CN104148009B - 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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- CN104148009B CN104148009B CN201410269879.XA CN201410269879A CN104148009B CN 104148009 B CN104148009 B CN 104148009B CN 201410269879 A CN201410269879 A CN 201410269879A CN 104148009 B CN104148009 B CN 104148009B
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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 is and in particular to one kind can quick Cr VI in naked eyes recognition detection water body
Composite bentonite material of ion and its preparation method and application.
Background technology
Chromium is a kind of metallic element being widely present in nature, is distributed mainly on rock, soil, big gas and water and biology
In body.Chromium distributed pole in soil is wide, and content range is very wide；In water body and air, chromium content is less, then contains in animal and plant body
Trace chromium.Nature chromium is mainly presented in trivalent chromium and Cr VI.Sugar in trivalent chromium participant and animal body and fat
The metabolism of fat, be human body mustn't trace element, Cr VI is then clear and definite harmful element, can make some albumen in blood of human body
The precipitation of matter, causes the diseases such as anemia, nephritis, neuritiss, contacts with Cr VI for a long time and also can cause respiratory inflammation, and induces
Pulmonary carcinoma or value volume cause invasive skin lesion, and serious sexavalence chromium poisoning also results in sexavalence chromium poisoning, or even dead.
According to statistics, Cr VI is mainly derived from chrome ore smelting, refractory material, plating, process hides, weaving, printing and dyeing, pigment, no
Chromium-containing waste gas, waste water and waste residue that rust steel welding, the industry such as cement and burning and exhausting go out etc..Cr VI is to be easiest to lead to allergy
One of metal, be only second to nickel, contact human skin is easily caused ulcer or anaphylaxiss.At present, the Cr VI in water body from
Son has very strong toxicity, has toxic and potential risk to human body and surrounding biologic, ecological environment etc..Cr VI has by force
Toxicity is it is generally recognized that its toxicity is chromic 100 times, and is easily absorbed by the body and accumulates in vivo.Cr VI passes through breathing
After system enters human body, rhinorrhea, sneeze, prurituss can be caused, go out nose bleeding, ulcer and perforation of nasal septum etc..Short-term is heavy dose of
Contact, contact site can produce ulcer, nasal mucosa stimulate, perforation of nasal septum.The Cr VI that absorption exceedes dosage leads to kidney
The damage of dirty and liver, nausea, intestines and stomach stimulations, gastric ulcer, spasm, or even death.A large amount of take in Cr VIs can produce carcinogenic,
The harmful effects such as mutagenesis, teratogenesis, the Center for Disease Control harmful toxic matter and disease registration administration (asdtr, cdc) are in 2007-
One of 2011 average annual materials that Cr VI is classified as first 20 preferential detections.Cr VI is determined by Environmental Protection Agency (epa)
For one of dangerous toxicant of 17 kinds of high concentrations.Hexavalent chromium compound oral lethal dose is about 1.5g, and in water body, content exceedes
0.1mg/l will produce intoxicating phenomenon.At present, Cr VI has become as one of index of China's enforcement overall control.China " city
Town Wastewater Treatment discharge standard " in specify chromic concentration must not exceed 0.5mg/l.Drinking Water health mark
Define hexavalent chromium concentration in accurate (gb5749 2006) and be less than 0.05mg/l.
In prior art, the method for determination of hexavalent chromium ion mainly have spectrophotometer method, flame atomic absorption spectrometry,
Oscillopolarographic titation, Kinetic spectrophotometery, flow injection spectrographic method etc..The pre-treating method of the most of sample of these methods is relatively
For complexity, and the instrument and equipment price being related to costly is not easy to popularization and uses, especially more remote at some
Area.
Content of the invention
It is an object of the invention to overcoming prior art defect, provide one kind can quick sexavalence in naked eyes recognition detection water body
The composite bentonite material of chromium ion.
Another object of the present invention is to providing the preparation method of above-mentioned composite bentonite material.
It is still another object of the present invention to provide the application of above-mentioned composite bentonite material.
The concrete technical scheme of the present invention is as follows:
A kind of can quickly in naked eyes recognition detection water body hexavalent chromium composite bentonite material, the core of this material is
Hydrophobic nano organic modified bentonite, this core is passed through the connection of its hydrophobic carbon chain and is modified with developer diphenylcarbazide,
This hydrophobic nano organic modified bentonite is formed by quaternary ammonium salt-modified, its smectite content ＞ 88%, and cation exchange is held
Measure as 80～130mmol/100g, whiteness is 76～95.
In a preferred embodiment of the invention, described quaternary ammonium salt be tetramethyl ammonium chloride, tetraethylammonium chloride, four
At least one in butyl ammonium chloride, dodecyl quaternary ammonium salt, cetyl quaternary ammonium salt and octadecyl quaternary ammonium salt.
A kind of preparation method of above-mentioned composite bentonite material, comprises the steps:
(1) developer and hydrophobic nano organic modified bentonite are weighed by the weight ratio of 1:2～200, pure with enough
After water uniformly mixes 10～300min at a temperature of 5～50 DEG C, pure water filters and must precipitate；
(2) be deposited at a temperature of 40～80 DEG C vacuum drying 1～48h by above-mentioned, described composite bentonite material.
In a preferred embodiment of the invention, described developer and hydrophobic nano organic modified bentonite weight
Amount ratio is 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 includes mechanical agitation, magnetic agitation
And ultrasound wave.
In a preferred embodiment of the invention, the described vacuum drying time is 1～24h.
A kind of method applying hexavalent chromium in above-mentioned composite bentonite material tests water body, comprises the steps:
(1) by weighing described composite bentonite material and pure water, serosity is mixed into the weight ratio of 1:1～200；
(2) serosity in step (1) is pipetted 0.3～20ml, be homogeneously added into and be placed in centre containing one layer of nitrocellulose
Water is filtered off on the vacuum filter of plain filter membrane, forms the uniform diaphragm that a thickness is 0.5～20mm；
(3) in 10～200ml liquid to be detected the 5～50% of Deca 0.5～5ml sulphuric acid, adjust ph value to 2.0 ±
0.5；
(4) liquid to be detected adjusting after ph is added on the uniform diaphragm of step (2) gained；
(5) after liquid to be detected completely through this uniform diaphragm and after developing the color, with the contrast of Standard Colors card, you can detected
Chromic content is contained in liquid.
The invention has the beneficial effects as follows:
1st, the detection method of the present invention is using having good absorption property and the high nanometer of itself whiteness to Organic substance
Organic modified bentonite, is dispersed in aqueous phase, forms the organic environment of a tiny area, as insoluble around its surface
Or the dissolving region of microsolubility Organic substance developer, also serve as their dispersants in aqueous phase, make use of nanometer organic simultaneously
Developer and hexavalent chromium in modified alta-mud absorption water, both can form distinctive color change, the change of its characteristic color
Change can be used as the reference frame of content of 6-valence Cr ions, and first Application original position naked eyes of heavy metal hexavalent chromium in water sample can be known
Other field of fast detection, has expanded the bentonitic application in analytical chemistry ambit；
2nd, the detection process of the present invention simple it is not necessary to by any detecting instrument, with low cost, and labor intensity is low；
3rd, the detection method of the present invention does not need, using any organic solvent, environmentally safe, to have ensured testing staff
Health；
4th, the test limit of the detection method of the present invention and conventional colorimetric method improves 50～1000 times, and test limit is less than 10.0 μ
g/l.
Brief description
Fig. 1 is prepared gradual change characteristic color in embodiments of the invention 2 with reference to card (0.3g nanometer organobentonite
Composite membrane, the prepare liquid of 100ml, detection liquid are 45min completely through the uniform diaphragm time)；
Fig. 2 is chromic recovery of standard addition curve (the linear dependence r in 0～60mg/l of embodiments of the invention 2
=0.9999)；
Fig. 3 is the correlation curve with characteristic color value for the hexavalent chromium concentration of embodiments of the invention 2.
Specific embodiment
Combine accompanying drawing below by way of specific embodiment technical scheme is further detailed and to describe.
Hydrophobic nano organic modified bentonite smectite content ＞ 88% in following embodiments, cation exchange is held
Measure as 80～130mmol/100g, whiteness is 76～95.
Embodiment 1
A kind of can quickly in naked eyes recognition detection water body hexavalent chromium composite bentonite material, the core of this material is
Hydrophobic nano organic modified bentonite, this core is connected with developer diphenylcarbazide by its hydrophobic carbon chain, and this is dredged
Water nano organic modified bentonite is formed by quaternary ammonium salt-modified, its smectite content ＞ 88%, and cation exchange capacity is
80～130mmol/100g, whiteness is 76～95.Described quaternary ammonium salt is tetramethyl ammonium chloride, tetraethylammonium chloride, tetrabutyl chlorine
Change at least one in ammonium, 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) developer and the organically-modified swelling of hydrophobic nano are weighed by the weight ratio (preferably 1:10～20) of 1:2～200
Soil, at a temperature of 5～50 DEG C, (preferably room temperature) uniformly mixes and (includes mechanical agitation, magnetic agitation and super with enough pure water
Sound wave) after 10～300min, pure water filters and must precipitate；
(2) be deposited at a temperature of 40～80 DEG C vacuum drying 1～48h (preferably 1～24h) by above-mentioned, described multiple
Close bentonite clay material.
Embodiment 2
Quick detection application process: weigh 10.0g by quaternary ammonium salt-modified hydrophobic nano organic modified bentonite
With the developer diphenylcarbazide of 1.0g, mass ratio is 10:1, is placed in the conical flask of 250ml of cleaning, adds 100ml's
Distilled water, is placed on magnetic stirring apparatuss after 5～50 DEG C of stirring 1h, formation serosity is standby.
Take the above-mentioned serosity of 5ml with clean liquid-transfering gun, equably 0.22 μm of new in vacuum apparatus nitro of Deca
On cellulose diaphragm, uniformly spread out and form the uniform diaphragm that a thickness is 0.5～20mm, with pure water to described composite bentonite
Material repeatedly washs, and removes undesired impurities.
100ml is contained the hexavalent chromium solution (ph=1～4) of standard series concentration, add vacuum filter dress one by one
Put in the container of upper strata, by concentration low to high, the described composite bentonite material got ready by brand-new one by one in same time
Expect uniform diaphragm, form the reference card of serial gradual change characteristic color, as shown in Figure 1.
Contain certain density hexavalent chromium solution in prepare liquid (ph=1～4), add vacuum apparatus upper strata container
In, with the former same time in by freshly prepd nanometer organobentonite function diaphragm, form prepare liquid color, with aforementioned ginseng
Picture ID compares, and obtains a reference value；Meanwhile, prepare liquid (Duplicate Samples) enters Precision measurement, obtains a detected value；Finally join
Examine value to contrast with detected value, determine the application performance of nanometer organobentonite function.As seen from Figure 1, sexavalence in prepare liquid
From between 0～200 μm/l, characteristic color has good differentiation to chromium concn.
By mark-on method, described composite bentonite material has in the recovery of standard addition that hexavalent chromium concentration is 0～60mg/l
Good is linear, 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 with numerical fitting, described composite bentonite material is in hexavalent chromium concentration and color
Have good linear between change, show that this functional material has linear trend (such as to the colour developing gradual change of hexavalent chromium feature
Shown in Fig. 3).
Embodiment 3
(1) the dodecyl sodium sulfate modified Nano bentonite of 10.0g and the developer diphenylcarbazide of 1.0g are weighed,
In mass ratio be 1:10, be placed in cleaning the conical flask of 250ml in, add 100ml distilled water, be placed on magnetic stirring apparatuss in
After 5～50 DEG C of stirring 1～5h, form serosity standby.
(2) use mark-on method, the distilled water of 600ml adds certain potassium dichromate, 3 parts of volumes of accurate measuring are
100ml liquid to be detected and 3 parts of volumes are the detection liquid as precision checking equipment for the 100ml；
(3) 3 parts of volumes in step (2) are carried out accurate detection for 100ml as the detection liquid of precision checking equipment, it is put down
Average is as the hexavalent chromium concentration value of this prepare liquid；
(4) according to following step, respectively by 3 parts of volumes of step (2) be 100ml liquid to be detected respectively by respective brand-new
Standby uniform diaphragm:
A, the serosity in step (1) is pipetted 0.3～20ml, be homogeneously added into be placed in and middle contain one layer of NC Nitroncellulose
Water is filtered off on the vacuum filter of filter membrane, forms the uniform diaphragm that a thickness is 0.5～20mm；
B, in 10～200ml liquid to be detected the 5～50% of Deca 0.5～5ml sulphuric acid, adjust ph value to 2.0 ±
0.5；
C, by adjust ph after liquid to be detected be slowly added on the uniform diaphragm of step b gained；
(5) after liquid to be detected completely through this uniform diaphragm and after developing the color, uniform diaphragm that detection in step (4) is finished
Color, is contrasted with standard proportional card, obtains hexavalent chromium concentration value in prepare liquid；
(6) concentration value that contrast standard ratio card in step (5) obtains is carried out school with the value of Precision measurement in step (3)
Right, obtain final concentration value, contrast the value obtaining more good.
Embodiment 4
(1) weigh hexadecyltrimethylammonium chloride modified Nano bentonite and the diphenylcarbazide of certain mass, press
Mass ratio is 1:10, is placed in the distilled water adding 100ml in the conical flask of 250ml of cleaning, puts at a temperature of 5～50 DEG C
After 0.5h～1h in the ultrasonic sound appratus, form serosity standby.
(2) use mark-on method, the tap water of 600ml adds certain potassium dichromate, 3 parts of volumes of accurate measuring are
100ml liquid to be detected and 3 parts of volumes are the detection liquid as precision checking equipment for the 100ml；
(3) 3 parts of volumes in step (2) are carried out accurate detection for 100ml as the detection liquid of precision checking equipment, it is put down
Average is as the hexavalent chromium concentration value of this prepare liquid；
(4) according to following step, respectively by 3 parts of volumes of step (2) be 100ml liquid to be detected respectively by respective brand-new
Standby uniform diaphragm:
A, the serosity in step (1) is pipetted 0.3～20ml, be homogeneously added into be placed in and middle contain one layer of NC Nitroncellulose
Water is filtered off on the vacuum filter of filter membrane, forms the uniform diaphragm that a thickness is 0.5～20mm；
B, in 10～200ml liquid to be detected the 5～50% of Deca 0.5～5ml sulphuric acid, adjust ph value to 2.0 ±
0.5；
C, by adjust ph after liquid to be detected be slowly added on the uniform diaphragm of step b gained；
(5) after liquid to be detected completely through this uniform diaphragm and after developing the color, uniform diaphragm that detection in step (4) is finished
Color, is contrasted with standard proportional card, obtains hexavalent chromium concentration value in prepare liquid；
(6) concentration value that contrast standard ratio card in step (5) obtains is carried out school with the value of Precision measurement in step (3)
Right, obtain final concentration value, contrast the value obtaining more good.
Embodiment 5
(1) the tetrabutylammonium chloride sodium modified Nano bentonite of 10.0g and the developer diphenylcarbazide of 0.5g are weighed,
In mass ratio be 1:20, be placed in cleaning the conical flask of 250ml in, add 100ml distilled water, be placed on magnetic stirring apparatuss in
After 5～50 DEG C of stirring 1h and 5h, form serosity standby.
(2) use mark-on method, the distilled water of 600ml adds certain potassium dichromate, 3 parts of volumes of accurate measuring are
100ml liquid to be detected and 3 parts of volumes are the detection liquid as precision checking equipment for the 100ml；
(3) 3 parts of volumes in step (2) are carried out accurate detection for 100ml as the detection liquid of precision checking equipment, it is put down
Average is as the hexavalent chromium concentration value of this prepare liquid；
(4) according to following step, respectively by 3 parts of volumes of step (2) be 100ml liquid to be detected respectively by respective brand-new
Standby uniform diaphragm:
A, the serosity in step (1) is pipetted 0.3～20ml, be homogeneously added into be placed in and middle contain one layer of NC Nitroncellulose
Water is filtered off on the vacuum filter of filter membrane, forms the uniform diaphragm that a thickness is 0.5～20mm；
B, in 10～200ml liquid to be detected the 5～50% of Deca 0.5～5ml sulphuric acid, adjust ph value to 2.0 ±
0.5；
C, by adjust ph after liquid to be detected be slowly added on the uniform diaphragm of step b gained；
(5) after liquid to be detected completely through this uniform diaphragm and after developing the color, diaphragm face that detection in step (4) is finished
Color, is contrasted with standard proportional card, obtains hexavalent chromium concentration value in prepare liquid；
(6) concentration value that contrast standard ratio card in step (5) obtains is carried out school with the value of Precision measurement in step (3)
Right, obtain final concentration value, contrast the value obtaining more good.
The above, only presently preferred embodiments of the present invention, therefore the scope of present invention enforcement can not be limited according to this, that is,
The equivalence changes made according to the scope of the claims of the present invention and description and modification, all should still belong in the range of the present invention covers.
Claims (6)
1. a kind of can quickly in naked eyes recognition detection water body hexavalent chromium composite bentonite material it is characterised in that: this material
The core of material is hydrophobic nano organic modified bentonite, and this core is passed through the connection of its hydrophobic carbon chain and is modified with developer hexichol
Phosphinylidyne two hydrazine, this hydrophobic nano organic modified bentonite pass through quaternary ammonium salt-modified form, its smectite content ＞ 88%, sun from
Sub- exchange capacity is 80～130mmol/100g, and whiteness is 76～95, and described quaternary ammonium salt is tetramethyl ammonium chloride, tetraethyl chlorination
At least one in ammonium, tetrabutylammonium chloride, dodecyl quaternary ammonium salt, cetyl quaternary ammonium salt and octadecyl quaternary ammonium salt, its
Preparation method comprises the steps:
(1) developer and hydrophobic nano organic modified bentonite are weighed by the weight ratio of 1:2～200, with enough pure water 5
After uniformly mixing 10～300min at a temperature of～50 DEG C, pure water filters and must precipitate；
(2) be deposited at a temperature of 40～80 DEG C vacuum drying 1～48h by above-mentioned, described composite bentonite material.
2. composite bentonite material as claimed in claim 1 it is characterised in that: described developer is organic with hydrophobic nano to be changed
The bentonitic weight of property is than for 1:10～20.
3. composite bentonite material as claimed in claim 1 it is characterised in that: the temperature of described step (1) be room temperature.
4. composite bentonite material as claimed in claim 1 it is characterised in that: described mixed uniformly mode includes machinery and stirs
Mix, magnetic agitation and ultrasound wave.
5. composite bentonite material as claimed in claim 1 it is characterised in that: the described vacuum drying time be 1～24h.
6. a kind of application claim 1 described in composite bentonite material tests water body in hexavalent chromium method, its feature
It is: comprise the steps:
(1) by weighing described composite bentonite material and pure water, serosity is mixed into the weight ratio of 1:1～200；
(2) serosity in step (1) is pipetted 0.3～20ml, be homogeneously added into and be placed in centre containing one layer of NC Nitroncellulose mistake
Water is filtered off on the vacuum filter of filter membrane, forms the uniform diaphragm that a thickness is 0.5～20mm；
(3) in 10～200ml liquid to be detected the 5～50% of Deca 0.5～5ml sulphuric acid, adjust ph value to 2.0 ± 0.5；
(4) liquid to be detected adjusting after ph is added on the uniform diaphragm of step (2) gained；
(5) after liquid to be detected completely through this uniform diaphragm and after developing the color, with the contrast of Standard Colors card, you can obtain detecting in liquid
Containing chromic content.
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| CN104826600B (en) * | 2015-05-05 | 2018-03-02 | 济南大学 | A kind of magnetic kleit preparation method |
| CN104826599A (en) * | 2015-05-05 | 2015-08-12 | 济南大学 | Preparation method of magnetic composite organic bentonite |
| CN106932388B (en) * | 2017-01-23 | 2019-11-26 | 中国第一汽车股份有限公司 | A kind of Cr VI detection indicator solution, preparation method and its application method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2276254A (en) * | 1939-06-16 | 1942-03-10 | Schinzel Karl | Color photography |
| CN1501066A (en) * | 2002-11-18 | 2004-06-02 | 上海师范大学 | Test piece for detecting hexavalent chromium and preparing method thereof |
| CN1959376A (en) * | 2005-11-03 | 2007-05-09 | 牛增元 | Method for detecting hexavalent chrome in dyed leather and product |
| CN102121905A (en) * | 2010-12-16 | 2011-07-13 | 上海交通大学 | Test strip for detecting heavy metal-chromium (Cr) in water quality and preparation method thereof |
Family Cites Families (2)
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|---|---|---|---|---|
| WO2009116669A1 (en) * | 2008-03-21 | 2009-09-24 | アークレイ株式会社 | Dry test instrument, method of measuring metal and method of producing dry test instrument |
| CN102980852A (en) * | 2011-09-02 | 2013-03-20 | 索尼公司 | Detection sheet, method, kit, and sensor for detection of heavy metal ions |
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2014
- 2014-06-17 CN CN201410269879.XA patent/CN104148009B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2276254A (en) * | 1939-06-16 | 1942-03-10 | Schinzel Karl | Color photography |
| CN1501066A (en) * | 2002-11-18 | 2004-06-02 | 上海师范大学 | Test piece for detecting hexavalent chromium and preparing method thereof |
| CN1959376A (en) * | 2005-11-03 | 2007-05-09 | 牛增元 | Method for detecting hexavalent chrome in dyed leather and product |
| CN102121905A (en) * | 2010-12-16 | 2011-07-13 | 上海交通大学 | Test strip for detecting heavy metal-chromium (Cr) in water quality and preparation method thereof |
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