CN106680052A - Preparation method of standard sample for inorganic components in urban sludge and standard sample prepared thereby - Google Patents
Preparation method of standard sample for inorganic components in urban sludge and standard sample prepared thereby Download PDFInfo
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- CN106680052A CN106680052A CN201611270474.3A CN201611270474A CN106680052A CN 106680052 A CN106680052 A CN 106680052A CN 201611270474 A CN201611270474 A CN 201611270474A CN 106680052 A CN106680052 A CN 106680052A
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- 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
- G01N2001/2893—Preparing calibration standards
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Abstract
The invention relates to a preparation method of a standard sample for inorganic components in urban sludge; the method comprises the steps of acquiring a sample; measuring preliminarily; soaking; mixing well; air-drying; drying by baking; mixing well for the second time, to be specific, mixing well again by means of pile shifting method; grinding, and screening; mixing well for the third time; primarily inspecting uniformity; subjecting the sample passing the primary inspection of uniformity to uniformity inspection, stability inspection, and fixed value and uncertainty estimation again so as to perform fixed value calibration on the sludge sample. According to the standard sample for inorganic matters in urban sludge prepared herein, results of standard recovery for sludge samples A and B are better than the results of both a soil standard sample and a precipitate standard sample. Therefore, the standard sample of sludge prepared by using the method is more suitable for the quality control in monitoring inorganic matters in sludge from urban sewage treatment plants and urban disposed sludge; by preparing the special standard sample of sludge, measurement results for sludge quality control process are more accurate, a sludge treatment process can be accurately guided, and late harmless treatment of sludge is facilitated.
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 obtained standard sample.
Background technology
As China's level of urbanization is improved constantly, sewage treatment facility builds high speed development, and by 2010, cities and towns were dirty
Water treatment capacity has reached 1.22 hundred million m3, up to more than 2600, " 12 " period will also increase sewage to urban wastewater treatment firm
The m of disposal ability 90,000,0003, increasing is built and is 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 substantial amounts of excess sludge is produced, 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, the t of year 60000000 will be broken through to the year two thousand twenty sludge yield.
The sludge of urban wastewater treatment firm is the accessory substance of sewage disposal, 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, causes the odor pollution air that sludge is distributed, and pathogen produces potential threat to human health.Especially with much money
Category, such as Cr, As, Hg, Ba and Be, easy polluted surface and ground water regime.The treatment of sludge is disposed and its innoxious, as
Regenerated resources are effectively using the great attention for having caused the Chinese government.Therefore, monitoring for inorganic content in sludge and grind
Study carefully and be also particularly important.
Accurately and reliably analyzing test data be sludge treatment disposal 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.At present, both at home and abroad still
There is not the sludge standard sample for monitoring city sludge indices.
The sludge monitoring of China is main to carry out quality control using soil or deposit standard sample, and these standard samples
The concentration level and matrix properties of definite value component have certain gap with real monitoring requirements, therefore, it is adapted to city in the urgent need to developing
Standard sample in town sludge of sewage treatment plant and cities and towns disposing sludge required for the monitoring quality control of inorganic matter.
The content of the invention
According to above-mentioned weak point, it is an object of the invention to provide the preparation of inorganic constituents standard sample in city sludge
Method and obtained standard sample.
To achieve the above object, technical program of the present invention lies in:The preparation of inorganic constituents standard sample in city sludge
Method, comprises the following steps:
(1) sample is gathered:Sludge after collection urban wastewater treatment firm dehydration;
(2) Preliminary Determination:The content of every inorganic matter in sludge is determined respectively;
(3) soak:The concentration of the sample according to required preparation, configures the standard liquid of respective concentration as soak,
Mud sample is placed in clean container, soak is uniformly added, at room temperature, mud sample was stirred repeatedly every 2~3 hours
1 time, sample is taken out after 48 hours, it is standby;
(4) mix:The mud sample that will be gathered, by mixer, is stirred, is mixed repeatedly;
(5) air-dry:Mixed sludge is divided at aeration-drying, carry out natural air drying;
(6) dry:To air-dry to the mud sample of leather hard, be placed in 40-60 DEG C of drying box dry it is aqueous to its
Rate ﹤ 5%;
(7) secondary mixing:Sample after drying is slowly fallen down to a central point, a conical sample heap is formed, by this
Sample is shoveled and picks and places another central point nearby by two relative positions of the sample heap in the same direction from cone bottom successively, is piled again new
Conical sample heap, be so repeated several times, by sample blending;
(8) grind and sieve:Sample fast-holding sample pulverizer after mixing is ground, the sample after grinding
By the standard screen of 80M;
(9) three mixings:Sample after sieving is mixed in mixing machine;
(10) bottle:Sample after mixing is sub-packed in in inner sealing lid, clean sample bottle;
(11) uniformity initial survey:10 bottles of samples are randomly selected, rear inductively coupled plasma is cleared up using microwave high pressure and is sent out
The multinomial inorganic content of spectrographic determination is penetrated, the sample parallel determination 10 times of every bottle of each index takes relative standard deviation and is less than
The qualified sample of 5.0% uniformity initial survey, standby inspection;
(12) the qualified sample of uniformity initial survey is carried out into uniformity testing, stability test, definite value again and is not known
The evaluation process of degree, definite value demarcation is carried out with to mud sample.
Preferably:The process of the uniformity testing is: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 respectively extracts 3 increments, each increment is individually carried out into constituent analysis,
Assay is carried out the calculating of uncertainty according to one-way analysis of variance method.
Preferably:The process of the stability test is:1 month, 3 months, 6 months, 9 months, l2 after packing
Stability is carried out respectively at individual month, 18 months, 24 months, 30 months, 36 months, 42 months, 48 months, 54 months and 60 months
Inspection, each time point randomly selects 3 bottles of samples, and 2 Parallel testings of every bottle of work are made with 3 bottles of grand means of sample detection result
It is the time point stability test result, assay is carried out into estimation of stability according to unitary linear fit model, calculates length
Phase unstability partial uncertainty.
Preferably:Described definite value process is:Using 10 laboratories, each laboratory is to 10 bottles of samples randomly selecting
Product carry out definite value, and every bottle determines 10 times, take its arithmetic average and represent a data, and each laboratory provides 10 data, adopts
With croup, this method is tested to the uniformity of every group of determination data;Each group is surveyed using Dixon criterions and Cochran criterions
Fixed number uniformity of average value and variance between is tested, and is standard value with the overall average for picking out exceptional value.
Preferably:The computational methods of the uncertainty evaluation are:
Wherein, ucharFor the uncertainty that cooperation is determined;ubbIt is the partial uncertainty of inhomogeneities between bottle;ultsIt is length
Phase instable partial uncertainty;S is grand mean standard deviation;P is the valid data group number for participating in statistics.
Preferably:Described uncertainty is expanded uncertainty UCRM, spreading factor k is equal to 2, UCRM=2 × uc。
The present invention also provides a kind of standard sample determined for inorganic content in city sludge, using as described above
Method is obtained.
The present invention also provides a kind of application of standard sample obtained in method as described above, for determining city sludge in
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, grinding, sieving, mixing, dress
After bottle, uniformity initial survey, uniformity testing, stability test, cooperation definite value and uncertainty evaluation, can be analyzed as sludge
The standard sample of journey.
(2) by sludge standard items obtained in the present invention, mark-on reclaims are carried out by mud sample A, B, its result is equal
Higher than soil changes and deposit standard sample.Therefore, sludge standard sample obtained in 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 disposing sludge.
(3) by preparing special sludge standard items, cause that measurement result is more defined in the quality control procedure of sludge
Really, contribute to accurately to instruct the processing procedure of sludge, beneficial to the later stage harmless treatment of sludge.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
The preparation method of inorganic constituents standard sample, comprises the following steps in city sludge:
(1) sample is gathered:Sludge after collection urban wastewater treatment firm dehydration;
(2) Preliminary Determination:The content of every inorganic matter in sludge is determined respectively;Each component contains in Preliminary Determination sludge
Amount, is in order to avoid because certain component content is too low, that is, when being near or below minimum detectability, it is impossible to as standard sample;
(3) soak:The concentration of the sample according to required preparation, configures the standard liquid of respective concentration as soak,
Mud sample is placed in clean container, soak is uniformly added, at room temperature, mud sample was stirred repeatedly every 2~3 hours
1 time, sample is taken out after 48 hours, it is standby;By soaking the standard liquid of various concentrations, various concentrations gradient can be prepared
Standard sample, so only need by preparation process of once sampling, you can obtain the standard sample of various concentration gradients, can be with
The detection of the sludge of different condition is applied to, it is pervasive strong, save operational sequence;
(4) mix:The mud sample that will be gathered, by mixer, is stirred, is mixed repeatedly;Wet mud sample is use up
May mix, be that the uniformity of the final standard sample for preparing lays the foundation;
(5) air-dry:Mixed sludge is divided at aeration-drying, carry out natural air drying;The mud sample one of collection
As moisture content be 60-80%, sample is tentatively dried, to moisture content 20% or so;It is easy to next step to be transferred in drying box to dry
It is dry;
(6) dry:To air-dry to the mud sample of leather hard, be placed in 40-60 DEG C of drying box dry it is aqueous to its
Rate ﹤ 5%;
(7) secondary mixing:Sample after drying is slowly fallen down to a central point, a conical sample heap is formed, by this
Sample is shoveled and picks and places another central point nearby by two relative positions of the sample heap in the same direction from cone bottom successively, is piled again new
Conical sample heap, be so repeated several times, by sample blending;3-4 times is generally mixed with to be advisable;
(8) grind and sieve:Sample fast-holding sample pulverizer after mixing is ground, the sample after grinding
By the standard screen of 80M;
(9) three mixings:Sample after sieving is mixed in mixing machine;By repeatedly mixing so that later stage definite value mistake
Error is reduced in journey;
(10) bottle:Sample after mixing is sub-packed in in inner sealing lid, clean sample bottle;
(11) uniformity initial survey:10 bottles of samples are randomly selected, rear inductively coupled plasma is cleared up using microwave high pressure and is sent out
The multinomial inorganic content of spectrographic determination is penetrated, the sample parallel determination 10 times of every bottle of each index takes relative standard deviation and is less than
The qualified sample of 5.0% uniformity initial survey, standby inspection;Because uniformity initial survey is only intended to select the preferable sample of the uniformity,
Therefore detected without to each constituent content, and select several constituent contents and detected, both can guarantee that sample
For the requirement of uniformity stabilization, the time of detection is saved again;
(12) the qualified sample of uniformity initial survey is carried out into uniformity testing, stability test, definite value again and is not known
Degree evaluation process, definite value demarcation is carried out with to mud sample.
Wherein, the process of uniformity testing is: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 respectively extracts 3 increments, and each increment is individually carried out into constituent analysis, and inspection is tied
Fruit carries out the calculating of uncertainty according to one-way analysis of variance method.
The process of stability test is:1 month after packing, 6 months, l2 month, 18 months, 24 months, 30 months,
Stability test is carried out respectively at 36 months, 42 months, 48 months, 54 months and 60 months, and each time point randomly selects 3 bottles
Sample, 2 Parallel testings of every bottle of work, using 3 bottles of grand means of sample detection result as the time point stability test result, will
Assay carries out estimation of stability according to unitary linear fit model, calculates secular instability partial uncertainty.
Definite value process is:Using 10 laboratories, each laboratory carries out definite value, every bottle to the 10 bottles of samples randomly selected
Determine 10 times, take its arithmetic average and represent a data, each laboratory provides 10 data, using croup this method to every
The uniformity of group determination data is tested;Using Dixon criterions and Cochran criterions to average value between each group determination data
Uniformity with variance is tested, and is standard value with the overall average for picking out exceptional value.
Wherein, the computational methods of uncertainty evaluation are:
Wherein, ucharFor the uncertainty that cooperation is determined;ubbIt is the partial uncertainty of inhomogeneities between bottle;ultsIt is 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 given with standard value and uncertainty.Standard value is mark to pick out the overall average of exceptional value
Quasi- value.
Uncertainty is expanded uncertainty UCRM, spreading factor k is equal to 2, UCRM=2 × uc。
A kind of standard sample determined for inorganic content in city sludge, is obtained using method as described before.
The application of standard sample obtained in a kind of method as described before, for determining 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 obtained in the sludge gathered to certain sewage treatment plant of Qingdao City carry out the result of definite value referring to table
1。
The city sludge standard sample definite value result (unit of table 1:mg/kg)
Sludge standard items and soil changes and deposit standard sample, which kind of standard items obtained in checking this method
It is more suitable for carrying out the quality control of mud sample, it is special to select the two sludge samples of sewage treatment plant of Qingdao City A and B of on July 4th, 2016
Product, carry out mark-on reclaims experiment with soil changes, deposit standard sample and sludge standard sample respectively, and detection project is
Cr, Ba, Hg, As and Be, using inductively coupled plasma emission spectrography after micro-wave digestion, Hg and As is using micro- for Cr, Ba, Be
Ripple clears up rear atomic fluorescence method.Each sample mark-on 8 times, obtains recovery of standard addition result as shown in table 2.
The recovery of standard addition result of table 2 is compared
As can be seen from Table 2, sludge standard sample carries out mark-on reclaims result and is above Soil standard to mud sample A, B
Sample and deposit standard sample.Therefore, it is more suitable for carrying out urban wastewater treatment by sludge standard sample obtained in this method
The quality control of Cr, Ba, Hg, As and Be monitoring in factory's sludge and cities and towns disposing sludge.
Due to make sludge standard items mud sample can according to sample difference and definite value result is different, therefore,
Every time make sludge standard items when be required to carry out definite value to it, can be only used for daily sludge quality control and other
Purposes.
Claims (8)
1. in city sludge inorganic constituents standard sample preparation method, it is characterised in that:Comprise the following steps:
(1) sample is gathered:Sludge after collection urban wastewater treatment firm dehydration;
(2) Preliminary Determination:The content of every inorganic matter in sludge is determined respectively;
(3) soak:The concentration of the sample according to required preparation, configures the standard liquid of respective concentration as soak, by dirt
Mud sample is placed in clean container, uniformly adds soak, at room temperature, stirring mud sample 1 time repeatedly every 2~3 hours,
Sample is taken out after 48 hours, it is standby;
(4) mix:The mud sample that will be gathered, by mixer, is stirred, is mixed repeatedly;
(5) air-dry:Mixed sludge is divided at aeration-drying, carry out natural air drying;
(6) dry:To air-dry to the mud sample of leather hard, be placed in 40-60 DEG C of drying box and dry to its moisture content ﹤
5%;
(7) secondary mixing:Sample after drying is slowly fallen down to a central point, a conical sample heap is formed, by this sample
Sample is shoveled and picks and places another central point nearby by two relative positions of the heap in the same direction from cone bottom successively, and new circle is piled again
Taper sample heap, is so repeated several times, by sample blending;
(8) grind and sieve:Sample fast-holding sample pulverizer after mixing is ground, the sample after grinding passes through
The standard screen of 80M;
(9) three mixings:Sample after sieving is mixed in mixing machine;
(10) bottle:Sample after mixing is sub-packed in in inner sealing lid, clean sample bottle;
(11) uniformity initial survey:10 bottles of samples are randomly selected, rear inductively coupled plasma launching light is cleared up using microwave high pressure
Spectrometry determines the content of multinomial inorganic matter, and the sample parallel determination 10 times of every bottle of each index takes relative standard deviation less than 5.0%
The qualified sample of uniformity initial survey, standby inspection;
(12) the qualified sample of uniformity initial survey is carried out into uniformity testing, stability test, definite value and uncertainty again to comment
The process estimated, definite value demarcation is carried out with to mud sample.
2. in city sludge according to claim 1 inorganic constituents standard sample preparation method, it is characterised in that:It is described
The process of uniformity testing is:Random synchronism extracts 3 groups of samples, every group 2O bottles, every group of sample is distributed into 3 different detections
Laboratory, every bottle of sample respectively extracts 3 increments, and each increment is individually carried out into constituent analysis, by assay according to single factor test
Method of analysis of variance carries out the calculating of uncertainty.
3. in city sludge according to claim 1 inorganic constituents standard sample preparation method, it is characterised in that:It is described
The process of stability test is:1 month after packing, 3 months, 6 months, 9 months, l2 month, 18 months, 24 months, 30
Stability test is carried out respectively at individual month, 36 months, 42 months, 48 months, 54 months and 60 months, and each time point takes out at random
Take 3 bottles of samples, 2 Parallel testings of every bottle of work, using 3 bottles of grand means of sample detection result as the time point stability test knot
Really, assay is carried out into estimation of stability according to unitary linear fit model, calculates secular instability partial uncertainty.
4. in city sludge according to claim 1 inorganic constituents standard sample preparation method, it is characterised in that:It is described
Definite value process be:Using 10 laboratories, each laboratory carries out definite value to the 10 bottles of samples randomly selected, and every bottle determines 10
It is secondary, take its arithmetic average and represent a data, each laboratory provides 10 data, using this method of croup to every group of measure
The uniformity of data is tested;Using Dixon criterions and Cochran criterions to average value and variance between each group determination data
Uniformity test, be standard value with the overall average for picking out exceptional value.
5. in city sludge according to claim 1 inorganic constituents standard sample preparation method, it is characterised in that:It is described
The computational methods of uncertainty evaluation are:
Wherein, ucharFor the uncertainty that cooperation is determined;ubbIt is the 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:
Described uncertainty is expanded uncertainty UCRM, spreading factor k is equal to 2, UCRM=2 × uc。
7. it is a kind of in city sludge inorganic content determine standard sample, it is characterised in that:Using such as claim 1 institute
The method stated is obtained.
8. the application of standard sample obtained in a kind of the method for claim 1, it is characterised in that:It is dirty for determining cities and towns
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 |
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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 |
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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 |
CN113405876A (en) * | 2021-07-15 | 2021-09-17 | 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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