CN104148009A - Composite bentonite material capable of quickly identifying hexavalent chromium ions in water with naked eyes as well as preparation method and application of material - Google Patents
Composite bentonite material capable of quickly identifying hexavalent chromium ions in water with naked eyes as well as preparation method and application of material Download PDFInfo
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- CN104148009A CN104148009A CN201410269879.XA CN201410269879A CN104148009A CN 104148009 A CN104148009 A CN 104148009A CN 201410269879 A CN201410269879 A CN 201410269879A CN 104148009 A CN104148009 A CN 104148009A
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Abstract
The invention discloses a composite bentonite material capable of quickly identifying hexavalent chromium ions in water with naked eyes as well as a preparation method and an application of the material. A core of the material is hydrophobic nano organic modified bentonite, wherein the core is connected with a color developing agent, namely diphenylcarbazide in a modifying manner through a hydrophobic carbon chain so as to form a novel composite bentonite material capable of identifying specificity of hexavalent chromium. The hydrophobic nano organic modified bentonite is prepared by modifying quaternary ammonium salt and has the characteristics that the content of montmorillonite is greater than 88%, cation exchange capacity is 80-130mmol/100g and the whiteness is 76-95. Through the composite bentonite material, the detection process is simple, no detection instrument is required, the cost is low, the labor intensity is low, no organic solvent is needed, the pollution to the environment is avoided, and the health of detection workers is guaranteed.
Description
Technical field
The invention belongs to water body detection technique field, be specifically related to composite bentonite material of hexavalent chromium in a kind of water body of naked eyes recognition detection fast and its preparation method and application.
Background technology
Chromium is a kind of metallic element that occurring in nature extensively exists, and is mainly distributed in rock, soil, atmosphere, water and organism.Chromium distributed pole in soil is wide, and content range is very wide; In water body and atmosphere, chromium content is less, contains trace chromium in animal and plant body.Nature chromium mainly exists with trivalent chromium and chromic form.Sugar in trivalent chromium participant and animal body and fatty metabolism, be human body mustn't trace element, Cr VI is clear and definite harmful element, can make the precipitation of some protein in blood of human body, cause the diseases such as anaemia, ephritis, neuritis, contact with Cr VI for a long time and also can cause respiratory inflammation, and bring out lung cancer or value volume causes invasive skin lesion, the poisoning Cr VI that also can cause of serious Cr VI is poisoning, even dead.
According to statistics, Cr VI be mainly derived from that the industries such as chrome ore smelting, refractory material, plating, process hides, weaving, printing and dyeing, pigment, stainless steel welding, cement and fire row emit containing chromium waste gas, waste water and waste residue etc.Cr VI is one of the easiest anaphylactic metal, is only second to nickel, and human body skin contact easily causes ulcer or allergic reaction.At present, the hexavalent chromium in water body has very strong toxicity, to human body with around biology, ecological environment etc. have toxic and potential risk.Cr VI has strong toxicity, it has been generally acknowledged that its toxicity is chromic 100 times, and is easily absorbed by the body and accumulation in vivo.Cr VI enters after human body by respiratory system, can cause rhinorrhea, sneezes, itch, go out nosebleed, ulcer and perforation of nasal septum etc.The contact of short-term heavy dose, can produce ulcer, schneiderian membrane stimulation, perforation of nasal septum in contact site.The Cr VI that absorption exceedes dosage cause kidney and liver damage, feel sick, intestines and stomach stimulation, gastric ulcer, spasm, even dead.A large amount of Cr VIs of taking in can produce the harmful effects such as carcinogenic, mutagenesis, teratogenesis, the Center for Disease Control harmful toxic matter and disease registration administration (ASDTR, CDC) one of 20 preferential materials that detect before 2007-2011 classifies Cr VI as every year.Environmental Protection Agency (EPA) is defined as Cr VI one of toxicant of 17 kinds of high concentration danger.Hexavalent chromium compound oral lethal dose is about 1.5g, and in water body, content exceedes 0.1mg/L and will produce intoxicating phenomenon.At present, Cr VI has become one of index of China's enforcement overall control.In China's " urban wastewater treatment firm pollutant emission standard ", the chromic concentration of regulation must not exceed 0.5mg/L.In standards for drinking water quality (GB5749-2006), specify that hexavalent chromium concentration is lower than 0.05mg/L.
In prior art, the method for determination of hexavalent chromium ion mainly contains spectrophotometer method, flame atomic absorption spectrometry, oscillopolarographic titation, dynamics photometry, flow injection spectroscopic methodology etc.The pre-treating method of the most of samples of these methods is comparatively complicated, and the instrument and equipment price relating to is comparatively expensive and be not easy to universal use, especially in some more remote areas.
Summary of the invention
The object of the invention is to overcome prior art defect, the composite bentonite material of hexavalent chromium in a kind of water body of naked eyes recognition detection is fast provided.
Another object of the present invention is to provide the preparation method of above-mentioned composite bentonite material.
A further object of the present invention is to provide the application of above-mentioned composite bentonite material.
Concrete technical scheme of the present invention is as follows:
The composite bentonite material of hexavalent chromium in a kind of water body of naked eyes recognition detection fast, the core of this material is hydrophobic nano organic modified bentonite, this core is connected and is modified with developer diphenylcarbazide by its hydrophobicity carbochain, this hydrophobic nano organic modified bentonite forms by quaternary ammonium salt-modified, its smectite content > 88%, cation exchange capacity is 80～130mmol/100g, and whiteness is 76～95.
In a preferred embodiment of the invention, described quaternary ammonium salt is at least one in tetramethyl ammonium chloride, etamon chloride, tetrabutylammonium chloride, dodecyl quaternary ammonium salt, cetyl quaternary ammonium salt and octadecyl quaternary ammonium salt.
A preparation method for above-mentioned composite bentonite material, comprises the steps:
(1) take developer and hydrophobic nano organic modified bentonite by the weight ratio of 1:2～200, evenly mix after 10～300min at the temperature of 5～50 DEG C with enough pure water, pure water washing and filtering must precipitate;
(2) by vacuum drying 1～48h at the above-mentioned temperature that is deposited in 40～80 DEG C, described composite bentonite material.
In a preferred embodiment of the invention, described developer and hydrophobic nano organic modified bentonite weight ratio are 1:10～20.
In a preferred embodiment of the invention, the temperature of described step (1) is room temperature.
In a preferred embodiment of the invention, described mixed uniformly mode comprises mechanical agitation, magnetic agitation and ultrasonic wave.
In a preferred embodiment of the invention, the described vacuum drying time is 1～24h.
A method of applying hexavalent chromium in above-mentioned composite bentonite material tests water body, comprises the steps:
(1) be mixed into slurries by taking described composite bentonite material and pure water with the weight ratio of 1:1～200;
(2) slurries in step (1) are pipetted to 0.3～20mL, add equably the vacuum filter upward filtration that contains one deck NC Nitroncellulose filter membrane in the middle of being placed in to anhydrate, the even diaphragm that formation one thickness is 0.5～20mm;
(3) in 10～200mL liquid to be detected, drip 5～50% the sulfuric acid of 0.5～5mL, regulate pH value to 2.0 ± 0.5;
(4) will regulate the liquid to be detected after pH to join on the even diaphragm of step (2) gained;
(5), after liquid to be detected sees through this even diaphragm colour developing completely, with Standard Colors card contrast, can obtain detecting and in liquid, contain chromic content.
The invention has the beneficial effects as follows:
1, detection method of the present invention adopts has good absorption property and a high nanometer organic modified bentonite of self whiteness to organic, be dispersed in water, its surface forms the organic environment of a tiny area around, as dissolving region insoluble or microsolubility organic matter developer, also the dispersant in water as them, utilized developer and hexavalent chromium in nanometer organic modified bentonite adsorbed water simultaneously, both can form distinctive change color, the variation of its characteristic color can be used as the reference frame of content of 6-valence Cr ions, the original position naked eyes of first Application heavy metal hexavalent chromium in water sample can fast recognition detection field, expand the bentonitic application at analytical chemistry ambit,
2, testing process of the present invention is simple, need to be by any detecting instrument, and with low cost, and labour intensity is low;
3, detection method of the present invention does not need to use any organic solvent, and environmentally safe has ensured testing staff's health;
4, the detectability of detection method of the present invention and traditional colorimetric method improves 50～1000 times, and detectability is lower than 10.0 μ g/L.
Brief description of the drawings
Fig. 1 be gradual change characteristic color prepared in embodiments of the invention 2 with reference to card (liquid to be measured of 0.3g nanometer organobentonite composite membrane, 100mL, detecting liquid, to see through the even diaphragm time be completely 45min);
Fig. 2 is the chromic recovery of standard addition curve (at the linear dependence R=0.9999 of 0～60mg/L) of embodiments of the invention 2;
Fig. 3 is the hexavalent chromium concentration of embodiments of the invention 2 and the correlation curve of characteristic color value.
Detailed description of the invention
By reference to the accompanying drawings technical scheme of the present invention is further detailed and is described by detailed description of the invention below.
Hydrophobic nano organic modified bentonite smectite content > 88% in following embodiment, cation exchange capacity is 80～130mmol/100g, whiteness is 76～95.
Embodiment 1
The composite bentonite material of hexavalent chromium in a kind of water body of naked eyes recognition detection fast, the core of this material is hydrophobic nano organic modified bentonite, this core is connected with developer diphenylcarbazide by its hydrophobicity carbochain, this hydrophobic nano organic modified bentonite forms by quaternary ammonium salt-modified, its smectite content > 88%, cation exchange capacity is 80～130mmol/100g, and whiteness is 76～95.Described quaternary ammonium salt is at least one in tetramethyl ammonium chloride, etamon chloride, tetrabutylammonium chloride, dodecyl quaternary ammonium salt, cetyl quaternary ammonium salt and octadecyl quaternary ammonium salt.
The preparation method of above-mentioned composite bentonite material comprises the steps:
(1) take developer and hydrophobic nano organic modified bentonite by the weight ratio of 1:2～200 (preferably 1:10～20), at the temperature of 5～50 DEG C, (preferably room temperature) evenly mixes after (comprising mechanical agitation, magnetic agitation and ultrasonic wave) 10～300min with enough pure water, and pure water washing and filtering must precipitate;
(2) by vacuum drying 1～48h (preferably 1～24h) at the above-mentioned temperature that is deposited in 40～80 DEG C, described composite bentonite material.
Embodiment 2
Fast detecting application process: what take 10.0g passes through quaternary ammonium salt-modified hydrophobic nano organic modified bentonite and the developer diphenylcarbazide of 1.0g, mass ratio is 10:1, be placed in the conical flask of clean 250mL, add the distilled water of 100mL, be placed on magnetic stirring apparatus in 5～50 DEG C and stir after 1h, form slurries for subsequent use.
The above-mentioned slurries of 5mL are got with clean liquid-transfering gun, drip equably on 0.22 μ m NC Nitroncellulose diaphragm new in vacuum apparatus, it is the even diaphragm of 0.5～20mm that uniform spreading open form becomes a thickness, described composite bentonite material is repeatedly washed with pure water, removes unnecessary impurity.
The hexavalent chromium solution (pH=1～4) that 100mL is contained to standard series concentration, add one by one in the container of vacuum apparatus upper strata, by the low to high beginning of concentration, in same time one by one by the even diaphragm of described composite bentonite material newly preparing, form serial gradual change characteristic color with reference to card, as shown in Figure 1.
In liquid to be measured (pH=1～4), contain certain density Cr VI solution, add in the container of vacuum apparatus upper strata, with in the former same time by freshly prepd nanometer organobentonite function diaphragm, form liquid color to be measured, compare with reference to card with aforementioned, obtain a reference value; Meanwhile, liquid to be measured (Duplicate Samples) enters accurate detection, obtains a detected value; Last reference value and detected value contrast, and determine the application performance of nanometer organobentonite function.As seen from Figure 1, in liquid to be measured, hexavalent chromium concentration is between 0～200 μ m/L, and characteristic color has good differentiation.
By mark-on method, the recovery of standard addition that described composite bentonite material is 0～60mg/L at hexavalent chromium concentration has good linearity, shows that this functional material has good adsorption effect and stability (as shown in Figure 2) to hexavalent chromium.
By specific hexavalent chromium concentration is carried out to numerical fitting, described composite bentonite material has good linearity between hexavalent chromium concentration and change color, shows that this functional material has linear trend (as shown in Figure 3) to hexavalent chromium feature colour developing gradual change.
Embodiment 3
(1) take the dodecyl sodium sulfate modified Nano bentonite of 10.0g and the developer diphenylcarbazide of 1.0g, be 1:10 in mass ratio, be placed in the conical flask of clean 250mL, add the distilled water of 100mL, be placed on magnetic stirring apparatus in 5～50 DEG C and stir after 1～5h, form slurries for subsequent use.
(2) use mark-on method, add certain potassium bichromate in the distilled water of 600mL, 3 parts of volumes of accurate measuring are that 100mL liquid to be detected and 3 parts of volumes are the detection liquid of 100mL as precision checking equipment;
(3) be that 100mL accurately detects as the detection liquid of precision checking equipment using 3 parts of volumes in step (2), its mean value is as the hexavalent chromium concentration value of this liquid to be measured;
(4), according to following step, be respectively that 100mL liquid to be detected passes through respectively freshly prepd even diaphragm separately by 3 parts of volumes of step (2):
A, the slurries in step (1) are pipetted to 0.3～20mL, add equably the vacuum filter upward filtration that contains one deck NC Nitroncellulose filter membrane in the middle of being placed in to anhydrate, the even diaphragm that to form a thickness be 0.5～20mm;
B, in 10～200mL liquid to be detected, drip 5～50% the sulfuric acid of 0.5～5mL, regulate pH value to 2.0 ± 0.5;
C, will regulate the liquid to be detected after pH slowly to join on the even diaphragm of step b gained;
(5) after liquid to be detected sees through this even diaphragm colour developing completely, by detecting complete even diaphragm color in step (4), contrast with standard proportional card, obtain hexavalent chromium concentration value in liquid to be measured;
(6) in concentration value contrast standard ratio card in step (5) being obtained and step (3), the accurate value detecting is proofreaded, and has obtained final concentration value, and the value that contrast obtains is comparatively good.
Embodiment 4
(1) take hexadecyltrimethylammonium chloride modified Nano bentonite and the diphenylcarbazide of certain mass, be 1:10 in mass ratio, be placed in the conical flask of clean 250mL, add the distilled water of 100mL, at the temperature of 5～50 DEG C, be placed in after ultrasonic sound appratus 0.5h～1h, form slurries for subsequent use.
(2) use mark-on method, add certain potassium bichromate in the running water of 600mL, 3 parts of volumes of accurate measuring are that 100mL liquid to be detected and 3 parts of volumes are the detection liquid of 100mL as precision checking equipment;
(3) be that 100mL accurately detects as the detection liquid of precision checking equipment using 3 parts of volumes in step (2), its mean value is as the hexavalent chromium concentration value of this liquid to be measured;
(4), according to following step, be respectively that 100mL liquid to be detected passes through respectively freshly prepd even diaphragm separately by 3 parts of volumes of step (2):
A, the slurries in step (1) are pipetted to 0.3～20mL, add equably the vacuum filter upward filtration that contains one deck NC Nitroncellulose filter membrane in the middle of being placed in to anhydrate, the even diaphragm that to form a thickness be 0.5～20mm;
B, in 10～200mL liquid to be detected, drip 5～50% the sulfuric acid of 0.5～5mL, regulate pH value to 2.0 ± 0.5;
C, will regulate the liquid to be detected after pH slowly to join on the even diaphragm of step b gained;
(5) after liquid to be detected sees through this even diaphragm colour developing completely, by detecting complete even diaphragm color in step (4), contrast with standard proportional card, obtain hexavalent chromium concentration value in liquid to be measured;
(6) in concentration value contrast standard ratio card in step (5) being obtained and step (3), the accurate value detecting is proofreaded, and has obtained final concentration value, and the value that contrast obtains is comparatively good.
Embodiment 5
(1) take the tetrabutylammonium chloride sodium modified Nano bentonite of 10.0g and the developer diphenylcarbazide of 0.5g, be 1:20 in mass ratio, be placed in the conical flask of clean 250mL, add the distilled water of 100mL, be placed on magnetic stirring apparatus in 5～50 DEG C and stir after 1h and 5h, form slurries for subsequent use.
(2) use mark-on method, add certain potassium bichromate in the distilled water of 600mL, 3 parts of volumes of accurate measuring are that 100mL liquid to be detected and 3 parts of volumes are the detection liquid of 100mL as precision checking equipment;
(3) be that 100mL accurately detects as the detection liquid of precision checking equipment using 3 parts of volumes in step (2), its mean value is as the hexavalent chromium concentration value of this liquid to be measured;
(4), according to following step, be respectively that 100mL liquid to be detected passes through respectively freshly prepd even diaphragm separately by 3 parts of volumes of step (2):
A, the slurries in step (1) are pipetted to 0.3～20mL, add equably the vacuum filter upward filtration that contains one deck NC Nitroncellulose filter membrane in the middle of being placed in to anhydrate, the even diaphragm that to form a thickness be 0.5～20mm;
B, in 10～200mL liquid to be detected, drip 5～50% the sulfuric acid of 0.5～5mL, regulate pH value to 2.0 ± 0.5;
C, will regulate the liquid to be detected after pH slowly to join on the even diaphragm of step b gained;
(5) after liquid to be detected sees through this even diaphragm colour developing completely, by detecting complete diaphragm color in step (4), contrast with standard proportional card, obtain hexavalent chromium concentration value in liquid to be measured;
(6) in concentration value contrast standard ratio card in step (5) being obtained and step (3), the accurate value detecting is proofreaded, and has obtained final concentration value, and the value that contrast obtains is comparatively good.
The above, be only preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence done according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (8)
1. the composite bentonite material of hexavalent chromium in naked eyes recognition detection water body fast, it is characterized in that: the core of this material is hydrophobic nano organic modified bentonite, this core is connected and is modified with developer diphenylcarbazide by its hydrophobicity carbochain, this hydrophobic nano organic modified bentonite forms by quaternary ammonium salt-modified, its smectite content > 88%, cation exchange capacity is 80～130mmol/100g, and whiteness is 76～95.
2. the composite bentonite material of hexavalent chromium in a kind of water body of naked eyes recognition detection fast as claimed in claim 1, is characterized in that: described quaternary ammonium salt is at least one in tetramethyl ammonium chloride, etamon chloride, tetrabutylammonium chloride, dodecyl quaternary ammonium salt, cetyl quaternary ammonium salt and octadecyl quaternary ammonium salt.
3. a preparation method for the composite bentonite material described in claim 1 or 2, is characterized in that: comprise the steps:
(1) take developer and hydrophobic nano organic modified bentonite by the weight ratio of 1:2～200, evenly mix after 10～300min at the temperature of 5～50 DEG C with enough pure water, pure water washing and filtering must precipitate;
(2) by vacuum drying 1～48h at the above-mentioned temperature that is deposited in 40～80 DEG C, described composite bentonite material.
4. preparation method as claimed in claim 3, is characterized in that: described developer and hydrophobic nano organic modified bentonite weight ratio are 1:10～20.
5. preparation method as claimed in claim 3, is characterized in that: the temperature of described step (1) is room temperature.
6. preparation method as claimed in claim 3, is characterized in that: described mixed uniformly mode comprises mechanical agitation, magnetic agitation and ultrasonic wave.
7. preparation method as claimed in claim 3, is characterized in that: the described vacuum drying time is 1～24h.
8. application rights requires a method for hexavalent chromium in the composite bentonite material tests water body described in 1 or 2, it is characterized in that: comprise the steps:
(1) be mixed into slurries by taking described composite bentonite material and pure water with the weight ratio of 1:1～200;
(2) slurries in step (1) are pipetted to 0.3～20mL, add equably the vacuum filter upward filtration that contains one deck NC Nitroncellulose filter membrane in the middle of being placed in to anhydrate, the even diaphragm that formation one thickness is 0.5～20mm;
(3) in 10～200mL liquid to be detected, drip 5～50% the sulfuric acid of 0.5～5mL, regulate pH value to 2.0 ± 0.5;
(4) will regulate the liquid to be detected after pH to join on the even diaphragm of step (2) gained;
(5), after liquid to be detected sees through this even diaphragm colour developing completely, with Standard Colors card contrast, can obtain detecting and in liquid, contain chromic content.
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| CN104826599A (en) * | 2015-05-05 | 2015-08-12 | 济南大学 | Preparation method of magnetic composite organic bentonite |
| CN104826600A (en) * | 2015-05-05 | 2015-08-12 | 济南大学 | Preparation method of magnetic kaolin |
| CN106932388A (en) * | 2017-01-23 | 2017-07-07 | 中国第汽车股份有限公司 | A kind of Cr VI detection indicator solution, its preparation method and its application method |
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