CN111982651A - Rapid microwave digestion treatment method for solid-containing residual oil - Google Patents
Rapid microwave digestion treatment method for solid-containing residual oil Download PDFInfo
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- 239000007787 solid Substances 0.000 title claims abstract description 69
- 238000000120 microwave digestion Methods 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 45
- 230000029087 digestion Effects 0.000 claims abstract description 141
- 239000002253 acid Substances 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000003921 oil Substances 0.000 claims description 68
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- 239000003517 fume Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000002133 sample digestion Methods 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000012528 membrane Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 238000004380 ashing Methods 0.000 description 9
- 239000002184 metal Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000001675 atomic spectrum Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000007415 particle size distribution analysis Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000000184 acid digestion Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000003250 coal slurry Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000010742 number 1 fuel oil Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
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Abstract
A rapid microwave digestion treatment method for solid residue oil comprises cleaning and drying a digestion tank, a 50ml or 100ml volumetric flask, a beaker and a glass rod; secondly, placing the sample containing the solid residue oil in an oven at 100-150 ℃ to be heated to be in a flowing state, weighing 0.3-0.8 g of sample in a digestion tank after uniformly stirring, and sequentially adding (8-10 ml) HNO into the digestion tank3、(2ml‑3ml)H2O2And (1ml-2ml) HCl; then placing the digestion tank filled with the sample into a microwave digestion instrument, presetting digestion conditions, and digesting; preferably, the digestion tank containing the sample is placed on an acid removing plate with the temperature of 180-220 ℃ until a drop of liquid is left in the digestion tank, the liquid is transferred into a volumetric flask for constant volume, the appearance of the sample is clear, slightly yellow or deep yellow after constant volume, the acid concentration is less than or equal to 2% after constant volume, and the label is marked; the invention has the characteristics of simple and convenient operation, high testing speed, good repeatability and high precision.
Description
Technical Field
The invention relates to the technical field of analysis and detection of solid residue oil-containing elements (metal elements and nonmetal elements), in particular to a rapid microwave digestion treatment method for solid residue oil.
Background
The coal oil co-refining and the light solid residue oil contain elements (nickel, vanadium, sulfur and the like) of raw material residual oil to be accurately measured and analyzed. The nickel element and the vanadium element in the raw material residual oil can poison the catalyst; and the sulfur element can promote the residual oil to be converted into light oil products. The contents of the elements are measured by an atomic spectrum analyzer, and the pretreatment of the sample is a key link of the atomic spectrum analysis such as AAS, ICP and the like; common sample pretreatment methods include ashing, extraction, acidolysis, high-pressure bomb dissolution and organic solvent dilution; the ashing method is specified according to IP501-2005 'determination of aluminum, silicon, vanadium, nickel, iron, sodium, calcium, zinc and phosphorus in residue fuel by ashing method and inductively coupled plasma emission spectrometry', and wet acidolysis is used for catalyst pretreatment; the method for treating the sample by the inorganic reagent treatment method is characterized in that: the sample treatment time is long, the chances of element loss or pollution are more, and the environmental pollution is large; the finished lubricating oil is diluted by an organic solvent; the treated sample of the organic reagent dilution method can only be soluble elements and the oil product does not contain solids.
The microwave digestion treatment of samples belongs to the field of wet acidolysis by an inorganic method, and the technology is characterized in that: the sample treatment time is short, and the oil containing solids can also be subjected to acidolysis; the usage amount of the sample and the reagent is small, and the environmental hazard degree is low; when a sample containing solid residue oil (toluene insoluble substance containing the solid residue oil is less than or equal to 25%) is treated by the existing microwave digestion method, the digestion is incomplete and incomplete, and the solid residue oil after the microwave digestion treatment still contains black solid powder. The solid containing solid residual oil mainly comprises carbon, mineral particles and a small amount of inorganic matters, and the particle size distribution of the solid is as follows: 0.1um-200um, because the matrix difference of the solid residue oil sample is very large, different digestion methods are needed to be adopted for different samples; in actual work, through a large number of experiments, an optimal digestion method for microwave digestion treatment of solid residue containing oil is confirmed by considering three aspects of sample weighing, acid system selection, acid using amount and digestion conditions.
Disclosure of Invention
In order to solve the problems of incomplete and incomplete digestion of solid residue oil-containing samples by the existing microwave digestion method, the invention aims to provide a rapid microwave digestion method for solid residue oil-containing samples, which can solve the problems of long treatment period, incomplete and incomplete acid digestion, residual solid particles in solution, large sample and reagent consumption and large environmental pollution, and has the advantages of simple operation, high test speed, good repeatability and high precision.
In order to achieve the purpose, the invention adopts the technical scheme that:
a rapid microwave digestion treatment method for solid-containing residual oil comprises the following steps:
step one, equipment preparation: cleaning the digestion tank, a 50ml or 100ml volumetric flask, a beaker and a glass rod, and drying in an oven at 105 +/-5 ℃ for 1-1.5 h;
step two, sample treatment: heating a sample containing solid residue oil in an oven at 100-150 ℃ to be in a flowing state, fully and uniformly stirring, and then sampling; weighing 0.3-0.8 g (accurate to 0.0001g) of uniform sample in a clean digestion tank, and sequentially adding (8-10 ml) HNO into the digestion tank3、(2ml-3ml)H2O2And (1ml-2ml) HCl;
step three, sample digestion: putting the digestion tank filled with the sample in the second step into a microwave digestion instrument, presetting digestion conditions, and starting the microwave digestion instrument;
step four, volume fixing stage: placing a digestion tank containing a test sample on an acid removing plate, setting the temperature of the acid removing plate between 180 ℃ and 220 ℃ until a drop of liquid remains in the digestion tank, transferring the liquid in the digestion tank into a 50ml or 100ml volumetric flask, then adding ultrapure water into the volumetric flask containing the test sample to the scale mark of the 50ml or 100ml volumetric flask, wherein the sample after constant volume is liquid with clear appearance, yellowish or deep yellow, the acid concentration of the sample after acid removing plate finishes constant volume is less than or equal to 2%, and labeling the label.
The digestion tank is a polytetrafluoroethylene tank with the volume of 50ml or 100 ml; if the silicon element of solid residue is measured, 0.5ml to 1ml of HF is added.
The water content of the solid residue oil-containing sample is less than 0.5 percent, and the content of toluene insoluble substances is less than or equal to 25 percent.
And (5) naturally standing the digestion tank of the sample added with the acid in the second step in a fume hood for 15-30 min, and then putting the digestion tank into a microwave digestion instrument.
The preset digestion conditions in the third step are as follows:
| step (ii) of | Temperature of | Power of | Duration of time | Magnetic stirring |
| Speed of power ramp-up | / | 800W-1000W | 20min-30min | Close off |
| Maintaining power | / | 800W-1000W | 20min-35min | Close off |
| Cooling down | 70℃ | 0W | / | Close off |
Note: 1) maximum rate of pressure increase: 0.3 bar/s;
2) maximum pressure: 55.0 bar;
3) limit of infrared temperature: 240 ℃;
4) internal temperature limit: at 260 ℃.
After the digestion is finished, if a small amount of residual solids exist in the digestion tank through visual observation, carrying out secondary digestion, and continuously adding (4ml-6ml) HNO into the digestion tank in sequence3、(1ml-3ml)H2O2(0.5ml-1ml) HCl, then putting the HCl into a microwave digestion instrument with preset digestion conditions, and starting the microwave digestion instrument; if the liquid in the digestion tank after the first digestion is clear and has no residual solid, the second digestion is not needed, namely the digestion process is completed.
The invention has the beneficial effects that:
1. the sample amount of the sample is small, the elements are completely dissolved in the digestion process, and the loss is almost avoided, so that the determination result is more real and reliable.
2. The microwave digestion process shortens the period of sample pretreatment.
3. And (3) discharging acid from the digested sample by using an acid removing plate, and obtaining a result that the relative deviation of the result of measuring the analysis element is the minimum when the acid concentration of the sample after constant volume is less than or equal to 2% through a large number of experiments.
In conclusion, the rapid microwave digestion treatment method for solid residue-containing oil has the advantages of simplicity and convenience in operation, high testing speed, good repeatability and high precision, and solves the problems of long time consumption and poor stability of actual sample pretreatment.
Detailed Description
A rapid microwave digestion treatment method for solid-containing residual oil comprises the following steps:
step one, equipment preparation: cleaning the digestion tank, a 50ml or 100ml volumetric flask, a beaker and a glass rod, and drying in an oven at 105 +/-5 ℃ for 1-1.5 h;
step two, sample treatment: heating the sample containing the solid residue oil in an oven at 100-150 ℃ to be in a flowing state, fully stirring uniformly, and sampling; weighing 0.3-0.8 g (accurate to 0.0001g) of uniform sample in a clean digestion tank, and sequentially adding (8-10 ml) HNO into the digestion tank3、(2ml-3ml)H2O2And (1ml-2ml) HCl;
step three, sample digestion: putting the digestion tank filled with the sample in the second step into a microwave digestion instrument, presetting digestion conditions, and starting the microwave digestion instrument;
step four, volume fixing stage: placing a digestion tank containing a sample on an acid removing plate, setting the temperature of the acid removing plate between 180 ℃ and 220 ℃ until a drop of liquid remains in the digestion tank, transferring the liquid in the digestion tank into a 50ml or 100ml volumetric flask, then adding ultrapure water into the volumetric flask containing the sample to the scale mark of the 50ml or 100ml volumetric flask, wherein the sample after constant volume is clear in appearance, yellowish or deep yellow, the acid concentration after constant volume is less than or equal to 2%, and the label marking is finished.
The digestion tank is a polytetrafluoroethylene tank with the volume of 50ml or 100 ml; if the content of silicon element in solid residue is measured, HF (0.5ml-1ml) is added.
The solid residue-containing sample contains water less than 0.5% and toluene insoluble substances less than or equal to 25%.
And (5) naturally standing the digestion tank added with the acid sample in the second step in a fume hood for 15-30 min, and then putting the digestion tank into a microwave digestion instrument.
The preset digestion conditions in the third step are as follows:
| step (ii) of | Temperature of | Power of | Duration of time | Magnetic stirring |
| Speed of power ramp-up | / | 800W-1000W | 20min-30min | Close off |
| Maintaining power | / | 800W-1000W | 20min-35min | Close off |
| Cooling down | 70℃ | 0W | / | Close off |
Note: 1) maximum rate of pressure increase: 0.3 bar/s;
2) maximum pressure: 55.0 bar;
3) limit of infrared temperature: 240 ℃;
4) internal temperature limit: at 260 ℃.
After the digestion is finished, if a small amount of residual solids exist in the digestion tank through visual observation, carrying out secondary digestion, and continuously adding (4ml-6ml) HNO into the digestion tank in sequence3、(1ml-3ml)H2O2(0.5ml-1ml) HCl, then putting the HCl into a microwave digestion instrument with preset digestion conditions, and starting the microwave digestion instrument; if no residual solid exists in the digestion tank after the first digestion, the second digestion is not needed, namelyAnd (5) finishing the digestion process.
Example 1
Selecting a sample with poor fluidity at room temperature, namely cracking tail oil of a suspension bed hydrogenation device, and measuring the content of toluene insoluble substances to be 6.43 percent; the kinematic viscosity at 135 ℃ is 330.62mm2S; after the mixture is kept at a constant temperature of 100 ℃ and is fully and uniformly stirred, 0.5697g of a sample is weighed in a beaker, hot toluene at 60 ℃ is added according to the solvent-oil ratio (toluene volume: sample mass) of 30:1, after ultrasonic treatment for 20min, micro-negative pressure filtration is carried out through a 0.1um glass fiber filter membrane under the pressure of 0.1Kpa, insoluble substances after toluene drying are all solids in the residual oil, and the solids are subjected to particle size distribution analysis, wherein the results are shown in the following table 1:
TABLE 1 solid particle size distribution content table of cracked tail oil
The rapid microwave digestion treatment method of the solid residue oil-containing sample comprises the following steps:
step one, cleaning a digestion tank, a 50ml volumetric flask, a beaker and a glass rod used in the test, and drying in an oven at 105 ℃ for 1 h;
step two, solid slag is contained
Heating the oil sample in a 150 ℃ oven to be in a flowing state, fully stirring uniformly, sampling, weighing 0.3446g and 0.3376g of parallel samples respectively, placing the samples into two digestion tanks, and adding 8ml of HNO into the two digestion tanks respectively3,2ml H2O21ml of HCl, then placing the digestion tank in a fume hood and standing for 15 min;
step three, covering the digestion tank which is kept stand in the fume hood in the step two with a cover, putting the digestion tank into a microwave digestion instrument, presetting digestion conditions, (see table 2) starting the microwave digestion instrument with the preset digestion conditions, and taking out the digestion tank after the digestion conditions are executed;
and step four, placing the digestion tank containing the sample on an acid removing plate, setting the temperature of the acid removing plate to be 200 ℃, until a drop of liquid remains in the digestion tank, transferring all the liquid in the digestion tank to a 50ml volumetric flask, adding ultrapure water into the volumetric flask containing the sample until a scale mark of 50ml is formed, wherein the appearance of the digestion sample after the sample is subjected to constant volume is clear yellowish liquid, and the acid concentration after the constant volume is less than or equal to 2%.
Referring to table 1, the particle size distribution data of the solid particles separated from the cracked tail oil in example 1 is between 0.1um and 200um, and the data comparison shows that the analysis result of the metal elements of the cracked tail oil treated by the rapid microwave digestion method of the present invention is better than the analysis result of the metal elements of the cracked tail oil treated by the conventional wet ashing method (see table 3 and table 4 for details).
TABLE 2 microwave digestion conditions set forth in the examples
| Step (ii) of | Temperature of | Power of | Duration of time | Magnetic stirring |
| Speed of power ramp-up | / | 900W | 20min | Close off |
| Maintaining power | / | 900W | 30min | Close off |
| Cooling down | 70℃ | 0W | / | Close off |
TABLE 3 analysis of metal element of cracked tail oil treated by rapid microwave digestion method
TABLE 4 analysis of metallic elements in wet ashing treatment of cracked tail oil
Example 2
Selecting a raw material of a suspension bed hydrogenation device, namely 20% of oil coal slurry (residual oil: coal powder is 80%: 20%) by mass ratio, and 19.89% of toluene insoluble substance; the kinematic viscosity at 135 ℃ is 84.62mm2S; after the mixture is kept at the constant temperature of 100 ℃ and fully stirred uniformly, 0.7882g of sample is weighed in a beaker, 60 ℃ hot toluene is added according to the solvent-oil ratio (toluene volume: sample mass) of 30:1, after ultrasonic treatment for 20min, the mixture is subjected to micro-negative pressure filtration under the pressure of 0.1Kpa through a 0.1um glass fiber filter membrane, insoluble substances after toluene drying are all solids in the residual oil, and the solids are subjected to particle size distribution analysis, wherein the results are shown in the following table 5:
TABLE 5 solid particle size distribution content table of kerosene co-refined stock oil
Treating the solid residue oil-containing sample by a rapid microwave digestion method:
step one, cleaning a digestion tank, a 50ml volumetric flask, a beaker and a glass rod, and drying in an oven at 100 ℃ for 1.5 h;
step two, placing the solid residue oil-containing sample in a 100 ℃ oven to be heated into a flowing state, fully stirring uniformly, sampling and respectively weighing 0.6754g and 0.7112g of parallel samples to be placed in two digestion tanks, and sequentially adding 8ml of HNO into the two digestion tanks3,2ml H2O21ml of HCl, then placing the digestion tank in a fume hood and standing for 15 min;
step three, covering the digestion tank which is kept still in the fume hood in the step two with a cover, putting the digestion tank into a microwave digestion instrument, presetting digestion conditions, and referring to table 2: starting the microwave digestion instrument with preset digestion conditions, taking out the digestion tank after the digestion conditions are executed, visually observing that a small amount of solid particles exist in sample liquid in the digestion tank, and continuously adding 4ml of HNO into the digestion tank in sequence3,、1ml H2O2And 0.5ml of HCl, starting preset digestion conditions, carrying out secondary microwave digestion, and taking out the digestion tank after the digestion conditions are executed;
and step four, placing the digestion tank containing the sample on an acid removing plate, setting the temperature of the acid removing plate to be 200 ℃, until a drop of liquid remains in the digestion tank, transferring all the liquid in the digestion tank to a 50ml volumetric flask, adding ultrapure water into the volumetric flask containing the sample to 50ml of scale mark, wherein the appearance of the digestion sample after constant volume is clear and yellowish liquid, and the acid concentration after constant volume is less than or equal to 2%.
Tables 6 and 7 show the comparison of the metal element content of the residual oil after the solid removal treatment by using two different filter membranes (0.1um filter membrane and 0.8um filter membrane), because the metal element of the solid particles (0.1um-0.8um) occupies a part of the metal element content of the residual oil filtered by the 0.8um filter membrane, the metal element content of the residual oil filtered by the 0.8um filter membrane is higher than that of the residual oil filtered by the 0.1um filter membrane; tables 8 and 9 are comparative tables showing the analysis results of the metal elements in the solid residue oil treated by the rapid microwave digestion method and the analysis results of the metal elements in the solid residue oil treated by the conventional wet ashing method. As trace loss of metal elements exists in the process of treating the residual oil by the traditional wet ashing method, comparison of data in tables 8 and 9 shows that the rapid microwave digestion method for treating the residual oil is superior to the traditional wet ashing method for treating the residual oil (the metal element data is measured by an ICP-AES instrument), tests compare 0.5%, 1%, 2%, 5% and 10% of samples with different acid concentrations, the influence of the acid concentration of less than or equal to 2% on the metal element detection result is the minimum, and the acid concentration after constant volume is selected to be less than or equal to 2%.
TABLE 6 residual oil feed after de-solidification (0.1um Filter Membrane)
TABLE 7 residual oil feed after de-solidification (0.8um Filter Membrane)
TABLE 8 data table for determining metal element content by microwave digestion treatment of solid residue-containing oil
TABLE 9 data table for determining content of metal elements in solid residue-containing oil treated by wet ashing method
Claims (9)
1. A rapid microwave digestion treatment method for solid-containing residual oil comprises the following steps:
step one, equipment preparation: cleaning the digestion tank, a 50ml or 100ml volumetric flask, a beaker and a glass rod, and drying in an oven at 105 +/-5 ℃ for 1-1.5 h;
step two, sample treatment: heating the sample containing the solid residue oil in an oven at 100-150 ℃ to be in a flowing state, fully stirring uniformly, and sampling; weighing 0.3-0.8 g (accurate to 0.0001g) of uniform sample in a clean digestion tank, and sequentially adding (8-10 ml) HNO into the digestion tank3、(2ml-3ml)H2O2And (1ml-2ml) HCl;
step three, sample digestion: putting the digestion tank filled with the sample in the second step into a microwave digestion instrument, presetting digestion conditions, and starting the microwave digestion instrument;
step four, volume fixing stage: placing a digestion tank containing a sample on an acid removing plate, setting the temperature of the acid removing plate between 180 ℃ and 220 ℃ until a drop of liquid remains in the digestion tank, transferring the liquid in the digestion tank into a 50ml or 100ml volumetric flask, then adding ultrapure water into the volumetric flask containing the sample to the scale mark of the 50ml or 100ml volumetric flask, wherein the sample after constant volume is clear in appearance, yellowish or deep yellow, the acid concentration after constant volume is less than or equal to 2%, and the label marking is finished.
2. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: the digestion tank in the first step is a polytetrafluoroethylene tank with the volume of 50ml or 100 ml; if the silicon element of solid residue is measured, HF (0.5ml-1ml) is added.
3. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: in the second step, the water content of the solid residue oil-containing sample is less than 0.5 percent, and the content of toluene insoluble substances is less than or equal to 25 percent.
4. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: and step two, placing the digestion tank containing the sample in a fume hood for naturally standing for 15-30 min, and then placing the digestion tank into a digestion instrument.
5. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: the preset digestion conditions in the third step are as follows:
Note: 1) maximum rate of pressure increase: 0.3 bar/s;
2) maximum pressure: 55.0 bar;
3) limit of infrared temperature: 240 ℃;
4) internal temperature limit: at 260 ℃.
6. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: after the digestion is finished, if a small amount of residual solids exist in the digestion tank through visual observation, carrying out secondary digestion, and continuously adding (4ml-6ml) HNO into the digestion tank in sequence3、(1ml-3ml)H2O2(0.5ml-1ml) HCl, then putting the HCl into a microwave digestion instrument with preset digestion conditions, and starting the microwave digestion instrument; if no residual solid exists in the digestion tank after the first digestion, the second digestion is not needed, namely the digestion process is completed.
7. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: and in the fourth step, the sample after volume fixing is a liquid with clear appearance, yellowish or deep yellow, and the acid concentration after volume fixing is less than or equal to 2%.
8. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: the method specifically comprises the following steps:
step one, cleaning a digestion tank, a 50ml volumetric flask, a beaker and a glass rod used in the test, and drying in an oven at 100 ℃ for 1.5 h;
step two, placing the sample containing the solid residue oil in a 150 ℃ oven to be heated into a flowing state, fully stirring uniformly, sampling, respectively weighing 0.3446g and 0.3376g of parallel samples, placing the samples into two digestion tanks, and sequentially adding 8ml of HNO into the two digestion tanks3,2ml H2O21ml of HCl, then placing the digestion tank in a fume hood and standing for 15 min;
step three, placing the digestion tank cover which is kept stand in the fume hood in the step two into a microwave digestion instrument, and presetting digestion conditions as follows:
Starting the microwave digestion instrument with preset digestion conditions, and taking out the digestion tank after the digestion conditions are executed;
and step four, placing the digestion tank containing the sample on an acid removing plate, setting the temperature of the acid removing plate to be 200 ℃, until a drop of liquid remains in the digestion tank, transferring all the liquid in the digestion tank to a 50ml volumetric flask, adding ultrapure water into the volumetric flask containing the sample until a scale mark of 50ml is formed, wherein the appearance of the digestion sample after the sample is subjected to constant volume is clear yellowish liquid, and the acid concentration after the constant volume is less than or equal to 2%.
9. The rapid microwave digestion treatment method for solid residue containing oil according to claim 1, characterized in that: the method specifically comprises the following steps:
step one, cleaning a digestion tank, a 50ml volumetric flask, a beaker and a glass rod used in the test, and drying in an oven at 105 ℃ for 1 h;
step two, placing the solid residue oil-containing sample in a 100 ℃ oven to be heated into a flowing state, fully stirring uniformly, sampling and respectively weighing 0.6754g and 0.7112g of parallel samples to be placed in two digestion tanks, and sequentially adding 8ml of HNO into the two digestion tanks3,2ml H2O21ml of HCl, then placing the digestion tank in a fume hood and standing for 15 min;
step three, placing the digestion tank cover which is kept stand in the fume hood in the step two into a microwave digestion instrument, and presetting digestion conditions as follows:
starting the microwave digestion instrument with preset digestion conditions, taking out the digestion tank after the digestion conditions are executed, finding that the sample liquid in the digestion tank contains a small amount of solid particles, and continuously adding 4ml of HNO into the digestion tank in sequence3,、1ml H2O2And 0.5ml of HCl, starting preset digestion conditions, carrying out secondary microwave digestion, and executing the digestion conditionsAfter the completion, taking out the digestion tank;
and step four, placing the digestion tank containing the sample on an acid removing plate, setting the temperature of the acid removing plate to be 200 ℃, until a drop of liquid remains in the digestion tank, transferring all the liquid in the digestion tank to a 50ml volumetric flask, adding ultrapure water into the volumetric flask containing the sample to 50ml of scale mark, wherein the appearance of the digestion sample after the sample is subjected to constant volume is clear yellowish liquid, and the acid concentration after the constant volume is less than or equal to 2%.
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