CN108169372B - Method for measuring complexing agent in electroplating wastewater - Google Patents
Method for measuring complexing agent in electroplating wastewater Download PDFInfo
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- CN108169372B CN108169372B CN201711402485.7A CN201711402485A CN108169372B CN 108169372 B CN108169372 B CN 108169372B CN 201711402485 A CN201711402485 A CN 201711402485A CN 108169372 B CN108169372 B CN 108169372B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention provides a method for measuring a complexing agent in electroplating wastewater, which comprises the following steps: s1: providing electroplating wastewater containing a complexing agent; s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected; s3: adding an internal standard substance into the first solution to be detected, stirring for 1-3h, concentrating under reduced pressure to dryness, then adding an acidifying reagent for dissolving, introducing nitrogen, concentrating to dryness, and obtaining an acidified sample; s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
Description
Technical Field
The invention relates to a method for measuring a complexing agent, in particular to a method for measuring a complexing agent in electroplating wastewater.
Background
The heavy metal pollution has the following characteristics of 1 and nondegradability, and any treatment method or microorganism can only change the valence of the heavy metal and the type of a compound but cannot degrade the heavy metal; 2. the toxicity is long-term and persistent, and some trace heavy metals can be converted into organic compounds with stronger toxicity under the action of microorganisms; 3. biological enrichment, which is a main characteristic of heavy metal pollution, some heavy metals can be enriched by tens of millions of times in organisms, and chronic poisoning is caused by accumulation in biological organs through a food chain, so that the health of the organisms is harmed; 3. trace heavy metals can produce toxic reaction, common heavy metals can produce toxicity within the concentration range of about 1.0-10.0mg/L, and heavy metals with strong toxicity, such as copper, can produce toxicity within the concentration range of 0.001-0.1 mg/L.
One of the main sources of the heavy metal wastewater is electroplating piece washing water, along with the stricter and stricter discharge standard of the electroplating wastewater, the high-efficiency removal of the complex heavy metal in the wastewater becomes a hotspot of current research, and a complexing agent has stronger chelating capacity and is a heavy metal trapping agent, so that the determination of the complexing agent is very important for determining the content of the heavy metal in the wastewater.
The determination of the complexing agent is influenced by a plurality of interference factors, and the method has important significance for eliminating the interference and improving the determination accuracy of the complexing agent.
Therefore, in order to solve the above problems, the present invention provides a method for rapidly and accurately measuring a complexing agent in electroplating wastewater.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for measuring a complexing agent in electroplating wastewater, comprising the steps of:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance into the first solution to be detected, stirring for 1-3h, concentrating under reduced pressure to dryness, then adding an acidifying reagent for dissolving, introducing nitrogen, concentrating to dryness, and obtaining an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
In one embodiment, the acidifying agent comprises one of hydrochloric acid, formic acid, acetic acid.
In one embodiment, the acidifying agent is formic acid.
In one embodiment, the internal standard is 1, 2-diaminopropane-N' -tetraacetic acid.
In one embodiment, the leacheate is a mixed solution of n-hexane and toluene.
In one embodiment, the volume ratio of n-hexane to toluene in the mixed solution of n-hexane and toluene in the eluent is (3-10): 1.
in one embodiment, the volume ratio of n-hexane to toluene in the mixed solution of n-hexane and toluene in the eluent is 7: 1.
in one embodiment, the eluent is a mixed solution of n-hexane and toluene.
In one embodiment, the volume ratio of n-hexane to toluene in the mixed solution of n-hexane and toluene in the eluent is (5-10): 1.
in one embodiment, the test parameters of the gas chromatography-mass spectrometry are: HP-5MS column (30 m.times.0.25 mm.times.0.25 μm); the column start temperature is 80 ℃; heating to 200 deg.C at a rate of 30 deg.C/min; then raising the temperature to 320 ℃ at the speed of 10 ℃/min, and keeping the temperature for 2 min; sample inlet temperature: 230 ℃; no shunt sampling; sample introduction volume: 2 mu L of the solution;
a source of negative chemical ions; reaction gas: methane; ionization energy: 60 eV; ion source temperature: at 210 ℃; connecting rod temperature: 220 ℃; an ion scan is selected.
The above-described and other features, aspects, and advantages of the present application will become more apparent with reference to the following detailed description.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" embraces the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer".
"interpolymer" means a polymer prepared by polymerizing at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is generally used to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is generally used to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing more monomers. "blend" means a polymer formed by two or more polymers being mixed together by physical or chemical means.
The invention provides a method for measuring a complexing agent in electroplating wastewater, which comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance into the first solution to be detected, stirring for 1-3h, concentrating under reduced pressure to dryness, then adding an acidifying reagent for dissolving, introducing nitrogen, concentrating to dryness, and obtaining an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
In one embodiment, the acidifying agent comprises one of hydrochloric acid, formic acid, acetic acid.
In one embodiment, the acidifying agent is formic acid.
In one embodiment, the internal standard is 1, 2-diaminopropane-N' -tetraacetic acid.
In one embodiment, the leacheate is a mixed solution of n-hexane and toluene.
In one embodiment, the volume ratio of n-hexane to toluene in the mixed solution of n-hexane and toluene in the eluent is (3-10): 1.
in one embodiment, the volume ratio of n-hexane to toluene in the mixed solution of n-hexane and toluene in the eluent is 7: 1.
in one embodiment, the eluent is a mixed solution of n-hexane and toluene.
In one embodiment, the volume ratio of n-hexane to toluene in the mixed solution of n-hexane and toluene in the eluent is (5-10): 1; preferably, the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the eluent is 8: 1.
the mass ratio of the acidified sample to the n-hexane in the invention is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20.
In one embodiment, the test parameters of the gas chromatography-mass spectrometry are: HP-5MS column (30 m.times.0.25 mm.times.0.25 μm); the column start temperature is 80 ℃; heating to 200 deg.C at a rate of 30 deg.C/min; then raising the temperature to 320 ℃ at the speed of 10 ℃/min, and keeping the temperature for 2 min; sample inlet temperature: 230 ℃; no shunt sampling; sample introduction volume: 2 mu L of the solution;
a source of negative chemical ions; reaction gas: methane; ionization energy: 60 eV; ion source temperature: at 210 ℃; connecting rod temperature: 220 ℃; an ion scan is selected.
The method comprises the steps of stabilizing the complexing agent in the electroplating wastewater by formaldehyde, further stabilizing by an internal standard substance and an acidifying reagent, purifying a sample by an eluent and detecting by a gas chromatography-mass spectrometry method to obtain the type and the content of the complexing agent.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the raw materials used are commercially available from national chemical reagents, unless otherwise specified.
Example 1
Sample 1: the complexing agent in this sample was EDTA at 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the content of EDTA in this sample was 0.99%.
Example 2
Sample 1: the complexing agent in this sample was EDTA, at a content of 2%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the content of EDTA in this sample was 0.99%.
Example 3
Sample 1: the complexing agent in this sample was EDTA at 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the content of EDTA in this sample was 1.97%.
Example 4
Sample 1: the complexing agent in this sample was NTA, at a level of 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the NTA content in this sample was 0.99%.
Example 5
Sample 1: the complexing agent in this sample was MGDA, at a level of 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the MGDA content in this sample was 0.98%.
Example 6
Sample 1: the complexing agent in this sample was 1,3-PDTA, with a content of 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the 1,3-PDTA content of this sample was 0.98%.
Comparative example 1
Sample 1: the complexing agent in this sample was EDTA at 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an acidification reagent formic acid into the first solution to be detected for dissolving, introducing nitrogen, and concentrating and drying to obtain an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected; the leacheate is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of the n-hexane and the toluene in the leacheate is 7: 1; the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of the n-hexane to the toluene in the mixed solution of n-hexane and toluene in the eluent is 8: 1; the mass ratio of the acidified sample to the n-hexane is 1: 5; the mass ratio of the acidified sample to the leacheate is 1: 12; the mass ratio of the acidified sample to the eluent is 1: 20;
s5: and detecting the second solution to be detected by using gas chromatography-mass spectrometry, and obtaining the type and content of the complexing agent (which is different from the embodiment in that no internal standard substance exists) through a standard control.
And (3) calculating the result: the content of EDTA in this sample was 0.90%.
Comparative example 2
Sample 1: the complexing agent in this sample was EDTA at 1%.
The method for measuring the complexing agent in the electroplating wastewater comprises the following steps:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance 1, 2-diaminopropane-N N 'N' -tetraacetic acid into the first solution to be detected, stirring for 1h, concentrating under reduced pressure to dryness, then adding an acidification reagent formic acid for dissolving, introducing nitrogen and concentrating to dryness to obtain an acidified sample;
s4: adding normal hexane into the acidified sample, and stirring to completely dissolve the normal hexane to obtain a second solution to be detected;
s5: and detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison.
And (3) calculating the result: the content of EDTA in this sample was 0.64%.
The data show that the method has simple operation steps, saves the detection cost, and can accurately, quickly, qualitatively and quantitatively analyze the type and the content of the complexing agent in the electroplating wastewater.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (3)
1. The method for measuring the complexing agent in the electroplating wastewater is characterized by comprising the following steps of:
s1: providing electroplating wastewater containing a complexing agent;
s2: adding formaldehyde into electroplating wastewater containing a complexing agent, and uniformly mixing to obtain a first solution to be detected;
s3: adding an internal standard substance into the first solution to be detected, stirring for 1-3h, concentrating under reduced pressure to dryness, then adding an acidifying reagent for dissolving, introducing nitrogen, concentrating to dryness, and obtaining an acidified sample;
s4: adding n-hexane into the acidified sample, transferring the acidified sample to a silica gel column purification column, eluting with an eluent, discarding the eluent, eluting with an eluent, and collecting the eluent to obtain a second solution to be detected;
s5: detecting the second solution to be detected by using a gas chromatography-mass spectrometry method, and obtaining the type and the content of the complexing agent through standard substance comparison; the internal standard substance is 1, 2-diaminopropane-N N 'N' -tetraacetic acid, the leacheate is a mixed solution of N-hexane and toluene, and the volume ratio of the N-hexane to the toluene in the leacheate is 7: 1, the eluent is a mixed solution of n-hexane and toluene, and the volume ratio of n-hexane to toluene in the eluent is 8: 1;
the complexing agent is one of EDTA, NTA, MGDA and 1, 3-PDTA;
test parameters of the gas chromatography-mass spectrometry: HP-5MS chromatographic column 30m × 0.25mm × 0.25 μm, column start temperature 80 deg.C; heating to 200 deg.C at a rate of 30 deg.C/min; then raising the temperature to 320 ℃ at the speed of 10 ℃/min, and keeping the temperature for 2 min; sample inlet temperature: 230 ℃; no shunt sampling; sample introduction volume: 2 mu L of the solution;
a source of negative chemical ions; reaction gas: methane; ionization energy: 60 eV; ion source temperature: at 210 ℃; connecting rod temperature: 220 ℃; an ion scan is selected.
2. The method for determining a complexing agent in electroplating wastewater according to claim 1, wherein the acidifying agent comprises one of hydrochloric acid, formic acid, and acetic acid.
3. The method for determining a complexing agent in electroplating wastewater according to claim 1, wherein said acidifying agent is formic acid.
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Citations (6)
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