CN103376302A - Novel testing method of carbon-containing organic substance - Google Patents

Novel testing method of carbon-containing organic substance Download PDF

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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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carbon
t0c
organic
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tc
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CN103376302B (en
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朱志平
周艺
赵永福
周瑜
陆海伟
付晶
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长沙理工大学
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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

一种含碳有机物的新型测定方法 A novel method for measuring organic carbonaceous

技术领域 FIELD

[0001] 本发明涉及一种含碳有机物的新型测定方法。 [0001] The present invention relates to a novel method for measuring the carbon-containing organic material. 具体地说,涉及一种易溶于水的含碳有机物的测定方法。 In particular, it relates to one kind of the carbonaceous organic substances soluble in water measurement method. 该新型测定方法以总有机碳(T0C)测定技术为基础,利用T0C测定仪作为分析手段,根据水溶液中总有机碳(T0C)含量和该有机物中固定的含碳百分比来实现该有机物质量浓度的测定。 In the novel method for measuring total organic carbon (T0C) technology, the use of analytical tools as T0C oximeter to achieve the organic substance concentration in the aqueous solution in accordance with the total organic carbon (T0C) and the content of organic carbon fixed percentage Determination. 该新型测定方法不仅无需样品前处理,测定速度快,灵敏度高,而且适用范围广,测定准确度高,非常适合于现场的在线监测。 The novel method for measuring not only do not need sample preparation, fast measurement speed, high sensitivity, and wide application range, high accuracy measurement, is ideal for online monitoring site.

背景技术 Background technique

[0002]目前,大部分有机物的定量测定都是通过色谱法(如气相色谱法、液相色谱法)、色谱-质谱联用法(如气相色谱-质谱联用法、液相色谱-质谱联用法)、光谱法(如紫外可见分光光度)而进行的,这些方法不仅灵敏度较低(检测限一般在mg/L级以上),而且单个样品测定耗时较长(有的一个样品测定要30min以上),甚至某些样品还需要进行各种前处理(如过滤、浓缩、柱前衍生等)之后,方可进行测定,给测定带来了不可避免的误差。 [0002] Currently, most of the organic substances are quantitatively determined by chromatography (e.g., gas chromatography, liquid chromatography), Chromatography - Mass Spectrometry (gas chromatography - mass spectrometry, liquid chromatography - mass spectrometry) , spectroscopy (e.g., UV-visible spectrophotometry) carried out, these methods are not only less sensitive (detection limit usually in mg / L and above), and a single sample measurement takes a long time (some for a sample measured over 30min) Thereafter, some samples even further require various pre-processing (e.g., filtered, concentrated, pre-column derivatization, etc.), before measurement, to bring the inevitable errors measured. 灵敏度偏低、操作繁琐、测定耗时、有可能引入误差等因素导致这些方法很难成为实时在线监测方法。 Low sensitivity, complicated operation, takes the measurement, is possible to introduce errors as a result of these factors is very difficult to be real-time online monitoring method. 上述测定方法中,要求溶剂必须为有机溶剂(如甲醇、乙醇、正己烷等),并不适用于有机物水溶液的浓度测定,即使勉强为之,也会给分析柱或者仪器带来不可逆的损坏。 The above-described measuring method, it is required to be solvent is an organic solvent (e.g. methanol, ethanol, n-hexane, etc.), are not suitable for the determination of the concentration of the aqueous organic, even barely worth, it will bring irreversible damage to the instruments or the analytical column. 另夕卜,某些新合成的有机物有可能在短期内并没有找到合适的测定方法,也可以参照本发明方法进行测定。 Another Bu Xi, certain novel organic compounds synthesized possible suitable assay method is not found in the short term, it may be determined with reference to the method of the present invention.

发明内容 SUMMARY

[0003] 本发明的目的就是为了提供一种含碳有机物的新型测定方法。 [0003] The object of the present invention is to provide a novel method for measuring the carbon-containing organic material.

[0004] 本发明技术方案如下: [0004] The technical solution of the present invention is as follows:

[0005] 1、一种含碳有机物的新型测定方法,其特征在于:以总有机碳(T0C)测定技术为基础,利用T0C测定仪作为分析手段,根据水溶液中总有机碳(T0C)含量和该有机物中固定的含碳百分比来实现该有机物质量浓度的测定; [0005] a novel method for measuring the carbon-containing organic material, characterized in that: the total organic carbon (T0C) measurement techniques based on the use as analytical tools T0C oximeter, (T0C) according to the content of total organic carbon in an aqueous solution and the fixed organic carbon to achieve measurement of the percentage of concentration of organic substances;

[0006] 2、检测分析过程主要在T0C仪上完成,其具体过程为: [0006] 2, mainly in the process of analysis of the instrument completes T0C, specific process is:

[0007] 1)在测定未知浓度的某含碳有机物样品前,用零水(超纯水,理论上完全不含碳)配置含碳量为1000mg/L的TC (总碳)、1C (总无机碳)标准储备溶液,所述TC标准储备液用优级纯邻苯二甲酸氢钾配置,1C标准储备液用碳酸钠和碳酸氢钠配置; [0007] 1) prior to assay a sample carbonaceous organics were unknown concentration, with zero water (ultrapure water, in theory, completely free of carbon) configured carbon content of 1000mg / L of TC (total carbon), 1C (total inorganic carbon) standard stock solution, the TC standard stock solution with pure class configuration, potassium hydrogen phthalate, 1C standard stock solution with sodium carbonate and bicarbonate configuration;

[0008] 2)根据待测有机物样品中的含碳量范围,分别选用TC、1C、NP0C(非挥发性有机碳)和P0C(挥发性有机碳)测定方法做出测定范围合适的TC、1C、NP0C和P0C标准曲线; [0008] 2) The scope of organic carbon content of the test sample, were selected TC, 1C, NP0C (non-volatile organic carbon) and P0C (volatile organic carbon) to make a determination of the appropriate measurement range TC, 1C , NP0C and P0C standard curve;

[0009] 3)根据2)中的标准曲线,建立方法文件,两方法文件分别为差减法测定和加和法测定,其中上述差减法测得的TOC = TC-1C,加和法测得的TOC = NP0C+P0C ; [0009] 3) the standard curve 2) the method of establishing a file, two files are methods Determination subtraction and the addition method, wherein said subtraction measured TOC = TC-1C, additivity is measured TOC = NP0C + P0C;

[0010] 4)最后,根据该待测有机物样品的酸碱性、含碳量选择3)中合适的方法文件对其进行T0C测定,得到T0C值,选取原则如下: [0010] 4) Finally, selected according to the pH, organic carbon content of the test sample 3) in a suitable method for its file T0C measured value obtained T0C, select the following principles:

[0011] 当T0C << 1C时,应采用加和法;[0012] 当TOC >> IC时,应采用差减法; [0011] When T0C << 1C, the method should be used and added; [0012] When the TOC >> IC, the subtraction should be used;

[0013] 当T0C ( 500 μ g/L时,应采用加和法,并选用高灵敏度催化剂; [0013] When T0C (500 μ g / L, should be added and method, and selects the high sensitivity of the catalyst;

[0014] 当样品溶液为强酸性或强碱性溶液时,应采用加和法; [0014] When the sample solution is strongly acidic or basic solution, adding and method should be used;

[0015] 3、该有机物固有含碳百分比的计算,假设该有机物分子式为CnHmOxNy,那么该有机物的含碳百分比为: [0015] 3, the percentage of organic carbon-containing inherent calculated, assuming that the organic substance of the formula CnHmOxNy, then the percentage of the carbon-containing organic material is:

[0016] ω (% ) = Χ100% [0016] ω (%) = Χ100%

[0017] 4、该有机物样品的质量浓度折算,Cm = TOC/ω,其单位与TOC单位一致。 [0017] 4, concentration of the organic substance sample conversion, Cm = TOC / ω, which is the same unit as the unit TOC.

[0018] 上述新型测定方法不仅操作简单,测定快速,而且还杜绝了前处理带来的人为误差;在采用高灵敏度催化剂的情况下,碳的检测下限低至10 μ g/L,灵敏度非常高;由于单个样品测定时间一般不超过lOmin,且能实现连续自动进样,因此非常适用于现场的在线检测。 [0018] The novel measurement method is not only simple, quick measurement, but also eliminate the human error caused by pre-treatment; in the case of high sensitivity of the catalyst, the lower detection limit as low carbon 10 μ g / L, the sensitivity is very high ; Since the individual sample measurement time is generally no more than lOmin, and can achieve continuous autosampler, so it is suitable for online testing site. 但是有一点,4中所述待测有机物样品必须为水溶液,且水中的本体T0C很低,相对于该有机物对整个溶液的T0C贡献值而言,其可以忽略不计。 But one thing, 4 in the test sample must be organic solution, and the water body is very low T0C, with respect to the organic substance in terms of contribution to the overall solution T0C, which is negligible.

具体实施方式 Detailed ways

[0019] 下面结合具体实施方式对本新型测定方法作进一步说明。 [0019] DETAILED DESCRIPTION The following embodiments of the present novel measurement method is further illustrated.

[0020] 实施例1:核电站二回路新型碱化剂乙醇胺的在线检测 [0020] Example 1: Novel Secondary Circuit line detection alkalizing agent ethanolamine

[0021] 乙醇胺是一种有机胺,因其强碱性、低汽液分配性和良好的热稳定性被越来越多地应用到核电站二回路当中。 [0021] An organic amine is ethanolamine, due to its strongly basic, low vapor-liquid distribution and good thermal stability are increasingly being applied to the circuit among the two nuclear power plants. 在我国大力发展第三代核电技术,乙醇胺水工况被确定为核电二回路水处理技术的情形下,给水中乙醇胺浓度的准确测定引起了业内专家的极大关注。 In the case of China to develop third-generation nuclear power technology, ethanolamine water condition is determined to be two nuclear power loop water treatment technology, to accurately determine the concentration of ethanolamine in water caused great concern to industry experts. 到目前为止,国内鲜见有关核电二回路乙醇胺的测定报道。 So far, the determination of domestic rare reports of two nuclear power circuit ethanolamine. 而国外采用离子色谱法测定给水中乙醇胺浓度也存在一定的弊端:如无机铵离子对乙醇胺的测定有极大的干扰,分析柱用到一定次数后必须更换,高浓度乙醇胺的测定必须进行稀释等。 The foreign using ion chromatography to ethanolamine concentration in water also has some disadvantages: such as inorganic ammonium ions interfere with the determination of great ethanolamine, analytical columns must be replaced after a certain number of uses, the determination of high concentrations of ethanolamine and the like must be diluted . 由于核电站二回路给水本体中的T0C含量很低,在20 μ g/L以下,而乙醇胺的含量在3500 μ g/L左右,即给水中T0C的主要贡献来自乙醇胺,因此可以采用该新型测定方法对核电站二回路乙醇胺进行在线实时检测。 Since the feed water of nuclear power plants T0C body in low levels, in the 20 μ g / L or less, and the content of diethanolamine is about 3500 μ g / L, i.e., the feed water from the main contribution T0C ethanolamine, the novel assay method can be employed of Secondary circuit ethanolamine-line real-time detection. 具体步骤如下: Specific steps are as follows:

[0022] 1)从给水取样回路取得有代表性的乙醇胺样品溶液; [0022] 1) to obtain a representative sample from the water solution of ethanolamine sample loop;

[0023] 2)在测定给水乙醇胺浓度前,用零水(超纯水,理论上完全不含碳)配置含碳量为1000mg/L的TC (总碳)、1C (总无机碳)标准储备溶液,所述TC标准储备液用优级纯邻苯二甲酸氢钾配置,1C标准储备液用优级纯碳酸钠和碳酸氢钠配置; [0023] 2) before measuring the concentration of feedwater ethanolamine, with zero water (ultrapure water, in theory, completely free of carbon) configured carbon content of 1000mg / L of TC (total carbon), 1C (total inorganic carbon) Standard stock solution, the TC standard stock solution with pure class configuration, potassium hydrogen phthalate, 1C standard stock solution with sodium carbonate and bicarbonate pure class configuration;

[0024] 3)根据给水中乙醇胺的浓度范围(0-10mg/L),分别选用TC、IC、NP0C (非挥发性有机碳)和P0C(挥发性有机碳)测定方法做出TC、IC、NP0C和P0C标准曲线。 [0024] 3) The ethanolamine in water to a concentration range (0-10mg / L), were selected (volatile organic carbon) Determination of TC, IC, NP0C (non-volatile organic carbon) and made P0C TC, IC, NP0C and P0C standard curve. 一条标准曲线仅需中一个浓度为10mg/L的标准TC或1C溶液(该标准溶液由2)中标准储备液稀释100倍得到),T0C仪可以根据设定的稀释倍数自动做出浓度分别为2mg/L、4mg/L、6mg/L、8mg/L和10mg/L的TC、1C、NP0C和P0C标准曲线。 A standard curve only in a concentration of 10mg / L standard solution 1C or TC (The standard solution consists of 2) standard stock solution was diluted 100 fold to give), T0C instrument dilution can be made automatically in accordance with set concentrations of 2mg / L, 4mg / L, 6mg / L, 8mg / L and 10mg / L of TC, 1C, NP0C and P0C standard curve.

[0025] 4)根据3)中的标准曲线,建立方法文件,两方法文件分别为差减法测定T0C和加和法测定T0C,其中上述差减法测得的TOC = TC-1C,加和法测得的TOC = NP0C+P0C ; [0025] 4) The calibration curve 3) the method of establishing a file, two files are measuring method measuring T0C T0C subtraction and summation law, wherein said subtraction measured TOC = TC-1C, additivity test We were TOC = NP0C + P0C;

[0026] 5)由于核电二回路给水中乙醇胺溶液呈强碱性,且含碳量在500 μ g/L以上,因此选用标准催化剂(无须选用高灵敏度催化剂)和加和法测定T0C,即TOC = NP0C+P0C。 [0026] 5) Since the two loops Nuclear ethanolamine solution to strongly alkaline water, and a carbon content of 500 μ g / L or more, catalyst selection criteria (selection of high sensitivity without catalyst) Canadian T0C and assay methods, i.e. TOC = NP0C + P0C.

[0027] 3、乙醇胺固有含碳百分比的计算,乙醇胺的分子式为CnHmOxNy,那么该有机物的含碳百分比为: [0027] 3, calculated inherent carbonaceous percent ethanolamine, ethanolamine formula CnHmOxNy, then the percentage of the carbon-containing organic material is:

[0028] ω (% ) = Χ100%= Χ100%= 39.34% [0028] ω (%) = Χ100% = Χ100% = 39.34%

[0029] 4、乙醇胺质量浓度的折算,Cm = TOC/ ω,单位与TOC单位一致。 [0029] 4, concentration of the conversion of ethanolamine, Cm = TOC / ω, the same unit as the unit TOC. 表1为实验室模拟核电站二回路水质工况测定给水中乙醇胺浓度的结果: The measurement results in Table 1 to the ethanolamine concentration in the water quality laboratory simulation Secondary Circuit conditions are:

[0030] 表1实验室模拟核电站二回路水工况下,T0C法测定给水中乙醇胺浓度的结果: [0030] Table 1 Secondary Circuit laboratory simulation water conditions, T0C result to the determination of the concentration of ethanolamine in water:

Figure CN103376302AD00051

[0033] 上述过程和结果表明:采用该新型测定方法测定核电站二回路给水中乙醇胺浓度,不仅操作简单,测定快速,而且还杜绝了前处理带来的人为误差;在采用高灵敏度催化剂的情况下,碳的检测下限可低至10 μ g/L,灵敏度非常高;再加之单个样品测定时间一般不超过lOmin,且能实现连续自动进样,因此非常适用于现场的在线监测。 [0033] The process and the results showed: Determination of Secondary Circuit diethanolamine concentration in water using a novel measurement method which is not only simple, quick measurement, but also eliminate the human error caused by pre-treatment; the case of high sensitivity catalyst detection limit may be as low carbon 10 μ g / L, the sensitivity is very high; single sample measurement time of generally not more than plus lOmin, and can achieve continuous autosampler, so it is suitable for online monitoring of the scene.

[0034] 实施例2:核电站精处理系统再生废液中乙醇胺浓度的检测 [0034] Example 2: Polishing System reproduction detecting nuclear power plant effluent concentration ethanolamine

[0035] 如实施例1所述,核电站二回路给水采用乙醇胺水工况后,凝结水精处理系统的树脂会因为不断地交换乙醇胺而达到饱和,饱和后的树脂中,阴、阳树脂分别主要以乙醇胺和氯化物的形式存在。 After [0035] As described in Example 1, ethanolamine feed water nuclear power plant water condition, condensate polishing system constantly exchange resin because of saturated ethanol amine, the resin saturation, male and female respectively, the main resin in the form of chloride and ethanolamine. 为保证凝结水精处理系统的处理效率,凝结水精处理系统运行一段时间后,必须用酸、碱进行再生,因此再生废液中会含有较高含量的乙醇胺。 To ensure efficient condensate polisher processing system, the water condensate polishing system for some time, to be regenerated with an acid, a base, and therefore the regeneration effluent will contain higher ethanolamines content.

[0036] 国外核电站废水排放标准中对C0D和N的要求特别严:2007年,分别为30和60mg/L,2008至2012年分别为20和40mg/L,预计2013年以后,分别为10和20mg/L。 [0036] Foreign nuclear power plant wastewater discharge requirements for C0D and N is particularly critical: 2007, respectively, 30 and 60mg / L, 2008 to 2012 were 20 and 40mg / L, 2013 after respectively 10 and 20mg / L. 每mg/L的乙醇胺中含2.36mg/L和0.23mg/L的N。 Per mg / L of ethanolamine containing 2.36mg / L and 0.23mg / L is N. 另外,乙醇胺有较强的生物毒性,在养鱼池塘中,允许最大乙醇胺浓度为0.5mg/L。 Further, ethanolamine strong toxicity, fish in the pond, the maximum allowable concentration of ethanolamine 0.5mg / L. 因此,对于即将采用乙醇胺水工况的我国第三代核电机组来说,对凝结水精处理系统的再生废液进行乙醇胺浓度的监测非常有必要。 Thus, ethanolamine for the upcoming third-generation hydraulic conditions of nuclear power plant, the regeneration waste water of condensate polishing system to monitor the concentration of the ethanolamine is necessary.

[0037] 测定步骤与实施例1基本一致,只是标准曲线的测定范围和方法文件需根据废液中T0C含量进行调整。 [0037] The procedure of Example 1 was measured basically the same, but the measurement range and the standard curve method file needs T0C in accordance with the content of the waste is adjusted. 该例中采用本新型方法测定乙醇胺浓度的另一大优势还在于:该方法测得的T0C值不仅可以经过换算得到废液中乙醇胺的准确浓度,还可以在一定范围内经过另一换算直接得到废液中C0D值。 This embodiment using the new method of measuring the concentration of diethanolamine present another advantage in that: the method T0C measured value may be subjected not only in terms of the exact concentration of the effluent ethanolamine, may also be within a certain range after the other directly converted C0D effluent values. 因此,核电运行人员可直接根据C0D值的大小确定再生废液是直接排放,还是经过一定的物理、化学和生物降解后再排放。 Thus, operation of nuclear power can directly determine the regeneration waste water is discharged directly or after a certain physical, chemical and biological degradation before discharge values ​​according to the size C0D.

Claims (4)

1.一种含碳有机物的新型测定方法,其特征在于:以总有机碳(TOC)测定技术为基础,利用T0C测定仪作为分析手段,根据水溶液中总有机碳(T0C)含量和该有机物中固定的含碳百分比来实现该有机物质量浓度的测定。 1. A novel method for measuring the carbon-containing organic material, characterized in that: the total organic carbon (TOC) measurement techniques based on the use as an analytical means T0C meter, total organic carbon according aqueous solution (T0C) and the organic matter content a fixed percentage of the carbon-containing organic material to achieve measurement of the mass concentration.
2.检测分析过程主要在T0C仪上完成,其具体过程为: 在测定未知浓度的某含碳有机物样品前,用零水(超纯水,理论上完全不含碳)配置含碳量为1000mg/L的TC (总碳)、IC (总无机碳)标准储备溶液,所述TC标准储备液用优级纯邻苯二甲酸氢钾配置,1C标准储备液用碳酸钠和碳酸氢钠配置; 根据待测有机物样品中的含碳量范围,分别选用TC、IC、NP0C (非挥发性有机碳)和P0C(挥发性有机碳)测定方法做出测定范围合适的TC、1C、NP0C和P0C标准曲线; 根据2 )中的标准曲线,建立方法文件,两方法文件分别为差减法测定和加和法测定,其中上述差减法测得的T0C=TC-1C,加和法测得的T0C=NP0C+P0C ; 最后,根据该待测有机物样品的酸碱性、含碳量选择3)中合适的方法文件对其进行T0C测定,得到T0C值,选取原则如下: 当T0C〈〈IC时, 应采用加和法; 当T0C»IC时,应采用差减法; 当T0C 2. detection analysis are completed on the instrument T0C, which is a specific process: a sample of a carbon-containing organic compounds before measuring an unknown concentration, with zero water (ultrapure water, in theory, completely free of carbon) configured carbon content of 1000mg / L, TC (total carbon), the IC (TIC) standard stock solution, the TC standard stock solution with pure class configuration, potassium hydrogen phthalate, 1C standard stock solution with sodium carbonate and bicarbonate configuration; the range of organic carbon content of the test sample, were selected TC, IC, NP0C (non-volatile organic carbon) and P0C (volatile organic carbon) to make a determination of the appropriate measurement range TC, 1C, NP0C standards and P0C curve; standard curve 2) the method of establishing a file, two files are measured subtraction method and the addition method for the assay, wherein said subtraction measured T0C = TC-1C, additivity measured T0C = NP0C + P0C; Finally, according to pH, organic carbon content of the test sample selection 3) in its file suitable method T0C measured value obtained T0C selecting principle is as follows: when T0C << IC, should additivity; when T0C »IC, subtraction should be used; when T0C ( 500 μ g/L时,应采用加和法,并选用高灵敏度催化剂; 当样品溶液为强酸性或强碱性溶液时,应采用加和法。 When the (500 μ g / L, should be added and method, and selects the high sensitivity of the catalyst; and when the sample solution is strongly acidic or basic solution, adding and method should be used.
3.该有机物固有含碳百分比的计算,假设该有机物分子式为CnHmOxNy,那么该有机物的含碳百分比为: 12& ω (%) = —-—~— X 100% 12aHhmL-S-lfe+14y 该有机物样品的质量浓度折算,Cm=T0C/co,其单位与T0C单位一致。 3. The percentage of the carbon-containing natural organic calculation, assuming the organic substance of the formula CnHmOxNy, then the percentage of the carbon-containing organic material is: 12 & ω (%) = --- ~ - X 100% 12aHhmL-S-lfe + 14y the organic substance concentration of the sample mass conversion, Cm = T0C / co, which is consistent with the unit T0C units.
4.权利4中所述待测有机物样品必须为水溶液,且水中的本体T0C值很低,相对于该有机物对整个溶液的T0C贡献值而言,其可以忽略不计。 4. The test claim 4 in an aqueous solution must be organic sample, and the body of water T0C low value, with respect to the organic solution of the entire T0C contribution, its negligible.
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