CN111896358A - Uniform dilution method for measuring COD (chemical oxygen demand) of high-concentration organic water sample - Google Patents
Uniform dilution method for measuring COD (chemical oxygen demand) of high-concentration organic water sample Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 238000003113 dilution method Methods 0.000 title claims abstract description 10
- 239000000126 substance Substances 0.000 title description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title description 6
- 229910052760 oxygen Inorganic materials 0.000 title description 6
- 239000001301 oxygen Substances 0.000 title description 6
- 238000001514 detection method Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000005070 sampling Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000007865 diluting Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 24
- 238000010790 dilution Methods 0.000 claims description 22
- 239000012895 dilution Substances 0.000 claims description 22
- 230000001804 emulsifying effect Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000000523 sample Substances 0.000 description 92
- 238000005259 measurement Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000004939 coking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012470 diluted sample Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1806—Biological oxygen demand [BOD] or chemical oxygen demand [COD]
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Abstract
A uniform dilution method for measuring COD of a high-concentration organic water sample comprises the following steps: step one, sampling: taking a representative water sample to be detected, and setting the COD concentration of the water sample to be eta0Setting the volume of a water sample to be detected as V; the amount of the water sample to be measured is more than or equal to 50 ml; a. if the volume of the water sample to be detected is less than or equal to 500ml, directly filling all the water sample into a sampling bottle; b. if the volume of the water sample to be detected is more than or equal to 500ml and less than or equal to 20L, a hand-held electric stirrer is used, a stirring head is placed at the bottom of the water sample, the water sample is stirred for 10 to 60 seconds, then 50 to 500ml of the water sample is sucked by a 50ml pipette within 5 minutes and injected into a sampling bottle. c. If the volume of the water sample to be detected is more than or equal to 20L, taking 100ml of the water sample at the top end of the liquid level, in the middle of the liquid level and at the bottom of the liquid by using a 50ml pipette respectively, and putting the water sample into a sampling bottle; the method is simple and convenient to operate, greatly shortens the time for diluting and detecting the organic water sample, and improves the accuracy of COD concentration detection.
Description
Technical Field
The invention relates to a uniform dilution method for measuring COD (chemical oxygen demand) of a high-concentration organic water sample, in particular to a uniform dilution method for exceeding the highest detection range and needing to be uniformly diluted when the COD is measured by the high-concentration organic water sample which is not dissolved in water. The method is particularly suitable for measuring the raw water COD concentration of a high-concentration organic water sample (COD is more than 100 ten thousand milligrams per liter) in the field of water treatment, and is also suitable for the pretreatment requirement that the high-concentration organic liquid containing organic impurities, oily clusters and poor fluidity needs to be uniformly diluted when the COD is measured.
Background
COD detection of water quality is an important index for chemical analysis of water treatment. At present, various methods are used for measurement, and the national standard method GB11914-89 specifically indicates that the maximum COD measurement upper limit value of an undiluted water sample is 700 mg/L. Water samples above this concentration need to be diluted for detection.
In the actual process, the original water sample is often higher than 700mg/L, the COD of similar coking wastewater is 3000-5000mg/L, the COD of the processed cutting emulsion is about 50000mg/L, and the COD of the mixed extractant of tributyl phosphate and sulfonated kerosene is about 2000000 mg/L. The COD of the raw water is far higher than the highest value of the measurement, and the uniform dilution treatment is needed. The organic components in the wastewater are insoluble in water, and can not be diluted uniformly by directly adding deionized water. In addition, organic substances inside the cutting emulsion are in a flocculation state, and need to be scattered and smashed and uniformly distributed in a water sample. How to dilute the chemical oxygen demand is not described in the method for measuring the chemical oxygen demand of GB11914-89, and the phenomenon of larger error caused by uneven dilution also exists in the actual detection process.
Disclosure of Invention
The invention aims to provide an even dilution method for measuring COD (chemical oxygen demand) by using a high-concentration organic water sample, which overcomes the defect that COD measurement result data is inaccurate because the COD can not be uniformly diluted by using the existing method for measuring COD by using the diluted high-concentration organic water sample.
A uniform dilution method for measuring COD of a high-concentration organic water sample comprises the following steps:
step one, sampling: taking a representative water sample to be detected, and setting the COD concentration of the water sample to be eta0Setting the volume of a water sample to be detected as V; the amount of the water sample to be measured is more than or equal to 50 ml;
a. if the volume of the water sample to be detected is less than or equal to 500ml, directly filling all the water sample into a sampling bottle;
b. if the volume of the water sample to be detected is more than or equal to 500ml and less than or equal to 20L, a hand-held electric stirrer is used, a stirring head is placed at the bottom of the water sample, the water sample is stirred for 10 to 60 seconds, then 50 to 500ml of the water sample is sucked by a 50ml pipette within 5 minutes and injected into a sampling bottle.
c. If the volume of the water sample to be detected is more than or equal to 20L, taking 100ml of the water sample at the top end of the liquid level, in the middle of the liquid level and at the bottom of the liquid by using a 50ml pipette respectively, and putting the water sample into a sampling bottle;
step two, pouring all the water samples obtained in the step one into a mixer I for uniform mixing, fully emulsifying and uniformly mixing the raw materials, and obtaining a uniformly mixed water sample to be detected; after being uniformly mixed, timely taking a proper amount of water sample for COD concentration detection;
a. if the COD concentration value is in the range measured by the detector, the COD detection value is eta1Turning to the step five;
b. if the COD concentration value is high and exceeds the measuring range of the detector, the next step is carried out,
step three, taking 20ml of the water sample to be detected from the water sample to be detected which is uniformly mixed in the mixer I, pouring the water sample to be detected into a dilution bottle, and adding 180ml of deionized water into the dilution bottle;
step four, cleaning the mixer I; pouring all the water samples in the dilution bottle in the previous step into a mixer I for uniform mixing, fully emulsifying and uniformly mixing the raw materials, and obtaining a uniformly mixed water sample; cleaning the dilution bottle; after water samples are uniformly mixed, timely taking a proper amount of water samples to carry out COD concentration detection;
a. if the COD concentration value is in the range measured by the detector, the COD detection value is eta1Turning to the step five;
b. if the COD concentration value is high and exceeds the measuring range of the detector, the step three is carried out,
step five, finishing the detection work, and detecting that the COD concentration value of the water sample to be detected is eta0:η0=10nη1(ii) a Wherein n is the number of times of diluting the water sample to be detected.
Wherein, the concrete method for uniformly mixing the water samples is that the mixer I is started to continuously stir for 0.5 min-10 min, so that the raw materials are fully emulsified and uniformly mixed.
The dilution flask described in step three and step four can also be replaced by blender II.
Compared with the prior art, the invention has the advantages that: the invention prepares the sample to be tested of COD by using the mixer to dilute evenly, and compared with the prior COD diluting and mixing method, the method has the following characteristics:
(1) the invention can uniformly dilute the water-insoluble organic water sample and ensure the accuracy of COD test.
(2) For a water-insoluble organic water sample, no matter how high the COD concentration is, the water-insoluble organic water sample can be quickly and uniformly diluted for many times by the method, and the detection result can be quickly calculated, so the detection is accurate;
(3) the invention prolongs the effective time of the water-insoluble organic water sample, prevents the water sample from layering within 1 year, and can effectively and accurately measure the COD value even after layering.
(4) The invention is effective to the pretreatment requirement that high-concentration organic liquid containing organic impurities, oily clusters and poor fluidity needs to be uniformly diluted when measuring COD.
(5) The method is simple and convenient to operate, greatly shortens the time for diluting and detecting the organic water sample, and improves the accuracy of COD concentration detection.
Drawings
FIG. 1 is a schematic flow chart of an embodiment of the process of the present invention;
FIG. 2 is a schematic view of a flow process according to an embodiment of the process of the present invention.
In the figure: 1 is the sampling bottle, 2 is blendor I, 3 is the dilution bottle, 4 is COD check out test set, 5 is blendor II.
The specific implementation mode is as follows:
a uniform dilution method for measuring COD of a high-concentration organic water sample comprises the following steps:
step one, sampling: taking a representative water sample to be detected, and setting the COD concentration of the water sample to be eta0Setting the volume of a water sample to be detected as V; the amount of the water sample to be measured is more than or equal to 50 ml;
a. if the volume of the water sample to be detected is less than or equal to 500ml, directly filling all the water sample into a sampling bottle;
b. if the volume of the water sample to be detected is more than or equal to 500ml and less than or equal to 20L, a hand-held electric stirrer is used, a stirring head is placed at the bottom of the water sample, the water sample is stirred for 10 to 60 seconds, then 50 to 500ml of the water sample is sucked by a 50ml pipette within 5 minutes and injected into a sampling bottle.
c. If the volume of the water sample to be detected is more than or equal to 20L, taking 100ml of the water sample at the top end of the liquid level, in the middle of the liquid level and at the bottom of the liquid by using a 50ml pipette respectively, and putting the water sample into a sampling bottle;
step two, pouring all the water samples obtained in the step one into a mixer I for uniform mixing, fully emulsifying and uniformly mixing the raw materials, and obtaining a uniformly mixed water sample to be detected; after being uniformly mixed, timely taking a proper amount of water sample for COD concentration detection;
a. if the COD concentration value is in the range measured by the detector, the COD detection value is eta1Turning to the step five;
b. if the COD concentration value is high and exceeds the measuring range of the detector, the next step is carried out,
step three, taking 20ml of the water sample to be detected from the water sample to be detected which is uniformly mixed in the mixer I, pouring the water sample to be detected into a dilution bottle, and adding 180ml of deionized water into the dilution bottle;
step four, cleaning the mixer I; pouring all the water samples in the dilution bottle in the previous step into a mixer I for uniform mixing, fully emulsifying and uniformly mixing the raw materials, and obtaining a uniformly mixed water sample; cleaning the dilution bottle; after water samples are uniformly mixed, timely taking a proper amount of water samples to carry out COD concentration detection;
a. if the COD concentration value is in the range measured by the detector, the COD detection value is eta1Turning to the step five;
b. if the COD concentration value is high and exceeds the measuring range of the detector, the step three is carried out,
step five, finishing the detection work, and detecting that the COD concentration value of the water sample to be detected is eta0:η0=10nη1(ii) a Wherein n is the number of times of diluting the water sample to be detected.
Wherein, the concrete method for uniformly mixing the water samples is that the mixer I is started to continuously stir for 0.5 min-10 min, so that the raw materials are fully emulsified and uniformly mixed.
The dilution flask described in step three and step four can also be replaced by blender II.
Pouring all the organic water samples to be detected into a mixer I, starting the mixer for mixing for 0.5-10 min, uniformly emulsifying and mixing (1), taking 50-500 ml of uniformly stirred water samples to enter a mixer II, simultaneously adding deionized water with a corresponding volume according to the dilution multiple to enter the mixer II (2), starting the mixer II to dilute, emulsify and mix (3), and taking a proper amount of diluted, emulsified and mixed water samples to perform COD detection.
Implementation scheme:
taking 50ml of waste bolt cleaning agent stock solution (COD value is calculated to be about 10000mg/L), pouring the waste bolt cleaning agent stock solution into a mixer I, covering a cutting tool bit cover, clicking a switch, starting a cutting tool bit at the rotating speed of 20000 revolutions per minute, and starting emulsification stirring. After emulsifying for 30 s. And (3) pouring 20ml of uniformly emulsified organic water sample I into a mixer II, pouring 180ml of deionized water, covering a cutting tool bit cover, clicking a switch, starting a cutting tool bit, rotating at the speed of 20000 rpm, and starting emulsifying and stirring. After emulsifying for 30s, taking 5ml of uniformly diluted emulsified water sample, and measuring the uniformly diluted water sample to obtain a COD of 975mg/L, a raw water sample of 9750mg/L, a repeated measurement result of 9830mg/L and an error of less than 1%. The accuracy of the method is verified.
The technical solution of the invention is as follows: a uniform dilution method for measuring COD of a high-concentration organic water sample comprises the following steps:
(1) sampling, and taking a representative water sample.
If the volume of the water sample is less than 500ml, the water sample is directly filled into a 500ml sampling bottle.
If the volume of the water sample is more than 500ml and less than 20L, a hand-held electric stirrer is used, a stirring head is placed at the bottom of the water sample, the water sample is stirred for 10 to 60 seconds, then 50 to 500ml of the water sample is sucked by a 50ml pipette within 5 minutes and injected into a 500ml sampling bottle.
If the volume of the water sample is more than 20L, 100ml of the water sample is respectively taken from the top of the liquid level, the middle of the liquid level and the bottom of the liquid by a 50ml pipette and is put into a 500ml sampling bottle.
(2) And (2) uniformly mixing the water sample obtained in the step (1). Here the water sample needs to be poured completely into the mixer I.
(3) Starting the mixer I, continuously stirring for 0.5-10 min to fully emulsify and uniformly mix the raw materials, obtaining a uniformly mixed water sample at the moment, and waiting for the water sampleMeasuring its COD as eta0。
(4) And (4) taking 20ml of the water sample to be detected in the step (3), pouring into a mixer II, adding 180ml of deionized water, and pouring into the mixer II. COD concentration eta of water sample0After diluted by 10 times, the concentration is reduced to 10 percent of the original concentration, namely eta1=0.1η0。
(5) And starting the mixer II, and continuously stirring for 0.5-10 min to fully mix the diluted water sample with the deionized water. Taking a proper amount of water sample to be detected, and carrying out COD detection to obtain eta1。
(6) And judging the reliability of the measurement result.
If eta1Within the accurate measurement range, the COD concentration eta of the original water sample can be calculated0=10η1。
If eta1If the accurate measurement range is less than the accurate measurement range, directly measuring eta of the step (2)0。
If eta1Higher than the accurate measurement range, and the reference step (7)
(7) Multiple dilution
And (5) taking 20ml and 180ml of deionized water from the diluted sample, and pouring into a cleaned mixer II. COD concentration eta of water sample0After 100 times of dilution, the concentration is reduced to 1 percent, namely eta2=0.01η0. Taking a proper amount of water sample to be detected, and carrying out COD detection to obtain eta2。
And (4) evaluating the reliability of the measurement result according to the step (6). If the water sample is still higher than the standard measurement range, repeating the step (7) and the step (6) until the diluted water sample etanWithin the accurate measurement range. Can calculate the COD concentration eta of the raw water sample0=10-nηn。
Further, the mixer in the step (2) comprises a base and a mixing cup, wherein the base is provided with a power line, a switch and a rotating motor, and the rotating speed of the motor is 300-. The mixing cup consists of a cutter head cover and a cup body. A rotatable cutting knife head is arranged on one side in the bottle on the knife head cover. The mixing cup has more than 100ml/200ml/500ml/1000ml and other optional dimensions. The water sample in the step (1) is required not to exceed 1/2 of the cup body, so that the excessive liquid volume and uneven mixing are prevented.
Further, in the step (3), the rotating machine starts to rotate when the switch is pressed every time, and the rotating time does not exceed 30 s. After each rotation was stopped, it was left to stand 10. The rotary machine 30s is then started again. The continuous rotation causes damage to the motor. The high-speed cutting tool bit can enable organic liquid to be cut into millimeter-sized small liquid drops to be uniformly dispersed in the water phase, and the process realizes the emulsification of the organic liquid.
Further, in the step (4), a proper amount of 10 ml-100 ml of the water sample which is uniformly stirred in the step (3) is taken, and after water is added according to the dilution ratio, the water sample and the water sample are poured into a mixer II together.
Further, blendor II is unanimous with blendor I, for the convenient name of code blendor I, blendor II.
Further, the mixing operation in the step (5) is consistent with that in the step (3). The COD testing process refers to the national COD detection standard to detect the water sample.
Claims (3)
1. A uniform dilution method for measuring COD of a high-concentration organic water sample comprises the following steps:
step one, sampling: taking a representative water sample to be detected, and setting the COD concentration of the water sample to be eta0Setting the volume of a water sample to be detected as V; the amount of the water sample to be measured is more than or equal to 50 ml;
a. if the volume of the water sample to be detected is less than or equal to 500ml, directly filling all the water sample into a sampling bottle;
b. if the volume of the water sample to be detected is more than or equal to 500ml and less than or equal to 20L, a hand-held electric stirrer is used, a stirring head is placed at the bottom of the water sample, the water sample is stirred for 10 to 60 seconds, then 50 to 500ml of the water sample is sucked by a 50ml pipette within 5 minutes and injected into a sampling bottle.
c. If the volume of the water sample to be detected is more than or equal to 20L, taking 100ml of the water sample at the top end of the liquid level, in the middle of the liquid level and at the bottom of the liquid by using a 50ml pipette respectively, and putting the water sample into a sampling bottle;
step two, pouring all the water samples obtained in the step one into a mixer I for uniform mixing, fully emulsifying and uniformly mixing the raw materials, and obtaining a uniformly mixed water sample to be detected; after being uniformly mixed, timely taking a proper amount of water sample for COD concentration detection;
a. if the COD concentration value is detectedWithin the measuring range of the measuring instrument, the COD detection value is eta1Turning to the step five;
b. if the COD concentration value is high and exceeds the measuring range of the detector, the next step is carried out,
step three, taking 20ml of the water sample to be detected from the water sample to be detected which is uniformly mixed in the mixer I, pouring the water sample to be detected into a dilution bottle, and adding 180ml of deionized water into the dilution bottle;
step four, cleaning the mixer I; pouring all the water samples in the dilution bottle in the previous step into a mixer I for uniform mixing, fully emulsifying and uniformly mixing the raw materials, and obtaining a uniformly mixed water sample; cleaning the dilution bottle; after water samples are uniformly mixed, timely taking a proper amount of water samples to carry out COD concentration detection;
a. if the COD concentration value is in the range measured by the detector, the COD detection value is eta1Turning to the step five;
b. if the COD concentration value is high and exceeds the measuring range of the detector, the step three is carried out,
step five, finishing the detection work, and detecting that the COD concentration value of the water sample to be detected is eta0:η0=10nη1(ii) a Wherein n is the number of times of diluting the water sample to be detected.
2. The method for evenly diluting a high concentration organic water sample for measuring COD according to claim 1, wherein the water sample is completely poured into the mixer I for even mixing, i.e. the mixer I is started and continuously stirred for 0.5-10 min, so that the raw materials are fully emulsified and evenly mixed.
3. The method for uniformly diluting a high-concentration organic water sample for measuring COD according to claim 1 or 2, wherein the dilution bottle in the third step and the fourth step is replaced by a blender II.
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CN114062096B (en) * | 2021-10-09 | 2023-04-21 | 武汉新烽光电股份有限公司 | Water sample dilution method for BOD on-line monitoring |
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CN113670861A (en) * | 2021-08-12 | 2021-11-19 | 力合科技(湖南)股份有限公司 | Total nitrogen analyzer and total nitrogen determination method |
CN114062096B (en) * | 2021-10-09 | 2023-04-21 | 武汉新烽光电股份有限公司 | Water sample dilution method for BOD on-line monitoring |
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