CN115524253A - Method for detecting content of water in solid waste of heavy metals such as copper and nickel - Google Patents
Method for detecting content of water in solid waste of heavy metals such as copper and nickel Download PDFInfo
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Abstract
The invention discloses a method for detecting the moisture content of heavy metal solid waste containing copper, nickel and the like, compared with the existing detection method, the method can greatly shorten the analysis and detection time, simplify the operation procedure, greatly reduce the energy consumption of steam, electricity and the like in a smelting production line and a raw material pretreatment stage for comprehensively recovering valuable metals by taking the heavy metal solid waste containing copper, nickel and the like with higher moisture content as raw materials, and better meet the requirements of central control detection analysis in the production process and serve for guiding production; meanwhile, the method has high detection precision, and improves the analysis efficiency while powerfully reducing the working strength of the laboratory staff.
Description
Technical Field
The invention belongs to the technical field of solid waste treatment, and particularly relates to a method for detecting the moisture content of heavy metal solid waste containing copper, nickel and the like.
Background
The national Standard on the determination of the Water and Dry matter content of solid waste (HJ 1222-2021) sets forth the scope of application of the test and the principles of the method, instruments and equipment, operating procedures, data processing, quality assurance and control, etc.
Before the standard is released, the moisture measurement in the solid waste (the sludge produced by precipitating or filter pressing the ash, the dust, the slag, the electroplating sludge, the industrial wastewater and the like) containing heavy metals such as copper, nickel, lead, zinc and the like does not form a uniform standard, the moisture content measurement in the actual operation process is carried out by referring to the standards of other industries, and most of the moisture content measurement are carried out by referring to the terms in the related standards of the moisture content measurement of iron ore, manganese ore and the like released in China.
The existing standard is compiled by using the relevant terms in the moisture content measurement standards of iron ore, manganese ore and the like, and the limitation in the application process is inevitable. Generally, the water content of iron ore and manganese ore is much lower than that of heavy metal solid waste containing copper, nickel and the like with higher water content, the sampling quantity difference of batch samples is very different, the former sample is weighed by tens of grams in the process of detecting and drying, the latter sample is weighed by at least 500 grams to ensure the accuracy of detecting the water content, and the actual operation process is controlled to be between 800 grams and 1000 grams. If only dozens of grams of heavy metal solid wastes containing copper, nickel and the like with higher moisture content are weighed in the sample detection drying process, the obtained moisture content data has larger difference from the actual data due to slight careless operation, large error and poor precision. Meanwhile, the requirements of the current standard on the corrosion resistance of detection instruments and equipment are not specified in detail, and the like. Under normal conditions, iron ore and manganese ore contain few, even trace and negligible corrosive substances such as acid and alkali; however, many types of hazardous wastes and solid wastes of heavy metals such as copper, nickel, lead, zinc and the like have high water content and contain a certain amount of acid radical ions (such as sulfate radicals, phosphate radicals, chloride radicals and the like), and the acid radical ions have certain corrosiveness to metal devices under certain conditions. The material requirements of the sample container in the standard only refer to that the sample container is waterproof and does not absorb moisture, and the aspects of acid corrosion resistance and the like are not described.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above problems and/or problems occurring in the prior art.
Therefore, the present invention is to provide a method for detecting the moisture content of heavy metal solid waste, such as copper and nickel, in order to overcome the disadvantages of the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the container is placed in an oven for drying, cooled and weighed to obtain a mass G1;
collecting a sample, placing the sample in a container, and weighing the total mass G2;
placing the container containing the sample in an oven for drying;
cooling and weighing the container and the total mass G3 of the sample after drying;
calculating the crude moisture content a of the sample;
and obtaining the final moisture content through data compensation and correction.
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: the container is a cover-free container, can resist water and medium and strong acid corrosion, and the thickness of the sample after being placed in the container and flattened is 1.5-2 cm.
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: and drying the container in an oven, wherein the drying temperature is 145-155 ℃, and the drying time is 5-10 min.
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: the mass of the sample is 800.0-1000.0 g.
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: and (3) drying the container containing the sample in an oven, wherein the drying temperature is 145-155 ℃, and the drying time is 4h.
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: the temperature rise rate of the oven is set within the range of 3-4 ℃/min.
As a preferable scheme of the method for detecting the moisture content of the solid waste water containing the heavy metals such as copper, nickel and the like, the method comprises the following steps: the crude moisture content of the sample is expressed as follows:
a＝(G3-G1)/G×100％
where a represents the crude moisture content of the sample, G represents the sample mass, and G = (G2-G1).
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: the final moisture content is expressed as follows:
W＝a+b
wherein W represents the final moisture content of the sample, a represents the crude moisture content of the sample, and b is a corrected value.
As a preferable scheme of the method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like, the method comprises the following steps: the difference between the moisture content data of the parallel samples measured by the method and the current standard method is not more than 2%.
The invention has the beneficial effects that:
(1) The method provided by the invention is simple to operate and short in detection time, the difference between the obtained water content detection result and the current national standard determination method is not more than 2.0% by improving the drying temperature, canceling the long-time constant-weight drying operation and correcting the water content result in a data compensation mode, the rapid central control analysis requirement in the production process can be met, and powerful data support is provided for efficiency improvement, yield increase, cost saving and consumption reduction.
(2) The water content data compensation correction table provided by the method is summarized based on long-time continuous analysis, tracking, improvement, comparison, correction, verification and the like of the determination working process of the water content of the copper-nickel-lead-zinc-containing heavy metal solid waste, has strong pertinence and good practicability for the detection of the water content of specific types of solid waste, can be used for supplementing or expanding the conventional determination standard of the water content of the solid waste, is suitable for the detection of the copper-nickel-containing heavy metal solid waste with low water content, and has more obvious detection effect on the high-water-content solid waste.
(3) The method of the invention puts clear requirements on the corrosion resistance of the detection instrument. The drying vessel for holding the sample to be detected adopts an enamel tray or a stainless steel tray which is resistant to high temperature and medium and strong acid and medium and strong alkali environments, thereby reducing or avoiding the pollution to the sample to the greatest extent so as to influence the precision of monitoring data and reduce errors.
(4) The method has certain reference and popularization values in the fields of solid waste recycling of heavy metals such as copper and nickel, pyrometallurgical smelting process, comprehensive recovery of valuable metals and the like, and has good development and application prospects.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The precision of the temperature control of the drying oven adopted in the embodiment of the invention is +/-1 ℃;
the container used in the embodiment of the invention has the length of 24 cm, the width of 16 cm and the depth of 3 cm;
the current standard determination method adopted in the invention is as follows: national Standard for determination of the Water and Dry matter content of solid waste (HJ 1222-2021);
table 1 is a moisture content data compensation correction table provided by the present invention.
The table is obtained by carrying out a large number of parallel tests, data comparative analysis, correction and verification summary on the table and the existing national standard detection method, wherein a in the table is the crude moisture content determined by the invention, and b is a correction value.
TABLE 1 data correction Compensation Table
Example 1
The embodiment provides a method for detecting the moisture content of solid waste of heavy metals such as copper and nickel.
Collecting samples strictly according to the HJ/T20 standard, immediately preparing the samples after collecting the samples, and measuring the moisture, wherein the mass unit adopted in the experiment is g, and the accuracy is 0.1g;
placing a waterproof and corrosion-resistant uncovered container with the length of 24 cm, the width of 16 cm and the depth of 3 cm in an oven, setting the heating rate of the oven to be 4 ℃/min, drying for 10min at the temperature of 150 ℃, taking out, cooling and weighing for later use, and marking as G1;
flatly paving a Gg solid waste sample in a dried and cooled container by using a sample spoon, wherein the thickness of the flatly paved sample is 1.5-2 cm, the total weight is weighed and recorded as G2, and the value range of G is 800.0-1000.0G;
placing the container containing the sample in an oven, and drying at 150 ℃ for 4h;
cooling and weighing the total mass of the sample and the container after drying, and marking as G3;
the crude moisture content a is calculated according to the following formula:
a＝(G3-G1)/G×100％
the final moisture content W, W = a + b, was calculated according to table 1.
Example 2
In this example, a sample having a moisture content in the range of 10 to 20% was measured;
according to the method, the sample of the embodiment is flatly paved in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content a =15.67% of the sample is calculated, and the compensation value b is corrected according to the table 1 to be 0.50%, so that the final moisture content W = a + b =16.17%;
the sample of this example was placed in a lidded container according to current standard assay methods, dried in an oven at 105 ℃ for 12 hours, weighed, and then dried continuously at intervals of 4 hours to constant weight, calculated to give a sample moisture content of 16.53%.
The difference between the method of the invention and the existing standard measuring method is 0.36 percent, and the result is credible within the error allowable range.
Example 3
In this example, a sample having a moisture content in the range of 10 to 20% was measured;
according to the method, the sample of the embodiment is flatly paved in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content a =18.21% of the sample is calculated, 0.50% is taken according to the corrected compensation value b of the table 1, and the final moisture content W = a + b =18.71% is obtained;
the sample of this example was placed in a lidded container according to current standard assay methods, dried in an oven at 105 ℃ for 12 hours, weighed, and then dried continuously at intervals of 4 hours to constant weight, calculated to give a sample moisture content of 19.23%.
The difference between the method of the invention and the current standard measuring method is 0.52 percent, and the result is credible within the error allowable range.
Example 4
In this example, a sample having a moisture content in the range of 20 to 30% was measured;
according to the method, the sample of the embodiment is flatly laid in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content a =23.53% of the sample is calculated, 0.80% is taken according to the corrected compensation value b of the table 1, and the final moisture content W = a + b =24.33% is obtained;
the sample of this example was placed in a lidded container according to current standard assay methods, dried in an oven at 105 ℃ for 12 hours, weighed, and then dried continuously at intervals of 4 hours to constant weight, calculated to give a sample moisture content of 24.96%.
The difference between the method of the invention and the existing standard measuring method is 0.57%, and the result is credible within the error allowable range.
Example 5
In this example, a sample having a moisture content in the range of 20 to 30% was measured;
according to the method, the sample of the embodiment is flatly paved in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content a =26.36% of the sample is calculated, and the compensation value b is corrected according to the table 1 to be 0.90%, so that the final moisture content W = a + b =27.26%;
according to the current standard determination method, the sample of the embodiment is placed in a container with a cover, dried in an oven at 105 ℃ for 12 hours and then weighed, and then continuously dried at intervals of 4 hours until the weight is constant, and the water content of the sample is 27.89% by calculation.
The difference between the method of the invention and the existing standard measuring method is 0.63 percent, and the result is credible within the error allowable range.
Example 6
In this example, a sample having a moisture content in the range of 30 to 40% was measured;
according to the method, the sample is flatly laid in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude water content a =33.19% of the sample is calculated, 1.20% is taken according to the corrected compensation value b in the table 1, and the final water content W = a + b =34.39% is obtained;
according to the current standard determination method, the sample of the embodiment is placed in a container with a cover, dried in an oven at 105 ℃ for 12 hours and then weighed, and then continuously dried at intervals of 4 hours until the weight is constant, and the water content of the sample is 35.41% by calculation.
The difference between the method of the invention and the current standard measuring method is 1.02 percent, and the result is credible within the error allowable range.
Example 7
In this example, a sample having a moisture content in the range of 30 to 40% was measured;
according to the method, the sample is spread in a container and then placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content a =36.84% of the sample is calculated, and the compensation value b is corrected according to the table 1 to obtain 1.30%, so that the final moisture content W = a + b =38.14%;
according to the current standard determination method, the sample of the embodiment is placed in a container with a cover, dried in an oven at 105 ℃ for 12 hours and then weighed, and then continuously dried at intervals of 4 hours until the weight is constant, and the water content of the sample is 39.21% by calculation.
The difference between the method of the invention and the existing standard measuring method is 1.07 percent, and the result is credible within the error allowable range.
Example 8
In this example, a sample having a moisture content in the range of 40 to 50% was measured;
according to the method, the sample in the embodiment is flatly laid in a container, and then is placed in an oven to be dried for 4h at 150 ℃, the crude water content a =42.04% of the sample is calculated, and the compensation value b is corrected according to the table 1 to obtain 1.55%, so that the final water content W = a + b =43.59%;
according to the current standard determination method, the sample of the embodiment is placed in a container with a cover, dried in an oven at 105 ℃ for 12 hours and then weighed, and then continuously dried at intervals of 4 hours until the weight is constant, and the moisture content of the sample is calculated to be 44.97%.
The difference between the method of the invention and the existing standard measuring method is 1.38%, and the result is credible within the error allowable range.
Example 9
In this example, a sample having a moisture content in the range of 40 to 50% was measured;
according to the method, the sample of the embodiment is flatly paved in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content a =47.11% of the sample is calculated, and the compensation value b is corrected according to the table 1 to obtain 1.65%, so that the final moisture content W = a + b =48.76%;
the sample of this example was placed in a lidded container according to current standard assay methods, dried in an oven at 105 ℃ for 12 hours, weighed, and then dried continuously at intervals of 4 hours to constant weight, calculated to give a sample moisture content of 49.95%.
The difference between the method of the invention and the existing standard measuring method is 1.19 percent, and the result is credible within the error allowable range.
Example 10
In the embodiment, a sample with the moisture content of 50-65% is measured;
according to the method, the sample of the embodiment is flatly paved in a container, and then is placed in an oven to be dried for 4 hours at 150 ℃, the crude moisture content of the sample is calculated to be a =56.48%, and the final moisture content W = a + b =58.88% by taking 2.0% of the corrected compensation value b according to the table 1;
according to the current standard determination method, the sample of the embodiment is placed in a container with a cover, dried in an oven at 105 ℃ for 12 hours and then weighed, and then continuously dried at intervals of 4 hours until the weight is constant, and the water content of the sample is 60.29% by calculation.
The difference between the method of the invention and the current standard measuring method is 1.41 percent, and the result is credible within the error allowable range.
Example 11
In the embodiment, a sample with the moisture content of 50-65% is measured;
according to the method, the sample is flatly paved in a container, then the sample is placed in an oven to be dried for 4h at 150 ℃, the crude moisture content of the sample is calculated to be a =61.17%, and the final moisture content W = a + b =63.37% is obtained by taking 2.20% of the corrected compensation value b according to the table 1;
according to the current standard determination method, the sample of the embodiment is placed in a container with a cover, dried in an oven at 105 ℃ for 12 hours and then weighed, and then continuously dried at intervals of 4 hours until the weight is constant, and the water content of the sample is 64.98% by calculation.
The difference between the method of the invention and the existing standard measuring method is 1.61%, and the result is credible within the error allowable range.
Comparative example 1
This comparative example is different from the above examples in that the drying temperature in the measurement method was adjusted to 160 ℃.
Table 2 compares the results of the measurements of samples with different water contents at this temperature with the current standard method;
TABLE 2 comparison of moisture content measurements
| Interval of water content of sample | Current standard method | Comparative example method | Determining the difference |
| 30％—40％ | 35.71％ | 30.13％ | 5.58％ |
| 40％—50％ | 47.26％ | 41.05％ | 6.21％ |
| 50％—65％ | 59.87％ | 51.34％ | 8.53％ |
In the drying process of the comparative example, the phenomena of flash combustion on the surface of the sample, flying out of fine particles of the sample and the like also occur, and meanwhile, the difference between the calculated final moisture content and the existing detection method is more than 5 percent and more than 0.36 to 1.61 percent of the detection method of the embodiment.
Compared with the existing detection method, the method has the advantages that the analysis and detection time can be greatly shortened, the operation procedure is simplified, the energy consumption of steam, electricity and the like in a smelting production line and a raw material pretreatment stage (solid waste drying) for comprehensively recovering valuable metals by taking the heavy metal solid waste with higher water content, copper, nickel and the like as raw materials can be greatly reduced, and the requirements of central control detection and analysis in the production process and the service of guiding production can be well met; meanwhile, the method has high detection precision, and improves the analysis efficiency while powerfully reducing the working strength of the laboratory staff.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A method for detecting the moisture content of heavy metal solid waste such as copper and nickel is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
placing the container in an oven for drying, cooling and weighing the container by mass G1;
collecting a sample, placing the sample in a container, and weighing the total mass G2;
placing the container containing the sample in an oven for drying;
cooling and weighing the container and the total mass G3 of the sample after drying;
calculating the crude water content a of the sample;
and obtaining the final moisture content through data compensation and correction.
2. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: the container is a cover-free container, can resist water and medium strong acid corrosion, and the thickness of the sample after being placed in the container and flattened is 1.5-2 cm.
3. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: and placing the container in an oven for drying, wherein the drying temperature is 145-155 ℃, and the drying time is 5-10 min.
4. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1 or 2, characterized by comprising the following steps: the mass of the sample is 800.0-1000.0 g.
5. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: and (3) drying the container containing the sample in an oven, wherein the drying temperature is 145-155 ℃, and the drying time is 4h.
6. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: the temperature rise rate of the oven is set within the range of 3-4 ℃/min.
7. The method for detecting the moisture content of the solid waste of heavy metals including copper and nickel according to claim 1, wherein: the crude moisture content of the sample is expressed as follows:
a＝(G3-G1)/G×100％
wherein a represents the crude moisture content of the sample, G represents the sample mass, and G = (G2-G1).
8. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: the mass unit is g, to the nearest 0.1g.
9. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: the final moisture content is expressed as follows:
W＝a+b
wherein W represents the final moisture content of the sample, a represents the crude moisture content of the sample, and b is a corrected value.
10. The method for detecting the moisture content of the solid waste of heavy metals containing copper, nickel and the like according to claim 1, which comprises the following steps: the difference between the moisture content data of the parallel samples measured by the method and the current standard method is not more than 2%.
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| CN202211054089.0A CN115524253A (en) | 2022-08-31 | 2022-08-31 | Method for detecting content of water in solid waste of heavy metals such as copper and nickel |
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| CN202211054089.0A CN115524253A (en) | 2022-08-31 | 2022-08-31 | Method for detecting content of water in solid waste of heavy metals such as copper and nickel |
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