CN106680052B - The preparation method of inorganic constituents standard sample and standard sample obtained in city sludge - Google Patents
The preparation method of inorganic constituents standard sample and standard sample obtained in city sludge Download PDFInfo
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Abstract
The present invention relates to the preparation method of inorganic constituents standard sample in city sludge, include the following steps: to acquire sample；Preliminary Determination；It impregnates；It mixes；It air-dries；Drying；Secondary mixing: it is mixed again using heap method is moved；It grinds and sieves；It mixes three times；Uniformity initial survey；The sample of uniformity initial survey qualification is subjected to uniformity testing, stability test, definite value and uncertainty evaluation process again, to carry out definite value calibration to mud sample.Through the invention in city sludge obtained inorganic matter standard sample, by carrying out mark-on reclaims to mud sample A, B, result is above soil changes and deposit standard sample.Therefore, sludge standard sample made from this method is more suitable for carrying out the quality control of inorganic matter monitoring in urban sewage treatment plant sludge and cities and towns disposition sludge.By preparing special sludge standard items, makes measurement result more accurate in the quality control procedure of sludge, facilitate the treatment process for accurately instructing sludge, conducive to the later period harmless treatment of sludge.
Description
Technical field
The present invention relates to city sludge process field, the preparation of inorganic constituents standard sample in city sludge is particularly related to
Method and standard sample obtained.
Background technique
With the continuous improvement of china's urbanization, sewage treatment facility builds high speed development, by 2010, cities and towns were dirty
Water treatment capacity has reached 1.22 hundred million m3, urban wastewater treatment firm will also increase sewage up to more than 2600 during " 12th Five-Year Plan "
90,000,000 m of processing capacity3, increase and build and building urban wastewater treatment firm up to more than 1800, to realize national emission reduction targets and pollution
Control, is made that tremendous contribution.
But the construction of sewage treatment plant puts into operation along with a large amount of excess sludge of generation, in terms of moisture content 80%, the whole nation
Year, sludge total output was quickly by 30,000,000 t of breakthrough.According to prediction, 60,000,000 t of year will be broken through to the year two thousand twenty sludge yield.
The sludge of urban wastewater treatment firm is the by-product of sewage treatment, be it is a kind of by organic debris, it is microorganism, inorganic
The extremely complex heterogeneous body of the compositions such as particle, colloid is the depots and most after all of domestic pollutant, industrial pollutants etc.
One of place.
With increasing year by year for China's treatment of town sewage and sludge quantum of output and sewage treatment plant, and domestic lack preferably dirt
Mud disposal technology, the odor pollution air for causing sludge to distribute, pathogen generate potential threat to human health.An especially huge sum of money
Belong to, such as Cr, As, Hg, Ba and Be, is easy polluted surface and ground water regime.The processing of sludge is disposed and its innoxious, as
Regenerated resources efficiently use the great attention for having caused the Chinese government.Therefore, it the monitoring for inorganic content in sludge and grinds
Studying carefully also is particularly important.
Accurately and reliably analysis test data be sludge processing disposition and its it is innoxious and effectively sharp as regenerated resources
Basis, and standard sample is Good Laboratory control and the essential etalon of environmental monitoring.Currently, both at home and abroad still
There is not the sludge standard sample for monitoring city sludge indices.
The sludge in China monitors and mainly uses soil or the progress quality control of deposit standard sample, and these standard samples
The concentration level and matrix properties of definite value component and real monitoring requirements have certain gap, and therefore, there is an urgent need to develop suitable city
Standard sample required for the monitoring quality of inorganic matter controls in town sludge of sewage treatment plant and cities and towns disposition sludge.
Summary of the invention
In view of the above deficiencies, the purpose of the present invention is to provide the preparations of inorganic constituents standard sample in city sludge
Method and standard sample obtained.
To achieve the above object, technical program of the present invention lies in the preparations of inorganic constituents standard sample in city sludge
Method includes the following steps:
(1) sample is acquired: the acquisition dewatered sludge of urban wastewater treatment firm；
(2) Preliminary Determination: the content of every inorganic matter in sludge is measured respectively；
(3) it impregnates: according to the concentration of required sample to be prepared, configuring the standard solution of respective concentration as soak,
Mud sample is placed in clean container, soak is uniformly added, at room temperature, stirred mud sample repeatedly every 2~3 hours
Sample is taken out after 1 time, 48 hours, it is spare；
(4) it mixes: by the mud sample of acquisition, by blender, being stirred, mixed repeatedly；
(5) it air-dries: mixed sludge is divided at aeration-drying, carry out natural air drying；
(6) it dries: will air-dry in the drying box for being placed in 40-60 DEG C to the mud sample of leather hard that be dried to its aqueous
Rate ﹤ 5%；
(7) secondary mixing: the sample after drying is slowly fallen down to a central point, a conical sample heap is formed, by this
Sample is successively shoveled pick-and-place another central point nearby from two relative positions at cone bottom in the same direction by sample heap, and is piled new
Conical sample heap, be so repeated several times, by sample blending；
(8) it grinds and sieves: the sample after mixing being ground with fast-holding sample pulverizer, the sample after grinding
Pass through the standard screen of 80M；
(9) it mixes three times: the sample after sieving is mixed in mixing machine；
(10) it bottles: the sample after mixing is sub-packed in in inner sealing lid, clean sample bottle；
(11) uniformity initial survey: randomly selecting 10 bottles of samples, and inductively coupled plasma body is sent out after being cleared up using microwave high pressure
The multinomial inorganic content of spectrographic determination is penetrated, every bottle of sample of each index is measured in parallel 10 times, and relative standard deviation is taken to be less than
The sample of 5.0% uniformity initial survey qualification, standby inspection；
(12) sample of uniformity initial survey qualification is subjected to uniformity testing, stability test, definite value again and is not known
The evaluation process of degree, to carry out definite value calibration to mud sample.
Preferably: the process of the uniformity testing are as follows: random synchronism 3 groups of samples of extraction, every group 2O bottles, by every group of sample
Product are distributed to 3 different testing laboratories, and every bottle of sample extracts 3 increments, and each increment is individually carried out constituent analysis,
Inspection result is carried out to the calculating of uncertainty according to one-way analysis of variance method.
Preferably: the process of the stability test are as follows: 1 month, 3 months, 6 months, 9 months, l2 after packing
Stability is carried out respectively at a month, 18 months, 24 months, 30 months, 36 months, 42 months, 48 months, 54 months and 60 months
It examines, each time point randomly selects 3 bottles of samples, and 2 Parallel testings of every bottle of work are made with the grand mean of 3 bottles of sample detection results
For the time point stability test as a result, inspection result is carried out estimation of stability according to unitary linear fit model, length is calculated
Phase unstability partial uncertainty.
Preferably: the definite value process are as follows: use 10 laboratories, each laboratory is to the 10 bottles of samples randomly selected
Product carry out definite value, and every bottle measures 10 times, its arithmetic average is taken to represent a data, and each laboratory provides 10 data, adopts
With croup, this method tests to the consistency of every group of determination data；Each group is surveyed using Dixon criterion and Cochran criterion
Fixed number consistency of average value and variance between is tested, to pick out the overall average of exceptional value as standard value.
Preferably: the calculation method of the uncertainty evaluation are as follows:
Wherein, ucharFor the uncertainty of cooperation measurement；ubbThe partial uncertainty of inhomogeneities between bottle；ultsFor length
Phase instable partial uncertainty；S is grand mean standard deviation；P is the valid data group number for participating in statistics.
Preferably: the uncertainty is expanded uncertainty UCRM, spreading factor k is equal to 2, UCRM=2 × uc。
The present invention also provides a kind of standard samples measured for inorganic content in city sludge, using as described above
Method is made.
The present invention also provides a kind of applications of standard sample made from method as described above, for measuring in city sludge
Total alkalinity, total zinc, total copper, total lead, total nickel, total cadmium, total boron, total potassium, total phosphorus, total nitrogen content.
The beneficial effects of the present invention are:
(1) sludge of sewage treatment plant's output by Preliminary Determination, immersion, mixing, drying, is ground up, sieved, mixes, fills
After bottle, uniformity initial survey, uniformity testing, stability test, cooperation definite value and uncertainty evaluation, it can be used as sludge and analyzed
The standard sample of journey.
(2) sludge standard items obtained through the invention, by carrying out mark-on reclaims to mud sample A, B, result is equal
Higher than soil changes and deposit standard sample.Therefore, sludge standard sample made from this method is more suitable for carrying out cities and towns
The quality control of inorganic content monitoring in sludge of sewage treatment plant and cities and towns disposition sludge.
(3) by preparing special sludge standard items, sludge quality control procedure make measurement result more subject to
Really, facilitate the treatment process for accurately instructing sludge, conducive to the later period harmless treatment of sludge.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
The preparation method of inorganic constituents standard sample, includes the following steps: in city sludge
(1) sample is acquired: the acquisition dewatered sludge of urban wastewater treatment firm；
(2) Preliminary Determination: the content of every inorganic matter in sludge is measured respectively；Each component contains in Preliminary Determination sludge
Amount, is in order to avoid since certain component content is too low, that is, when being near or below minimum detectability, being not used as standard sample；
(3) it impregnates: according to the concentration of required sample to be prepared, configuring the standard solution of respective concentration as soak,
Mud sample is placed in clean container, soak is uniformly added, at room temperature, stirred mud sample repeatedly every 2~3 hours
Sample is taken out after 1 time, 48 hours, it is spare；By impregnating the standard solution of various concentration, various concentration gradient can be prepared
Standard sample, only need to can be obtained the standard sample of a variety of concentration gradients by once sampling preparation process in this way, can be with
The detection of sludge applied to different condition, it is pervasive strong, save operational sequence；
(4) it mixes: by the mud sample of acquisition, by blender, being stirred, mixed repeatedly；Wet mud sample is use up
It may mix, the uniformity of the standard sample finally to prepare lays the foundation；
(5) it air-dries: mixed sludge is divided at aeration-drying, carry out natural air drying；The mud sample one of acquisition
As moisture content be 60-80%, sample is tentatively dried, until moisture content 20% or so；It is dried convenient for being transferred in drying box in next step
It is dry；
(6) it dries: will air-dry in the drying box for being placed in 40-60 DEG C to the mud sample of leather hard that be dried to its aqueous
Rate ﹤ 5%；
(7) secondary mixing: the sample after drying is slowly fallen down to a central point, a conical sample heap is formed, by this
Sample is successively shoveled pick-and-place another central point nearby from two relative positions at cone bottom in the same direction by sample heap, and is piled new
Conical sample heap, be so repeated several times, by sample blending；Generally mixing with 3-4 times is advisable；
(8) it grinds and sieves: the sample after mixing being ground with fast-holding sample pulverizer, the sample after grinding
Pass through the standard screen of 80M；
(9) it mixes three times: the sample after sieving is mixed in mixing machine；By repeatedly mixing, so that later period definite value mistake
Error is reduced in journey；
(10) it bottles: sample after mixing is sub-packed in in inner sealing lid, clean sample bottle；
(11) uniformity initial survey: randomly selecting 10 bottles of samples, and inductively coupled plasma body is sent out after being cleared up using microwave high pressure
The multinomial inorganic content of spectrographic determination is penetrated, every bottle of sample of each index is measured in parallel 10 times, and relative standard deviation is taken to be less than
The sample of 5.0% uniformity initial survey qualification, standby inspection；Since uniformity initial survey is only intended to select the preferable sample of the uniformity,
Therefore do not have to detect each constituent content, and select several constituent contents and detected, both can guarantee sample
The requirement stable for uniformity, and save the time of detection；
(12) sample of uniformity initial survey qualification is subjected to uniformity testing, stability test, definite value again and is not known
Evaluation process is spent, to carry out definite value calibration to mud sample.
Wherein, the process of uniformity testing are as follows: random synchronism extracts 3 groups of samples, every group 20 bottles, every group of sample is distributed to
3 different testing laboratories, every bottle of sample extract 3 increments, and each increment is individually carried out constituent analysis, tie examining
Fruit carries out the calculating of uncertainty according to one-way analysis of variance method.
The process of stability test are as follows: 1 month after packing, 6 months, l2 months, 18 months, 24 months, 30 months,
Stability test is carried out at 36 months, 42 months, 48 months, 54 months and 60 months respectively, each time point randomly selects 3 bottles
Sample, 2 Parallel testings of every bottle of work as a result, will using the grand mean of 3 bottles of sample detection results as the time point stability test
Inspection result carries out estimation of stability according to unitary linear fit model, calculates secular instability partial uncertainty.
Definite value process are as follows: use 10 laboratories, each laboratory carries out definite value to 10 bottles of samples randomly selecting, and every bottle
Measurement 10 times takes its arithmetic average to represent a data, and each laboratory provides 10 data, using croup this method to every
The consistency of group determination data is tested；Using Dixon criterion and Cochran criterion to average value between each group determination data
It tests with the consistency of variance, to pick out the overall average of exceptional value as standard value.
Wherein, the calculation method of uncertainty evaluation are as follows:
Wherein, ucharFor the uncertainty of cooperation measurement；ubbThe partial uncertainty of inhomogeneities between bottle；ultsFor length
Phase instable partial uncertainty；S is grand mean standard deviation；P is the valid data group number for participating in statistics.
Final definite value result is provided with standard value and uncertainty.Standard value is to pick out the overall average of exceptional value as mark
Quasi- value.
Uncertainty is expanded uncertainty UCRM, spreading factor k is equal to 2, UCRM=2 × uc。
A kind of standard sample measured for inorganic content in city sludge, is made using foregoing method.
The application of standard sample made from a kind of foregoing method, for measuring the total alkalinity in city sludge, total
Zinc, total copper, total lead, total nickel, total cadmium, total boron, total potassium, total phosphorus, total nitrogen content.
Sludge standard items made from sludge to the acquisition of certain sewage treatment plant, Qingdao City carry out the result of definite value referring to table
1。
1 city sludge standard sample definite value result (unit: mg/kg) of table
For sludge standard items made from this method and soil changes and deposit standard sample, which kind of standard items verified
It is more suitable for carrying out the quality control of mud sample, it is special to select two sludge samples of sewage treatment plant, Qingdao City A and B on July 4th, 2016
Product carry out mark-on reclaims test with soil changes, deposit standard sample and sludge standard sample respectively, and detection project is
Cr, Ba, Hg, As and Be, Cr, Ba, Be use inductively coupled plasma emission spectrography after micro-wave digestion, Hg and As using micro-
Atomic fluorescence method after wave resolution.Each sample mark-on 8 times, obtaining recovery of standard addition, the results are shown in Table 2.
2 recovery of standard addition result of table compares
As can be seen from Table 2, sludge standard sample carries out mark-on reclaims result to mud sample A, B and is above Soil standard
Sample and deposit standard sample.Therefore, the sludge standard sample as made from this method is more suitable for carrying out urban wastewater treatment
The quality control of Cr, Ba, Hg, As and Be monitoring in factory's sludge and cities and towns disposition sludge.
Due to production sludge standard items mud sample can according to the difference of sample and definite value the result is that different,
It is required to carry out definite value to it when production sludge standard items every time, the quality that can be only used for daily sludge controls and other
Purposes.
Claims (8)
1. the preparation method of inorganic constituents standard sample in city sludge, characterized by the following steps:
(1) sample is acquired: the acquisition dewatered sludge of urban wastewater treatment firm；
(2) Preliminary Determination: the content of every inorganic matter in sludge is measured respectively；
(3) it impregnates: according to the concentration of required sample to be prepared, configuring the standard solution of respective concentration as soak, it will be dirty
Mud sample product are placed in clean container, and soak is uniformly added, and at room temperature, are stirred mud sample 1 time repeatedly every 2~3 hours,
Sample is taken out after 48 hours, it is spare；
(4) it mixes: by the mud sample of acquisition, by blender, being stirred, mixed repeatedly；
(5) it air-dries: mixed sludge is divided at aeration-drying, carry out natural air drying；
(6) it dries: will air-dry in the drying box for being placed in 40-60 DEG C to the mud sample of leather hard and be dried to its moisture content ﹤
5%；
(7) secondary mixing: the sample after drying is slowly fallen down to a central point, a conical sample heap is formed, by this sample
Sample is successively shoveled pick-and-place another central point nearby from two relative positions at cone bottom in the same direction by heap, and piles new circle
Taper sample heap, is so repeated several times, by sample blending；
(8) it grinds and sieves: the sample after mixing being ground with fast-holding sample pulverizer, the sample after grinding passes through
The standard screen of 80M；
(9) it mixes three times: the sample after sieving is mixed in mixing machine；
(10) it bottles: sample after mixing is sub-packed in in inner sealing lid, clean sample bottle；
(11) uniformity initial survey: randomly selecting 10 bottles of samples, and inductively coupled plasma body emits light after being cleared up using microwave high pressure
Spectrometry measures the content of multinomial inorganic matter, and every bottle of sample of each index is measured in parallel 10 times, takes relative standard deviation less than 5.0%
Uniformity initial survey qualification sample, standby inspection；
(12) sample of uniformity initial survey qualification uniformity testing, stability test, definite value and uncertainty is carried out again to comment
The process estimated, to carry out definite value calibration to mud sample.
2. the preparation method of inorganic constituents standard sample in city sludge according to claim 1, it is characterised in that: described
The process of uniformity testing are as follows: random synchronism extracts 3 groups of samples, and every group 20 bottles, every group of sample is distributed to 3 different detections
Laboratory, every bottle of sample extract 3 increments, and each increment is individually carried out constituent analysis, by inspection result according to single factor test
The calculating of method of analysis of variance progress uncertainty.
3. the preparation method of inorganic constituents standard sample in city sludge according to claim 1, it is characterised in that: described
The process of stability test are as follows: 1 month, 3 months, 6 months, 9 months, l2 months, 18 months, 24 months, 30 after packing
Stability test is carried out respectively at a month, 36 months, 42 months, 48 months, 54 months and 60 months, and each time point is taken out at random
Take 3 bottles of samples, 2 Parallel testings of every bottle of work, using the grand mean of 3 bottles of sample detection results as the time point stability test knot
Inspection result is carried out estimation of stability according to unitary linear fit model, calculates secular instability partial uncertainty by fruit.
4. the preparation method of inorganic constituents standard sample in city sludge according to claim 1, it is characterised in that: described
Definite value process are as follows: use 10 laboratories, each laboratory carries out definite value, every bottle of measurement 10 to 10 bottles of samples randomly selecting
It is secondary, take its arithmetic average to represent a data, each laboratory provides 10 data, using this method of croup to every group of measurement
The consistency of data is tested；Using Dixon criterion and Cochran criterion to average value and variance between each group determination data
Consistency test, to pick out the overall average of exceptional value as standard value.
5. the preparation method of inorganic constituents standard sample in city sludge according to claim 1, it is characterised in that: described
The calculation method of uncertainty evaluation are as follows:
Wherein, ucharFor the uncertainty of cooperation measurement；ubbThe partial uncertainty of inhomogeneities between bottle；ultsFor for a long time not
The partial uncertainty of stability；S is grand mean standard deviation；P is the valid data group number for participating in statistics.
6. according to claim 1 or 5 in city sludge inorganic constituents standard sample preparation method, it is characterised in that:
The uncertainty is expanded uncertainty UCRM, spreading factor k is equal to 2, UCRM=2 × uc。
7. a kind of standard sample measured for inorganic content in city sludge, it is characterised in that: using such as claim 1 institute
The method stated is made.
8. a kind of application of standard sample made from the method as described in claim 1, it is characterised in that: for measuring cities and towns dirt
Total alkalinity, total zinc in mud, total copper, total lead, total nickel, total cadmium, total boron, total potassium, total phosphorus, total nitrogen content.
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| CN110736800A (en) * | 2019-11-07 | 2020-01-31 | 济南海关技术中心 | pentachlorophenol standard sample in soil and preparation method thereof |
| RU2731696C1 (en) * | 2020-03-18 | 2020-09-08 | Общество с ограниченной ответственностью «Научно-производственное объединение «Метрология» | Method for production of standard sample of mass fraction of heavy metals in agricultural products |
| RU2753971C1 (en) * | 2020-09-10 | 2021-08-25 | Общество с ограниченной ответственностью "Научно-производственное объединение "Метрология" | Method for producing a standard sample of the mass fraction of heavy metals in food products |
| CN112394123A (en) * | 2021-01-21 | 2021-02-23 | 中国农业科学院农业环境与可持续发展研究所 | Preparation method of deposit dioxin standard substance |
| CN113405876B (en) * | 2021-07-15 | 2022-10-18 | 陈传禄 | Automatic batch processing and analyzing device for hexavalent chromium in solution |
| CN113960287A (en) * | 2021-10-22 | 2022-01-21 | 中国地质科学院地球物理地球化学勘查研究所 | Uncertainty determination method and system for undetected elements of uniformity of geological standard substance |
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