CN105466738A - Chemical sample preparation method for testing trace quantity of elemental chromium in soil and sewage - Google Patents
Chemical sample preparation method for testing trace quantity of elemental chromium in soil and sewage Download PDFInfo
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- CN105466738A CN105466738A CN201410428077.9A CN201410428077A CN105466738A CN 105466738 A CN105466738 A CN 105466738A CN 201410428077 A CN201410428077 A CN 201410428077A CN 105466738 A CN105466738 A CN 105466738A
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Abstract
The invention provides a method for testing the trace quantity of elemental chromium in soil and sewage by using a total reflection X-ray fluorescence (TXRF) instrument. The method comprises the following steps: weighing a soil digestion solution or sewage sample and adding acid to establish an acidic reagent environment; adding a potassium permanganate solution to oxidize trivalent chromium ions into hexavalent chromium ions; successively adding an extraction agent and hydrochloric acid to extract the chromium ions; dropwisely adding an extracted chromium ion organic phase solution onto quartz glass and carrying out constant-temperature titration film preparation; and drying a film prepared through titration and placing the dried film on a TXRF sample platform for scanning test. According to the invention, extraction technology is applied to testing with the TXRF instrument for the first time, a methyl isobutyl ketone (MIBK) reagent extraction method is employed, so elemental chromium in the soil digestion solution or other aqueous solution samples is separated from other substrate elements; thus, the spectral peaks of other elements and background interference are reduced during testing.
Description
Technical field
The invention belongs to water quality and soil monitoring field, be specifically related to the one chemistry method for making sample of a kind of total Reflection X-ray Fluorescence Spectrometry (TXRF) instrument testing soil and Chromium in Sewage constituent content, be particularly useful for the trace analysis of chromium element.
Background technology
China is since reform and opening-up, and economic high speed, steady, sustainable growth, achieve remarkable achievement.Accompany with it, the pressure of environmental protection also strengthens year by year, and pollution is totally still in a higher level.For water environment, at present, the Proposals of Water Resources of China the threat of severe contamination, industrial waste water and exhausting sewage discharge in a large number in rivers,lakes and seas and soil, the day water and quality of groundwater are worsened increasingly, more exacerbate the pressure of water resource, serious constrains expanding economy, compromises the health of the mankind.
Harmonious co-existence between man and nature is one of six essential characteristics of harmonious socialist society.To this, central authorities are by the important goal being classified as Eleventh Five-Year Plan with the strategic task of friendly environment society of building a resource-conserving society.At field of environment protection, central authorities and governments at all levels continue to increase input, and Policy Toward and the market demand it is also proposed a series of new requirement to environment supervision instrument and equipment, and these require that main manifestations is:
1. the requirement of pair accuracy of instrument and function is more and more higher, is ensureing under the prerequisite that instrument stabilizer runs, is requiring that portability is stronger, to meet the requirement of relevant department's Emergent detection.
2. the requirement of pair detection sample sample preparation aspect is: quick, accurately sample preparation, with the content value facilitating all kinds of testing tool to test out various pollution element fast and accurately.
3. the secondary pollution problem in sample preparation and test process, the use requiring method for making sample the least possible test sample and the chemical reagent of secondary environmental pollution may be caused.
The advantages such as TXRF total reflection X-ray fluorescence spectrometer is high with measuring accuracy, easy to carry are just applied by scene field tests of meeting an urgent need at present more and more widely.
The excitation principle of TXRF instrument is different from the excitation principle of common XRF instrument, it requires X ray in atmosphere or in vacuum to plunder the surface being emitted through sample test platform lower than the angle of critical angle, eliminate simple X ray relevant or incoherent scattering phenomenon on reflecting body, scattering background is reduced, reduces and detect lower limit.Its principle of reflection is shown in accompanying drawing 1.
Based on above-mentioned total reflection principle, test in sample making course at TXRF, need ensure that sample drop fixes on film very thin for one deck on load sample platform, the sample of surface irregularity does not reach the effect of total reflection, directly affects measuring accuracy and detection limit.
The TXRF instrument test principle applied in the market is identical, all applies the total reflection principle of X ray, in test process, sample is directly made fluid film titration and dry test on load sample sheet.In test process, its background noise and relevant interference element can bring sizable error to test.
Summary of the invention
The present invention is directed to the defect of prior art, required tested elemental chromium utilized the method for extraction, adopt liquid--liquid is separated, and by the extract titration masking test containing tested elemental chromium, eliminates the interference between element completely.
A chemical method for making sample for testing soil and Chromium in Sewage element trace, is characterized in that: comprise the following steps,
A. measure soil digested solusion or the sewage sample of 80ml-90ml, import in volumetric flask stand-by;
B. in volumetric flask, add acid solution, set up the reagent environment under acid condition;
C. in above-mentioned mixed liquor, add the liquor potassic permanganate that concentration is the 500 μ L of 1%, fully shake all, 3 valency chromium ions in tested soil digested solusion or sewage are all oxidized to 6 valency chromium ions;
D. the extractant of 1ml-3ml is added in volumetric flask, fully jolt, extractant is fully contacted with mixed liquor;
E. add the hydrochloric acid of 8ml-10ml and shake all, 6 valency chromium elements in volumetric flask and hydrochloric acid reaction are generated containing chromium complex, and being extracted agent extraction in the reaction, then continuing to jolt 2 minutes, extractant is fully contacted with water-soluble solution;
F. volumetric flask is normally put static 2 minutes on the table, now mixed solution completes liquid-liquid separation, organic extractant phase solution containing tested elemental chromium ion floats on aqueous phase solution upper strata, and the chromium element in soil digested solusion or sewage sample extracts completely, completes the enrichment of chromium element;
G. be placed on thermostat by the quartz glass plate that TXRF tests, the chromium ion organic phase solution of measured amounts drops on quartz glass plate and carries out constant temperature titration masking;
H. titration masking is placed on the enterprising line scanning test of TXRF example platform after dripping film drying.
As preferably, the acid solution added in described step b is red fuming nitric acid (RFNA), described in add red fuming nitric acid (RFNA) content be 1ml-3ml.
As preferably, in order to ensure that extraction completely, between described step c and described steps d, further comprising the steps of, the mixed liquor being added with liquor potassic permanganate to be mixed and after static 1 minute, import in wide mouth beaker, heated at constant temperature platform be heated to seethe with excitement and keep 3 minutes, make 3 valency chromium ions in mixing material more cmpletely be oxidized to 6 valency chromium ions.
As preferably, the extractant in described steps d is hexone.
As preferably, the addition of described extractant is 2.2ml.
As preferably, the chromium ion organic phase solution measuring 10 μ L-40 μ L in described step g drops on quartz glass plate and carries out constant temperature titration masking.
As preferably, in described step g, the temperature of constant temperature titration masking is 90 degree.
Compared with prior art, the present invention has the following advantages;
1. in the middle of the test first abstraction technique being applied to total reflection X ray fluorescence instrument.
2. the present invention uses the reagent extracting process of MIBK (hexone), and the chromium element in soil digested solusion or other aqueous sample and other base metals are separated, and reduces spectrum peak and the background interference of other elements in test process.
3. the sample after extraction, under the effect of MIBK (hexone), is separated into aqueous phase and organic phase, uses liquid-transfering gun to extract organic phase tens μ L and once can drip film test, reaches that sample preparation is convenient, the effect of anti-secondary pollution.
4. after extraction process, use the method for liquid enrichment masking, reduce the Monitoring lower-cut of TXRF instrument chromium element.
5. experimental verification test, uses TXRF apparatus measures soil digested solusion and all kinds of Chromium in Sewage constituent content detection limit can reach 5 below ppb.
Accompanying drawing explanation
Figure 1 shows that X ray reflection schematic diagram in TXRF instrument;
Figure 2 shows that test flow chart of the present invention.
Embodiment
As shown in Figure 2, the method for testing of a kind of TXRF instrument test soil and Chromium in Sewage element trace, comprises the following steps:
A. first measure soil digested solusion or the sewage sample of 80ml-90ml, import in volumetric flask stand-by;
B. add red fuming nitric acid (RFNA) 1ml-3ml, adjustment reagent environment, ensures that extractive reaction carries out under suitable acid condition; Mixed solution after acid adding is shaken up rear static stand-by;
C. be titrated in above-mentioned mixed solution by the liquor potassic permanganate 500 μ l of 1% concentration, fully shake up, now mixed liquor takes on a red color.Adding liquor potassic permanganate object is that 3 valency chromium ions in tested soil digested solusion or sewage are all oxidized to 6 valency chromium ions, extracts for MIBK;
D. getting MIBK (hexone) 1ml-3ml adds in volumetric flask, fully jolts, extractant is fully contacted with mixed solution, and the preferred content adding MIBK is 2.2ml;
E. measure in hydrochloric acid 8ml-10ml instillation volumetric flask and shake up, 6 valency chromium elements in volumetric flask and hydrochloric acid reaction are generated containing chromium network and thing, and is extracted by MIBK in course of reaction, then continue to jolt 2 minutes, MIBK is fully contacted with water-soluble solution;
F. then volumetric flask is normally put static 2 minutes on the table, now mixed solution will complete liquid--and liquid is separated, organic extractant phase solution containing tested elemental chromium ion floats on aqueous phase solution upper strata, chromium element in soil digested solusion or sewage sample extracts completely, completes the enrichment of chromium element;
G. be placed on thermostat by the quartz glass plate that TXRF tests, the chromium ion organic phase solution drawing 10 μ l-40 μ l drops on quartz glass plate and carries out 90 DEG C of constant temperature titration maskings;
H. titration masking is placed the enterprising line scanning test of TXRF example platform after dripping film drying.
As preferred steps, in order to ensure that extraction completely, further comprising the steps of between above-mentioned steps c and steps d, the mixed liquor being added with liquor potassic permanganate to be mixed and after static 1min, import in wide mouth beaker, heated at constant temperature platform is heated to seethe with excitement and is cooled to room temperature, through heating after keeping 3min, make 3 valency chromium ions in sample more cmpletely be oxidized to 6 valency chromium ions, ensure extraction completely.
Embodiment disclosed herein is exemplary, and it is only to explain the present invention, and is not limitation of the present invention, and the improvement that those skilled in the art will envision that and expansion are included in protection scope of the present invention.
Claims (7)
1. a chemical method for making sample for testing soil and Chromium in Sewage element trace, is characterized in that: comprise the following steps,
A. measure soil digested solusion or the sewage sample of 80ml-90ml, import in volumetric flask stand-by;
B. in volumetric flask, add acid solution, set up the reagent environment under acid condition;
C. add at volumetric flask the liquor potassic permanganate that concentration is the 500 μ L of 1%, fully shake all, 3 valency chromium ions in tested soil digested solusion or sewage are all oxidized to 6 valency chromium ions;
D. the extractant of 1ml-3ml is added in volumetric flask, fully jolt, extractant is fully contacted with mixed liquor;
E. add the hydrochloric acid of 8ml-10ml and shake all, 6 valency chromium elements in volumetric flask and hydrochloric acid reaction are generated containing chromium complex, and being extracted agent extraction in the reaction, then continuing to jolt 2 minutes, extractant is fully contacted with water-soluble solution;
F. volumetric flask is normally put static 2 minutes on the table, now mixed solution completes liquid-liquid separation, organic extractant phase solution containing tested elemental chromium ion floats on aqueous phase solution upper strata, and the chromium element in soil digested solusion or sewage sample extracts completely, completes the enrichment of chromium element;
G. the quartz glass plate that TXRF tests is placed on thermostat, draws a certain amount of chromium ion organic extractant phase solution and drop on quartz glass plate and carry out constant temperature titration masking;
H. titration masking is placed on the enterprising line scanning test of TXRF example platform after dripping film drying.
2. the chemical method for making sample of testing soil according to claim 1 and Chromium in Sewage element trace, is characterized in that: the acid solution added in described step b is red fuming nitric acid (RFNA), described in add red fuming nitric acid (RFNA) content be 1ml-3ml.
3. the chemical method for making sample of testing soil according to claim 1 and Chromium in Sewage element trace, it is characterized in that: in order to ensure that extraction completely, between described step c and described steps d, further comprising the steps of, the mixed liquor being added with liquor potassic permanganate to be mixed and after static 1 minute, import in wide mouth beaker, heated at constant temperature platform be heated to seethe with excitement and keep 3 minutes, make 3 valency chromium ions in mixing material more cmpletely be oxidized to 6 valency chromium ions.
4. the chemical method for making sample of testing soil according to claim 1 and Chromium in Sewage element trace, is characterized in that: the extractant in described steps d is hexone.
5. the chemical method for making sample of the testing soil according to claim 1 or 4 and Chromium in Sewage element trace, is characterized in that: the addition of described extractant is 2.2ml.
6. the chemical method for making sample of testing soil according to claim 1 and Chromium in Sewage element trace, is characterized in that: the chromium ion organic phase solution measuring 10 μ L-40 μ L in described step g drops on quartz glass plate and carries out constant temperature titration masking.
7. the chemical method for making sample of testing soil according to claim 1 and Chromium in Sewage element trace, is characterized in that: in described step g, the temperature of constant temperature titration masking is 90 degree.
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Citations (5)
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| JP2004333364A (en) * | 2003-05-09 | 2004-11-25 | Matsushita Electric Ind Co Ltd | Total reflection x-ray fluorescence analysis method and analysis apparatus |
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| CN102507454A (en) * | 2011-10-31 | 2012-06-20 | 中国科学院宁波材料技术与工程研究所 | Method for detecting trivalent chromium ions |
| US20120264225A1 (en) * | 2005-09-01 | 2012-10-18 | Mitsuhiro Oki | Method of quantitative analysis of hexavalent chromium in chromate coating and method for controlling hazardous element in encapsulating resin of resin encapsulation semiconductor device |
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| JP2004333364A (en) * | 2003-05-09 | 2004-11-25 | Matsushita Electric Ind Co Ltd | Total reflection x-ray fluorescence analysis method and analysis apparatus |
| US20120264225A1 (en) * | 2005-09-01 | 2012-10-18 | Mitsuhiro Oki | Method of quantitative analysis of hexavalent chromium in chromate coating and method for controlling hazardous element in encapsulating resin of resin encapsulation semiconductor device |
| CN101178357A (en) * | 2007-12-12 | 2008-05-14 | 上海大学 | Methods for detecting the content of chromium ion in soil |
| CN102411001A (en) * | 2011-08-08 | 2012-04-11 | 山东汇金彩钢有限公司 | Method for rapid detection of hexavalent chromium ions in sewage |
| CN102507454A (en) * | 2011-10-31 | 2012-06-20 | 中国科学院宁波材料技术与工程研究所 | Method for detecting trivalent chromium ions |
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