CN102478468A - Device and method for measuring water-soluble ions in solid sample - Google Patents
Device and method for measuring water-soluble ions in solid sample Download PDFInfo
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- CN102478468A CN102478468A CN2010105602945A CN201010560294A CN102478468A CN 102478468 A CN102478468 A CN 102478468A CN 2010105602945 A CN2010105602945 A CN 2010105602945A CN 201010560294 A CN201010560294 A CN 201010560294A CN 102478468 A CN102478468 A CN 102478468A
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- 239000007787 solid Substances 0.000 title claims abstract description 30
- 150000002500 ions Chemical class 0.000 title abstract description 23
- 238000000034 method Methods 0.000 title abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 60
- 210000004907 gland Anatomy 0.000 claims description 54
- 238000005259 measurement Methods 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 8
- 229920002379 silicone rubber Polymers 0.000 claims description 8
- 238000005352 clarification Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 4
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- 238000000691 measurement method Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 6
- 239000012153 distilled water Substances 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 6
- 239000011573 trace mineral Substances 0.000 description 10
- 235000013619 trace mineral Nutrition 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000002689 soil Substances 0.000 description 7
- 239000004945 silicone rubber Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 125000001183 hydrocarbyl group Chemical group 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 239000011435 rock Substances 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 3
- 239000011785 micronutrient Substances 0.000 description 3
- 235000013369 micronutrients Nutrition 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
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- 238000000605 extraction Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910002552 Fe K Inorganic materials 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
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- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
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- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
The invention discloses a device and a method for measuring water-soluble ions in a solid sample. The device comprises a bottle body, a bottle cap and a magnetic stirrer. A sealing ring is arranged between the bottle cap and the bottle body, and the bottle cap and the bottle body are connected by threads; the bottle cover is provided with an air inlet and an air outlet, the air inlet and the air outlet are provided with sealing covers, and the air inlet and the air outlet are in threaded connection with the sealing covers; the bottom in the bottle body is provided with a magnetic stirrer. Putting a solid sample into a bottle body of the device, adding distilled water, introducing inert gas, driving air out from an air outlet, uniformly stirring by using a magnetic stirrer, and standing to clarify a solution; the clear solution can be measured. The device and the method avoid the influence of air, extract a plurality of water-soluble ion components, do not need enrichment, can be directly analyzed, improve the accuracy and the repeatability of an analysis result, and have wide application.
Description
Technical field
The present invention relates to oil and gas geochemistry exploration technique field, say further, relate in a kind of solid sample water-soluble attitude ion measurement with device and assay method.
Background technology
Having found 40 in oil ash surplus, the modern analysis method plants trace element; Mainly migrate to the face of land with underground water with the trace element in the hydrocarbon-bearing pool, analyze the composition and the content of the water-soluble attitude ion of corresponding formation sample and can infer the oily information of underlying formation in view of the above with water-soluble attitude ionic means.
Current; In the oil and gas geochemistry exploration technique, the trace element analysis method of extracting in soil, the rock is to dissolve appearance with chloroazotic acid, measures with spectral instrument; What measure is the total content of soil part trace element; Be primary trace element and migration source content of elements sum in the soil, wherein primary micronutrient levels is represented as the background of soil content, has hydrocarbon-bearing pool migration source content of elements comprising the oil and gas geochemistry information of underlying formation.Existing problems: if primary micronutrient levels is very high, migration source content of elements variation tendency is just not obvious, also just can't judge the oil and gas geochemistry information of underlying formation.
In recent years; In the big investigation of land resources geology field; The Elemental Speciation Analysis method more and more receives field workers' such as geochemistry, environmental chemistry and agricultural sciences great attention in the pedotheque, the main trace element that adopts the vibration extraction method to extract sample intermediate ion exchange state (comprising water-soluble attitude), carbonate combined state, humic acid combined state, iron and manganese oxides combined state, strong organic combined state forms such as (comprising the partial vulcanization thing).
At present; Also do not extract water-soluble attitude ion determination method and apparatus in the solid samples such as soil, rock separately; For overcoming the above problems, it is more and more urgent to develop in the solid samples such as a kind of suitable extraction soil, rock water-soluble attitude ion determination method and apparatus.
Summary of the invention
Reconnoitre the technological existing problem of trace element in the solid sample of extracting for solving oil and gas geochemistry, the invention provides in a kind of solid sample water-soluble attitude ion measurement and use device and method.Can extract the water-soluble attitude ion of hydrocarbon-bearing pool migration source trace element in the solid samples such as soil, rock, guarantee to analyze the accuracy of data and effectively obtain the oil and gas geochemistry information that sample contained.
The purpose of this invention is to provide in a kind of solid sample water-soluble attitude ion measurement and use device.
Determinator of the present invention comprises bottle and bottle cap, and bottle is placed on the magnetic stirring apparatus, and the bottle inner bottom part is placed magnetic agitation.
In the said bottle cap screw thread is arranged, bottle cap adopts with bottle and is threaded; Being provided with O-ring seal between bottle cap and the bottle seals; Bottle cap preferably is provided with anti-skidding line outward.
Air intake opening and gas outlet are set on the said bottle cap, and air intake opening is provided with the air intake opening gland bonnet, in the air intake opening gland bonnet screw thread is arranged, and the air intake opening gland bonnet adopts with air intake opening and is threaded; The gas outlet is provided with the gas outlet gland bonnet, in the gland bonnet of gas outlet screw thread is arranged, and the gas outlet gland bonnet adopts with the gas outlet and is threaded; Be provided with sealing gasket between air intake opening gland bonnet, gas outlet gland bonnet and the bottle cap; Said air intake opening gland bonnet, gas outlet gland bonnet preferably are provided with anti-skidding line outward.
The quantity of air intake opening, gas outlet respectively is preferably more than one; And symmetry or evenly distribution on bottle cap; On at least one air intake opening gland bonnet blow vent is set, the air intake opening below is connected with draft tube in the bottle, and draft tube can select for use the suitable and harder plastic tube of size directly to insert air intake opening.
The material of the above O-ring seal and sealing gasket is preferably silicon rubber.
Said bottle is preferably transparent, wide-mouth bottle; The bottle subscript is marked with scale.
Said bottle can be processed with transparent material, optimization polycarbonate, and the bottle shape can be to shapes such as cylinder, rectangular parallelepiped, squares, and is preferably cylindric.
Two of the object of the invention provides water-soluble attitude ion measurement method in a kind of solid sample.
Comprise following steps:
(1) solid sample is put into the bottle of the water-soluble attitude ion measurement of said solid sample with device, adding distil water covers tight bottle cap, air intake opening gland bonnet and gas outlet gland bonnet;
(2) open the gas outlet gland bonnet, in bottle, feed inert gas through draft tube, drive air away, cover tight gas outlet gland bonnet, leave standstill after evenly, make the solution clarification with magnetic stirrer from the gas outlet from air intake opening;
(3) open bottle cap, extract clarified solution with pipettor and measure.
Specific operation process is following:
The sample pretreatment technology: bottle cap is opened in (1), takes by weighing solid sample 10-100g in sample bottle, adds magnetic agitation, adds 100-300mL distilled water, the bottle cap of screwing, air intake opening gland bonnet and gas outlet gland bonnet; If solid sample is also can directly carry out pre-service by above-mentioned steps (1) without dried and crushed after the fresh pedotheque collection; If solid sample is not a fresh sample, in order to be easy to disperse, can the solid sample that dry be pulverized, preferably be dispersed to 74-100 μ m.
(2) open the gas outlet gland bonnet, feed sufficient N with syringe needle through air intake opening silicone rubber seal pad, draft tube from blow vent
2Or other inert gas is to drive air away, the preferred 5-10min of duration of ventilation; The gas outlet gland bonnet of screwing is extracted the syringe needle of air intake opening, is under (25 ± 5) ℃ condition in temperature, and is even with magnetic stirrer, preferably stirs 0.5-3.0h, leaves standstill 12-24h, makes the solution clarification of sample top;
(3) open bottle cap, extract the 10-50ml clarified solution with pipettor and measure.
Described mensuration can comprise the various analytical tests that need carry out water-soluble attitude ion in the solid sample in the prior art, for example comprises following various analytical technology:
1. measure water-soluble attitude elements K, Na, Ca, Mg, Fe, Al, Cd, Co, Cr, Cu, Mn, V, Ni, Pb, Zn etc. with plasma emission spectrometer (ICP-OES);
2. measure water-soluble attitude zwitterion: F with ion chromatograph (IC)
-, Cl
-, SO
4 2-, NO
3 -, NO
2 -, AC
-, K
+, Na
+, Ca
2+, Mg
2+, Al
3+, Cu
2+, Zn
2+Deng;
3. measure water-soluble attitude trace elements As, Hg, Sb, Bi etc. with atomic fluorescence appearance (AFS); Measure water-soluble attitude trace element W, Mo with polarograph; Dichromate method is measured Fe
2+
Sample bottle in the sample pretreatment apparatus and corollary apparatus are that polycarbonate is processed, and sealing gasket is a silastic material, and the sample bottle entire body is transparent, cylinder wide-mouth and be marked with the volume scale, and the back sample rapid reloading of being convenient to sample is unified and state observation with volume.The bottle inner wall smooth is convenient to clean, and is reusable.Selected material hardness of the present invention and elasticity are suitable, and general external force can not cause damage to it, is convenient to field construction and transportation.Between bottle cap and bottle, all adopt screw type to be threaded (detachably) between gland bonnet and bottle cap, after this device assembled, vacuumize from arbitrary reserved opening, in 24 hours, vacuum tightness is not seen obvious decline, good sealing effect.Under service condition, no stripping of bottle itself and volatilization organic component can not produce sample and pollute.
The present invention has adopted and has filled N
2Deng inert gas shielding, sealing, stirring and dissolving technology; Avoided air influence; Can more fully come out the water-soluble attitude ion dose in the solid sample and redox and new precipitation reaction can not take place component, the water-soluble attitude ion component that is extracted is many, and need not enrichment; Can directly analyze, improve precision of analysis and repeatability.
The present invention can handle dozens of even more sample simultaneously; Required reagent, material are few; The pre-service cost is low, according to the variation tendency of water-soluble attitude ion component and content on horizontal section or the longitudinal profile, can to a certain degree judge the oily information of underlying formation hydrocarbon-bearing pool.In the oil-gas exploration application test, obtained good effect.
Description of drawings
Fig. 1 sealed sample bottle structure figure
Description of reference numerals
1-1 air intake opening gland bonnet; 1-2 gas outlet gland bonnet; 2-1 air intake opening sealing gasket; 2-2 gas outlet sealing gasket; 3 gas outlets; 4 bottle caps; 5 bottles (mark scale); 6 distilled water; 7 solid samples; 8 magnetic stirring apparatuss; 9 blow vents; 10 O-ring seals; 11 draft tube; 12 magnetic agitation.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
As shown in Figure 1, water-soluble attitude ion measurement is used device in the solid sample of present embodiment, comprising:
Comprise bottle 5 and bottle cap 4, in the bottle cap 4 screw thread is arranged, be provided with silicone rubber O-ring 10 between bottle cap 4 and the bottle 5 and seal, bottle cap 4 adopts with bottle 5 and is threaded;
An air intake opening and a gas outlet 3 are set on the bottle cap 4, being distributed on the bottle cap symmetrically, air intake opening is provided with air intake opening gland bonnet 1-1, in the air intake opening gland bonnet 1-1 screw thread is arranged, and the air intake opening gland bonnet adopts with air intake opening and is threaded; Gas outlet 3 is provided with gas outlet gland bonnet 1-2, in the gland bonnet 1-2 of gas outlet screw thread is arranged, and gas outlet gland bonnet 1-2 adopts with the gas outlet and is threaded; Be provided with the silicone rubber seal pad between air intake opening gland bonnet 1-1, gas outlet gland bonnet 1-2 and the bottle cap 4;
Bottle is positioned on the magnetic stirring apparatus 8, and the bottle inner bottom part is placed magnetic agitation 12;
On the air intake opening gland bonnet 1-1 blow vent 9 is set, the air intake opening below is connected with draft tube 11 in the bottle, and draft tube 11 is the plastic tube of hard, directly inserts the air intake opening below;
Bottle cap 4, air intake opening gland bonnet 1-1, gas outlet gland bonnet 1-2 all have anti-skidding line;
Bottle 5 is processed for polycarbonate, and bottle is shaped as cylindric, and wide-mouth has scale on the bottle.
Embodiment 2
Above prosperous moral gas field, the distant basin of pine, drill through 1.5-1.6m pedotheque under the face of land with fried dough twist, dried and crushed is to 74-100 μ m.Open bottle cap, take by weighing solid sample 50g in sample bottle, add magnetic agitation, add 150mL distilled water.Open the gas outlet gland bonnet, feed sufficient N with syringe needle through air intake opening silicone rubber seal pad, draft tube from air intake opening
2Driving air away from the gas outlet, duration of ventilation 5min, the gas outlet gland bonnet of screwing is extracted the syringe needle of air intake opening, is under 25 ℃ of conditions in temperature, and is even with magnetic stirrer, stirs 1.5h, leaves standstill 24h, makes the solution clarification of sample top.Extract the 10mL clarified solution with pipettor and measure F with ion chromatograph
-, Cl
-, SO
4 2-, NO
3 -, NO
2 -, AC
-, K
+, Na
+, Ca
2+, Mg
2+Deng; Extract the 20mL clarified solution and measure Fe with dichromate method
2+Measure the result and see table 1.
Water-soluble attitude ion concentration (μ g/g) in the pedotheque of top, prosperous moral gas field, the loose distant basin of table 1
| The appearance number | Ca 2+ | Fe 2+ | K + | Mg 2+ | Na + | F - | CL - | NO 3 - | SO 4 2- | AC - | NO 2 - |
| CA01 | 44.72 | 0.31 | 2.97 | 38.97 | 342.08 | 46.29 | 146.48 | 7.17 | 71.04 | 0.65 | 0.69 |
| CA02 | 21.80 | 0.39 | 5.62 | 16.40 | 569.60 | 34.21 | 112.67 | 12.82 | 362.54 | 0.47 | 0.38 |
| CA03 | 24.92 | 0.36 | 4.87 | 31.04 | 406.40 | 67.58 | 81.83 | 5.55 | 91.41 | 0.58 | 0.46 |
| CA04 | 31.70 | 2.63 | 5.08 | 14.28 | 515.20 | 30.92 | 97.87 | 5.14 | 83.48 | 0.54 | 0.44 |
| CA05 | 44.36 | 0.46 | 5.51 | 12.01 | 843.60 | 31.68 | 180.11 | 5.82 | 558.45 | 0.51 | 0.39 |
| CA06 | 47.84 | 0.19 | 3.66 | 6.43 | 223.24 | 7.66 | 56.66 | 2.88 | 87.38 | 0.44 | 0.19 |
| CA07 | 76.56 | 0.01 | 2.38 | 17.88 | 118.00 | 9.09 | 61.01 | 2.10 | 56.32 | 0.26 | 0.19 |
| CA08 | 59.36 | 0.53 | 2.31 | 14.78 | 155.84 | 7.77 | 90.17 | 2.93 | 45.78 | 0.36 | 0.21 |
Above gas field, new field, Sichuan, drill through 1.5-1.6m pedotheque under the face of land with fried dough twist, dried and crushed is to 74-100 μ m.Open bottle cap, take by weighing solid sample 50g in sample bottle, add magnetic agitation, add 150mL distilled water.Open the gas outlet gland bonnet, feed sufficient N with syringe needle through air intake opening silicone rubber seal pad, draft tube from air intake opening
2Driving air away from the gas outlet, duration of ventilation 5min, the gas outlet gland bonnet of screwing is extracted the syringe needle of air intake opening, is under 25 ℃ of conditions in temperature, and is even with magnetic stirrer, stirs 1.5h, leaves standstill 24h, makes the solution clarification of sample top.Extracting the 40mL clarified solution with pipettor measures with plasma emission spectrometer.Measure the result and see table 2.
Table 2 plasma emission spectrometry is measured water-soluble micronutrient levels (μ g/g) in the pedotheque of gas field, new field, Sichuan
| The sample name | Al | Ca | Fe | K | Mg | Na |
| B1 | 0.80 | 119.10 | 0.05 | 2.42 | 17.52 | 14.64 |
| B2 | 0.96 | 88.26 | 0.07 | 2.07 | 10.15 | 10.51 |
| B3 | 0.50 | 207.30 | 0.01 | 3.56 | 24.03 | 110.70 |
| B4 | 2.41 | 83.28 | 1.31 | 1.61 | 13.26 | 12.02 |
| B5 | 0.42 | 41.06 | 0.37 | 0.36 | 9.16 | 2.36 |
| B6 | 2.06 | 68.28 | 0.59 | 0.61 | 5.87 | 3.39 |
| B7 | 1.07 | 93.72 | 0.46 | 2.70 | 11.54 | 9.01 |
| B8 | 5.73 | 88.14 | 3.52 | 3.28 | 11.64 | 7.57 |
| B9 | 42.44 | 81.84 | 21.47 | 6.52 | 21.73 | 14.24 |
| B10 | 1.19 | 91.14 | 0.10 | 0.92 | 11.86 | 11.07 |
| B11 | 0.57 | 54.25 | 0.17 | 0.60 | 10.73 | 6.04 |
| B12 | 0.96 | 160.92 | 0.02 | 1.53 | 18.88 | 11.93 |
| B13 | 1.03 | 89.04 | 0.32 | 1.25 | 17.34 | 11.60 |
| B14 | 0.02 | 25.15 | 0.02 | 0.33 | 4.97 | 0.68 |
| B15 | 14.56 | 21.48 | 1.60 | 1.50 | 5.78 | 4.55 |
| B16 | 0.57 | 45.64 | 0.01 | 1.21 | 13.73 | 2.18 |
Above Shandong Dongying Depression square king oil field, drill through 1.5-1.6m pedotheque under the face of land with fried dough twist, dried and crushed is to 74-100 μ m.Open bottle cap, take by weighing solid sample 50g in sample bottle, add magnetic agitation, add 150mL distilled water.Open the gas outlet gland bonnet, feed sufficient N with syringe needle through air intake opening silicone rubber seal pad, draft tube from air intake opening
2Driving air away from the gas outlet, duration of ventilation 5min, the gas outlet gland bonnet of screwing is extracted the syringe needle of air intake opening, is under 25 ℃ of conditions in temperature, and is even with magnetic stirrer, stirs 1.5h, leaves standstill 24h, makes the solution clarification of sample top.Extract the 10mL clarified solution with pipettor and measure F with ion chromatograph
-, Cl
-, SO
4 2-, NO
3 -, NO
2 -, AC
-, K
+, Na
+, Ca
2+, Mg
2+Deng; Extract the 20mL clarified solution and measure Fe with dichromate method
2+Measure the result and see table 3.
Water-soluble attitude ion concentration (μ g/g) in table 3 Shandong Dongying Depression square top, the king oil field pedotheque
| The appearance number | Ca 2+ | Fe 2+ | K + | Mg 2+ | Na + | F - | CL - | NO 3 | SO 4 2- | AC - | NO 2 - |
| PC1 | 105.52 | 0.04 | 2.55 | 31.70 | 83.40 | 2.19 | 93.64 | 16.01 | 274.79 | 0.18 | 0.14 |
| PC2 | 125.92 | 0.10 | 4.48 | 40.40 | 254.64 | 4.31 | 76.50 | 4.67 | 325.30 | 0.32 | 0.07 |
| PC3 | 100.96 | 0.14 | 2.93 | 19.01 | 176.52 | 3.06 | 243.17 | 74.16 | 610.58 | 0.10 | 0.06 |
| PC4 | 432.00 | 0.03 | 4.15 | 123.12 | 211.16 | 2.48 | 82.99 | 30.90 | 467.76 | 0.34 | 0.08 |
| PC5 | 278.20 | 0.04 | 5.64 | 103.60 | 215.40 | 2.17 | 103.53 | 4.81 | 2402.00 | 0.27 | 0.07 |
| PC6 | 143.56 | 0.05 | 7.69 | 44.08 | 96.80 | 2.19 | 105.65 | 177.63 | 1417.38 | 0.30 | 0.07 |
| PC7 | 188.96 | 0.05 | 4.51 | 42.72 | 89.88 | 2.15 | 56.92 | 8.98 | 500.49 | 0.34 | 0.07 |
| PC8 | 83.24 | 0.29 | 2.21 | 17.24 | 43.56 | 2.24 | 62.23 | 78.86 | 684.00 | 0.03 | 0.26 |
| PC9 | 357.12 | 0.01 | 7.56 | 146.08 | 216.92 | 2.41 | 29.57 | 53.81 | 128.20 | 0.12 | 0.04 |
| PC10 | 84.28 | 0.20 | 6.54 | 21.04 | 36.03 | 1.55 | 226.12 | 3.78 | 1399.10 | 0.15 | 0.05 |
| PC11 | 99.32 | 0.05 | 3.31 | 71.64 | 346.68 | 2.83 | 69.47 | 37.82 | 330.35 | 0.13 | 0.06 |
| PC12 | 66.60 | 0.45 | 2.87 | 16.02 | 180.32 | 4.74 | 415.07 | 70.06 | 391.65 | 0.03 | 0.06 |
| PC13 | 87.48 | 0.11 | 2.71 | 22.66 | 66.00 | 3.90 | 70.23 | 97.74 | 276.63 | 0.08 | 0.05 |
| PC14 | 354.52 | 0.02 | 5.27 | 83.84 | 181.04 | 2.17 | 44.29 | 78.03 | 151.04 | 0.07 | 0.05 |
| PC15 | 152.36 | 0.02 | 2.76 | 57.04 | 93.88 | 1.73 | 255.53 | 310.43 | 1306.54 | 0.20 | 0.05 |
| PC16 | 552.80 | 0.02 | 5.88 | 145.00 | 193.24 | 5.10 | 82.59 | 214.10 | 488.26 | 0.17 | 0.05 |
| PC17 | 202.96 | 0.01 | 5.96 | 48.32 | 77.28 | 2.17 | 223.40 | 296.98 | 2470.43 | 0.31 | 0.06 |
| PC18 | 49.04 | 1.86 | 3.17 | 8.11 | 148.16 | 1.65 | 53.82 | 55.18 | 719.93 | 0.12 | 0.07 |
Claims (8)
1. water-soluble attitude ion measurement is used device in the solid sample, comprises bottle and bottle cap, it is characterized in that:
In the said bottle cap screw thread is arranged, be provided with O-ring seal between bottle cap and the bottle and seal, bottle cap adopts with bottle and is threaded;
Air intake opening and gas outlet are set on the said bottle cap, and air intake opening is provided with the air intake opening gland bonnet, in the air intake opening gland bonnet screw thread is arranged, and the air intake opening gland bonnet adopts with air intake opening and is threaded; The gas outlet is provided with the gas outlet gland bonnet, in the gland bonnet of gas outlet screw thread is arranged, and the gas outlet gland bonnet adopts with the gas outlet and is threaded; Be provided with sealing gasket between air intake opening gland bonnet, gas outlet gland bonnet and the bottle cap;
Said bottle is positioned on the magnetic stirring apparatus, and the bottle inner bottom part is placed magnetic agitation.
2. device as claimed in claim 1 is characterized in that:
The quantity of said air intake opening, gas outlet respectively is more than one, and symmetry or evenly distribution on bottle cap.
3. like each described device of claim 1～2, it is characterized in that:
On said at least one air intake opening gland bonnet blow vent is set, the air intake opening below is connected with draft tube in the bottle.
4. sealing sampling bottle as claimed in claim 3 is characterized in that:
Said bottle cap, air intake opening gland bonnet, gas outlet gland bonnet all have anti-skidding line.
5. device as claimed in claim 1 is characterized in that:
The material of said O-ring seal and sealing gasket is a silicon rubber.
6. device as claimed in claim 1 is characterized in that:
Said bottle is transparent, wide-mouth bottle; The bottle subscript is marked with scale.
7. device as claimed in claim 6 is characterized in that:
Said bottle is that polycarbonate is processed, and bottle is shaped as cylindric.
8. water-soluble attitude ion measurement method in the solid sample adopts and measures with device like water-soluble attitude ion measurement in the described solid sample of one of claim 1～7, comprises following steps:
(1) solid sample is put into the bottle of the water-soluble attitude ion measurement of said solid sample with device, adding distil water covers tight bottle cap, air intake opening gland bonnet and gas outlet gland bonnet;
(2) open the gas outlet gland bonnet, in bottle, feed inert gas through draft tube, drive air away, cover tight gas outlet gland bonnet, leave standstill after evenly, make the solution clarification with magnetic stirrer from the gas outlet from air intake opening;
(3) open bottle cap, extract clarified solution with pipettor and measure.
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| CN105092314A (en) * | 2014-05-23 | 2015-11-25 | 中国石油化工股份有限公司 | Apparatus for collecting head-space gas, and method using apparatus |
| CN111413190A (en) * | 2019-01-07 | 2020-07-14 | 东莞东阳光科研发有限公司 | Carbon-coated lithium iron phosphate digestion device, digestion method and detection method |
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