CN103376302A - Novel testing method of carbon-containing organic substance - Google Patents
Novel testing method of carbon-containing organic substance Download PDFInfo
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- CN103376302A CN103376302A CN2012101164353A CN201210116435A CN103376302A CN 103376302 A CN103376302 A CN 103376302A CN 2012101164353 A CN2012101164353 A CN 2012101164353A CN 201210116435 A CN201210116435 A CN 201210116435A CN 103376302 A CN103376302 A CN 103376302A
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Abstract
The invention discloses a novel testing method of carbon-containing organic substance. The method is based on the TOC (Total Organic Carbon) testing technology, a TOC tester is used as an analysis tool, and test on mass concentration of the organic substance is realized according to the TOC content in water solution and the fixed carbon percentage in the organic substance. The novel testing method is free from any sample pretreatment, is quick in test, high in sensitivity, wide in application range and high in testing accuracy, thereby being very suitable for on-site online monitoring.
Description
Technical field
The present invention relates to a kind of measurement method of carbonaceous organic material.Specifically, the assay method that relates to a kind of carbonaceous organic material soluble in water.This measurement method is take total organic carbon (TOC) determination techniques as the basis, utilize the TOC analyzer as analysis means, recently realize the mensuration of this organism quality concentration according to carbon containing percentage fixing in total organic carbon in the aqueous solution (TOC) content and this organism.This measurement method not only need not sample pre-treatments, and finding speed is fast, and is highly sensitive, and applied widely, and accuracy of measurement is high, is very suitable for on-the-spot on-line monitoring.
Background technology
At present, most of organic quantitative measurement all is (such as vapor-phase chromatography by chromatography, liquid phase chromatography), the chromatograph-mass spectrometer coupling method is (such as GC-MS(gas chromatography-mass spectrography), Liquid Chromatography-Mass Spectrometry), spectroscopic methodology (such as the UV, visible light spectrophotometric) and carrying out, these methods are sensitivity lower (detectability is generally more than the mg/L level) not only, and single sample is measured grow (sample determination that has is wanted more than the 30min) consuming time, even some sample also needs to carry out various pre-treatments (as filtering, concentrated, column front derivation etc.) afterwards, can measure, bring inevitable error to mensuration.Sensitivity is on the low side, complex operation, mensuration are consuming time, might introduce the factors such as error causes these methods to be difficult to become realtime on-line monitoring method.In the said determination method, require solvent to be necessary for organic solvent (such as methyl alcohol, ethanol, normal hexane etc.), and be not suitable for the concentration determination of organic aqueous solution, even reluctantly for it, bring irreversible damage also can for analytical column or instrument.In addition, some organism that newly synthesizes might not find suitable assay method in a short time, can measure with reference to the inventive method yet.
Summary of the invention
Purpose of the present invention is exactly for a kind of measurement method of carbonaceous organic material is provided.
Technical solution of the present invention is as follows:
1, a kind of measurement method of carbonaceous organic material, it is characterized in that: take total organic carbon (TOC) determination techniques as the basis, utilize the TOC analyzer as analysis means, recently realize the mensuration of this organism quality concentration according to carbon containing percentage fixing in total organic carbon in the aqueous solution (TOC) content and this organism;
2, detect analytic process and mainly finish at the TOC instrument, its detailed process is:
1) before certain carbonaceous organic material sample of measuring unknown concentration, with zero water (ultrapure water, complete carbon containing not in theory) the configuration carbon content is TC (total carbon), IC (total inorganic carbon (TIC)) the standard inventory solution of 1000mg/L, described TC standard reserving solution disposes with the pure Potassium Hydrogen Phthalate of top grade, and the IC standard reserving solution disposes with sodium carbonate and sodium bicarbonate;
2) according to the carbon content scope in the organic matter samples to be measured, select respectively TC, IC, NPOC (non-volatile organic carbon) and POC (volatile organic carbon) assay method to make the suitable TC of measurement range, IC, NPOC and POC typical curve;
3) according to 2) in typical curve, method for building up file, two method files are respectively minusing and measure and add and method is measured, wherein the TOC=TC-IC that records of above-mentioned minusing adds the TOC=NPOC+POC that records with method;
4) last, select 3 according to Acidity of Aikalinity, the carbon content of this organic matter samples to be measured) in suitable method file it carried out TOC measure, obtain the TOC value, selection principle is as follows:
When TOC＜＜during IC, should adopt to add and method;
When TOC＞＞during IC, should adopt minusing;
When TOC≤500 μ g/L, should adopt to add and method, and select the high sensitivity catalyzer;
When sample solution is highly acid or strong alkali solution, should adopt to add and method;
3, the calculating of the intrinsic carbon containing number percent of this organism supposes that this organic molecule formula is CnHmOxNy, and this organic carbon containing number percent is so:
ω(％)＝×100％
4, the mass concentration of this organic matter samples conversion, Cm=TOC/ ω, its unit is consistent with TOC unit.
Above-mentioned measurement method is not only simple to operate, measures fast, but also has stopped the personal error that pre-treatment brings; In the situation that adopts the high sensitivity catalyzer, the detection lower limit of carbon is low to moderate 10 μ g/L, and sensitivity is very high; Because the single sample minute generally is no more than 10min, and can realize continuous auto injection, therefore be highly suitable for on-the-spot online detection.But have a bit, organic matter samples to be measured is necessary for aqueous solution described in 4, and the body TOC in the water is very low, and with respect to the TOC contribution margin of this organism for whole solution, it can be ignored.
Embodiment
Below in conjunction with embodiment this measurement method is described further.
Embodiment 1: the online detection of the novel basifier monoethanolamine of nuclear power station secondary loop
Monoethanolamine is a kind of organic amine, because its strong basicity, low vapour-liquid distributivity and good thermal stability are applied in the middle of the nuclear power station secondary loop more and more.Greatly develop the generation Ⅲ nuclear power technology in China, the monoethanolamine water condition is confirmed as under the situation of nuclear power secondary circuit water technology, and the Accurate Determining of monoethanolamine concentration has caused expert's very big concern in the feedwater.Up to the present, the mensuration of domestic rarely seen relevant nuclear power secondary circuit monoethanolamine report.Also there is certain drawback in monoethanolamine concentration in the ion-chromatographic determination feedwater and abroad adopt: the mensuration such as Inorganic Ammonium ion pair monoethanolamine has great interference, analytical column is used behind certain number of times and must be changed, and the mensuration of high concentration ethanol amine must be diluted etc.Because the TOC content in the nuclear power station secondary loop feedwater body is very low, below 20 μ g/L, and the content of monoethanolamine is about 3500 μ g/L, namely therefore the main contributions of TOC can adopt this measurement method that the nuclear power station secondary loop monoethanolamine is carried out online in real time detection from monoethanolamine in the feedwater.Concrete steps are as follows:
1) obtains representational monoethanolamine sample solution from the feedwater sampling loop;
2) before measuring feedwater monoethanolamine concentration, with zero water (ultrapure water, complete carbon containing not in theory) the configuration carbon content is TC (total carbon), IC (total inorganic carbon (TIC)) the standard inventory solution of 1000mg/L, described TC standard reserving solution disposes with the pure Potassium Hydrogen Phthalate of top grade, and the IC standard reserving solution disposes with the pure sodium carbonate of top grade and sodium bicarbonate;
3) according to the concentration range (0-10mg/L) of monoethanolamine in the feedwater, select respectively TC, IC, NPOC (non-volatile organic carbon) and POC (volatile organic carbon) assay method to make TC, IC, NPOC and POC typical curve.Article one, 100 times of the standard TC that concentration was 10mg/L during typical curve only needed or the dilutions of IC solution (this standard solution is by 2) Plays storing solution obtain), the TOC instrument can be made TC, IC, NPOC and the POC typical curve that concentration is respectively 2mg/L, 4mg/L, 6mg/L, 8mg/L and 10mg/L automatically according to the extension rate of setting.
4) according to 3) in typical curve, method for building up file, two method files are respectively minusing and measure TOC and add and method is measured TOC, wherein the TOC=TC-IC that records of above-mentioned minusing adds the TOC=NPOC+POC that records with method;
5) since in the nuclear power secondary circuit feedwater ethanolamine solutions be strong basicity, and carbon content is more than 500 μ g/L, so selection standard catalyzer (need not select the high sensitivity catalyzer) and adding and method mensuration TOC, i.e. TOC=NPOC+POC.
3, the calculating of the intrinsic carbon containing number percent of monoethanolamine, the molecular formula of monoethanolamine is CnHmOxNy, this organic carbon containing number percent is so:
ω(％)＝×100％＝×100％＝39.34％
4, the conversion of monoethanolamine mass concentration, Cm=TOC/ ω, unit is consistent with TOC unit.Table 1 is measured the result of monoethanolamine concentration in the feedwater for laboratory simulation nuclear power station secondary loop working condition of water quality:
Under the table 1 laboratory simulation nuclear power station secondary loop water condition, the TOC method is measured the result of monoethanolamine concentration in the feedwater:
Said process and result show: adopt this measurement method to measure monoethanolamine concentration in the nuclear power station secondary loop feedwater, and not only simple to operate, measure fast, but also stopped the personal error that pre-treatment brings; In the situation that adopts the high sensitivity catalyzer, the detection lower limit of carbon can be low to moderate 10 μ g/L, and sensitivity is very high; The single sample minute generally is no more than 10min in addition, and can realize continuous auto injection, therefore is highly suitable for on-the-spot on-line monitoring.
Embodiment 2: the detection of monoethanolamine concentration in the nuclear power station precision processing system regeneration liquid waste
As described in Example 1, after the monoethanolamine water condition is adopted in the nuclear power station secondary loop feedwater, the resin of condensed water precision processing system can reach capacity because constantly exchange monoethanolamine, and in the resin after saturated, the yin, yang resin mainly exists with monoethanolamine and muriatic form respectively.For guaranteeing the treatment effeciency of condensed water precision processing system, condensed water precision processing system must be regenerated, so can contain the monoethanolamine of high level in the regeneration liquid waste with acid, alkali after operation a period of time.
Tight especially to the requirement of COD and N in the external nuclear power station wastewater discharge standard: 2007, be respectively 30 and 60mg/L, be respectively 20 and 40mg/L in 2008 to 2012, estimate after 2013, be respectively 10 and 20mg/L.The N that contains 2.36mg/L and 0.23mg/L in the monoethanolamine of every mg/L.In addition, monoethanolamine has stronger bio-toxicity, and in piscina, allowing maximum monoethanolamine concentration is 0.5mg/L.Therefore, for China's generation Ⅲ nuclear power unit that is about to adopt the monoethanolamine water condition, the monitoring of the regeneration liquid waste of condensed water precision processing system being carried out monoethanolamine concentration is necessary very much.
Determination step and embodiment 1 are basically identical, and just the measurement range of typical curve and method file need to adjust according to TOC content in the waste liquid.Another the large advantage that adopts this novel method to measure monoethanolamine concentration in this example also is: the TOC value that the method records not only can obtain through converting the accurate concentration of monoethanolamine in the waste liquid, can also convert through another within the specific limits and directly obtain COD value in the waste liquid.Therefore, the nuclear power operations staff can directly determine that according to the size of COD value regeneration liquid waste is direct discharging, or through again discharging after certain physics, chemistry and the biodegradation.
Claims (4)
1. the measurement method of a carbonaceous organic material, it is characterized in that: take total organic carbon (TOC) determination techniques as the basis, utilize the TOC analyzer as analysis means, recently realize the mensuration of this organism quality concentration according to carbon containing percentage fixing in total organic carbon in the aqueous solution (TOC) content and this organism.
2. detect analytic process and mainly finish at the TOC instrument, its detailed process is:
Before certain carbonaceous organic material sample of measuring unknown concentration, with zero water (ultrapure water, complete carbon containing not in theory) the configuration carbon content is the TC(total carbon of 1000mg/L), the IC(total inorganic carbon (TIC)) standard inventory solution, described TC standard reserving solution disposes with the pure Potassium Hydrogen Phthalate of top grade, and the IC standard reserving solution disposes with sodium carbonate and sodium bicarbonate;
According to the carbon content scope in the organic matter samples to be measured, select respectively TC, IC, the non-volatile organic carbon of NPOC() and the POC(volatile organic carbon) assay method makes the suitable TC of measurement range, IC, NPOC and POC typical curve;
According to 2) in typical curve, method for building up file, two method files are respectively minusing and measure and add and method is measured, wherein the TOC=TC-IC that records of above-mentioned minusing adds the TOC=NPOC+POC that records with method;
At last, select 3 according to the Acidity of Aikalinity of this organic matter samples to be measured, carbon content) in suitable method file it carried out TOC measure, obtain the TOC value, selection principle is as follows:
When TOC＜＜during IC, should adopt to add and method;
As TOC〉〉 during IC, should adopt minusing;
When TOC≤500 μ g/L, should adopt to add and method, and select the high sensitivity catalyzer;
When sample solution is highly acid or strong alkali solution, should adopt to add and method.
3. the calculating of the intrinsic carbon containing number percent of this organism supposes that this organic molecule formula is C
nH
mO
xN
y, this organic carbon containing number percent is so:
ω（%）=
×100%
The mass concentration conversion of this organic matter samples, C
m=TOC/ ω, its unit is consistent with TOC unit.
4. organic matter samples to be measured is necessary for aqueous solution described in the right 4, and the body TOC value in the water is very low, and with respect to the TOC contribution margin of this organism for whole solution, it can be ignored.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677765A (en) * | 2017-10-31 | 2018-02-09 | 浙江圣安化工股份有限公司 | A kind of method for deriving Production by Catalytic Combustion Process measure hydroxylamine salt organic residue based on TOC |
| CN110118744A (en) * | 2019-06-24 | 2019-08-13 | 江苏沥环科技有限公司 | A kind of method of total content of organic carbon in detection water |
Citations (3)
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| JPH05302920A (en) * | 1992-04-24 | 1993-11-16 | Shimadzu Corp | Carbon measuring apparatus |
| US20080198381A1 (en) * | 2007-02-21 | 2008-08-21 | Teledyne Tekmar Company | Pressurized detectors substance analyzer |
| CN201488944U (en) * | 2009-08-10 | 2010-05-26 | 重庆川仪自动化股份有限公司 | Total organic carbon (TOC) analyzer |
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- 2012-04-19 CN CN201210116435.3A patent/CN103376302B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05302920A (en) * | 1992-04-24 | 1993-11-16 | Shimadzu Corp | Carbon measuring apparatus |
| US20080198381A1 (en) * | 2007-02-21 | 2008-08-21 | Teledyne Tekmar Company | Pressurized detectors substance analyzer |
| CN201488944U (en) * | 2009-08-10 | 2010-05-26 | 重庆川仪自动化股份有限公司 | Total organic carbon (TOC) analyzer |
Non-Patent Citations (3)
| Title |
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| 周明浩等: "饮用水致突变前体物水生腐殖酸研究进展", 《重庆环境科学》, vol. 18, no. 3, 15 June 1996 (1996-06-15), pages 49 - 52 * |
| 彭朝辉 等: "天然水体中腐殖酸的分析方法", 《东北水利水电》, vol. 26, no. 8, 15 August 2008 (2008-08-15), pages 59 - 60 * |
| 殷旭慧: "水质监测中总有机碳测定方法之比较", 《工业水处理》, vol. 27, no. 8, 20 August 2007 (2007-08-20), pages 56 - 58 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677765A (en) * | 2017-10-31 | 2018-02-09 | 浙江圣安化工股份有限公司 | A kind of method for deriving Production by Catalytic Combustion Process measure hydroxylamine salt organic residue based on TOC |
| CN110118744A (en) * | 2019-06-24 | 2019-08-13 | 江苏沥环科技有限公司 | A kind of method of total content of organic carbon in detection water |
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