CN101256123A - Pumping-filtering method and apparatus for quantitatively extracting nano educt - Google Patents
Pumping-filtering method and apparatus for quantitatively extracting nano educt Download PDFInfo
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- CN101256123A CN101256123A CNA2007101151259A CN200710115125A CN101256123A CN 101256123 A CN101256123 A CN 101256123A CN A2007101151259 A CNA2007101151259 A CN A2007101151259A CN 200710115125 A CN200710115125 A CN 200710115125A CN 101256123 A CN101256123 A CN 101256123A
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Abstract
The invention provides a nanometer precipitate fixed quantity abstraction pumping filtration method and a pumping filtration arrangement, which belongs to the field of nanometer precipitate quantitative determination technique, the device includes a pumping filtration machine, a waste liquor collecting flask, a sand core funnel, a cleaning nozzle, a supporting stand, an electrolyzing tank, a carrier frame and so on, using the device to carry the process of pumping filtration solves the loss of precipitate in the transfer process existing in the nanometer precipitate quantitative analysis procedure usually used at present, and improves the accuracy of nanometer precipitate fixed quantity abstraction. The arrangement integrates electrolysis, cleaning and pumping filtration, which reduces the trouble of electrolysing solution in the transfer process, and improves the test precision and provides exact data for new product development.
Description
Technical field
The present invention relates to a kind of nanometer precipitate quantitative measurement technology, particularly a kind of nanometer precipitate dose suction filtration method and suction filtration device.
Technical background
Precipitation strength is to improve the important means of the performance of steel, the quantitative test of nanometer precipitate is the steps necessary of high tough new product development, existing more advanced nanometer precipitate dose method is, at first sample is carried out electrolysis in electrolysis cup, the powder that then electrolysis is obtained flushing, transfers on the filter paper, with electrolytic corrosion liquid by the cotton synthetic mistake filter core of acetone and pickling, the washing filtering core, to cross the filter core powder collection and transfer on the filter paper, carry out suction filtration, obtain clean nanometer powder.The 4th page of Chinese periodical " metallurgical analysis " 1992 the 2nd phase provides a kind of when unstable and fine precipitated phase quantitative test " in the steel cleaning method ", the shortcoming that above method exists is, nanometer powder liquid repeatedly shifts, cause the loss of certain amount of nano powder in the transfer process, influence result's accuracy.
Summary of the invention
For overcoming the defective of prior art, solve the loss of nanometer precipitate in transfer process that exists in the nanometer precipitate quantitative test process commonly used at present, improve the accuracy of nanometer precipitate dose, the invention provides a kind of nanometer precipitate dose suction filtration method and special-purpose suction filtration device.
Technical scheme of the present invention is as follows:
A kind of nanometer precipitate dose suction filtration method, step is as follows:
(1) sample production
The steel specimen size: cylindric rod iron, diameter of phi 10～15mm, long 100～200mm requires smooth surface, and roughness is not done specific requirement, and at one end there is a chase at 2～4mm place, is used for fixing the metal copper wire as anode;
(2) electrolyte quota, composed as follows by weight percentage:
Tetramethyl sal-ammoniac 5%～20%, diacetone 5%～20%, methyl alcohol 60%～90% are hybridly prepared into electrolytic solution;
(3) sample pretreatment:
Sample is put into above-mentioned electrolytic solution, electrolysis temperature-5 ℃～-30 ℃, current density 0.02～0.05A/cm2, electrolysis time 30～120 minutes is after electrolysis finishes, sample is taken out, scrub specimen surface with glue head glass bar, with 1% citric acid ethanolic solution flushing sample, till sample is clean, dry up with hair dryer, it is standby that sample is weighed;
This step is preelectrolysis, only as formal electrolysis pretreatnlent of sample; Be in order to obtain the weight difference of electrolysis sample accurately and further to remove the dirt of specimen surface and impurity carries out this step operation.
(4) sample electrolysis:
The electrolytic solution of step (2) is put into the electrolytic tank of this covering device, and the sample that step (3) was handled is put into the electrolytic solution of electrolytic tank again, electrolysis temperature-5 ℃～-30 ℃, current density 0.02～0.05A/cm2, electrolysis time 30～120 minutes., and dry up and weigh until totally with 1% citric acid ethanolic solution flushing specimen surface; Open the draining switch of electrolytic solution bottom, electrolytic solution and washing fluid are progressively put into following sand core funnel, carry out suction filtration;
(5) suction filtration:
Allow filtrate flow into the sand core funnel the inside together with electrolysate, open the dynamo-electric source of suction filtration and begin suction filtration, till suction filtration is done, with the residue on the 1% citric acid ethanolic solution flushing electrolysis sample, again with absolute ethyl alcohol flushing electrolysis sample, take out filter membrane, and wipe clean the electrolysate of leaving over of sand core funnel the inside with filter paper, filter membrane and filter paper are put into conical flask in the lump, in conical flask, pour the concentrated sulphuric acid into, decompose the sample electrolyte on filter membrane and filter paper and filter membrane and the filter paper, the sample electrolysis precipitate in the collection liquid is in order to the usefulness of next step quantitative test.
A kind of suction filtration device that is used for the special use of above-mentioned nanometer precipitate dose suction filtration method, comprise: suction filtration machine, waste collection bottle, sand core funnel, cleaning mouth, support, electrolytic tank and carriage, it is characterized in that waste collection bottle bottleneck and sand core funnel are tightly connected by frosting, the sand core funnel side pipe links to each other with the suction filtration machine by the suction filtration pipe, core and filter membrane are equipped with in going up in the bucket of sand core funnel, and filter membrane is positioned at the core top; The sand core funnel top is the electrolytic tank that is fixed on the support, and bottom of electrolytic tank is a leakage fluid dram.
Described waste collection bottle is fixed on the carriage.
Described electrolytic tank is made by stainless steel.
In the described electrolytic tank electrolytic solution is housed.
Described electrolytic tank top has the metal copper wire of hanging sample to be fixed on the support.
There is the cleaning mouth described electrolytic tank top.Clean mouth and also can respectively establish one in the sample both sides above electrolytic tank.
Connect flexible pipe under the described bottom of electrolytic tank leakage fluid dram, clamp flexible pipe as switch with iron clamp.Also can under described bottom of electrolytic tank leakage fluid dram, be connected to the stainless-steel tube of switch.
When using, under-5 ℃～-30 ℃ low temperature, operates in this this device.
When apparatus of the present invention are used, sample can be hung on the metal copper wire as anode, electrolytic tank is as negative electrode, sample immerses in the electrolytic solution can finish electrowinning process, then with the switch opens below the electrolytic tank, allow the waste liquid of finishing electrowinning process and electrolytic solution by core and filter membrane, can obtain clean nanometer powder on the filter membrane with as quantitative test.
The invention solves the loss of precipitate in transfer process that exists in the nanometer precipitate quantitative test process commonly used at present, improved the accuracy of nanometer precipitate dose.This device has reduced the trouble of electrolytic solution in transfer process, thereby has improved test accuracy, for new product development provides accurate data because electrolysis, flushing, suction filtration are integrated in one.
Description of drawings
Fig. 1 is apparatus of the present invention synoptic diagram, and Fig. 2 is the sand core funnel synoptic diagram in the suction filtration device of the present invention.
Wherein: 1-suction filtration machine, 2-suction filtration pipe, 3-waste collection bottle, the 4-sand core funnel, 5-core, 6-switch, 7-electrolytic solution, the 8-sample, 9-cleans mouth, 10-metal copper wire, 11-support, 12-filter membrane and husky core stationary installation, the 13-electrolytic tank, 14,15, the 16-carriage, the 17-filter membrane, 18-sand core funnel side pipe, going up of 19-sand core funnel struggles against.
Embodiment
Embodiment 1:
Present embodiment as shown in Figure 1, comprise: suction filtration machine 1, waste collection bottle 3, sand core funnel 4, cleaning mouth 9, support 11, electrolytic tank 13 and carriage 14,15,16, it is characterized in that waste collection bottle 3 is fixed on the carriage 16, waste collection bottle 3 bottlenecks tops and sand core funnel 4 are tightly connected by matte surface, the sand core funnel side pipe 18 of sand core funnel 4 one sides links to each other with suction filtration machine 1 by suction filtration pipe 2, core 5 and filter membrane 17 are equipped with in sand core funnel 4 the insides, filter membrane 17 is positioned at core 5 tops, is fixed by filter membrane and husky core stationary installation 12; Sand core funnel 4 tops are the electrolytic tanks 13 that are fixed on the support 11, and electrolytic tank 13 belows connect flexible pipe, clamp flexible pipe as switch 6 with iron clamp, and electrolytic solution 7 is housed in the electrolytic tank 13; Side, electrolytic tank 13 top is to clean mouth 9, is metal copper wire 10 directly over the electrolytic tank 13, can hang sample 8, and package unit is positioned in the big volume refrigerator.Described electrolytic tank 13 is made by stainless steel.
Embodiment 2:
As shown in Figure 1, a kind of nanometer precipitate dose suction filtration method, step is as follows:
(1) sample production:
The steel specimen size: cylindric rod iron, diameter of phi 15mm, long 200mm requires smooth surface, and roughness is not done specific requirement, and at one end there is a chase at the 4mm place, will be fastened on this chase place as the metal copper wire 10 of anode;
(2) electrolyte quota:
Composed as follows, by weight percentage:
Tetramethyl sal-ammoniac 20%, diacetone 20%, methyl alcohol 60% are mixed with electrolytic solution;
(3) sample pretreatment:
This electrolytic process does not carry out in the electrolytic tank shown in Fig. 1 13, only as the formally pre-service of electrolysis sample 8;
(4) sample electrolysis:
(5) suction filtration:
Allow filtrate flow into sand core funnel 4 the insides together with electrolysate, open suction filtration machine 1 power supply and begin suction filtration, till suction filtration is done,, wash with absolute ethyl alcohol again with 1% citric acid ethanolic solution flushing residue, take out filter membrane 17, and wipe clean the electrolysate of leaving over of sand core funnel 4 the insides with filter paper, and put into conical flask in the lump, pour the concentrated sulphuric acid into and decompose experimental sample and filter membrane filter paper, collect the usefulness of active principle, under-30 ℃ of low temperature, operate when this device uses in order to next step quantitative test.
Embodiment 3:
As shown in Figure 1, a kind of nanometer precipitate dose suction filtration method, step is as follows:
(1) sample production:
The steel sample is made Φ 12mm, and the rod iron of long 100mm requires smooth surface, and at one end there is a chase at the 2mm place, so that the fixed anode wiring;
(2) electrolyte quota:
By weight percentage: 10% tetramethyl sal-ammoniac, 10% diacetone, 80% methyl alcohol is mixed with solution;
(3) sample pretreatment:
This electrolytic process does not carry out in the electrolytic tank shown in Fig. 1 13, only as the formally pre-service of electrolysis sample 8;
(4) sample electrolysis:
(5) suction filtration:
Filtrate is put into sand core funnel 4 together with electrolysate, open suction filtration machine 1 power supply and begin suction filtration, till suction filtration is done, with 1% citric acid ethanolic solution flushing residue, wash with absolute ethyl alcohol again, take out filter membrane 17, and wipe clean electrolysate on the filter bowl with filter paper, put into the 250ml conical flask, pour the 20ml concentrated sulphuric acid into and decompose experimental sample and filter membrane filter paper, surely dissolve in the 100ml volumetric flask after the test solution clarification, collect the usefulness of active principle, under-30 ℃ of low temperature, operate when this device uses in order to next step quantitative test.
Embodiment 4:
As shown in Figure 1, a kind of nanometer precipitate dose suction filtration method, step is as follows:
(1) sample production:
The steel specimen size: Φ 10mm, long 100mm requires smooth surface, and roughness is not done specific requirement, and at one end there is a chase at the 2mm place, will be fastened on this chase place as the metal copper wire 10 of anode;
(2) electrolyte quota:
Composed as follows, by weight percentage:
Tetramethyl sal-ammoniac 5, diacetone 5%, methyl alcohol 90% are mixed with electrolytic solution;
(3) sample pretreatment:
This electrolytic process does not carry out in the electrolytic tank shown in Fig. 1 13, only as the formally pre-service of electrolysis sample 8;
(4) sample electrolysis:
(5) suction filtration:
Allow filtrate flow into sand core funnel 4 the insides together with electrolysate, open suction filtration machine 1 power supply and begin suction filtration, till suction filtration is done,, wash with absolute ethyl alcohol again with 1% citric acid ethanolic solution flushing residue, take out filter membrane 17, and wipe clean the electrolysate of leaving over of sand core funnel 4 the insides with filter paper, and put into conical flask in the lump, pour the concentrated sulphuric acid into and decompose experimental sample and filter membrane filter paper, collect the usefulness of active principle, under-5 ℃ of low temperature, operate when this device uses in order to next step quantitative test.
Claims (8)
1. nanometer precipitate dose suction filtration method, step is as follows:
(1) sample production
The steel specimen size: cylindric rod iron, diameter of phi 10～15mm, long 100～200mm requires smooth surface, and roughness is not done specific requirement, and at one end there is a chase at 2～4mm place, is used for fixing the metal copper wire as anode;
(2) electrolyte quota, composed as follows by weight percentage:
Tetramethyl sal-ammoniac 5%～20%, diacetone 5%～20%, methyl alcohol 60%～90% are hybridly prepared into electrolytic solution;
(3) sample pretreatment:
Sample is put into above-mentioned electrolytic solution, electrolysis temperature-5 ℃～-30 ℃, current density 0.02～0.05A/cm2, electrolysis time 30～120 minutes is after electrolysis finishes, sample is taken out, scrub specimen surface with glue head glass bar, and with 1% citric acid ethanolic solution flushing sample, till sample is clean, dry up with hair dryer, it is standby that sample is weighed;
(4) sample electrolysis:
The electrolytic solution of step (2) is put into electrolytic tank, and the sample that step (3) was handled is put into the electrolytic solution of electrolytic tank again, electrolysis temperature-5 ℃～-30 ℃, current density 0.02～0.05A/cm2, electrolysis time 30～120 minutes; , and dry up and weigh until totally with 1% citric acid ethanolic solution flushing specimen surface; Open the draining switch of electrolytic solution bottom, electrolytic solution and washing fluid are progressively put into following sand core funnel, carry out suction filtration;
(5) suction filtration:
Allow filtrate flow into the sand core funnel the inside together with electrolysate, open the dynamo-electric source of suction filtration and begin suction filtration, till suction filtration is done, with the residue on the 1% citric acid ethanolic solution flushing electrolysis sample, again with absolute ethyl alcohol flushing electrolysis sample, take out filter membrane, and wipe clean the electrolysate of leaving over of sand core funnel the inside with filter paper, filter membrane and filter paper are put into conical flask in the lump, in conical flask, pour the concentrated sulphuric acid into, decompose the sample electrolyte on filter membrane and filter paper and filter membrane and the filter paper, the sample electrolysis precipitate in the collection liquid is in order to the usefulness of next step quantitative test.
2, a kind of suction filtration device that is used for the described nanometer precipitate of claim 1 dose suction filtration method, comprise: suction filtration machine, waste collection bottle, sand core funnel, cleaning mouth, support, electrolytic tank and carriage, it is characterized in that waste collection bottle bottleneck and sand core funnel are tightly connected by frosting, the sand core funnel side pipe links to each other with the suction filtration machine by the suction filtration pipe, core and filter membrane are equipped with in going up in the bucket of sand core funnel, and filter membrane is positioned at the core top; The sand core funnel top is the electrolytic tank that is fixed on the support, and bottom of electrolytic tank is a leakage fluid dram.
3, suction filtration device as claimed in claim 2 is characterized in that described waste collection bottle is fixed on the carriage.
4, suction filtration device as claimed in claim 2 is characterized in that described electrolytic tank made by stainless steel.
5, suction filtration device as claimed in claim 2 is characterized in that in the described electrolytic tank electrolytic solution being housed.
6, suction filtration device as claimed in claim 2 is characterized in that described electrolytic tank top has the metal copper wire of hanging sample to be fixed on the support.
7, suction filtration device as claimed in claim 2 is characterized in that there is the cleaning mouth described electrolytic tank top.
8, suction filtration device as claimed in claim 2 is characterized in that connecing flexible pipe under the described bottom of electrolytic tank leakage fluid dram, clamps flexible pipe as switch with iron clamp.
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| CN2007101151259A CN101256123B (en) | 2007-11-30 | 2007-11-30 | Pumping-filtering method and apparatus for quantitatively extracting nano educt |
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| CN2007101151259A CN101256123B (en) | 2007-11-30 | 2007-11-30 | Pumping-filtering method and apparatus for quantitatively extracting nano educt |
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| CN101256123B CN101256123B (en) | 2010-07-14 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866053A (en) * | 2012-09-14 | 2013-01-09 | 济南市环境保护科学研究院 | Durable organic matter large-volume water sample separation and concentration device |
| CN105920895A (en) * | 2016-07-03 | 2016-09-07 | 肖雄 | Graphene oxide suction filtration device |
| CN107376488A (en) * | 2017-08-15 | 2017-11-24 | 江苏省环境监测中心 | Suitable for the filtration in-situ system of the water sample containing heavy metal |
| CN117110128A (en) * | 2023-10-24 | 2023-11-24 | 中国航发北京航空材料研究院 | Quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0668244A1 (en) * | 1994-02-18 | 1995-08-23 | National Research Development Corporation | Effluent treatment involving electroflotation |
| CN100593706C (en) * | 2007-03-29 | 2010-03-10 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN201107229Y (en) * | 2007-11-30 | 2008-08-27 | 莱芜钢铁集团有限公司 | Continuous type nanometer precipitate fixed quantity abstraction pumping filtration apparatus |
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2007
- 2007-11-30 CN CN2007101151259A patent/CN101256123B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866053A (en) * | 2012-09-14 | 2013-01-09 | 济南市环境保护科学研究院 | Durable organic matter large-volume water sample separation and concentration device |
| CN102866053B (en) * | 2012-09-14 | 2015-01-07 | 济南市环境保护科学研究院 | Durable organic matter large-volume water sample separation and concentration device |
| CN105920895A (en) * | 2016-07-03 | 2016-09-07 | 肖雄 | Graphene oxide suction filtration device |
| CN107376488A (en) * | 2017-08-15 | 2017-11-24 | 江苏省环境监测中心 | Suitable for the filtration in-situ system of the water sample containing heavy metal |
| CN117110128A (en) * | 2023-10-24 | 2023-11-24 | 中国航发北京航空材料研究院 | Quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy |
| CN117110128B (en) * | 2023-10-24 | 2024-01-30 | 中国航发北京航空材料研究院 | Quantitative test method for gamma' -phase mass fraction in nickel-based powder superalloy |
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