CN101308064B - Agitation type cadmium reduction rod preparation method - Google Patents
Agitation type cadmium reduction rod preparation method Download PDFInfo
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- CN101308064B CN101308064B CN 200810071398 CN200810071398A CN101308064B CN 101308064 B CN101308064 B CN 101308064B CN 200810071398 CN200810071398 CN 200810071398 CN 200810071398 A CN200810071398 A CN 200810071398A CN 101308064 B CN101308064 B CN 101308064B
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Abstract
Disclosed is a process for preparing a stirring cadmium reduction rod, which relates to a cadmium reduction rod. The invention provides a method for producing the stirring cadmium reduction rod by using a copper-plated cadmium film as a reducing medium to stir to reduce nitrate in the water sample into nitrite, and comprising the following steps of: cleaning the stirring magneton respectively with organic solvent and water, and making at least two ring-shaped grooves on the surface of the stirring magneton after the magneton is dried in order to allow water sample flowing through the grooves while stirring; soaking the cadmium film into an acid solution, removing oxide from the cadmium film and then rinsing the cadmium film with water to be neutral; wrapping the stirring magneton which is made with the grooves with the pretreated cadmium film to produce a stirring rod; and soaking the stirring rod into a bivalent copper ion solution, plating a copper layer on the cadmium film, then rinsing the copper-plated cadmium film with water to remove the residual copper ion solution on the surface, as a result, the stirring cadmium reduction rod is produced.
Description
Technical field
The present invention relates to a kind of cadmium reduction rod, especially relate to a kind ofly take copper facing cadmium film as reducing medium, can the limit be the preparation method of the agitation type cadmium reduction rod of nitrite with the nitrate reduction in the water sample when stir on the limit.
Background technology
The Cadmium column reduction method is to measure at present nitrate (NO
3 -) common method, its process is: the cadmium grain of certain particle diameter is immersed in certain density Cu
2+In the solution, make the cadmium grain plate layer of copper, then be seated in and make the cadmium reduction column in the glass tube, the water sample that will contain nitrate passes through the cadmium reduction column with certain flow rate, and then nitrate is reduced into nitrite, then nitrite P-aminobenzene-sulfonamide diazotising, again with hydrochloric acid N-(1-naphthyl) ethylenediamine coupling, form azo dyes rosy, measure in the 540nm place, obtain the content of nitrate.Though the method has higher reduction efficiency to nitrate, troublesome poeration, air easily enter the cadmium post and produce bubble, cause reduction efficiency unstable, even damage the cadmium post.(Zhang Tianhui, Wang Haiying, the Heilungkiang environment circular such as Zhang Tianhui, 2003,27 (1): 88-89) then directly with copper facing cadmium grain and nitrate sample mix to be measured, certain hour vibrates in oscillator, thereby nitrate reduction is become nitrite, and the recycling spectrophotometric method is measured.Though the method has solved the impact of traditional cadmium post bubble, very loaded down with trivial details during cadmium grain regeneration step, be difficult to reclaim and use.Therefore be necessary to develop the mode of operation of new Cadmium column reduction.
Summary of the invention
The present invention aims to provide a kind of take copper facing cadmium film as reducing medium, can the limit be the preparation method of the agitation type cadmium reduction rod of nitrite with the nitrate reduction in the water sample when stir on the limit.
Technical scheme of the present invention is as reducing medium take the cadmium film, it is wrapped on the notched stirring magneton, namely make agitation type cadmium reduction rod after the copper facing, this rod can be when stirring is nitrite with the nitrate reduction in the water sample, have and need not to fill post, easy and simple to handle, can be repeatedly used, use procedure can not produce the advantages such as bubble.
Agitation type cadmium reduction rod of the present invention is provided with the stirring magneton, stirs magneton and is provided with at least 2 road annular grooves, is stirring magneton surface parcel one deck cadmium film.Described annular groove is preferably 2～36 roads.
The present invention includes following steps:
1) stirs scribing of magneton groove: will stir magneton and clean with organic solvent and water respectively, and after the drying, make at least 2 road annular grooves stirring the magneton surface, in order to allow water sample mobile by groove when stirring;
2) pre-service of cadmium film: the cadmium film is inserted acid solution soak, remove the oxide on the cadmium film, then the water flushing is to neutral;
3) the cadmium film is at the parcel that stirs on the magneton: pretreated cadmium film is wrapped on the reeded stirring magneton of making, makes stirring rod;
4) copper facing of cadmium film: place bivalent cupric ion solution to soak stirring rod, at cadmium film plating layer of metal copper, then use water rinse copper facing cadmium film, remove the copper ion solution of its remained on surface, namely get agitation type cadmium reduction rod.
The length that stirs magneton is preferably 0.5～5.0cm, stirs the magneton shape and can be olive shape or cylindrical etc., and organic solvent can be selected at least a in ethanol, acetone, the methyl alcohol etc., best 2～36 roads of annular groove.
The thickness of cadmium film is preferably 0.025～1.0mm, and the area of cadmium film is preferably 1.0～30cm
2, number percent by volume, the concentration of acid solution is 1.0%～20%, and the time of immersion is preferably 0.5～10min, and described acid is preferably at least a in hydrochloric acid, sulfuric acid or the nitric acid etc.
Number percent by volume, the concentration of bivalent cupric ion solution is preferably 0.5%～10%, and the time of immersion is preferably 0.5～20min, and described bivalent cupric ion solution can be used copper-bath, copper chloride solution or Schweinfurt green solution.
The present invention utilizes copper facing cadmium film as the reductive agent of nitrate, can be when stirring be nitrite with the nitrate reduction in the water sample, have that preparation is simple, easy to operate, the reduction rod long service life and use in can not produce the advantage such as bubble.Can prepare length, reduction rod that thickness is different by demand in the practical application.
Description of drawings
Fig. 1 is the structural representation of the agitation type cadmium reduction rod that makes of the embodiment of the invention 2.
Fig. 2 is the SEM figure of cadmium film after the acid treatment in the embodiment of the invention 2.
Fig. 3 is the SEM figure of cadmium film after the copper facing in the embodiment of the invention 2.
Embodiment
The present invention is further illustrated below by embodiment.
1) stir scribing of magneton groove: get the long olive-type of a 0.5cm and stir magneton, use respectively methyl alcohol, distilled water cleans, and then oven dry carves 2 road grooves on its surface.
2) pre-service of cadmium film: get a thickness 0.025mm, area 1.0cm
2, insert 1.0ml, concentration is to soak 0.5min in the sulfuric acid solution of 1.0% (V/V) to remove the oxide on the cadmium film, then the water flushing is to neutral.
3) parcel of cadmium film on the stirring magneton: above-mentioned pretreated cadmium film is wrapped on the notched stirring magneton, makes stirring rod.
4) copper facing of cadmium film: it is that the copper chloride solution of 0.5% (m/V) soaks 0.5min that above-mentioned stirring rod is placed 1.0ml concentration, make the cadmium film plate certain metallic copper, then use gently rinsing copper facing cadmium film of distilled water water, remove its surperficial copper chloride solution, namely get agitation type cadmium reduction rod.
Referring to Fig. 1～3, scribing of stirring magneton groove is similar to Example 1, is acetone but clean used organic solvent, and stirring magneton 1 is column type, length 3.0cm, cutting 12 roads.The cadmium film thickness is 0.1mm, area 15cm
2, be the hydrochloric acid solution immersion 3min of 10% (V/V) with concentration, remove its surperficial oxide, then extremely neutral with distilled water flushing.This cadmium film is wrapping on the stirring magneton of cutting and makes stirring rod.This rod inserted in the copper-bath that 50ml concentration is 2.0% (m/V) soak 1.0min, make and plate layer of metal copper on the cadmium film, then with distilled water rinsing copper facing cadmium film 2 gently, remove residual copper-bath, namely get agitation type cadmium reduction rod.Fig. 1 provides the structural representation of the agitation type cadmium reduction rod that the embodiment of the invention 2 makes, and Fig. 2 provides the SEM figure of cadmium film after the acid treatment in the embodiment of the invention 2, and Fig. 3 provides the SEM figure of cadmium film after the copper facing in the embodiment of the invention 2.
Embodiment 3
It is similar to Example 1 to stir scribing of magneton groove, is ethanol but clean used organic solvent, and the stirring magneton is column type, length 5.0cm, cutting 36 roads.The cadmium film thickness is 1.0mm, area 30cm
2, be the hydrochloric acid solution immersion 10min of 20% (V/V) with concentration, remove its surperficial oxide, then extremely neutral with distilled water flushing.This cadmium film is wrapping on the stirring magneton of cutting and makes stirring rod.This rod inserted in the Schweinfurt green solution that 100ml concentration is 10% (m/V) soak 20min, make and plate layer of metal copper on the cadmium film, then with distilled water rinsing copper facing cadmium film gently, remove residual Schweinfurt green solution, namely get agitation type cadmium reduction rod.
Embodiment 4
Get the water sample 100ml that contains nitrate, add the NH of 3ml
4Cl buffer solution adjust pH to 8.0 is put into water sample with the agitation type cadmium reduction rod of embodiment 2, stirs reduction 30min.Get the supernatant 50ml of water sample after stirring in color comparison tube, the P-aminobenzene-sulfonamide solution that adds 1.0ml 1% (m/V), behind 1.0min, add again two hydrochloric acid of 1.0ml 0.1% (m/V)-1-naphthodiamide solution, colour developing, after stablizing 5.0min, detect at the 540nm place with spectrophotometer, measure light absorption value.
Embodiment 5
Get Bank in Shenhu Bay water sample 100ml, behind Filter paper filtering, add the NH of 3ml
4Cl buffer solution adjust pH to 8.0 is put into water sample with the agitation type cadmium reduction rod of embodiment 2, stirs reduction 30min.Get the supernatant 50ml of water sample after stirring in color comparison tube, the P-aminobenzene-sulfonamide solution that adds 1.0ml 1% (m/V), behind 1.0min, add again two hydrochloric acid of 1.0ml 0.1% (m/V)-1-naphthodiamide solution, colour developing, after stablizing 5.0min, detect at the 540nm place with spectrophotometer, recording light absorption value is 0.424.
Claims (10)
1. the preparation method of an agitation type cadmium reduction rod is characterized in that may further comprise the steps:
1) stirs scribing of magneton groove: will stir magneton and clean with organic solvent and water respectively, and after the drying, make at least 2 road annular grooves stirring the magneton surface, in order to allow water sample mobile by groove when stirring;
2) pre-service of cadmium film: the cadmium film is inserted acid solution soak, remove the oxide on the cadmium film, then the water flushing is to neutral;
3) the cadmium film is at the parcel that stirs on the magneton: pretreated cadmium film is wrapped on the reeded stirring magneton of making, makes stirring rod;
4) copper facing of cadmium film: place bivalent cupric ion solution to soak stirring rod, at cadmium film plating layer of metal copper, then use water rinse copper facing cadmium film, remove the copper ion solution of its remained on surface, namely get agitation type cadmium reduction rod.
2. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1, the length that it is characterized in that stirring magneton is 0.5～5.0cm.
3. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 or 2, it is characterized in that stirring magneton is that olive shape stirs magneton or cylindrical stirring magneton.
4. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 is characterized in that organic solvent is selected from least a in ethanol, acetone, the methyl alcohol.
5. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 is characterized in that annular groove is 2～36 roads.
6. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1, the thickness that it is characterized in that the cadmium film is 0.025～1.0mm; The area of cadmium film is 1.0～30cm
2
7. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 is characterized in that by volume number percent, and the concentration of acid solution is 1.0%～20%, and the time of immersion is 0.5～10min.
8. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 is characterized in that described acid is at least a in hydrochloric acid, sulfuric acid or the nitric acid.
9. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 is characterized in that by volume number percent, and the concentration of bivalent cupric ion solution is 0.5%～10%, and the time of immersion is 0.5～20min.
10. the preparation method of a kind of agitation type cadmium reduction rod as claimed in claim 1 is characterized in that described bivalent cupric ion solution is copper-bath, copper chloride solution or Schweinfurt green solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200810071398 CN101308064B (en) | 2008-07-12 | 2008-07-12 | Agitation type cadmium reduction rod preparation method |
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| CN 200810071398 CN101308064B (en) | 2008-07-12 | 2008-07-12 | Agitation type cadmium reduction rod preparation method |
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| CN101308064A CN101308064A (en) | 2008-11-19 |
| CN101308064B true CN101308064B (en) | 2013-04-17 |
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| CN112458471A (en) * | 2020-10-23 | 2021-03-09 | 武汉拓材科技有限公司 | Cleaning device and method for ultra-high-purity cadmium rod |
| CN114085008B (en) * | 2021-12-07 | 2023-04-07 | 中原环保股份有限公司 | Environment-friendly method treatment process of ammonium nitrate condensation wastewater |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1973944A (en) * | 2006-09-25 | 2007-06-06 | 厦门大学 | Making process of integral stirring rod for solid phase extraction |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1973944A (en) * | 2006-09-25 | 2007-06-06 | 厦门大学 | Making process of integral stirring rod for solid phase extraction |
Non-Patent Citations (1)
| Title |
|---|
| 茅惠明.血清中硝酸盐的镀铜镉还原测定法.临床检验杂志.1995,13(1),6-8. * |
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