CN110954638B - Method for judging stability of hydrogen sulfide content in excess sludge - Google Patents
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- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8859—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample inorganic compounds
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Abstract
The invention discloses a method for judging the stability of hydrogen sulfide content in excess sludge. The invention mainly comprises the following steps: the method comprises the steps of sample collection, standard curve establishment, sample pretreatment, gas phase measurement and data processing. Taking fresh excess sludge, dividing a sample into nine parts according to an equal division principle in the sampling process, taking a middle part of the sample as an experimental sample, and storing the experimental sample in a sampling tank at a low temperature. The invention samples for multiple times (such as three times) at the same sampling point, measures the concentration change of the same sampling point at different time, can provide data guidance for hydrogen sulfide in the residual sludge of the sewage treatment plant, and effectively controls the hydrogen sulfide pollution of the residual sludge of the sewage treatment plant.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for judging the stability of hydrogen sulfide content in excess sludge.
Background
Hydrogen sulfide is an acute virulent, and inhalation of a small amount of high-concentration hydrogen sulfide can be fatal in a short time. Low concentrations of hydrogen sulfide have an effect on the eye, respiratory system and central nervous system. Hydrogen sulfide is extremely soluble in organic amines. Also has greater solubility in caustic solutions. The combustion in excess oxygen produces sulfur dioxide and water, and when the oxygen supply is insufficient, water and free sulfur are produced. Is stable at room temperature. The water soluble sulfur-free water soluble water solution is weakly acidic, and can slowly become turbid due to sulfur separated out by oxidation when contacting with air. Can be burnt in air to produce blue flame and generate SO 2 And H 2 O, S and H are formed in the case of air deficiency 2 And O. Ultra-high toxicity, even dilute hydrogen sulfide, has an irritant effect on respiratory tract and eyes and causes headache, and is dangerous to life at a concentration of 1mg/L or more, so that H is prepared and used 2 S should be performed in a fume hood.
The concentration of hydrogen sulfide in a mud area of a sewage treatment plant is higher, and the hydrogen sulfide can damage the environment and surrounding workers. Therefore, the detection of the content of the hydrogen sulfide in the excess sludge is significant for reducing the pollution of the hydrogen sulfide.
At present, the determination methods of hydrogen sulfide in the market are numerous, but most methods detect whether the hydrogen sulfide in the workshop air and the environmental air of the sewage treatment plant exceeds the standard, the research on the content of the hydrogen sulfide in the residual sludge is not carried out, the content of the hydrogen sulfide in the residual sludge is researched, the operation of the deodorization device of the sewage treatment plant can be accurately controlled, and the waste of resources is reduced.
Disclosure of Invention
The invention aims to solve the problems and provides a method for judging the stability of the content of hydrogen sulfide in excess sludge, which provides data guidance for hydrogen sulfide in excess sludge of a sewage treatment plant and effectively treats hydrogen sulfide pollution of the excess sludge of the sewage treatment plant.
In order to achieve the above object, the present invention provides a method for determining stability of hydrogen sulfide content in excess sludge, comprising:
1) collecting samples:
collecting excess sludge of a sludge treatment workshop of a sewage treatment plant for multiple times at different time points to respectively obtain the excess sludge at different time points;
2) establishment of a standard curve:
preparing hydrogen sulfide gases with different concentrations by using hydrogen sulfide standard gas to obtain gas chromatography peak areas of the hydrogen sulfide gases with different concentrations, and obtaining a standard curve of the hydrogen sulfide by linear fitting;
3) and (3) processing of a sample:
adding the residual sludge into a headspace sample injection bottle, adding hydrochloric acid and NaCl solid, then adding deionized water, capping and sealing to enable hydrogen sulfide in the sample to overflow, and obtaining a treated sample;
4) gas chromatographic determination of the sample:
performing gas chromatography determination on the treated sample to obtain the area of a gas chromatography peak, substituting the area into the standard curve of the hydrogen sulfide in the step 2) to obtain the content of the hydrogen sulfide in the treated sample, and recording the content as a, b and the like according to the sampling time sequence;
5) judging the stability of the hydrogen sulfide content:
and if the a/b is 0.8-1.2, judging that the hydrogen sulfide content of the excess sludge in the sludge treatment workshop of the sewage treatment plant is stable.
Preferably, the detection method comprises the following steps:
a method for judging the stability of the content of hydrogen sulfide in excess sludge is characterized by comprising the following steps:
1) collecting samples:
collecting excess sludge of a sludge treatment workshop of a sewage treatment plant for multiple times at different time points to respectively obtain the excess sludge at different time points;
2) establishment of a standard curve:
preparing hydrogen sulfide gases with different concentrations by using hydrogen sulfide standard gas to obtain gas chromatography peak areas of the hydrogen sulfide gases with different concentrations, and obtaining a standard curve of the hydrogen sulfide by linear fitting;
3) and (3) processing of a sample:
adding the residual sludge into a headspace sample injection bottle, adding hydrochloric acid and NaCl solid, then adding deionized water, capping and sealing to enable hydrogen sulfide in the sample to overflow, and obtaining a treated sample;
4) gas chromatographic determination of the sample:
performing gas chromatography determination on the treated sample to obtain the area of a gas chromatography peak, substituting the area into the standard curve of the hydrogen sulfide in the step 2) to obtain the content of the hydrogen sulfide in the treated sample, and recording the content as a, b and the like according to the sampling time sequence;
5) judging the stability of the hydrogen sulfide content:
and if the a/b is 0.8-1.2, judging that the hydrogen sulfide content of the excess sludge in the sludge treatment workshop of the sewage treatment plant is stable.
As a preferred scheme, the excess sludge of a sludge treatment workshop of a sewage treatment plant is collected by a freezing sampling tank, the freezing sampling tank is of an inner-outer double-layer barreled structure, an inner barrel is used for sample preservation, the surface of an outer barrel is coated with a heat insulation material, and liquid nitrogen is added between the two barrels before sampling. The freezing sampling tank is used for sampling, so that the original property of the sludge can be fully retained, and workers can be prevented from being frostbitten.
Preferably, in the step 2), the concentration of hydrogen sulfide gas with different concentrations is 0mg/L, 0.15-0.25mg/L, 0.35-0.45mg/L, 0.55-0.65mg/L, 0.75-0.85mg/L and 0.95-1 mg/L.
Preferably, in step 2), the hydrogen sulfide gas has concentrations of 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L and 1 mg/L.
Preferably, in the step 3), the dosage ratio of the excess sludge, the hydrochloric acid and the NaCl solid is 2 g: (0.04-0.06) mL: (0.8-1.2) g.
As a preferred scheme, when the headspace sampling bottle is used for processing a sample, the headspace sampling program is set as follows: heating the sample to 60 ℃, the temperature of the transmission line is 100 ℃, the temperature of the injection needle is 95 ℃, the constant temperature time of the headspace bottle is 30min, the pressure balance time is 1min, and then performing the step 4). And the content of volatile hydrogen sulfide in the solid excess sludge is measured by headspace sampling, so that the steps of sample pretreatment are reduced.
As a preferred scheme, when gas chromatography is carried out, the sample injection method is temperature programming, and the program is as follows: the initial temperature was 35 deg.C, held for 10min, ramped up to 120 deg.C at 20 deg.C/min, held for 4min, ramped up to 220 deg.C at 25 deg.C/min, held for 2.5 min.
As a preferred scheme, when gas chromatography is carried out, the temperature of a sample inlet is 250 ℃, the flow rate of a column is 1.0mL/min, the purging flow of a spacer is 3mL/min, the sample introduction volume is 1uL, a sample introduction liner pipe is a shunt liner pipe, and the shunt ratio is 3: 1.
Preferably, the detector is an FPD detector and the column is Agilent DB-SULFUR SCD when gas chromatography is performed.
Preferably, the proper operation of the sludge treatment plant of the sewage treatment plant is determined prior to sample collection.
As a further preferable scheme, in the sampling process of fresh excess sludge, a sample can be divided into nine parts according to an equal division principle, the middle part of the sample is taken as an experimental sample, and the experimental sample is stored in a sampling tank at a low temperature. Such as placing in a refrigerator for freezing.
The invention has the beneficial effects that:
1. the invention uses a self-made freezing sampling tank for sampling during sampling, takes fresh excess sludge, divides the sample into a plurality of parts (such as nine parts) according to an equal division principle preferably in the sampling process, takes a middle part of the sample as an experimental sample, and stores the experimental sample in the sampling tank at low temperature. And sampling is carried out for multiple times (such as three times) at the same sampling point, and the concentration change of the same sampling point at different time is measured, so that data guidance can be provided for the hydrogen sulfide in the residual sludge of the sewage treatment plant, and the hydrogen sulfide pollution of the residual sludge of the sewage treatment plant can be effectively treated.
2. The headspace sample injection bottle is adopted to measure the content of hydrogen sulfide in the excess sludge, and the method has the characteristics of simple operation, high sensitivity, accurate measurement result and the like.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
In the embodiment of the invention, the structure of the specially-made freezing sampling tank is specifically as follows: freezing sample jar is two inside and outside circular steel drums, interior bucket diameter 8mm, urceolus diameter 10mm, high 15cm, and the lid is fixed on the urceolus, and diameter 10mm opens the lid when needing the sample, has got the sample after, adds a certain amount of liquid nitrogen between the bucket of the inside and outside, then fixes the lid, and one prevents that the measuring thing of sample from volatilizing, and two prevents that the sample from shining and falling. The heat insulating material is wrapped on the edge of the outer barrel, so that personnel can be prevented from being frostbitten after liquid nitrogen is added. The edge of the outer cylinder is provided with two vent holes with the diameter of 1cm, so that the liquid nitrogen is prevented from volatilizing to cause burst hazard. The addition of liquid nitrogen allows the sample to be kept at a lower temperature during the field to the laboratory, maintaining as much of the original properties of the sample as possible.
Example 1
Detecting hydrogen sulfide in excess sludge of a sludge treatment workshop A of a certain sewage treatment plant.
Step one, sample collection: before sample collection, the normal operation of a sludge treatment plant of a sewage treatment plant needs to be determined. Sampling by using a special freezing sampling tank, taking fresh excess sludge, dividing a sample into nine parts according to an equal division principle in the sampling process, taking a middle part of the sample as an experimental sample, and storing the experimental sample in the sampling tank at a low temperature; after the first sampling, samples were taken every 3 hours at the same sampling point, twice in total.
Step two, establishing a standard curve: the standard gas with certain concentration is configured into the standard gas with the following concentration: 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L and 1mg/L, and introducing sample by gas chromatography, wherein the sample introduction method comprises temperature programming and the program comprises the following steps: the initial temperature was 35 deg.C, held for 10min, ramped up to 120 deg.C at 20 deg.C/min, held for 4min, ramped up to 220 deg.C at 25 deg.C/min, held for 2.5 min. The injection inlet temperature is 250 ℃, the column flow rate is 1.0mL/min, the spacer purge flow is 3mL/min, the injection volume is 1ul, the injection liner tube is a shunt liner tube, and the shunt ratio is 3: 1. The detector is FPD detector, and the chromatographic column is Agilent DB-SULFUR SCD. Obtaining a standard curve by linear fitting of peak areas measured by gas chromatography: y is 0.9962x-0.0021, wherein y represents the concentration of hydrogen sulfide, and x represents the peak area of gas chromatography.
Step three, sample treatment: and collecting a fresh sample, and placing the fresh sample in a refrigerator for freezing treatment. And (3) adding 2g of excess sludge into a headspace sampling bottle, adding a drop of hydrochloric acid and 1g of NaCl solid into the sample, adding 5mL of deionized water into the sample at one time by using a liquid transfer device, and quickly covering and sealing the sample to ensure that hydrogen sulfide in the sample is easier to overflow. The headspace sampling program is set as that the sample is heated to 60 ℃, the temperature of the transmission line is 100 ℃, the temperature of the sampling needle is 95 ℃, the headspace bottle is stable for 30min, the pressure balance time is 1min, and then the sample is injected.
Step four, gas chromatography determination: and (3) feeding the sample treated by headspace sample injection into a gas chromatograph, wherein the sample injection method comprises the following steps of: the initial temperature was 35 deg.C, held for 10min, ramped up to 120 deg.C at 20 deg.C/min, held for 4min, ramped up to 220 deg.C at 25 deg.C/min, held for 2.5 min. The sample injection volume is 1uL, the sample injection liner tube is a shunt liner tube, the detector is an FPD detector, and the chromatographic column is Agilent DB-SULFUR SCD. The peak area was determined by gas chromatography.
Step five, judging the stability of the hydrogen sulfide content: and substituting the measured sample peak area into X in the standard curve, and calculating the content Y of the hydrogen sulfide in the residual sludge. The result obtained by the first sampling is 0.35mg/L, the result obtained by the second sampling is 0.31mg/L, and the result obtained by the second sampling is slightly lower than the result obtained by the first sampling, but the difference is not great, which indicates that the content of hydrogen sulfide in the residual sludge in different time periods is relatively stable.
Example 2
Detecting hydrogen sulfide in excess sludge of a sludge treatment workshop A of a certain sewage treatment plant.
The difference from example 1 is that in step one, samples were taken at 5-hour intervals.
The standard curve of the example 1 is used, the result of the first sampling is 0.37mg/L, the result of the second sampling is 0.36mg/L, and the result of the second sampling is slightly lower than the result of the first sampling, but the difference is not great, which indicates that the content of hydrogen sulfide in the residual sludge in different time periods is relatively stable.
While embodiments of the present invention have been described above, the above description is illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (7)
1. A method for judging the stability of the content of hydrogen sulfide in excess sludge is characterized by comprising the following steps:
1) collecting samples:
collecting excess sludge of a sludge treatment workshop of a sewage treatment plant for multiple times at different time points to respectively obtain the excess sludge at different time points;
2) establishment of a standard curve:
preparing hydrogen sulfide gases with different concentrations by using hydrogen sulfide standard gas to obtain gas chromatography peak areas of the hydrogen sulfide gases with different concentrations, and performing linear fitting to obtain a standard curve of the hydrogen sulfide;
3) and (3) processing of a sample:
adding the residual sludge into a headspace sample injection bottle, adding hydrochloric acid and NaCl solid, then adding deionized water, capping and sealing to enable hydrogen sulfide in the sample to overflow, and obtaining a treated sample;
4) gas chromatographic determination of the sample:
performing gas chromatography determination on the treated sample to obtain the area of a gas chromatography peak, substituting the area into the standard curve of the hydrogen sulfide in the step 2) to obtain the content of the hydrogen sulfide in the treated sample, and recording the content as a and b according to the sampling time sequence;
5) judging the stability of the hydrogen sulfide content:
if the a/b =0.8-1.2, judging that the hydrogen sulfide content of the excess sludge in the sludge treatment workshop of the sewage treatment plant is stable;
collecting residual sludge in a sludge treatment workshop of a sewage treatment plant by using a freezing sampling tank, wherein the freezing sampling tank is of an inner-outer double-layer barreled structure, an inner barrel is used for sample preservation, the surface of an outer barrel is coated with a heat insulation material, liquid nitrogen is added between the two barrels before sampling, and the edge of the outer barrel is provided with a plurality of vent holes;
wherein, when using the headspace sample introduction bottle to handle the sample, the headspace sample introduction program sets up to: heating the sample to 60 ℃, the temperature of the transmission line is 100 ℃, the temperature of the sample injection needle is 95 ℃, the constant temperature time of the headspace bottle is 30min, the pressure balance time is 1min, and then carrying out the step 4);
wherein, when gas chromatography is used for measurement, the sample introduction method is temperature programming, and the program is as follows: the initial temperature was 35 deg.C, held for 10min, ramped up to 120 deg.C at 20 deg.C/min, held for 4min, ramped up to 220 deg.C at 25 deg.C/min, held for 2.5 min.
2. The method of claim 1, wherein the method comprises the steps of:
1) collecting samples:
collecting fresh excess sludge of a sludge treatment workshop of a sewage treatment plant every 2-5 h to respectively obtain excess sludge at different time points, and storing at 0-4 ℃;
2) establishment of a standard curve:
preparing hydrogen sulfide gases with different concentrations in a concentration range of 0mg/L-1mg/L by using hydrogen sulfide standard gas to obtain gas chromatography peak areas of the hydrogen sulfide gases with different concentrations, and obtaining a standard curve of the hydrogen sulfide by linear fitting;
3) and (3) processing of a sample:
adding residual sludge into a headspace sample injection bottle, adding hydrochloric acid and NaCl solid, adding deionized water, capping and sealing to enable hydrogen sulfide in the sample to overflow, thus obtaining a treated sample, wherein the material-liquid ratio of the residual sludge to the deionized water is 2 g: (4-6) mL;
4) gas chromatographic determination of the sample:
performing gas chromatography determination on the treated sample to obtain the area of a gas chromatography peak, substituting the area into the standard curve of the hydrogen sulfide in the step 2) to obtain the content of the hydrogen sulfide in the treated sample, and recording the content as a and b according to the sampling time sequence;
5) judging the stability of the hydrogen sulfide content:
and if the a/b =0.8-1.2, judging that the hydrogen sulfide content of the excess sludge of the sludge treatment workshop of the sewage treatment plant is stable.
3. The method according to claim 1 or 2, wherein in step 2), the hydrogen sulfide gas has a concentration of 0mg/L, 0.15-0.25mg/L, 0.35-0.45mg/L, 0.55-0.65mg/L, 0.75-0.85mg/L, 0.95-1 mg/L.
4. The method according to claim 1 or 2, wherein in step 2), the hydrogen sulfide gas has a concentration of 0mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1 mg/L.
5. The method according to claim 1 or 2, wherein in step 3), the ratio of the amount of excess sludge, hydrochloric acid and NaCl solids is 2 g: (0.04-0.06) mL: (0.8-1.2) g.
6. The method according to claim 1 or 2, wherein, when the gas chromatography is performed, the injection port temperature is 250 ℃, the column flow rate is 1.0mL/min, the spacer purge flow is 3mL/min, the injection volume is 1 μ L, the injection liner is a split liner, and the split ratio is 3: 1.
7. The method according to claim 1 or 2, wherein, when performing gas chromatography measurements, the detector is an FPD detector and the chromatography column is Agilent DB-self cdr SCD.
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| CN103063790B (en) * | 2011-10-20 | 2015-04-29 | 攀钢集团西昌钢钒有限公司 | Method for detecting hydrogen sulfide content in coal gas |
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| CN106290660A (en) * | 2016-11-10 | 2017-01-04 | 同济大学 | A kind of fast, the method for sulfurous gas in accurate quantitative analysis biogas |
| CN106824209B (en) * | 2016-12-05 | 2019-07-23 | 上海大学 | The method for preparing porous material processing hydrogen sulfide contamination gas using mixing sludge |
| CN107401867B (en) * | 2017-07-17 | 2023-06-13 | 浙江万里学院 | Liquid nitrogen freezing and storing device for lifting aquatic products |
| CN107543903A (en) * | 2017-08-25 | 2018-01-05 | 北京林业大学 | A kind of method and apparatus for monitoring dewatering technology of mud ammonia and hydrogen sulfide on-line |
| CN107640443A (en) * | 2017-09-30 | 2018-01-30 | 广东产品质量监督检验研究院 | One kind detection sample stored frozen device |
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