into other modules, and then realizes the function of cleaning.
Above-mentioned chemical reaction module includes reagent set, disengaging sample device, digestion pool；
The reagent set includes can be used for the reagent for realizing resolution reaction, general to select：Proton acid reagent is (such as：The concentrated sulfuric acid),
Permanganate agent is (such as：Potassium permanganate), redox reagent is (such as：The nitrite such as sodium nitrite).
The disengaging sample device can be realized such as：Liquid reagent in the equipment such as digestion tube outputs and inputs function.
Some digestion tubes are equipped with above-mentioned digestion pool；Such digestion tube is in the arrangement of queue, which can be circular team
Row, or the queue of any geometry is (such as：Square, diamond shape etc.), its quantity and queue mode by Index Instrument specification
Or the needs of client be adjusted with it is customized.
Each digestion tube has unique corresponding numbering, which is summarized in the mainboard program of Index Instrument, in order to realize
The tracking of digestion tube state, each digestion tube is also provided with independent infrared induction equipment, monitoring water level equipment, flow monitoring are set
Standby to wait monitoring equipment, all equipment can be in real time by status data transfers into mainboard program, and mainboard program is according to each
The status data of digestion tube carries out the arrangement of operating process and deploys to ensure effective monitoring and control of illegal activities.
Above-mentioned analysis detection module includes gas detection equipment；
The gas detection equipment is the specific implementation device of GPMAS methods.
Wherein, at least one sample is included in above-mentioned sample sets；
Mentioned reagent group memory contains at least one reagent；
Sample in above-mentioned sample sets enters chemical reaction module by sample introduction equipment, via disengaging sample device input resolution pipe
It is interior；
Mentioned reagent group turn on disengaging sample device, via passing in and out sample device to digestion tube delivery of therapeutic agents；
Above-mentioned disengaging sample device circulates according to time beat between each digestion tube, input sample or reagent, and is examined to analysis
Survey module output and complete the sample after resolution；
Above-mentioned gas detection device carries out chemical analysis to completing the sample after clearing up.
Further, the permanganate index analyzer of a kind of continuous sample introduction provided by the invention, also with such spy
Point：I.e., above-mentioned disengaging sample device includes transfer device and more siphunculus；
Above-mentioned transfer device drives more siphunculus to be circulated according to time beat between each digestion tube；
Wherein, above-mentioned more siphunculus are equipped with some mutually independent paths；
Above-mentioned path turns on correspondingly with each reagent in reagent set, for conveying classes of agents；
Above-mentioned path is also turned on sample introduction module, for inputting various samples；
Above-mentioned path is also turned on analysis detection module, for exporting the sample after various completions are cleared up；
And/or
Above-mentioned chemical reaction module further includes waste liquor treatment equipment；
Above-mentioned waste liquor treatment equipment switches circulation between digestion tube, discharges waste liquid.
The waste liquid can be that all kinds of waste liquids, the processes of the discharge such as cleaning waste liquid, reaction remaining waste can be to be aggregated into
Concentration discharge is carried out in liquid waste collector, or during operation, is directly arranged by the pipeline connected with device external
Go out, or discharged by the vapor liquid equilibrium such as linker equipment.
Further, the permanganate index analyzer of a kind of continuous sample introduction provided by the invention, it is characterised in that：I.e.,
Above-mentioned sample introduction module further includes at least one sample switching device, is used for realization the switching of multiple sample room paths.
Further, the permanganate index analyzer of a kind of continuous sample introduction provided by the invention, also with such spy
Point：I.e., above-mentioned analysis detection module further includes reaction reagent group, gas-liquid separation equipment, waste collection equipment；
Wherein, at least one reaction reagent is included in above-mentioned reaction reagent group；The reaction reagent is can be by sodium nitrite
The reagent of nitric oxide or nitrogen dioxide is reduced to, it is general to select acid (such as：Hydrochloric acid, citric acid etc.), fatty alcohol (such as：Methanol, second
Alcohol, propyl alcohol etc.).
Above-mentioned reaction reagent is with completing the sample after resolution, in branch or the input gas-liquid separation equipment gone the same way；I.e., this is anti-
After answering reagent to import a mixing chamber by equipment such as communicating pipes with completing the sample after clearing up, then input gas-liquid separation and set
In standby, or the reaction reagent is inputted in gas-liquid separation equipment, when inputting respectively respectively with completing the sample after resolution by two-way
When, the input speed of two-way liquid should be controlled respectively by equipment such as flow-limiting valves.
Above-mentioned gas-liquid separation equipment is equipped with gas passage and fluid passage；Be respectively used to conveying reaction generation gas with
And reserve liquid after reacting remaining or cleaning；
Above-mentioned gas passage is turned on gas detection equipment；Realize the detection of gas；Under normal circumstances, it is more preferable in order to realize
Detection result, the cleaning equipment such as drier can be also equipped with the path of the conducting.
Aforesaid liquid passage is turned on waste collection equipment.
Can be to be arranged by the pipeline connected with device external when the waste collection equipment reaches certain limit
Go out, or discharged by the vapor liquid equilibrium such as linker equipment.
Further, the permanganate index analyzer of a kind of continuous sample introduction provided by the invention, also with such spy
Point：I.e., it is equipped with heating equipment in above-mentioned digestion pool；
And/or above-mentioned gas-liquid separation equipment is equipped with heating equipment；
And/or above-mentioned reaction reagent is equipped with heating equipment to the pipeline that gas-liquid separation equipment conveys；
And/or the sample after above-mentioned completion resolution is equipped with heating equipment to the pipeline that gas-liquid separation equipment conveys.
Such heating equipment can be controlled by the control button or front end display screen on instrument surface, also can by mainboard program come
Actively heat (such as：When sensing that instrument starts or sample is ready, the program of automatic start heating).
Further, the permanganate index analyzer of a kind of continuous sample introduction provided by the invention, also with such spy
Point：I.e., pipeline handover module is further included；
Above-mentioned pipeline handover module is respectively turned on sample introduction module, analysis detection module and chemical reaction module, realizes sample introduction
Module, analysis detection module and the switching for chemically reacting path between module.
Further, the permanganate index analyzer of a kind of continuous sample introduction provided by the invention, also with such spy
Point：I.e., above-mentioned pipeline handover module is equipped with more siphunculus switching valve, injection port, bidirectional interface, outlet, and/or waste liquid ports；
Above-mentioned injection port, bidirectional interface, outlet, waste liquid port realized by more siphunculus switching valves two-way between each outlet or
Multinomial conducting；
Wherein, above-mentioned injection port is turned on sample introduction equipment；
Above-mentioned bidirectional interface is turned on disengaging sample device；
Above-mentioned outlet is turned on entering gas-liquid separation equipment or analyzing the path of detection module；
Above-mentioned waste liquid port is turned on waste collection equipment.
The function and effect of the present invention：
The present invention provides a kind of test method of gas-phase molecular absorption spectrometry method test permanganate index, and according to this side
Method has designed and developed brand-new permanganate index analyzer, has filled up the domestic and international blank in this field.This method and instrument
The release of device will solve sample turbidity and colourity interference problem in permanganate index test, improve the efficiency and quality of test.
Gas molecule in space spectroscopic analysis methods widely using in permanganate index test is promoted at the same time.
The invention discloses a kind of automation stream that permanganate index in water is measured based on gas molecule in space spectral absorption method
Cheng Fangfa, and a kind of brand-new permanganate index analyzer is devised based on this flow and method.This method and instrument have with
Lower obvious advantage：
1. technical flow design is rationally ingenious, digestion process is designed using the thought of queue in software subject, by disappearing
Intermittent analysis flow is converted to the continuous analysis process of sustainable sample introduction by the design of solution pipe queue, substantially increases analysis effect
Rate.Solves the stability problem of efficiency in conventional method and its nitrous acid in practical applications.
2. the instrument based on this method design takes full advantage of the advantage of GPMAS analysis methods, solves national standard method
The colourity of GB11892-89 and the interference problem of turbidity：Since permanganate index is converted into gas, by gas from water sample
Measured again after separation, the colourity and turbidity of sample would not interference experiment results.
3. based on the instrument of this method design, rectification journey full automation, it is not necessary to manual intervention.Avoid because operation
Precision problem caused by reason, also greatly increases the production efficiency.
Brief description of the drawings
The structure diagram of attached drawing 1, permanganate index analyzer provided in this embodiment；
The structure diagram for clearing up queue of attached drawing 2, permanganate index analyzer provided in this embodiment；
The structure diagram for the permanganate index analyzer that attached drawing 3, the variation one of the present embodiment provide；
The structure diagram for the permanganate index analyzer that attached drawing 4, the variation two of the present embodiment provide.
Embodiment
As shown in Figure 1, permanganate index analyzer provided in this embodiment include sample introduction module, chemical analyzer module,
Analyze detection module.
Sample introduction module, including sample sets, sampling pump P1, switching valve V1 and V2；
Wherein, include in sample sets independently be used to store sample (sample to be tested), standard specimen (standard sample) and pure
Three liquid storage containers of water (cleaning solution)；
Sample is connected with switching valve V1 respectively with the liquid output pipe of standard specimen, by control switching valve V1 realize sample and
Sample introduction selection and switching, the output terminal of switching valve V1 between standard specimen are equipped with a liquid output pipe turned on switching valve V2；
The liquid output pipe of pure water is connected with switching valve V2, and pure water and switching valve V1 ends are realized by controlling switching valve V2
Selection and switching between the liquid of output, the output terminal of switching valve V2 are turned on sampling pump P1, for by sample, standard specimen or pure
Water is exported to resolution Queue module；
Chemically react module, including reagent set, sampling pump P2, digesting equipment, switching valve V3；
Wherein, three storages for being used to store the concentrated sulfuric acid, potassium permanganate and sodium nitrite independently are included in reagent set
Liquid container；
Digesting equipment includes digestion pool, digestion tube and multichannel pin；Several digestion tubes, the resolution are equipped with the digestion pool
Pond is furnished with water bath with thermostatic control heating unit, as shown in Fig. 2, the digestion tube is in the arrangement of queue, which moves with polar coordinates
Device 3 is controlled, with the rotation of mechanical arm by coordinate position each by the rotating connection of mechanical arm by polar coordinates telecontrol equipment
Circulation between digestion tube.
As shown in Figure 1, the liquid output pipe of the concentrated sulfuric acid, potassium permanganate and sodium nitrite is connected with sampling pump P2 respectively,
Sampling pump P2 and the conducting that multichannel pin is in a plurality of circuit, realize that the concentrated sulfuric acid, potassium permanganate and sodium nitrite pass through sampling pump P2
Being pumped in multichannel pin independently, and then entered by multichannel pin in digestion tube；Meanwhile multichannel pin be additionally provided with to
A few sample intake passage that is independent, being turned on switching valve V3, for by the sample in autosampler module, standard specimen or pure water
In input resolution pipe.Its amount of being pumped into can be calculated by computer and obtain or be set by the operating personnel of front equipment end.
The output terminal with sampling pump P1, multichannel pin connect switching valve V3 into sample outlet end respectively, and equipped with an output
End is connected with analysis detection module, and switching valve V3 can realize the work of Three models.
Operating mode A., which works as, to be needed the sample in autosampler module, standard specimen or pure water input resolution Queue module
When, switching valve V3 can be set to conducting a-b ends, and then sample, standard specimen or pure water are directly flowed into what is specified by multichannel pin
In digestion tube；
Operating mode B., can be by switching valve when needing the pure water input in autosampler module analyzing detection module
V3 is set to conducting a-c ends, and then pure water is directly inputted in analysis detection module；
Operating mode C. when need will clear up complete sample/standard specimen or cleaning after water input analysis detection module when,
Switching valve V3 can be set to conducting b-c ends, and then by the water after clearing up the sample/standard specimen completed or cleaning directly by more logical
In road pin input analysis detection module.
Analysis detection module includes reaction reagent the storage box, sampling pump P3 and P4, gas-liquid separation equipment, gas collection
Device, detector and waste liquid pool；
Wherein, which contains the reaction reagents such as the acid reacted with nitrite and fatty alcohol, leads to
Cross sampling pump P3 to be pumped into gas-liquid separation equipment, its amount of being pumped into can calculate the operation for obtaining or passing through front equipment end by computer
Personnel are set.
The liquid inputted by the c ends of switching valve V3, is pumped into gas-liquid separation equipment by sampling pump P4, when the liquid being pumped into
During sample/standard specimen that body is completed for resolution, reacted in gas-liquid separation equipment with reaction reagent, it reacts the gas produced
After the completion of being collected by gas collector, it is delivered to detector end and carries out sample detection and analysis, it reacts remaining liquid then
It is discharged into waste liquid pool；When solution after the liquid being pumped into is the cleaning of pure water or digestion tube, directly in company with gas-liquid separation equipment
Solution is discharged into waste liquid pool together after cleaning.
The carrying out practically step of the said equipment is as follows：
Step 1: nitrite standard specimen successively sample introduction is formed sample queue, 5-10 is kept the temperature at a temperature of 80-100 DEG C
After minute, chemical analysis is carried out one by one to it, and make absorbance standard curve；
Step 2: the pipeline and equipment that are flowed through to step 1 nitrite standard specimen, are cleaned automatically with pure water；
Step 3: keeping temperature, to digestion tube N sample introductions, acid and permanganate are added, waits interval time to be specified；
Step 4: to digestion tube N+1, N+2, N+3......N+n of queue successively, the action of repeat step three, until institute
Some digestion tubes complete sample introduction or total time-consuming reaches setting time, and n is natural number；
Step 5: when the stand-by period of digestion tube N having reached setting time, nitrite is added into digestion tube N, into
Row redox reaction；
Step 6: after redox reaction is completed, after partly or entirely the extracting of liquid in digestion tube N, with acid,
Fatty alcohol is reacted, and the analysis result of the gas phase analysis absorption spectrum of the gas obtained according to reaction, measures nitrous acid solution
Concentration, and recorded after calculating corresponding permanganate index；
Step 7: the pipeline and equipment that are flowed through to the sample in digestion tube N, are cleaned automatically with pure water；
Step 8: keeping temperature, sample to be tested and digestive reagent are added into digestion tube N, waits interval time to be specified；
The process is after the liquid in a digestion tube in queue is drawn into the link of analysis, continues to complete to the cleaning
Digestion tube in the follow-up sample to be tested of addition, it is achieved thereby that continuously, the effect analyzed in sample introduction
Step 9: N=N+1, next digestion tube under turning, the action of repeat step five to eight is until next digestion tube is sky
When；
Wherein, in step 1, when the concentration of sodium nitrite standard specimen is different, after each standard specimen completes sample introduction, to this
The pipeline and equipment that standard specimen flows through, are cleaned automatically with pure water, while after each standard specimen completes analysis, which is flowed through
Pipeline and equipment, cleaned automatically with pure water；
Between step three and four, when the sample of digestion tube N and digestion tube N+n is different sample, in digestion tube N
In sample complete sample introduction after, the pipeline and equipment that are flowed through to the sample, are cleaned automatically with pure water.
By taking the detection of 5 groups of samples as an example, the principle of its carrying out practically is as follows：
1. chemically react module：Water-bath is preheating to 100 degree.
2 sample introduction modules：Next idle digestion tube in auto injection to resolution Queue module.
3 chemical reaction modules：Concentrated sulfuric acid solution is added to the digestion tube of new sample introduction, adds liquor potassic permanganate, heating disappears
Solution a period of time.
4 chemical reaction modules：Digestion tube to having completed Specimen eliminating, it is unnecessary using excessive nitrite solution reduction
Potassium permanganate.
5. chemically react module：Digestion tube to having completed reduction reaction, takes out remaining sodium nitrite solution,
It is input to analysis detection module.
6. analyze detection module：With the mixture that acid is medium, fatty alcohol is catalyst, with step 5 gained sodium nitrite
Solution is pumped into analysis detection together.Analyze detection module and use gas molecule in space spectral absorption method measure nitrous acid solution concentration.And
Permanganate index is calculated according to the relation (such as formula one) of sodium nitrite and permanganic acid acid potassium amount.
Permanganate index (O2, mg/L) and=(C1×8×V1)/(7×V2)
C1For nitrite solution concentration, unit is mg/L；
V1It is nitrous acid solution cumulative volume in step 4, unit is ml；
8：It is the molal weight of oxygen (1/2O)；
7：It is the molal weight of nitrogen (1/2N)；
V1：It is the sample volume of sample, unit is ml.
7. following step 2-6 repeatedly, analyzed until all samples and complete
There are 5 digestion tubes in the resolution queue of above-mentioned example, each sample need to heat 30 minutes, this multichannel pin is each
Work on digestion tube needs to complete in 6 minutes altogether.
According to the announcement and teaching of example below, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula make a change and modification.Therefore, the invention is not limited in the embodiment for being disclosed below and describing, to the present invention's
Digestion tube number, heating time, processing are time-consuming, the amount of sample and reagent, and the modifications and changes of the parameter such as reagent concentration also should
When fall into the present invention scope of the claims in.
The variation one of the present embodiment：
As shown in figure 3, switching valve V3 is connected with waste liquid pool, when needing to discharge the liquid in digestion tube, conducting can be passed through
Liquid in digestion tube is directly discharged into the effect of waste liquid pool to realize by b-d ends.
The variation two of the present embodiment：
As shown in figure 4, further include waste liquid pool in resolution Queue module and go out sample pump P5；
This goes out sample pump P5 one end and is connected with going out sample device, and the other end is connected with waste liquid pool, this goes out control pair of the sample device by system
Digestion tube in be cleaned/cleaning carries out the output function of waste liquid, and liquid is delivered in waste liquid pool by going out sample pump P5.
Claims (10)
- A kind of 1. assay method of the permanganate index of continuous sample introduction, it is characterised in that：In pipelined fashion in digestion tube Following process is performed in queue successively:Sample introduction process, reaction process, analysis detection process；Wherein, the sample introduction process is that continuous uninterrupted or continuous sample introduction and digestive reagent by the appointed interval time, form sample Product queue；The reaction process is, with specified time beat, each sample in the sample queue reacted for completion resolution, automatically The addition reaction reagent of change, carries out redox reaction；The analysis detection process is to carry out gas-phase molecular absorption spectrometry analysis and height for the sample for completing redox reaction The calculating of mangaic acid salt index.
- A kind of 2. assay method of the permanganate index of continuous sample introduction as claimed in claim 1, it is characterised in that：Further include Cleaning process；After the analysis for completing a sample or one group of sample detects process and/or sample introduction process, cleaning process is automatically switched to；The cleaning process is, equipment that cleaning solution flows through the sample for completing to analyze detection process and/or sample introduction process and/ Or the process that pipeline is cleaned.
- A kind of 3. assay method of the permanganate index of continuous sample introduction as claimed in claim 2, it is characterised in that specific work Skill step is as follows：Step 1: nitrite standard specimen successively sample introduction to each digestion tube is formed sample queue, protected at a temperature of 80-100 DEG C After 5-10 minutes warm, analysis detection is carried out one by one to it, and make absorbance standard curve；Step 2: keeping temperature, sample to be tested and digestive reagent are added into digestion tube N, waits interval time to be specified, it is described Digestive reagent is acid and permanganate；Step 3: digestion tube N+1, N+2, N+3......N+n into queue, the action of repeat step two successively, until owning Digestion tube complete sample to be tested and the addition of digestive reagent or total time-consuming reaches the digestion time of setting, N and n are nature Number；Step 4: when the stand-by period of digestion tube N having reached the digestion time of setting, nitrite is added into digestion tube N, Carry out redox reaction；Step 5: after redox reaction is completed, after partly or entirely the extracting of liquid in digestion tube N, with acid, fat Alcohol is reacted, and the analysis result of the gas phase analysis absorption spectrum of the gas obtained according to reaction, calculates corresponding permanganate Recorded after index；Step 6: the pipeline and/or equipment that are flowed through to digestion tube N and sample, are cleaned automatically with pure water；Step 7: keeping temperature, sample to be tested and digestive reagent are added into digestion tube N, waits interval time to be specified；Step 8: next digestion tube is gone to, repeat step four to seven, until all samples to be tested complete chemical analysis；Wherein, exist In step 1, after each digestion tube completes standard specimen sample introduction, the pipeline and equipment that are flowed through to the standard specimen, are carried out automatic clear with pure water Wash, while after each standard specimen completes analysis, the pipeline and equipment that are flowed through to the standard specimen, are cleaned automatically with pure water；In step 3 and seven, after each digestion tube completes the addition of sample to be tested and digestive reagent, to the sample to be tested The pipeline flowed through, is cleaned automatically with pure water；In step 6, when there is liquid residual in digestion tube N, then after first discharging the remaining waste in digestion tube N, then to digestion tube The pipeline and/or equipment that N and sample flow through, are cleaned automatically with pure water.
- A kind of 4. permanganate index analyzer of continuous sample introduction, it is characterised in that：Including sample introduction module, chemical reaction module, Analyze detection module；The sample introduction module includes sample sets, sample introduction equipment；The chemical reaction module includes reagent set, disengaging sample device, digestion pool；Some digestion tubes are equipped with the digestion pool；The analysis detection module includes gas detection equipment；Wherein, at least one sample is included in the sample sets；The reagent set memory contains at least one reagent；Sample in the sample sets enters chemical reaction module by sample introduction equipment, via in disengaging sample device input resolution pipe；The reagent set turn on disengaging sample device, via passing in and out sample device to digestion tube delivery of therapeutic agents；The disengaging sample device circulates according to time beat between each digestion tube, input sample or reagent, and detects mould to analysis The sample after resolution is completed in block output；The gas detection equipment carries out chemical analysis to completing the sample after clearing up.
- A kind of 5. permanganate index analyzer of continuous sample introduction as claimed in claim 4, it is characterised in that：The disengaging sample device includes transfer device and more siphunculus；The transfer device drives more siphunculus to be circulated according to time beat between each digestion tube；Wherein, more siphunculus are equipped with some mutually independent paths；The path turns on correspondingly with each reagent in reagent set, for conveying classes of agents；The path is also turned on sample introduction module, for inputting various samples；The path is also turned on analysis detection module, for exporting the sample after various completions are cleared up；And/orThe chemical reaction module further includes waste liquor treatment equipment；The waste liquor treatment equipment switches circulation between digestion tube, discharges waste liquid.
- A kind of 6. permanganate index analyzer of continuous sample introduction as claimed in claim 4, it is characterised in that：The sample introduction module further includes at least one sample switching device, is used for realization the switching of multiple sample room paths.
- A kind of 7. permanganate index analyzer of continuous sample introduction as claimed in claim 4, it is characterised in that：The analysis detection module further includes reaction reagent group, gas-liquid separation equipment, waste collection equipment；Wherein, at least one reaction reagent is included in the reaction reagent group；The reaction reagent is with completing the sample after resolution, in branch or the input gas-liquid separation equipment gone the same way；The gas-liquid separation equipment is equipped with gas passage and fluid passage；The gas passage is turned on gas detection equipment；The fluid passage is turned on waste collection equipment.
- A kind of 8. permanganate index analyzer of continuous sample introduction as described in claim 4-7 is any, it is characterised in that：Heating equipment is equipped with the digestion pool；And/or the gas-liquid separation equipment is equipped with heating equipment；And/or the reaction reagent is equipped with heating equipment to the pipeline that gas-liquid separation equipment conveys；And/or the sample after the completion resolution is equipped with heating equipment to the pipeline that gas-liquid separation equipment conveys.
- A kind of 9. permanganate index analyzer of continuous sample introduction as described in claim 4-8 is any, it is characterised in that：Further include pipeline handover module；The pipeline handover module be respectively turned on sample introduction module, analysis detection module and chemical reaction module, realize sample introduction module, Analyze detection module and chemically react the switching of path between module.
- A kind of 10. permanganate index analyzer of continuous sample introduction as claimed in claim 9, it is characterised in that：The pipeline handover module is equipped with more siphunculus switching valve, injection port, bidirectional interface, outlet, and/or waste liquid ports；The injection port, bidirectional interface, outlet, waste liquid port are realized two-way or multinomial between each outlet by more siphunculus switching valves Conducting；Wherein, the injection port is turned on sample introduction equipment；The bidirectional interface is turned on disengaging sample device；The outlet is turned on entering gas-liquid separation equipment or analyzing the path of detection module；The waste liquid port is turned on waste collection equipment.
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Application publication date: 20180424 |