CN102313706A - Digestion and determination method of heavy metals in waste dust-collecting bag - Google Patents
Digestion and determination method of heavy metals in waste dust-collecting bag Download PDFInfo
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- CN102313706A CN102313706A CN201110142301A CN201110142301A CN102313706A CN 102313706 A CN102313706 A CN 102313706A CN 201110142301 A CN201110142301 A CN 201110142301A CN 201110142301 A CN201110142301 A CN 201110142301A CN 102313706 A CN102313706 A CN 102313706A
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Abstract
The invention discloses a digestion and determination method of heavy metals in a waste dust-collecting bag, and relates to microwave digestion of the waste bags generated by iron and steel smelting and non-ferrous metal smelting (such as lead-zinc smelting and copper smelting). The method comprises the following steps: mixing the waste dust-collecting bag with a digestion acid system composed of nitric acid, hydrogen peroxide and hydrofluoric acid in a polytetrafluoroethylene-sealed pressurized digestion tank at normal temperature, shaking up and keeping standing overnight; and performing the microwave digestion under certain conditions and then performing heavy metal determination. By adopting the method, the waste dust-collecting bag is made into a digestion solution, and flame atomic absorption spectroscopy (FAAS) is further adopted for determining the content of the heavy metals in the digestion solution.
Description
Technical field
The present invention relates to the pre-treatment of micro-wave digestion in the waste and old dust-removal cloth-bag determining heavy metals process and the method for Instrument measuring; Specially refer to clearing up and assay method of heavy metal in a kind of waste and old dust-removal cloth-bag that smelting iron and steel, lead-zinc smelting industry produce, belong to field of environment engineering.
Background technology
Waste and old dust-removal cloth-bag is mainly derived from exhaust gas volumns such as iron and steel, non-ferrous metal metallurgy, thermal power plant, cement mill, steam boiler and produces the sack cleaner in the bigger industry exhaust-gas treatment operation.Along with sack cleaner tenure of use increases, that cloth bag has occurred is aging, damaged, burn and problem such as obstruction, has produced the problem of environmental pollution of waste and old dust-removal cloth-bag thereupon.Common cloth bag mainly is divided into man-made fiber cloth bag and spun glass cloth bag.Spun glass cloth bag principal ingredient is silicon dioxide, aluminium oxide, calcium oxide, boron oxide, magnesium oxide, sodium oxide molybdena etc.Spun glass filter bag skin is a cloth, and internal layer uses spun glass.The man-made fiber cloth bag mainly comprises terylene, polyimide fiber, aromatic polyamide fibre, polyphenylene sulfide fibre (PPS) etc.Waste and old dust-removal cloth-bag also contains poisonous and harmful substances such as some exhaust gas dusts and heavy metal except the starting material that comprise new cloth bag.If unprocessed direct entering environment, waste and old dust-removal cloth-bag very easily causes secondary pollution to underground water, soil etc. through immersion, erosion and the seepage of rainwater, harm humans healthy.
About the pollution characteristic of heavy metal in the waste and old dust-removal cloth-bag and the present domestic relevant report of not seeing of research of recycling and resource thereof.Maximum harm is heavy metal pollution to industries such as non-ferrous metal metallurgy (smelting like lead-zinc smelting, copper), iron and steel to environment, and along with the widespread use of sack cleaner in these industries, the heavy metal pollution problem that thereupon produces is also serious day by day.
Summary of the invention
For addressing the above problem, the purpose of this invention is to provide clearing up and assay method of heavy metal in a kind of waste and old dust-removal cloth-bag, for the recycling of next step waste and old dust-removal cloth-bag provides scientific basis.
To achieve these goals, the present invention adopts following technical scheme:
In a kind of waste and old dust-removal cloth-bag heavy metal clear up and assay method may further comprise the steps:
(1) at first waste and old dust-removal cloth-bag is cut into the rectangle of 20cm * 10cm with scissors, flying dust is separated with cloth bag through the mode of manual work or mechanical beating.Waste and old dust-removal cloth-bag after patting is carried out patting repeatedly once more and weighing more than three times, and the mass change before and after patting is less than 5%.Waste and old dust-removal cloth-bag after the constant weight use scissors shred to volume be 0.25～0.50cm
3Rectangular parallelepiped, above-mentioned sample is placed baking oven, and down oven dry 24 h are subsequent use in 105 ℃;
(2) take by weighing the above-mentioned waste and old dust-removal cloth-bag for preparing of 0.3～0.5g and place the full teflon seal supercharging of FR21 type counteracting tank, add by 7～10ml HNO
3, 1～3ml massfraction 30% H
2O
2With the acid system of clearing up of 1～3ml HF (hydrofluorite) composition, screw and clear up cover, solution is rocked for several times hold over night.The about 20min of acid is caught up with in water-bath behind the micro-wave digestion (100 ℃), and the use volume fraction is 2% HNO
3The medium washing is dissolved the appearance cup 3 times, is incorporated in to be equipped with in the 50 ml volumetric flasks to survey;
(3) running parameter of flame atomic absorption spectrophotometer is set, titer Cu, Zn, Pb, Cr, Ni and Cd is carried out full dose measure and the drawing standard curve, then sample solution in the step (2) is carried out the mensuration of above-mentioned six heavy metal species.
The micro-wave digestion program is made up of following three steps in the said step (2):
| Step | Power (W) | Heating-up time (min) | Temperature (℃) | Retention time (min) |
| 1 | 1600 | 5 | 120 | 5 |
| 2 | 1600 | 5 | 160 | 5 |
| 3 | 1600 | 5 | 200 | 30 |
Waste and old dust-removal cloth-bag is 1:30～1:48 with clearing up the acid system ratio in the said step (2), and wherein waste and old dust-removal cloth-bag mass unit is gram, and sour volume unit is a milliliter.
Clearing up acid system in the said step (2) is by HNO
3, H
2O
2Form with HF, its optimum volume ratio is: 10:2:2.
The condition of work of flame atomic absorption spectrophotometer is following in the said step (3):
| Element | Cu | Cr | Cd | Ni | Pb | Zn |
| Wavelength/nm | 324.7 | 357.9 | 228.8 | 232.0 | 283.3 | 213.9 |
| Slit/nm | 0.4 | 0.4 | 0.4 | 0.2 | 0.4 | 0.4 |
| Lamp current/mA | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 |
| Burner height/mm | 6 | 8 | 6.5 | 7 | 5 | 7 |
| Air pressure/Mpa | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Acetylene pressure/Mpa | 0.09 | 0.09 | 0.09 | 0.09 | 0.09 | 0.09 |
| Air mass flow/(Lmin -1) | 7.0 | 7.0 | 7.0 | 7.0 | 7.0 | 7.0 |
| Acetylene flow/(Lmin -1) | 1.0 | 2.5 | 1.5 | 1.2 | 1.5 | 1.0 |
Beneficial effect of the present invention:
This method is that the acid system of at normal temperatures waste and old dust-removal cloth-bag and nitric acid, oxydol and hydrofluorite being formed of clearing up mixes in teflon seal supercharging counteracting tank, shakes all, and hold over night carries out carrying out determining heavy metals after the micro-wave digestion under certain condition.The present invention is prepared into digestion solution with waste and old dust-removal cloth-bag, further adopts flame atomic absorption spectrometry (FAAS) to measure its content of beary metal.
Embodiment
(1) starting material of the present invention
Test specimen picks up from four kinds of different operations of certain iron and steel enterprise and lead-zinc smelting factory sintering mill (plant).Its basic proterties is seen table 1.
Table 1 cloth bag fundamental property
| The cloth bag source | The cloth bag type | Working temperature ℃ | Instantaneous temperature ℃ | Filtering feature | Wearing quality | Hydrolytic stability | Acid resistance | Alkali resistance | Inoxidizability |
| Converter | Terylene (polyester) | 135 | 150 | Well | Well | Relatively poor | Generally | Relatively poor | Better |
| Blast furnace | Spun glass | 250 | 280 | Generally | Generally | Well | Relatively poor | Generally | Well |
| Electric furnace | Acrylic fibers+glass | 125 | 140 | Better | Better | Better | Better | Generally | Better |
| Coking | Mei Tasi (aromatic polyamide) | 180 | 220 | Well | Well | Generally | Generally | Generally | Better |
| Sintering | Spun glass | 250 | 300 | Generally | Generally | Well | Relatively poor | Generally | Well |
(2) case study on implementation
Embodiments of the invention are described in the back at present:
Embodiment 1
Under the normal temperature and pressure, the lead-zinc smelting factory waste and old dust-removal cloth-bag in sintering mill (plant) that takes by weighing 105 ℃ of dry 24h of 0.3g places the full teflon seal supercharging of FR21 type counteracting tank, adds 7mlHNO respectively
3(GR), 1mlH
2O
2(30%, GR) and 1mlHF (GR); 10mlHNO
3(GR), 3mlH
2O
2(30%, GR) and 3mlHF (GR) screw and clear up cover, solution are rocked several times hold over night.The about 20min of acid is caught up with in water-bath behind the micro-wave digestion (100 ℃), and the use volume fraction is 2% HNO
3The molten appearance cup of medium washing 3 times is incorporated in to be equipped with in the 50ml volumetric flask and surveys, and the running parameter of FAAS instrument is set, and the sample-digestion solution after full dose is cleared up carries out Cu, Zn, Pb, Cr, Ni, Cd full dose mensuration.Experimental result sees Table 2, table 3.
Table 2 micro-wave digestion test effect
| Sequence number | Clear up acid system | Clear up effect |
| 1 | 7mlHNO 3、1mlH 2O 2、1mlHF | Clarification, transparent, light yellow |
| 2 | 10mlHNO 3、3mlH 2O 2、3mlHF | Clarification, transparent, light yellow |
The waste and old dust-removal cloth-bag of table 3 is cleared up back determining heavy metals result (mgkg
-1
)
| Sequence number | Cu | Pb | Cd | Ni | Zn | Cr |
| 1 | 90.05 | 4667.33 | 378.69 | 10.63 | 10977.13 | Do not detect |
| 2 | 100.95 | 4866.12 | 431.51 | 13.62 | 12977.11 | Do not detect |
Embodiment 2
Under the normal temperature and pressure, the waste and old dust-removal cloth-bag of steel plant's converter that takes by weighing 105 ℃ of dry 24h of 0.5g places the full teflon seal supercharging of FR21 type counteracting tank, adds 10mlHNO
3(GR), 2 mlH
2O
2(30%, GR) and 2ml HF (GR) screw and clear up cover, solution are rocked several times hold over night.The about 20min of acid is caught up with in water-bath behind the micro-wave digestion (100 ℃), and the use volume fraction is 2% HNO
3The molten appearance cup of medium washing 3 times is incorporated in to be equipped with in the 50ml volumetric flask and surveys, and the running parameter of FAAS instrument is set, and the sample after full dose is cleared up and the digestion solution of contaminated soil national standard material carry out Cu, Zn, Pb, Cr, Ni, Cd full dose mensuration.Experimental result sees Table 4, table 5.
Table 4 micro-wave digestion test effect
| Sequence number | Waste and old dust-removal cloth-bag kind | Clear up effect |
| 1 | The waste and old dust-removal cloth-bag of converter | Clarification, transparent, light yellow |
| 2 | The waste and old dust-removal cloth-bag of blast furnace | Clarification, transparent, light yellow |
| 3 | The waste and old dust-removal cloth-bag of electric furnace | Clarification, transparent, light yellow |
| 4 | The waste and old dust-removal cloth-bag of coking | Clarification, transparent, light yellow |
The waste and old dust-removal cloth-bag of table 5 is cleared up back determining heavy metals result (mgkg
-1)
| Sequence number | Cu | Pb | Cd | Ni | Zn | Cr |
| 1 | 34.94 | 2884.29 | 4.11 | 28.08 | 881.81 | 1.17 |
| 2 | 10.16 | 44.94 | 4.35 | 23.94 | 944.456 | 10.61 |
| 3 | 95.52 | 1585.65 | 11.29 | 34.97 | 4012.21 | 13.86 |
| 4 | 321.81 | 93.49 | 3.73 | 27.01 | 4670.03 | 3.64 |
Embodiment 3
Under the normal temperature and pressure, the waste and old dust-removal cloth-bag of steel plant's blast furnace that takes by weighing 105 ℃ of dry 24h of 0.4g places the full teflon seal supercharging of FR21 type counteracting tank, adds 10mlHNO3 (GR), 2 mlH
2O
2(30%, GR) and 2ml HF (GR) screw and clear up cover, solution are rocked several times hold over night.The about 20min of acid is caught up with in water-bath behind the micro-wave digestion (100 ℃); Using volume fraction is that 2% HNO3 medium washing is dissolved the appearance cup 3 times; Be incorporated in to be equipped with in the 50ml volumetric flask and survey; The running parameter of FAAS instrument is set, and the digestion solution of sample after full dose is cleared up and contaminated soil national standard material carries out Cu, Zn, Pb, Cr, Ni, Cd full dose mensuration.Experimental result sees Table 4, table 5.
Embodiment 4
Of embodiment 3, different is that test specimen is the waste and old dust-removal cloth-bag of steel plant's electric furnace, and experimental result is seen table 4, table 5.
Embodiment 5
Of embodiment 3, different is that test specimen is the waste and old dust-removal cloth-bag of steel plant's coke oven, and experimental result is seen table 4, table 5.
Claims (4)
1. the clearing up and assay method of heavy metal in the waste and old dust-removal cloth-bag is characterized in that this method may further comprise the steps:
(1) at first waste and old dust-removal cloth-bag is cut into the rectangle of 20cm * 10cm; Mode through manual work or mechanical beating is separated flying dust with cloth bag; Waste and old dust-removal cloth-bag after patting is carried out patting repeatedly once more and weighing more than three times; Mass change before and after patting is less than 5%, the waste and old dust-removal cloth-bag after the constant weight shred to volume be 0.25～0.50cm
3Rectangular parallelepiped, above-mentioned sample is placed baking oven, and down oven dry 24 h are subsequent use in 105 ℃;
(2) take by weighing the above-mentioned waste and old dust-removal cloth-bag for preparing of 0.3～0.5g and place full teflon seal supercharging counteracting tank, add by 7～10ml HNO
3, 1～3ml massfraction 30% H
2O
2With the acid system of clearing up of 1～3ml HF composition, screw and clear up cover, solution is rocked for several times hold over night; Sour 20min is caught up with in 100 ℃ of water-baths behind the micro-wave digestion, and the use volume fraction is 2% HNO
3The medium washing is dissolved the appearance cup 3 times, is incorporated in to be equipped with in the 50 ml volumetric flasks to survey;
(3) running parameter of flame atomic absorption spectrophotometer is set, titer Cu, Zn, Pb, Cr, Ni and Cd is carried out full dose measure and the drawing standard curve, then sample solution in the step (2) is carried out the mensuration of above-mentioned six heavy metal species.
2. according to claim 1 clearing up and assay method is characterized in that: the micro-wave digestion program is made up of following three steps in the said step (2):
According to claim 1 clearing up and assay method is characterized in that: waste and old dust-removal cloth-bag is 1:30～1:48 with clearing up the acid system ratio in the said step (2), and wherein waste and old dust-removal cloth-bag mass unit is gram, and sour volume unit is a milliliter.
3. according to claim 1 clearing up and assay method is characterized in that: clearing up acid system in the said step (2) is by HNO
3, H
2O
2Form with HF, its volume ratio is 10:2:2.
4. according to claim 1 clearing up and assay method is characterized in that: the condition of work of flame atomic absorption spectrophotometer is following in the said step (3):
。
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|---|---|---|---|
| CN 201110142301 CN102313706B (en) | 2011-05-30 | 2011-05-30 | Digestion and determination method of heavy metals in waste dust-collecting bag |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110142301 CN102313706B (en) | 2011-05-30 | 2011-05-30 | Digestion and determination method of heavy metals in waste dust-collecting bag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102313706A true CN102313706A (en) | 2012-01-11 |
| CN102313706B CN102313706B (en) | 2013-02-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110142301 Expired - Fee Related CN102313706B (en) | 2011-05-30 | 2011-05-30 | Digestion and determination method of heavy metals in waste dust-collecting bag |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879346A (en) * | 2012-09-29 | 2013-01-16 | 神华集团有限责任公司 | Measuring method for content of metal elements in polymer resin |
| CN103207171A (en) * | 2013-04-25 | 2013-07-17 | 浙江海拓环境技术有限公司 | Digestion method of electroplating chromium mud |
| CN103411909A (en) * | 2013-09-03 | 2013-11-27 | 江苏沥泽生化科技有限公司 | Method for detecting silver content in nano-silver dressing |
| CN104792720A (en) * | 2015-05-15 | 2015-07-22 | 福建中烟工业有限责任公司 | Method for measuring titanium element or titanium dioxide content in diacetate cellulose tow |
| CN105466916A (en) * | 2015-11-11 | 2016-04-06 | 巴彦淖尔市飞尚铜业有限公司 | Method for rapid combined measurement of lead and zinc in copper smelting soot |
| CN105928926A (en) * | 2016-04-19 | 2016-09-07 | 攀钢集团研究院有限公司 | Sample preparation method and detection method for water-soluble heavy metal elements in solid waste |
| CN109557079A (en) * | 2018-11-06 | 2019-04-02 | 河钢股份有限公司 | The ICP-OES measuring method of constituent content in sintering dust separation ash |
| CN112378868A (en) * | 2020-10-16 | 2021-02-19 | 苏州特瑞思塑胶有限公司 | Method for detecting content of metal components in polyphenylene sulfide |
| CN112557243A (en) * | 2020-11-13 | 2021-03-26 | 瀚蓝绿电固废处理(佛山)有限公司 | Method for analyzing selenium form in fly ash |
| CN114739926A (en) * | 2022-04-08 | 2022-07-12 | 新疆维吾尔自治区产品质量监督检验研究院 | Method for measuring residual quantity of harmful heavy metals in printing ink |
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Cited By (13)
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| CN102879346A (en) * | 2012-09-29 | 2013-01-16 | 神华集团有限责任公司 | Measuring method for content of metal elements in polymer resin |
| CN103207171A (en) * | 2013-04-25 | 2013-07-17 | 浙江海拓环境技术有限公司 | Digestion method of electroplating chromium mud |
| CN103207171B (en) * | 2013-04-25 | 2015-05-13 | 浙江海拓环境技术有限公司 | Digestion method of electroplating chromium mud |
| CN103411909A (en) * | 2013-09-03 | 2013-11-27 | 江苏沥泽生化科技有限公司 | Method for detecting silver content in nano-silver dressing |
| CN104792720A (en) * | 2015-05-15 | 2015-07-22 | 福建中烟工业有限责任公司 | Method for measuring titanium element or titanium dioxide content in diacetate cellulose tow |
| CN105466916A (en) * | 2015-11-11 | 2016-04-06 | 巴彦淖尔市飞尚铜业有限公司 | Method for rapid combined measurement of lead and zinc in copper smelting soot |
| CN105928926A (en) * | 2016-04-19 | 2016-09-07 | 攀钢集团研究院有限公司 | Sample preparation method and detection method for water-soluble heavy metal elements in solid waste |
| CN109557079A (en) * | 2018-11-06 | 2019-04-02 | 河钢股份有限公司 | The ICP-OES measuring method of constituent content in sintering dust separation ash |
| CN112378868A (en) * | 2020-10-16 | 2021-02-19 | 苏州特瑞思塑胶有限公司 | Method for detecting content of metal components in polyphenylene sulfide |
| CN112557243A (en) * | 2020-11-13 | 2021-03-26 | 瀚蓝绿电固废处理(佛山)有限公司 | Method for analyzing selenium form in fly ash |
| CN112557243B (en) * | 2020-11-13 | 2021-11-19 | 瀚蓝绿电固废处理(佛山)有限公司 | Method for analyzing selenium form in fly ash |
| CN114739926A (en) * | 2022-04-08 | 2022-07-12 | 新疆维吾尔自治区产品质量监督检验研究院 | Method for measuring residual quantity of harmful heavy metals in printing ink |
| CN114739926B (en) * | 2022-04-08 | 2022-11-22 | 新疆维吾尔自治区产品质量监督检验研究院 | Method for measuring residual quantity of harmful heavy metals in printing ink |
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