CN103091148A - Pretreatment method for measuring ammonia nitrogen in living sewage - Google Patents
Pretreatment method for measuring ammonia nitrogen in living sewage Download PDFInfo
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- CN103091148A CN103091148A CN2013100064850A CN201310006485A CN103091148A CN 103091148 A CN103091148 A CN 103091148A CN 2013100064850 A CN2013100064850 A CN 2013100064850A CN 201310006485 A CN201310006485 A CN 201310006485A CN 103091148 A CN103091148 A CN 103091148A
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Abstract
The invention discloses a pretreatment method for measuring ammonia nitrogen in living sewage, and belongs to the field of water quality index detection. In the conventional national standard, no targeted pretreatment methods aiming at the characteristics of the living sewage are proposed, and the problems that the absorbance of a blank sample is high, the measurement error is large, the adding standard recovery does not reach the standard and the like exist. The pretreatment method comprises the following steps of: directly measuring the ammonia nitrogen concentration of the living sewage so as to be used as a pre-estimation value; carrying out static settlement on a sample to be measured for 9-10min; diluting by adding distilled water according to a pre-estimation value, wherein the ammonia nitrogen concentration of the sample after being diluted is 0.8-1.0mg/L and the volume of the sample after being diluted is 90-100ml; adding 1-1.2mL of zinc sulfate solution of which the concentration is 90-100g/L into the sample; uniformly mixing; adjusting the pH to be at 10.4-10.6 by using a sodium hydroxide solution of which the concentration is 240-250g/L; uniformly mixing; carrying out static settlement for 2-3min; putting 55-60mL of supernate after the static settlement into a centrifugal tube; centrifuging for 7-10min in a speed of 3000-5000rpm; and measuring the supernate. The relative error of the pretreatment method is not larger than 2.5%, the added standard recovery is 98-105%, and the blank absorbance is less than 0.050, so that the requirements of water quality monitoring are met.
Description
Technical field
The invention belongs to the water-quality guideline detection field, be specifically related to the preprocess method that the one way of life sewage ammonia nitrogen is measured.
Background technology
2011, national surface water totally was slight pollution, and the ammonia nitrogen total emission volumn is 260.4 ten thousand tons, descends 1.52% than the last year, and wherein, agricultural sources ammonia nitrogen discharge capacity is 82.6 ten thousand tons, descends 0.41% than the last year; But lake (reservoir) eutrophication problem is still outstanding, and in 26 state control emphasis lakes (reservoir) of monitoring, lake (reservoir) ratio of I-III class, IV-V class and bad V class water quality is respectively 42.3%, 50.0% and 7.7%.Ammonia and nitrogen pollution is the major reason of China's water environment crisis.
At present, municipal sewage plant, Industrial Wastewater Treatment facility have all carried out technological innovation for the removal of ammonia nitrogen, to alleviate the water environment crisis.The Gas-phase Molecular Absorption Spectrometry ammonia nitrogen is little owing to disturbing, and reliability is high, measure accurately, and be desirable assay method.But because the method is high to the instrument and equipment requirement, be difficult to extensive universal, present, ammonia nitrogen determination mainly adopts the nessler reagent spectrophotometric method, but in actual monitoring, finds that former water total nitrogen concentration is often less than the actual measurement ammonia nitrogen concentration, measure checking by kjeldahl nitrogen, show that the ammonia nitrogen determination result is higher; During ammonia nitrogen determination, disturbing factor is more, and the wavelength in assay method is comparatively responsive for colloid and suspension, and conventional pre-service is disturbed large to measurement result; Remove technique for the nitrogen take nitrosation-anaerobic ammoxidation autotrophic denitrification technique as representative, because it requires fixing ammonia nitrogen and nitrite nitrogen ratio, the error of ammonia nitrogen has caused great impact to process control and integrated artistic treatment effect, makes this technique be difficult to bring into play its low energy consumption, dynamical advantage.
In the appraisement system of assay method, blank absorbency and accuracy are major criterions.Blank absorbency reaction the method requires blank absorbency less than 0.05 for the reliability and the susceptibility that approach the substrate concentration of measuring lower limit usually; Accuracy refers to the degree of closeness of measured value and actual value, recovery of standard addition commonly used represents, namely measuring under liquid system, by adding wherein the normal fluid of known accurate concentration, measure its alluvial and the recovery, it has reflected the actual sewage system for the influence degree of measuring matrix, and the General Requirements recovery of standard addition requires 95-105%, recovery of standard addition measurement result bigger than normal is bigger than normal, and recovery of standard addition measurement result less than normal is less than normal.The mode of direct coagulation and filtration is adopted in the pre-service of GB, does not give and corresponding preprocess method for concrete water quality characteristics, and after causing pre-service, blank absorbency is high, and is insensitive for ammonia nitrogen determination, and error is large; Coagulation process needs to carry out under alkali condition, and the ammonia nitrogen in water body is volatile; Use filter paper in filter process, the ammonia nitrogen in filter paper causes larger interference to sample; Recovery of standard addition can not reach the GB requirement; Error at measurment is generally more than 10%." urban wastewater treatment firm pollutant emission standard " one-level A standard for country promulgates requires total nitrogen less than 15mg/L, and ammonia nitrogen is less than 5mg/L, and 10% error will have a strong impact on the judgement to treatment effect.
Need the ammonia nitrogen determination preprocess method that proposes to be applicable to the sanitary sewage system badly, eliminate the interference in the ammonia nitrogen determination process, make recovery of standard addition reach 95-105% and measure accuracy requirement to satisfy, for the monitoring of water quality and the regulation and control of technique provide reliable basis.
Summary of the invention
The object of the invention is to provide a kind of interference of eliminating colloid, suspension etc. in sanitary sewage, measures the preprocess method of accuracy to guarantee the sanitary sewage ammonia nitrogen concentration.
The preprocess method that the one way of life sewage ammonia nitrogen is measured is characterized in that:
1) directly measure the ammonia nitrogen concentration of sanitary sewage without pre-service, as discreet value;
2) sanitary sewage sample to be measured is staticly settled 9-10min, adopts distilled water diluting according to discreet value, make Sample Dilution after ammonia nitrogen concentration at 0.8-1.0mg/L, after dilution, volume is 90-100mL;
3) adding 1-1.2mL concentration in sample after dilution is the solution of zinc sulfate of 90-100g/L, mixing, and the sodium hydroxide solution adjusting pH that is 240-250g/L with concentration is 10.4-10.6, mixing staticly settles 2-3min;
4) the supernatant 55-60mL that gets after staticly settling is placed in centrifuge tube, adopts the 3000-5000 rev/min of centrifugal 7-10 of rotating speed minute, gets supernatant and measures.
Compare with existing ammonia nitrogen determination preprocess method, the present invention has following beneficial effect:
1) compare GB suggestion preprocess method, by coagulation after first dilution, make ammonia nitrogen concentration less than 1mg/L, can prevent that the adding of highly basic in preprocessing process, pH from improving the measurement result that the ammonia nitrogen volatilization that causes causes less than normal;
2) compare GB suggestion preprocess method, filter by centrifugal replacement, can prevent in filter paper with ammonia nitrogen to be infected with the caused measurement result of sample bigger than normal; And with centrifugal alternative filtration, the suspension less than the filter paper hole in liquid can be separated from sample, make pre-service after sample contain hardly suspension, blank absorbency is less than 0.050, blank disturb little;
3) after sample pretreatment, accuracy of measurement is high, and relative error is less than 2.5%, and recovery of standard addition is 98%～105%;
4) compare distillation and wait preprocess method, the present invention is simple to operate, and is low for equipment requirements, is easy to promote.
Description of drawings
Fig. 1 as reference, determines the relative error of this preprocess method with the gas-phase molecular absorption spectrometry method, and carries out the mark-on recovery test, mark-on concentration 25mg/L for adopting this method actual measurement sanitary sewage ammonia nitrogen concentration.Water sampling is 50 altogether, measurement result relative error 2.16 ± 0.37%, and recovery of standard addition is 98-105%
Embodiment
Embodiment 1
Be the contrast pretreating effect, experiment adopts 3 kinds of preprocess methods that Ammonia Nitrogen in Municipal Wastewater is measured, and wherein method 1 is without the direct dilution metering of pre-service; Method 2 is recommended preprocess method in GB GB7479-87, measures after coagulation, precipitation, filtration, dilution; Method 3 adopts dilution, coagulation, precipitation, centrifugal rear mensuration, is the method for the invention.Working sample is residential quarter, Beijing septic tank effluent, ammonia nitrogen concentration 60-100mg/L, and after pre-service, ammonia nitrogen determination adopts the nessler reagent spectrophotometric method, each sample preparation and measure 3 Duplicate Samples.Titer is by the pure ammonium sulfate of accurate weighing top grade, and dilution in volumetric flask, constant volume configure, and concentration is 100.00 ± 0.05mg/L.The Gas-phase Molecular Absorption Spectrometry ammonia nitrogen disturbs lower, and stability and accuracy are higher, as reference value, measure 10 Duplicate Samples with the method measurement result.
Method 1, sample staticly settles to be got supernatant 1.00mL after 10min and is placed in the 50mL color comparison tube, measures ammonia nitrogen concentration after being diluted to the 50.00mL groove, and water sampling is 30 altogether, blank absorbency is 0.012 ± 0.008 measurement result relative error 10.16 ± 6.48%, and recovery of standard addition is 109-115%.
Method 2 is measured after coagulation, precipitation, filtration, dilution.Sample is staticly settled 10min; Get supernatant 100mL, adding 1mL concentration is the solution of zinc sulfate of 100g/L, mixing, then to add 0.1-0.2mL concentration be the sodium hydroxide solution of 250g/L, and regulating pH is 10.5, mixing staticly settles 3min until a large amount of flocculent deposit produces; Getting supernatant 10mL employing repeatedly filters without the qualitative filter paper of ammoniacal liquor drip washing; Get and filter rear sample 2.00mL, be diluted to 50.00mL and measure ammonia nitrogen concentration, water sampling is 35 altogether, and blank absorbency is 0.087 ± 0.027, measurement result relative error 9.16 ± 6.48%, and recovery of standard addition is 83-91%.
Method 3 is carried out pre-service by the method for the invention, adopts dilution, coagulation, precipitation, centrifugal rear mensuration.
1) the sanitary sewage sample is staticly settled 10min, get supernatant 2.00mL, to 100mL, after dilution, sample concentration is 0.8-1.0mg/L with distilled water diluting;
2) after the dilution sample to add 1mL concentration be the solution of zinc sulfate of 100g/L, mixing, then to add 0.1-0.2mL concentration be the sodium hydroxide solution of 250g/L, regulating pH is 10.5, mixing staticly settles 3min;
3) the supernatant 60mL that gets after staticly settling is placed in centrifuge tube, adopts 5000 rev/mins of rotating speeds centrifugal 8 minutes, gets supernatant 50mL, adopts nessler reagent spectrophotometry ammonia nitrogen concentration.
Water sampling is 50 altogether, and blank absorbency is 0.035 ± 0.011, measurement result relative error 2.16 ± 0.37%, and recovery of standard addition is 98-105%.
Claims (1)
1. the preprocess method measured of one way of life sewage ammonia nitrogen is characterized in that:
1) directly measure the ammonia nitrogen concentration of sanitary sewage without pre-service, as discreet value;
2) sanitary sewage sample to be measured is staticly settled 9-10min, adopts distilled water diluting according to discreet value, make Sample Dilution after ammonia nitrogen concentration at 0.8-1.0mg/L, after dilution, volume is 90-100mL;
3) adding 1-1.2mL concentration in sample after dilution is the solution of zinc sulfate of 90-100g/L, mixing, and the sodium hydroxide solution adjusting pH that is 240-250g/L with concentration is 10.4-10.6, mixing staticly settles 2-3min;
4) the supernatant 55-60mL that gets after staticly settling is placed in centrifuge tube, adopts the 3000-5000 rev/min of centrifugal 7-10 of rotating speed minute, gets supernatant and measures.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103674867A (en) * | 2013-11-29 | 2014-03-26 | 中国科学院电子学研究所 | Method for detecting ammonia nitrogen concentration of water sample |
| CN104483304A (en) * | 2014-12-16 | 2015-04-01 | 上海微谱化工技术服务有限公司 | Analysis method of solid cleaning agent |
| CN105021599A (en) * | 2014-09-29 | 2015-11-04 | 邓光 | Method for detecting ammonia nitrogen in water |
| CN105334208A (en) * | 2015-04-09 | 2016-02-17 | 中国科学院城市环境研究所 | Method for determining ammonia nitrogen in trace amount of solution under interference of iron and copper metal ions |
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| CN102393392A (en) * | 2011-10-26 | 2012-03-28 | 天津生机集团股份有限公司 | Reagent kit for rapidly detecting ammonium and nitrogen in water for aquaculture and detection method thereof |
| CN102721656A (en) * | 2012-06-20 | 2012-10-10 | 苏州国环环境检测有限公司 | Method for determining ammonia nitrogen content in water through Nessler reagent spectrophotometric method |
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Patent Citations (2)
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| CN102393392A (en) * | 2011-10-26 | 2012-03-28 | 天津生机集团股份有限公司 | Reagent kit for rapidly detecting ammonium and nitrogen in water for aquaculture and detection method thereof |
| CN102721656A (en) * | 2012-06-20 | 2012-10-10 | 苏州国环环境检测有限公司 | Method for determining ammonia nitrogen content in water through Nessler reagent spectrophotometric method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103674867A (en) * | 2013-11-29 | 2014-03-26 | 中国科学院电子学研究所 | Method for detecting ammonia nitrogen concentration of water sample |
| CN103674867B (en) * | 2013-11-29 | 2015-12-30 | 中国科学院电子学研究所 | The detection method of ammonia nitrogen concentration of water sample |
| CN105021599A (en) * | 2014-09-29 | 2015-11-04 | 邓光 | Method for detecting ammonia nitrogen in water |
| CN104483304A (en) * | 2014-12-16 | 2015-04-01 | 上海微谱化工技术服务有限公司 | Analysis method of solid cleaning agent |
| CN105334208A (en) * | 2015-04-09 | 2016-02-17 | 中国科学院城市环境研究所 | Method for determining ammonia nitrogen in trace amount of solution under interference of iron and copper metal ions |
| CN105334208B (en) * | 2015-04-09 | 2018-12-04 | 中国科学院城市环境研究所 | A kind of iron, copper metal ion interfere the measuring method of ammonia nitrogen in lower micro solution |
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Application publication date: 20130508 |