CN106153789A - The evaporating column measured for trace amounts of bromine hydrochlorate and the system of mensuration - Google Patents
The evaporating column measured for trace amounts of bromine hydrochlorate and the system of mensuration Download PDFInfo
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- CN106153789A CN106153789A CN201510204853.1A CN201510204853A CN106153789A CN 106153789 A CN106153789 A CN 106153789A CN 201510204853 A CN201510204853 A CN 201510204853A CN 106153789 A CN106153789 A CN 106153789A
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Abstract
The invention provides a kind of evaporating column measured for trace amounts of bromine hydrochlorate, including packed column, in packed column, be filled with anion exchange resin absorption material.Present invention also offers a kind of mensuration system measured for trace amounts of bromine hydrochlorate, comprise: an evaporating column, one guard column, one analytical column, one electric conductivity detector, when sample enters evaporating column, the aniones such as the bromate in the online adsorption sample of evaporating column are so that anion is enriched on evaporating column, leacheate flows through evaporating column makes the aniones such as bromate elute from evaporating column, analytical column is entered after then flowing through guard column, analytical column isolates bromate, and detect through electric conductivity detector, wherein evaporating column comprises packed column, packed column is filled with anion exchange adsorbing material.By using evaporating column, in conjunction with large volume sample injection, it is achieved that the on-line preconcentration of bromate, improve bromate and measure sensitivity and the precision of system.
Description
Technical field
The present invention relates to the mensuration of trace amounts of bromine hydrochlorate, particularly relate to efficiently measure the evaporating column of trace amounts of bromine hydrochlorate and mensuration system.
Background technology
Along with the raising day by day of people's living standard, the safety of drinking water receives much attention already with health problem, and carcinogen therein people especially are concerned about
One of focus.Bromate (BrO3 -) it is the bromide ion (Br in drinking water-) the important inorganic byproduct of one of generation after ozonization, also it is time chlorine
Acid sodium is as product during disinfectant solution.1992, the use Safety Examination report that World Health Organization (WHO) (WHO) delivers confirms that bromate is one
Plant oxidisability carcinogen, mainly can cause kidney and the bladder body generation canceration of animal.International cancer research institution (IARC) assert that bromate is 2B
Level potential carcinogen.Research shows, when people drink all the life containing the drinking water that bromate is 5.0 μ/gL or 0.5 μ/gL, its carcinogenic danger degree is respectively
It is 10-4Or 10-5。
Many countries have been that the content of bromate sets limit value when formulating water standard.In Environmental Protection Agency (US EPA) drinking water standard
The maximum permissible concentration of regulation bromate is 10 μ g/L, it is desirable to value is to can't check.2004 World Health Organization (WHO) (WHO) by " drinking water quality
Standard " in bromate limit value be changed to 10 μ g/L from 25 μ g/L.The existing national standard " natural mineral water " (GB8537-2008) of China,
" drinking water sanitary standard " (GB5749-2006), and the industry standard " urban water supply water standard " (CJ/T206-2005) that the Ministry of Construction promulgates,
All the content of bromate is defined to 10 μ g/L.
Bromate is as disinfection byproduct (DBP), and the content in drinking water is the lowest, the usually less than μ g/L order of magnitude.Therefore, research underwater trace and
The assay method of ultra trace bromate is significant, is also necessary.
The method of bromate in water that measures at present mainly includes gas chromatography, the chromatography of ions, spectrophotography etc..Wherein the chromatography of ions relies on
Simple to operate, it is not necessary to a large amount of chemical reagent, there is the advantage of higher sensitivity and accuracy, extremely analyze the favor of worker.US EPA will
The chromatography of ions is classified as the standard method measuring bromate.In ion chromatography water, the means that predominantly detect of bromate have Suppressor conductivity detection method, post
Rear derivative uv detection method, chromatography of ions-inductively coupled plasma mass spectrometry method (IC-ICP-MS) and chromatography of ions-electron spray mass spectrometry
(IC-ESI-MS)。
Suppressor conductivity detection method is simple to operate, environmental friendliness, but its sensitivity is the poorest.Generally use the mode of large volume quantitative loop direct injected to carry
High sensitivity.Sampling volume is many between 100-500 μ L, and detection limit scope is many between 0.2-5.0 μ g/L.At present, China's national standard method is " raw
Live the drinking water standard method of inspection " (GB/T5750-2006) recommends use bromate in water with ion chromatography, Suppressor conductivity detection, sample introduction body
Long-pending 500 μ L, detection limit only has 5 μ g/L.
The higher method of sensitivity has post-column derivation ultraviolet method, inductively coupled plasma mass spectrometry (ICP-MS) and electron spray mass spectrometry
(ESI-MS).Wherein the more difficult control of the condition of post-column derivation, complex operation, and derivative reagent are the most harmful；Energy anti-interference with mass spectrometry
Power is strong, but instrument and running expense are expensive, promote the use of by a definite limitation.
Along with the requirement of drinking water quality is improved day by day so that the detection limit using Suppressor conductivity detection method to measure at present is gradually difficult to meet to measure want
Asking, urgent need precision is higher, stability preferably measures system.The evaporating column of the on-line preconcentration bromate that the present invention relates to and mensuration system, for measuring
Trace bromate provides solution efficient, simple, highly sensitive, can reach 0.01 μ g/L, than the existing sensitivity generally analyzing method
(0.1～5 μ g/L) improves at least one order of magnitude, can effectively solve the problem that current methods medium sensitivity is not enough.
Summary of the invention
It is an object of the invention to measure, for bromate of the prior art, the weak point that system exists, measure for trace amounts of bromine hydrochlorate
Mensuration system improved.
According to the purpose of the present invention, the invention provides a kind of evaporating column measured for trace amounts of bromine hydrochlorate, including packed column, its feature
It is, in packed column, is filled with anion exchange resin absorption material.
Preferably, evaporating column also comprises two connecting portions being positioned at packed column two ends, and connecting portion has the hole communicated with packed column, in order to
Liquid passes through to flow in or out packed column from hole.
Further, adsorbing material is quaternized polystyrene-divinylbenzene crosslinking material.
Present invention also offers a kind of mensuration system measured for trace amounts of bromine hydrochlorate, comprise: an evaporating column, a guard column, an analysis
Post, an electric conductivity detector, when sample enters evaporating column, the anion such as the bromate in the online adsorption sample of evaporating column is so that anion
Being enriched on evaporating column, leacheate flows through evaporating column makes the aniones such as bromate elute from evaporating column, after then flowing through guard column
Entering analytical column, analytical column isolates bromate, and detects through electric conductivity detector, it is characterised in that evaporating column comprises packed column, fills out
Fill and post is filled with anion exchange adsorbing material.
Preferably, adsorbing material is anion exchange resin absorption material.
Further, adsorbing material is quaternized polystyrene-divinylbenzene crosslinking material.
Preferably, evaporating column also comprises two connecting portions being positioned at packed column two ends, and connecting portion has the hole communicated with packed column, in order to
Liquid passes through to flow in or out packed column from hole.
Further, mensuration system also comprises an injector that sample can be loaded to evaporating column.Further, mensuration system also comprises
One six-way valve, six-way valve has the first hole, the second hole, the 3rd hole, the 4th hole, the 5th hole and the 6th hole being arranged in order.
Further, by the first of six-way valve to the 6th hole respectively with injector, the two ends of evaporating column, guard column, leacheate, with
And sewer pipe is connected, to be controlled the connection order of clematis stem valve opening by switching six-way valve, realize loading concentration, removal waste fluid, pouring respectively
Wash, separation etc..
Further, the first hole is connected with injector, and the second hole is connected with the two ends of evaporating column respectively with the 5th hole, the 3rd hole and protection
Post is connected, and the 4th hole is connected with leacheate, and the 6th hole is waste liquid outlet.
Further, injector is automatic sampler, comprises a sample introduction and controls loop, and sample introduction controls loop and sets according to microcomputer or artificial
Setup control injector inputs the sample of set amount in mensuration system.
By using evaporating column to substitute the quantitative loop in existing determining instrument, in conjunction with large volume sample injection, it is achieved online enrichment bromate,
Substantially increase mensuration system to the sensitivity of bromate and precision, the order of magnitude of 0.1-0.01 μ g/L can be easily reached, with existing
Technology is compared, and substantially increases mensuration system to the Detection capability of trace level bromate and precision.Further, quantitative loop is changed into concentration
The operation of post is very simple, changes the least to existing determining instrument.And the evaporating column regeneration that the present invention uses is conveniently, repeatable utilization,
It is greatly reduced cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of the trace amounts of bromine hydrochlorate mensuration system of the first-selected embodiment of the present invention.
Fig. 2 be the first-selected embodiment of the present invention mensuration system in the generalized section of evaporating column structure.
Fig. 3 is the bromate routine sample introduction chromatography of ions comparison diagram with concentrated sample introduction of the first-selected embodiment of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the present invention it is further detailed and illustrates.
As it is shown in figure 1, the trace amounts of bromine hydrochlorate of the first-selected embodiment of the present invention measures system comprises an injector 10, an evaporating column 12,
One guard column 14, an analytical column 16, an electric conductivity detector 18.
Sample solution is injected into evaporating column 12 by injector 10, and sample includes that bromate is enriched in evaporating column in interior anion
On 12.Using the online generator of leacheate, generate highly purified potassium hydroxide leacheate, leacheate flows through evaporating column 12 by enrichment
The anion comprising bromate elutes from evaporating column 12, flows through guard column 14, after being separated by analytical column 16, and conductance
Detector 18 detects.Appearance time is qualitative, and peak area quantification obtains the concentration of bromate.
In first-selected embodiment, after eluting, liquid first flows through guard column, after pollutant therein are trapped, then flow into analytical column and enters
Row Anion separation.In this way, reduce the pollutant damage to analytical column in sample, to improve the use longevity of analytical column as far as possible
Order, stablize its separating effect.And guard column is as easily-consumed products, can regularly replace.
In this first-selection embodiment, injector 10 is automatic sampler, has a sample feeding controller, it is preferred that a sample introduction controls
Loop, is connected with computer, is set by computer program, can control the amount of each loading of injector 10, such as every time 5ml.Is having him
In embodiment, it is also possible to by the microprocessor of other forms in addition to computer or be manually set, or by artificial
Inject the amount controlling each loading.The amount relevant to detection limit (in certain limit, applied sample amount is the biggest, and detection limit is the lowest) of loading every time,
Therefore corresponding applied sample amount can also be set according to actual measurement environment and mensuration requirement.In other embodiments, for measuring
For system, injector can not be the part that mensuration system carries, but the accessory that can additionally configure.
As in figure 2 it is shown, evaporating column 12 comprises packed column 122, and lay respectively at the connecting portion 124,126 at packed column 122 two ends.
Connecting portion 124,126 is respectively provided with a hole, flows in or out evaporating column 12 to allow sample to pass therethrough.Packed column 122 is filled out
It is filled with anion exchange adsorbing material, particularly anion exchange resin absorption material, the most quaternized polystyrene-divinyl
Base benzene crosslinking material.Adsorbing material is graininess, particle diameter substantially 11 μm.The size first-selection internal diameter of packed column is 4mm, long
Degree is 50mm.In other embodiments, adsorbing material and packed column also can possess other shapes, size.
First-selected ground, connects injector 10, evaporating column 12, guard column 14 by a six-way valve 20, provided liquid discharge entrance,
Waste fluid channel and leacheate passage, by controlling six-way valve 20 rotor with stator relative to the switching of position, form different liquid
Body flow channel, thus control the approach that liquid flows through.Six-way valve 20 has six holes, definition be connected with injector for the first hole,
Six holes of six-way valve 20 respectively be the first hole 205, hole the 204, the 5th, hole the 203, the 4th, the 201, second hole the 202, the 3rd, hole,
6th hole 206.In first-selected embodiment, the first hole 201 is connected with injector 10, the second hole 205, hole the 202, the 5th respectively with
The two ends of evaporating column 12 connect, and the 3rd hole 203 is connected with guard column 14, and the 4th hole 204 is leacheate entrance, and the 6th hole 206 is
The waste liquid outlet of evaporating column 12.
As it is shown in figure 1, for six-way valve part, solid line is the stream of loading (Load) state, dotted line is sample introduction (Inject) shape
The stream of state.
Loading (Load) state: six-way valve is placed in loading state, injector 10, by sample solution, is pressed into by the first hole 201,
Flowing out from the second hole 202, a connection end 124 of concentrated post 12 flows into evaporating column 12, and the anion in sample solution, including bromine
Acid group and other matrix ions, the adsorbing material displacement sorption being concentrated in post 12, it is retained on evaporating column 12, it is achieved bromate exists
Enrichment on evaporating column 12, and the waste liquid after sample solution is enriched connects end 126 to the 5th hole 205, through the from another of evaporating column
Six holes 206 are flowed out.Loading (Load) stream of sample is: injector 10,201, second hole 202, the first hole of six-way valve, dense
Hole 206, contracting post the 12, the 5th hole the 205, the 6th, waste fluid container.Under this state of six-way valve, the stream of leacheate is: drip washing
Liquid generator, the 4th hole 203, hole the 204, the 3rd of six-way valve, guard column 14, analytical column 16, electric conductivity detector 18.
Sample introduction (Inject) state: when after testing sample solution all (such as: 5mL) press-in evaporating column, six-way valve switch to into
Sample (Inject) state, makes leacheate connect with evaporating column 12, and gradient increases the ionic strength of leacheate, by evaporating column 12
The anion including bromate of enrichment elutes, and after flowing through guard column 14, enters analytical column 16 and isolates bromate, then
Detected by electric conductivity detector 18.Stream now is: leacheate generator, the 4th hole 205, hole the 204, the 5th of six-way valve, concentration
Hole 203, post the 12, second hole the 202, the 3rd, guard column 14, analytical column 16, electric conductivity detector 18.
Experiment one:
In order to verify the effect of evaporating column, it is analyzed by the following method:
(1) compound concentration is the bromate solution of 5.12 μ g/L；
(2) conventional sample introduction 25 μ L, does not use evaporating column to be enriched with bromate ion, and wherein 25 μ L are existing detecting instrument
The quantitative loop volume generally used during sample introduction, detects and calculates the bromate peak area of non-concentrated sample introduction；
(3) sample introduction 5mL, by evaporating column on-line preconcentration bromate ion；
(4) detect and calculate the peak area of bromate after concentration；
(5) (2), (3), (4) step are repeated twice, comprehensive 3 measurement results, measure after not concentrating mensuration, concentration
Bromate peak area there were significant differences, and be computed showing that the enrichment factor of evaporating column is about 240 times, such as Fig. 3
Shown is bromate routine sample introduction in this experiment (that is: non-concentrated sample introduction) (as shown in A in Fig. 3) with concentrate into
The comparison of the chromatography of ions figure of sample (as shown in B in Fig. 3), arrow is oriented to the chromatography of ions peak of bromate.
Empirical tests, evaporating column is notable to the concentrated effect of bromate.Certainly, enrichment factor also can occur because of the difference of sample size size
Change, but relative to conventional sample introduction, due to the existence of evaporating column so that sample size rises to ml rank, so electricity from μ L rank
The amount leading the bromate that detector detects increases with decades of times or hundreds times, thus greatly reduces the detection limit of bromate, can relatively hold
Change places and reach the rank of 0.1-0.01 μ g/L, drastically increase sensitivity.
Experiment two:
Measure system linearity scope for measuring the present invention, draw calibration curve by the following method:
(1) preparing the bromate standard solution of variable concentrations, concentration range is between 0.0551.2 μ g/L；
(2) this mensuration system, respectively the bromate standard solution sample introduction 5ml to variable concentrations are used；
(3) detect and calculate testing result；
(4) statistical result, is concluded that bromate concentration linear relationship between 0.05-51.2 μ g/L is good, the range of linearity
At least 3 orders of magnitude, correlation coefficient >=0.9995.
Experiment three:
In order to verify that the present invention measures the detection limit of system, it is measured by the following method and analyzes:
(1) preparing the bromate standard solution of 7 part of 0.05 μ g/L, empirically the step analysis of two measures；
(2) specify according to HJ168-2010, calculate the standard deviation S of 7 parallel assays, by method detection limit computing formula
MDL=3.143 × S,
Obtaining in the case of sample size is 5ml, the present invention measures the detection limit of system, and the least concentration that can detect is
0.01μg/L.As it was previously stated, enrichment factor can change because sample size change, therefore can when concrete mensuration according to
The detection limit needed, suitable adjustment sample size.
It is above the present invention is measured the qualification of system for trace amounts of bromine hydrochlorate mensuration.
When needing the mensuration system using the present invention that testing sample carries out bromate concentration mensuration, following steps are used to be measured:
(1) first use the method and steps of experiment two, mensuration system is calibrated, if the linear relationship of calibration result is good, then
Meaning to measure working state of system good, calibration curve can be used；
(2) the mensuration system using the present invention the most again testing sample is carried out loading (Load), concentration, eluting sample introduction (Inject),
Separate, detect, and calculate the bromate concentration of testing sample.
Experiment four:
The mensuration system using the present invention is analyzed detection to commercially available tri-kinds of pure water of A, B, C, and carries out recovery of standard addition mensuration,
Result is as shown in table 1.Data result shows, this assay method accuracy can meet analysis requirement.
The bromate of 1: three kind of commercially available pure water of table measures
Above content provide only the preferred embodiment of the present invention.Those skilled in the art are according to provided by the present invention
Word describes, accompanying drawing and claims can it is readily conceivable that the present invention limited without departing from claims design and
Under conditions of scope, may be made that multiple obvious change, substitute and revise.Protection scope of the present invention is determined by claim.
Claims (16)
1. the evaporating column measured for trace amounts of bromine hydrochlorate, including packed column, it is characterised in that be filled with anion in described packed column
Crossover resin absorption material.
2. the evaporating column measured for trace amounts of bromine hydrochlorate as claimed in claim 1, it is characterised in that described evaporating column also comprises to be positioned to be filled out
Filling two connecting portions at post two ends, described connecting portion has the hole communicated with described packed column, in order to liquid passes through from described hole
To flow in or out packed column.
3. the evaporating column measured for trace amounts of bromine hydrochlorate as claimed in claim 1, it is characterised in that described adsorbing material is quaternized
Polystyrene-divinylbenzene crosslinking material.
4. the evaporating column measured for trace amounts of bromine hydrochlorate as claimed in claim 1, it is characterised in that described adsorbing material is graininess,
Particle diameter substantially 11 μm.
5. the evaporating column measured for trace amounts of bromine hydrochlorate as claimed in claim 2, it is characterised in that the internal diameter of described packed column is 4mm,
A length of 50mm.
6. the evaporating column measured for trace amounts of bromine hydrochlorate as claimed in claim 2, it is characterised in that described evaporating column can be directly connected to
One bromate measure system six-way valve on thus on-line preconcentration bromate.
7. the mensuration system measured for trace amounts of bromine hydrochlorate, comprises: an evaporating column, a guard column, an analytical column, a Conductivity detection
Device, when sample enter described evaporating column, described evaporating column adsorb the aniones such as the bromate in described sample online so that the moon from
Sub-on-line preconcentration is on described evaporating column, and leacheate flows through described evaporating column makes the aniones such as described bromate from described evaporating column
Eluting, enter described analytical column after then flowing through described guard column, described analytical column isolates bromate, and through described electricity
Lead detector detection, it is characterised in that described evaporating column comprises packed column, described packed column is filled with anion exchange and inhales
Enclosure material.
8. the mensuration system measured for trace amounts of bromine hydrochlorate as claimed in claim 7, it is characterised in that the suction filled in described evaporating column
Enclosure material is anion exchange resin absorption material.
9. the mensuration system measured for trace amounts of bromine hydrochlorate as claimed in claim 7, it is characterised in that the suction filled in described evaporating column
Enclosure material is quaternized polystyrene-divinylbenzene crosslinking material.
10. the mensuration system measured for trace amounts of bromine hydrochlorate as claimed in claim 7, it is characterised in that described evaporating column also comprises
Being positioned at two connecting portions at packed column two ends, described connecting portion has the hole communicated with described packed column, in order to liquid is from described hole
In by flow in or out described packed column.
The 11. mensuration systems measured for trace amounts of bromine hydrochlorate as claimed in claim 7, it is characterised in that the internal diameter of described packed column
For 4mm, a length of 50mm.
12. mensuration systems measured for trace amounts of bromine hydrochlorate as claimed in claim 7, it is characterised in that described adsorbing material is
Granular, particle diameter substantially 11 μm.
The 13. mensuration systems measured for trace amounts of bromine hydrochlorate as claimed in claim 7, it is characterised in that described mensuration system is also wrapped
Containing an injector that described sample can be loaded to described evaporating column.
The 14. mensuration systems measured for trace amounts of bromine hydrochlorate as claimed in claim 13, it is characterised in that described mensuration system is also wrapped
Containing a six-way valve, described six-way valve have be arranged in order the first hole, the second hole, the 3rd hole, the 4th hole, the 5th hole and
6th hole.
The 15. mensuration systems measured for trace amounts of bromine hydrochlorate as claimed in claim 14, it is characterised in that by described six-way valve
First to the 6th hole respectively with described injector, the two ends of described evaporating column, described guard column, described leacheate and waste liquid
Pipe is connected, and to control the connection order of described clematis stem valve opening by switching six-way valve, realizes large volume loading, the denseest respectively
Contracting, removal waste fluid, drip washing, separation etc..
The 16. mensuration systems measured for trace amounts of bromine hydrochlorate as claimed in claim 14, it is characterised in that described first hole is with described
Injector is connected, described second hole with the 5th hole respectively two ends with described evaporating column be connected, described 3rd hole and described guard column
Being connected, described 4th hole is connected with described leacheate, and described 6th hole is waste liquid outlet.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510204853.1A CN106153789A (en) | 2015-04-23 | 2015-04-23 | The evaporating column measured for trace amounts of bromine hydrochlorate and the system of mensuration |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510204853.1A CN106153789A (en) | 2015-04-23 | 2015-04-23 | The evaporating column measured for trace amounts of bromine hydrochlorate and the system of mensuration |
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| US20100187175A1 (en) * | 2007-06-29 | 2010-07-29 | Christ Water Technology Ag | Treatment of water with hypobromite solution |
| CN102411035A (en) * | 2011-08-25 | 2012-04-11 | 浙江大学 | New method for detecting trace amount bromate |
| CN102539568A (en) * | 2011-12-31 | 2012-07-04 | 杭州市质量技术监督检测院 | Ion chromatography method for detecting iodate and bromate in cosmetic |
| CN103558331A (en) * | 2013-10-31 | 2014-02-05 | 大连大公环境检测有限公司 | Method for detecting bromate in drinking water |
| CN204807521U (en) * | 2015-04-23 | 2015-11-25 | 刘晶 | A evaporating column and survey system for trace bromate survey |
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2015
- 2015-04-23 CN CN201510204853.1A patent/CN106153789A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100187175A1 (en) * | 2007-06-29 | 2010-07-29 | Christ Water Technology Ag | Treatment of water with hypobromite solution |
| CN102411035A (en) * | 2011-08-25 | 2012-04-11 | 浙江大学 | New method for detecting trace amount bromate |
| CN102539568A (en) * | 2011-12-31 | 2012-07-04 | 杭州市质量技术监督检测院 | Ion chromatography method for detecting iodate and bromate in cosmetic |
| CN103558331A (en) * | 2013-10-31 | 2014-02-05 | 大连大公环境检测有限公司 | Method for detecting bromate in drinking water |
| CN204807521U (en) * | 2015-04-23 | 2015-11-25 | 刘晶 | A evaporating column and survey system for trace bromate survey |
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| Title |
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| YALI SHI等: "A Novel Simplified Column-Switching Technique for the Determination of Traces of Bromate in High Concentration Matrices", 《MICROCHIM ACTA》 * |
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