A kind of precision instrument atomizer incrustation detergent
Technical field
The present invention relates to analytical chemistry technical field of measurement and test more particularly to a kind of analysis precision instrument atomizer incrustation cleanings
Agent.
Background technology
In recent years, with the progress of science and technology, inductive coupling plasma emission spectrograph (ICP-AES), full spectrum are straight
The highly sensitive large-scale instrument such as plasma emission spectrometer (ICAP) and Inductively coupled plasma mass spectrometry instrument (ICP-MS) is read to obtain
Extensive use is arrived, which with different sample pre-treatments is combined, has made significant headway, emerged by people
Many new technologies, new method, and the means of testing is applied to geological prospecting and Methods of Regional field, achieve notable achievement.
At abroad, inductive coupling plasma emission spectrograph (ICP-AES) and icp ms
(ICP-MS) highly sensitive large-scale instrument has obtained extensively should in fields such as geology, metallurgy, agricultural, environmental protection, oil and chemical industry
With;In the past 20 years, ICP-AES and ICP-MS large-scale precision instruments have also obtained tremendous development in China, substantially there is certain reality
The analysis inspection center of power is provided with both instruments, especially ore sample analysis, food analysis, environmental sample point
Analysis.
Inductive coupling plasma emission spectrograph and icp ms are in specific test sample application
In, commonly using a kind of ICP atomizers, such atomizer is different from that atomizer for medically applying air wetting.ICP mists
Change device is double-layer structure, and outer tube is carrier gas access, and inner tube is sample cell, mainly by a kind of dress of prepare liquid quality sample atomization analysis
It puts, main and fog chamber is used cooperatively.
During specific test sample, when being particularly the sample being acidified after some alkali fusions, extremely easily in capillary
Salinity incrustation is formed at wall and nozzle, causes to block, so as to seriously affect atomizing effect, drips splashing liquid pearl at nozzle so that atomization
Effect declines, and the sensitivity of Instrument measuring element seriously reduces, and then influences accuracy and the precision of measurement result.Solution at present
Certainly this problem, there are two common methods, and one kind is to block nozzle, is passed through a large amount of gases, carries out blowback;Another kind is exactly single
Pure uses diluted acid to carry out invading bubble flushing.But both approaches poor effect, and even if can be used after treated, but
It cannot use for a long time, can only finally use new ICP atomizers instead, therefore ICP atomizers are consumptive materials, instrument company is not also protected
It repaiies.The market price of ICP atomizers is generally 4000-30000 yuan and differs, and price is relatively expensive, and replacement frequency is very fast, therefore
ICP atomizers become the serious burden of analysis measuring unit.Therefore, inventing a kind of ICP atomizers incrustation detergent has very
Important meaning.
ICP atomizers capillary tube inner wall and nozzle go out salinity incrustation comparison of ingredients complexity.Such as the sample being acidified after alkali fusion
Product, the crucible type of alkali fusion selection is important influence factor, using nickel crucible alkali fusion, then incrustation ingredient is mostly nickel and sodium,
Using corundum crucible, then its ingredient is mostly aluminium and sodium, is then iron and sodium using iron crucible alkali fusion.For the molten sample of acid, ICP
Atomizer capillary tube inner wall and nozzle go out salinity incrustation and occur more slow, but use for a long time, atomizer will also result in resistance
Plug, the incrustation ingredient that acidified sample generates are generally the elements such as copper, lead, zinc, iron, tungsten, molybdenum, tin, silicon, such as the production of Pb-Zn deposits sample
Raw incrustation ingredient is lead zinc, and the incrustation ingredient of ironstone sample is mostly iron.
The content of the invention
The present invention provides a kind of precision instrument atomizer incrustation detergent, can remove the various incrustation in ICP atomizers.
In order to solve the above technical problem, the present invention provides precision instrument atomizer incrustation detergent be realized in
's:
A kind of precision instrument atomizer incrustation detergent, deionized water, chloroazotic acid, metal-chelator, surfactant, except silicon
Agent loses agent and corrosion protection agent except silicon increases.
Optionally, the metal-chelator is EDETATE SODIUM, citric acid, tartaric acid, oxalic acid and sodium gluconate.
Optionally, the surfactant is cetane sulfonate, octadecyl dihydroxy ethyl glycine betaine and hexadecane three
Methyl bromide ammonium.
Optionally, the desiliconizing agent is fluoboric acid class.
Optionally, the desiliconizing agent is tetrafluoro boric acid.
Optionally, it is described except silicon increases erosion agent as sodium tripolyphosphate.
Optionally, corrosion protection agent is Boratex.
Optionally, the deionized water, chloroazotic acid, metal-chelator, surfactant, desiliconizing agent, increase erosion agent and corruption except silicon
Losing protectant mass ratio is:1000~2000:100~400:30~50:10~20:10~20:3~5:10~20.
Optionally, the quality of EDETATE SODIUM in the metal-chelator, citric acid, tartaric acid, oxalic acid and sodium gluconate
Than for:10:5:5:5:10.
Optionally, cetane sulfonate, octadecyl dihydroxy ethyl glycine betaine and hexadecane three in the surfactant
The mass ratio of methyl bromide ammonium is:10:5:5.
The present invention use deionized water as solvent, purity height, it is ensured that free from admixture in solvent, be conducive to solute dissolving and
Ensure that not having other reactions occurs..
Metal-chelator, which can eliminate, is accumulated in metal dirt in atomizer mouth.EDETATE SODIUM is common metal chelating agent,
Complex reaction can occur with alkali metal, rare earth element and transition metal etc., generate soluble complex;Citric acid and tartaric acid tool
There is scattered and stable metal ion, make it stable in solution, the two especially has the metals such as tungsten tin molybdenum complexing well to make
With tungsten tin molybdenum easily generates sediment in an acidic solution, and has the presence of tartaric acid and citric acid, this metal ion can be with
It is stabilized in acid solution.Sodium gluconate scale prevention ability is strong:To calcium, magnesium, molysite has very strong complexing power, so resistance
Dirt is very capable, especially to Fe3+There is fabulous chelation.Oxalic acid has very strong complexing with metal ion, can be with transition
Property metal ion combine, form soluble complex.
Surfactant is sodium cetanesulfonate, octadecyl dihydroxy ethyl glycine betaine and cetyl trimethyl bromination
Ammonium;The former is anion surfactant, and both rear is zwitterionic surfactant, is respectively provided under acid and alkaline condition
Excellent stability is both a kind of good surfactant of water solubility, has wetting, emulsification, scattered, foam and decontamination
Ability.Surfactant, which can eliminate, is accumulated in dirt in atomizer mouth.
Desiliconizing agent is fluoboric acid class, and optimal is tetrafluoro boric acid.Fluoboric acid class in an acidic solution, could be formed with effect ingredient
Fluorine ion, the ion pair element silicon have complexing, can eliminate and be accumulated in silicon dirt in atomizer mouth.
It is sodium tripolyphosphate except silicon increases erosion agent, the substance is to removing silicon effect with facilitation.
Corrosion protection agent is Boratex, this component is key component.In fluoric acid salt in an acidic solution, Boratex can be with
Generation weak acid boric acid is combined with hydrogen ion in solution, with fluorine ion complex reaction can occur for boric acid, so as to reduce hydrofluoric acid
Harm, plays the role of protection.
Precision instrument atomizer incrustation detergent provided by the invention, water are solvent, and chloroazotic acid is lytic agent, and chelating agent is complexed
Metal ion, and activating agent is to promote fouled surface activity, is conducive to incrustation and enters solution;Desiliconizing agent is used for except silicon, except silicon
Increase erosion agent as the catalyst except silicon, corrosion protection agent removes the hydrogen ion generated in chloroazotic acid scale removal and generated in desiliconizing agent scale removal
Fluorine ion.
Precision instrument atomizer incrustation detergent provided by the invention has removal incrustation effect ideal, and the time is short, is easy to
Operation, it is safe.Precision instrument atomizer incrustation detergent provided by the invention is suitble to the incrustation of ICP atomizers to remove work
Make, application is strongly professional, easy to operate, cleaning effect is good, at low cost, small toxicity.It fits to ICP atomizer corrosiveness very littles,
It is higher to remove incrustation efficiency, effect is preferable.Inexpensively, advantage of lower cost is easy for construction effective for the prices of raw materials.
During the experiment of the present invention, inventor has found the mass ratio of precision instrument atomizer incrustation detergent each component
The best results in scope provided by the invention during ambient weather cold, will increase deionized water and the amount of chloroazotic acid;Chloroazotic acid it is dense
Degree is not easy excessive, and when heating, smell is too dense, is pernicious to people, and if very little, effect is bad;Chelating agent:It is sufficient, still
Dissolubility is bad if excessively high, not into solution.Surfactant:Concentration is too big, and bubble is too big, moreover, dissolubility is in low temperature
It waits, does not dissolve;Desiliconizing agent:Concentration is too dense, easy etching glass vessel.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, following embodiment carries out the present invention
It is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit
The present invention.
The preparation of precision instrument atomizer incrustation detergent of the present invention
Embodiment one
It calculates by quality ratio, by deionized water 1000g, chloroazotic acid 100g, sodium gluconate 10g, DETA 10g, tartaric acid
5g, citric acid 5g, oxalic acid 5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 5g, cetyl sulphur
Sour sodium 10g, tetrafluoro boric acid 10g, sodium tripolyphosphate 5g, Boratex 10g, are sufficiently stirred mixing in a reservoir.Above-mentioned raw materials remove
Outside ionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration uses.
Embodiment two
It calculates by quality ratio, by deionized water 1000g, chloroazotic acid 200g, sodium gluconate 10g, DETA 10g, tartaric acid
5g, citric acid 2.5g, oxalic acid 2.5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 5g, hexadecane
Base sodium sulfonate 5g, tetrafluoro boric acid 15g, sodium tripolyphosphate 3g, Boratex 15g, are sufficiently stirred mixing in a reservoir.Above-mentioned raw materials,
In addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration makes
With.
Embodiment three
It calculates by quality ratio, by deionized water 1000g, chloroazotic acid 150g, sodium gluconate 15g, DETA 15g, tartaric acid
7.5g, citric acid 7.5g, oxalic acid 5g, octadecyl dihydroxy ethyl glycine betaine 2.5g, cetyl trimethylammonium bromide 2.5g, ten
Six sodium alkyl sulfonate 5g, tetrafluoro boric acid 20g, sodium tripolyphosphate 4g, Boratex 20g, are sufficiently stirred mixing in a reservoir.Above-mentioned original
Material, in addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration
It uses.
Example IV
It calculates by quality ratio, by deionized water 1000g, chloroazotic acid 170g, sodium gluconate 10g, DETA 10g, tartaric acid
5g, citric acid 7.5g, oxalic acid 7.5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 3g, hexadecane
Base sodium sulfonate 5g, tetrafluoro boric acid 18g, sodium tripolyphosphate 4g, Boratex 18g, are sufficiently stirred mixing in a reservoir.Above-mentioned raw materials,
In addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration makes
With.
Embodiment five
It calculates by quality ratio, by deionized water 1000g, chloroazotic acid 120g, sodium gluconate 10g, DETA 10g, tartaric acid
10g, citric acid 7.5g, oxalic acid 7.5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 8g, 16
Sodium alkyl sulfonate 5g, tetrafluoro boric acid 13g, sodium tripolyphosphate 3g, Boratex 13g, are sufficiently stirred mixing in a reservoir.Above-mentioned original
Material, in addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration
It uses.
Embodiment six
It calculates by quality ratio, by deionized water 2000g, chloroazotic acid 400g, sodium gluconate 10g, DETA 10g, tartaric acid
10g, citric acid 7.5g, oxalic acid 7.5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 8g, 16
Sodium alkyl sulfonate 5g, tetrafluoro boric acid 13g, sodium tripolyphosphate 3g, Boratex 13g, are sufficiently stirred mixing in a reservoir.Above-mentioned original
Material, in addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration
It uses.
Embodiment seven
It calculates by quality ratio, by deionized water 1500g, chloroazotic acid 300g, sodium gluconate 10g, DETA 10g, tartaric acid
5g, citric acid 2.5g, oxalic acid 2.5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 5g, hexadecane
Base sodium sulfonate 5g, tetrafluoro boric acid 15g, sodium tripolyphosphate 3g, Boratex 15g, are sufficiently stirred mixing in a reservoir.Above-mentioned raw materials,
In addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration makes
With.
Embodiment eight
It calculates by quality ratio, by deionized water 1800g, chloroazotic acid 400g, sodium gluconate 10g, DETA 10g, tartaric acid
5g, citric acid 2.5g, oxalic acid 2.5g, octadecyl dihydroxy ethyl glycine betaine 5g, cetyl trimethylammonium bromide 5g, hexadecane
Base sodium sulfonate 5g, tetrafluoro boric acid 15g, sodium tripolyphosphate 3g, Boratex 15g, are sufficiently stirred mixing in a reservoir.Above-mentioned raw materials,
In addition to deionized water, the purity of all components is that analysis is pure.Chloroazotic acid is according to hydrochloric acid and nitric acid 3:1 ratio situ configuration makes
With.
After configuring precision instrument atomizer incrustation detergent according to above-mentioned eight embodiments, the cleaning of any embodiment is used
Agent starts to clean ICP atomizers.In ambient weather colder season, select deionized water and chloroazotic acid content higher as far as possible
Detergent.The ICP atomizers for needing to clean are put into beaker, 2 zeolites or tile is put down gently, adds in above-mentioned solution, make
Liquid level cover all ICP atomizers, heated using controllable temperature device, slightly boiling 30-60 minutes, cool down.Leather glove is taken to take
Go out ICP atomizers, 4 times or more are cleaned with clear water, then using washes of absolute alcohol 3 times, after naturally dry, you can use.Clearly
Ultrasonic cleaning cannot be never used during washing, high temperature is made sure to keep in mind and acutely seethes with excitement, because the capillary at ICP atomizers center is easily
It is broken.
ICP atomizers occur after dirt or after obstruction, and atomizing effect will become the element very poor, instrument is gathered
Signal value will be greatly lowered.There are incrustation ICP atomizers in setting use, and the elemental signals value that instrument is gathered is I0;Make
ICP atomizers after being cleaned with cleaning agent of the present invention, the elemental signals value that instrument is gathered are I, setting K=I ÷ I0.When K is big
When 1, illustrate that the atomizing effect of ICP atomizers cleaning is good, so as to react the cleaning performance that cleaning agent has had dirt;Work as K
During less than 1, illustrating the atomizing effect of ICP atomizers cleaning becomes worse, and damage is caused to atomizer so as to react cleaning agent.
When K is equal to or is approximately equal to 1, then reacting cleaning agent does not have dirt any effect.
Instrument and its running parameter:6300 Radial of ICAP compose the direct-reading plasma emission spectrometer (U.S. entirely
ThermoFisher companies).Instrument operating condition is:RF power 1150W aid in gas (Ar) flow velocity 1.0L/min, atomizer pressure
Power 0.20MPa, wriggling revolution speed 50r/min, long wave time for exposure 10s, shortwave time for exposure 15s, 1~20s of the time of integration, from
Dynamic integration.
Chosen elements use for europium Eu, Eu generally as internal standard element.What the analysis spectral line selected as instrument of Eu was recommended
First spectral line 381.967nm, the spectral line signal is sensitive, i.e., under relatively low concentration conditions, signal value is all very high, buckle back
Scape model selection is the double buttons in left and right.
Test method:Take 5 ICP atomizers for incrustation occurred, press surface condition carry out and on tell the tool of example
Body implementation just tests comparison.Data below preheats what is measured after 1 hour under instrument optimum state in instrument.
1 ICP atomizer cleaning performance tables of table
By above-mentioned table 1 as can be seen that the detergent of the application present invention has ICP atomizers removal incrustation energy well
Power.As can be seen that precision instrument atomizer incrustation detergent provided by the invention is suitble to ICP from above-described embodiment and table 1
The incrustation of atomizer removes work, and application is strongly professional, easy to operate, cleaning effect is good, at low cost, small toxicity.It fits to ICP mists
Change device corrosiveness very little, removal incrustation efficiency is higher, and effect is preferable.The prices of raw materials inexpensively, apply by advantage of lower cost
Work is easily and effectively.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.