CN109696410A - A kind of polyethers production waste water dissolubility COD rapid detection method - Google Patents
A kind of polyethers production waste water dissolubility COD rapid detection method Download PDFInfo
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- CN109696410A CN109696410A CN201910105387.XA CN201910105387A CN109696410A CN 109696410 A CN109696410 A CN 109696410A CN 201910105387 A CN201910105387 A CN 201910105387A CN 109696410 A CN109696410 A CN 109696410A
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- Prior art keywords
- cod
- polyester wastewater
- detection method
- polyethers
- wastewater
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- 239000002351 wastewater Substances 0.000 title claims abstract description 59
- 238000001514 detection method Methods 0.000 title claims abstract description 23
- 229920000570 polyether Polymers 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title description 5
- 229920000728 polyester Polymers 0.000 claims abstract description 46
- 238000001228 spectrum Methods 0.000 claims abstract description 11
- 238000004458 analytical method Methods 0.000 claims abstract description 9
- 238000007619 statistical method Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000002835 absorbance Methods 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 7
- 238000010219 correlation analysis Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 4
- 239000012898 sample dilution Substances 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 238000012360 testing method Methods 0.000 abstract description 7
- 238000002211 ultraviolet spectrum Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- DOBUSJIVSSJEDA-UHFFFAOYSA-L 1,3-dioxa-2$l^{6}-thia-4-mercuracyclobutane 2,2-dioxide Chemical compound [Hg+2].[O-]S([O-])(=O)=O DOBUSJIVSSJEDA-UHFFFAOYSA-L 0.000 description 1
- 238000010220 Pearson correlation analysis Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000556 factor analysis Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229940074994 mercuric sulfate Drugs 0.000 description 1
- 229910000372 mercury(II) sulfate Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Abstract
The present invention relates to a kind of polyethers to produce waste water dissolubility COD rapid detection method.The present invention finds out polyethers characteristic spectrum in conjunction with statistical analysis, and establish linear relationship with dissolubility COD by analysis Polyester wastewater ultraviolet spectra fingerprint characteristic.The present invention realizes the quick detection to Polyester wastewater dissolubility COD, and comparison routine COD detection method is compared, and can greatly reduce COD detection time cost.Meanwhile, it is capable to greatly save COD test reagent cost, while COD detection can be eliminated and cause environmental pollution, there is high economy and environmental benefit.
Description
Technical field
The invention belongs to sewage detection technical fields, and in particular to a kind of polyethers production waste water dissolubility COD is quickly detected
Method.
Background technique
Currently, the production waste water COD detection of petrochemical industry polyethers generally uses rapid-digestion spectrophotometry (HJ/T399-
2007) it is analyzed, for instructing the debugging and operational management of petrifaction sewage treatment facility.Current routine COD detection method pair
Although it is more accurate that Polyester wastewater COD analyzes result, takes a long time, generally need 2h or more.Meanwhile COD test medicament is main
For potassium bichromate, the concentrated sulfuric acid, silver sulfate, mercuric sulfate etc., these medicaments are expensive and can cause seriously to pollute to environment.Cause
How this shortens the COD testing time, addition noble metal or heavy metal medicament is avoided to make under the premise of guaranteeing COD test accurately
With being the current COD test technical issues that need to address.
Summary of the invention
The technical problem to be solved by the present invention is to be directed to the deficiency of existing COD detection technique, provide suitable for petrochemical industry row
Industry Polyester wastewater dissolubility COD rapid detection method.
The present invention finds out polyethers characteristic spectrum in conjunction with statistical analysis by analysis Polyester wastewater ultraviolet spectra fingerprint characteristic,
And linear relationship is established with dissolubility COD.By detecting Polyester wastewater characteristic spectrum absorbance, Polyester wastewater can be directly obtained
Dissolubility COD value.
To achieve the above object, the present invention adopts the following technical scheme: a kind of polyethers production waste water dissolubility COD is quickly examined
Survey method, by analyzing Polyester wastewater ultraviolet spectra fingerprint characteristic, binding factor analysis and correlation analysis find out polyethers feature
Spectrum, and correlation curve is established with dissolubility COD, by detecting Polyester wastewater characteristic spectrum absorbance, can directly obtain
Polyester wastewater dissolubility COD value.
Specifically comprise the following steps:
1) Polyester wastewater is repeatedly sampled, is sampled number 5-15 times, adjust pH=7.0 ± 0.1, it is dilute through deionized water
It releases, and removes oil removal with 0.45 μm of filter membrane；
2) it carries out ultraviolet-visible spectrum to sample to sweep entirely, scanning wavelength range is 200nm-500nm；
3) it using factorial analysis and correlation analysis screening and the optimal spectral wavelength of Polyester wastewater COD correlation, and builds
Vertical correlation curve；
4) Polyester wastewater water sample to be measured is taken, pH=7.0 ± 0.1 is adjusted, is diluted through deionized water, and gone with 0.45 μm of filter membrane
Oil removal；
5) ultraviolet-visible spectrophotometer is utilized, it is dilute in the ultraviolet characteristic spectrum wavelength measurement Polyester wastewater of Polyester wastewater
Rear sample absorbance value is released, absorbance and COD relation curve, as Polyester wastewater COD concentration are substituted into；
Polyester wastewater statistics water sample extension rate is determined according to its absorbance in the step 2), is inhaled after guaranteeing water sample dilution
Shading value is between 0.5-2.5.
Ultraviolet-visible spectrophotometer zeroing is returned to zero using deionized water in the step 3).
Polyester wastewater water sample extension rate to be measured is determined according to its absorbance in the step 4), is inhaled after guaranteeing water sample dilution
Shading value is between 0.5-2.5.
Ultraviolet-visible spectrophotometer zeroing is returned to zero using deionized water in the step 5).
Inventive principle
Polyester wastewater mainly contains terephthalic acid (TPA) and phenol, this type organic is in ultraviolet-visible spectrum UV200-
250nm has obvious absorption.It is counted by multiple repairing weld, finds out Polyester wastewater ultraviolet absorptivity and wavelength COD in a linear relationship,
The value of COD is determined by detecting Polyester wastewater absorbance value under the ultraviolet wavelength.
Calculation formula:
CODCr(mg/L)=(a × UV+b) × n
Wherein: a, b are UV characteristic wavelength and COD correlation curve slope and intercept, after the numerical value is by statistically linear fitting
It obtains；
UV is the absorbance with the highest UV wavelength of the Polyester wastewater COD degree of correlation；
N is extension rate.
Beneficial effect
The present invention finds out polyethers characteristic spectrum in conjunction with statistical analysis by analysis Polyester wastewater ultraviolet spectra fingerprint characteristic,
And linear relationship is established with dissolubility COD.The present invention realizes the quick detection to Polyester wastewater dissolubility COD, compares routine COD
Detection method is compared, and COD detection time cost can be greatly reduced.Meanwhile, it is capable to COD test reagent cost is greatlyd save, and
COD detection can be eliminated and cause environmental pollution, there is high economy and environmental benefit.
Present invention detection speed is quick, is highly suitable for developing Polyester wastewater COD on-line checking.
Detailed description of the invention
Fig. 1 is ultraviolet-visible full scan figure.
Fig. 2 is correlation analysis figure.
Fig. 3 is embodiment COD and UV208 linear fitting diagram.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment
The present invention is applied to Tianjin petrifaction sewage treatment plant Polyester wastewater COD and quickly detects, comprising the following steps:
One, the foundation of standard curve
(1) in petrifaction sewage factory, Polyester wastewater sampled point is repeatedly sampled, and utilizes rapid-digestion spectrophotometry (HJ/T399-
2007) analysis Polyester wastewater COD is carried out；
(2) Polyester wastewater water sample adjusts pH=7.0 ± 0.1, removes oil removal with 0.45 μm of filter membrane, dilute through deionized water
20 times and constant volume are released, to guarantee UV absorbance between 0.5-2.5.Ultraviolet-visible full scan (figure is carried out to water sample after dilution
1)；
(3) through factorial analysis and correlation analysis (Fig. 2 and table 1), factorial analysis is aobvious by gained spectral absorbance and corresponding COD
Show UV208And UV210With COD strong correlation, Correlation analysis showed UV208Absorbance and COD correlation are best, establish mark through fitting
Directrix curve is COD=(44.005 × UV208+20.650)×20,R2=0.940, linear fit is as shown in Figure 3；
1 Pearson correlation analysis of table
Two, Polyester wastewater COD is quickly detected
(1) Polyester wastewater water sample is taken, pH=7.0 ± 0.1 is adjusted, dilutes 20 times through deionized water, guarantees that absorbance exists
0.5-2.5, and oil removal is removed through 0.45 μm of filter membrane；
(2) ultraviolet-visible spectrophotometer is utilized, it is dilute in the ultraviolet characteristic spectrum wavelength measurement Polyester wastewater of Polyester wastewater
Rear sample absorbance value is released, absorbance and COD relation curve, as Polyester wastewater COD concentration (table 2) are substituted into.
The COD value of the present invention of table 2 and rapid-digestion spectrophotometry COD value
The measurement result of the invention method and national standard rapid-digestion spectrophotometry is still it can be seen from upper table 2
Compare identical, for petrochemical industry Polyester wastewater, the relative error of COD is in the range of -17.05%~16.72%.This
Kind analysis precision meets the requirement of the operation of petrochemical industry Polyester wastewater sewage treatment facility and self-test.
Although the preferred embodiment of the present invention is described above, the invention is not limited to above-mentioned specific
Embodiment, the above mentioned embodiment is only schematical, is not restrictive, those skilled in the art
Under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, it can also make very
Multi-form specific transformation, within these are all belonged to the scope of protection of the present invention.
Claims (6)
1. a kind of polyethers produces waste water dissolubility COD rapid detection method, which is characterized in that by analyzing Polyester wastewater ultraviolet light
Fingerprint characteristic is composed, finds out polyethers characteristic spectrum in conjunction with statistical analysis, and establish linear relationship with dissolubility COD, it is poly- by detecting
Ether wastewater characteristic spectrum absorbance can directly obtain Polyester wastewater dissolubility COD value.
2. a kind of polyethers according to claim 1 produces waste water dissolubility COD rapid detection method, which is characterized in that its
It is characterized in that, specifically comprises the following steps:
1) Polyester wastewater is sampled, adjusts pH=7.0 ± 0.1, is diluted through deionized water, and is outstanding with 0.45 μm of filter membrane removal
Floating object；
2) it carries out ultraviolet-visible spectrum to sample to sweep entirely, scanning wavelength range is 200nm-500nm；
3) using factorial analysis and correlation analysis screening and the optimal spectral wavelength of Polyester wastewater COD correlation, and phase is established
Close curve；
4) Polyester wastewater water sample to be measured is taken, pH=7.0 ± 0.1 is adjusted, is diluted through deionized water, and is outstanding with 0.45 μm of filter membrane removal
Floating object；
5) ultraviolet-visible spectrophotometer is utilized, after the ultraviolet characteristic spectrum wavelength measurement Polyester wastewater dilution of Polyester wastewater
Sample absorbance value substitutes into absorbance and COD relation curve, as Polyester wastewater COD concentration.
3. a kind of polyethers according to claim 2 produces waste water dissolubility COD rapid detection method, which is characterized in that institute
It states Polyester wastewater statistics water sample extension rate in step 1) and determines that absorbance value exists after guaranteeing water sample dilution according to its absorbance
Between 0.5-2.5.
4. a kind of polyethers according to claim 2 produces waste water dissolubility COD rapid detection method, which is characterized in that institute
Ultraviolet-visible spectrophotometer zeroing in step 2) is stated to return to zero using deionized water.
5. a kind of polyethers according to claim 2 produces waste water dissolubility COD rapid detection method, which is characterized in that institute
It states the water sample extension rate to be measured of Polyester wastewater in step 4) to be determined according to its absorbance, absorbance value exists after guaranteeing water sample dilution
Between 0.5-2.5.
6. a kind of polyethers according to claim 2 produces waste water dissolubility COD rapid detection method, which is characterized in that institute
Ultraviolet-visible spectrophotometer zeroing in step 5) is stated to return to zero using deionized water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110987860A (en) * | 2019-12-18 | 2020-04-10 | 松辽水资源保护科学研究所 | COD detection method based on infrared technology |
| CN111929265A (en) * | 2020-10-09 | 2020-11-13 | 天津市赛普新锐仪器科技有限公司 | Accurate compensation determination method for COD and/or BOD of domestic sewage |
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Application publication date: 20190430 |