静态顶空分析的新理论、新技术及其在制浆造纸中的应用
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摘要
静态顶空分析技术，是一种定量准确、灵敏度和自动化程度高的气相萃取检测技术。该技术不仅成功地消除了样品基质溶剂及非挥发性组分对GC分析的影响和对仪器的损害，而且大大简化了样品的预处理步骤、节约了时间、避免了在样品准备过程中被检测物质的流失，十分适合于对基质复杂性高的样品（如制浆造纸工业中的废液、纸品、原料等）进行分析检测。然而，顶空分析技术进样理论的不完善性及新技术的欠缺，使得它还不能对制浆造纸研究中很多难检测被分析物进行准确分析、甚至不能分析。因此，建立适应现实需求的顶空分析技术的新理论、新技术以及相应检测方法的开发，对于改善制浆造纸工业分析方法的研究现状、进而提高对相关科学问题展开研究的可能性和研发速度具有十分重要的现实意义。
为了保证顶空分析技术的进样准确性、提高检测灵敏度，通过对顶空分析的制样平衡、高温平衡、加压平衡、放压平衡四种平衡态下的物料衡算、压力衡算、并综合温度效应，建立了静态顶空分析技术的进样理论基础及灵敏度分析体系。研究了相平衡体系和SFV-FET、SPV-FET、SNV-FET四种典型顶空分析技术中溶质全挥发率、检测灵敏度与溶剂饱和蒸汽压、温度、气液分配系数、定量环体积之间的关系，并给出了提高检测灵敏度的方式。建立了顶空加压过程的非平衡态动态模型，并利用空气中的氧气做示踪剂建立了一种检测样品体积或密度的示踪检测方法。
以全挥发理论的灵敏度分析结果为出发点，为了提高极难挥发的被检测物质的检测灵敏度、解决水相样品高温HS-GC-MS检测的困难，开发了溶剂全固化-溶质全挥发顶空分析技术。该技术成功避免了溶剂高温下大量挥发对气相中被检测物质的稀释，降低了放压过程中气相体积膨胀系数，并消除了被检测物质气液平衡系数对全挥发率的影响（样品最大允许进样量仅与全固化试剂用量相关），极大地提高了检测的灵敏度（2～6个数量级）；同时，避免了溶剂对气相色谱柱分离、检测器的影响，使得水相样品进行高温HS-GC-MS分析成为可能。并建立了氧脱木素废液及纸浆洗涤滤液中低浓度甲醇的检测方法，相比传统全挥发技术该方法的定量限（60ppb）提高了约1800倍。
结合上述建立的低浓度甲醇检测方法，分别研究了麦草浆、南方松硫酸盐浆、高卡伯值桉木浆及低卡伯值桉木浆在氧脱木素过程中的甲醇生成规律，建立了适合描述四种浆料甲醇生成的修正一级动力学模型，并结合木素脱除的动力学模型及纸浆黏度的变化给出了四种纸浆氧脱木素过程中甲醇生成量的控制方案。研究发现：麦草浆和两种桉木浆的甲醇生成动力学参数具有一致性，且其甲醇生成量与卡伯值之间的线性关系不受氧脱木素条件影响；而对于南方松木浆的氧脱木素过程，提高反应温度和用碱量不仅可在更短时间内达到目标卡伯值（并保证了纸浆的黏度）、更可显著降低氧脱木素过程中甲醇的生成量（>50%）。
在相反应转化顶空分析应用中，分别基于高锰酸钾、碘酸钾在酸性体系下的反应特性，建立了漂白废液中残余过氧化氢和草酸根含量的高灵敏度、批量检测方法；并依托硼氢化钠在碱性条件下的高选择性，建立了纸巾和微胶囊乳液中甲醛含量的间接检测方法。结果表明，在本研究确定的反应条件下，四种方法均能满足实际样品的定量限要求（H_2O_22.8ppm，C_2O_4~-13ppm，CH_2O7.7ppm，CH_2O5.7ppm），且具有很好的选择性（有效屏蔽了干扰组分）、准确性（RSD>95%）和可靠性（回收率95%～105%）。另外，还利用样品的破坏性预处理方式，以42.5%磷酸为反应介质通过对反应和检测条件的优化建立了纸浆中甲醇含量的检测方法，经验证该方法具有很高的检测限（66ppm）、准确性（RSD>96.5%）、及可靠性（回收率93%～102%）。
利用示踪顶空分析技术，分别结合顶空的两相非稳态平衡和三相稳态分配平衡建立了高温高浓流体粘度及纳米微乳液颗粒平均粒径、挥发性组分的液-固吸附平衡常数的检测模型。证实了使用两相非稳态平衡示踪检测模型对高温（110℃）高浓（固形物53%～75%）黑液粘度的适用性；并将三相稳态检测模型应用于纳米级聚苯乙烯微乳液的粒径分析中（采用甲苯作示踪技术），结果表明利用该方法检测纳米颗粒平均粒径的方法是完全可行的，并最终确定了甲苯的液-固体系吸附平衡常数（2651cm-1）。
采用高压-溶剂全挥发顶空分析技术建立了气相中挥发性组分浓度与GC检测信号之间比例系数的检测方法，并将其应用于纸品中甲醇向空气的脱附研究中；建立了纸品中甲醇释放的动力学模型，确定了纸品在不同存放密度及环境温度下达到国家室内甲醇限量标准所需的时间、给出了相应的通风条件建议。利用多次顶空抽提技术建立了原位检测过氧化氢漂白过程中氧气生成动态变化的研究方案，并结合具体条件给出了不同体系下氧气生成量与反应条件的关系。
As a vapor-phase extraction technique, static headspace gas chromatography (HS-GC) isan indirect detection technology with high accuracy, sensitivity and automaticity. HSextraction is not only successful in eliminating the effects of solvent and non-volatilecomponents in sample matrix on GC analysis or the possible damage to instrument system,but also greatly simplifies the steps of sample pretreatment, saves time, and avoids the analyteloss during sample preparation. It is very suitable for the determination of analytes in processsamples with high complexity of matrices, such as raw materials, waste effluents, andproducts in pulp and paper industry. However, as a relatively new technology, there is still agreat potential to explore some new theories and techniques for the headspace based analysis,from which the quantification for many difficult industrial samples can be performed byHS-GC.
In order to improving the accuracy and detection sensitivity in headspace analysis, wehave established some new theories of headspace sampling based on mass balance, pressurebalance, and pressure and temperature effects at the equilibrium states. The relations ofanalyte evaporation rate and detection sensitivity with the solvent saturated vapor pressure,temperature, gas-liquid partition coefficient, and sample loop volume have been investigatedfor the typical headspace analysis’ techniques, i.e., phase equilibrium, solvent fullvaporization-full evaporation technique (FET), solvent partial vaporization-FET,non-volatile solvent-FET. Several methodologies have developed for improving the detectionsensitivity in headspace analysis. Moreover, a tracing (using oxygen in sample vial air)detection method that is able to measure the sample’ density/volume has been established.
In order to improve detection sensitivity for trace amount of volatile analytes andovercome the water-vapor problem met in HS-GC-MS analysis for aqueous samples, asolvent full solidification full evaporation technique (SFS-FET) has been developed. Thistechnique can avoid the dilution of solvent vaporization on analytes in vapor, reduce theexpansion coefficient of gas phase in headspace vial during venting, and eliminate the effectof gas-liquid coefficient of analytes on its evaporation rate. The SFS-FET could not onlygreatly increase the detection sensitivity (from2to6orders of magnitude), but also avoid theimpacts of solvent on GC detector and its column separation, which makes it possible toconduct a HS-GC-MS analysis at high temperature for aqueous samples. The limits ofquantification in the new method were60ppb, which is1800times low of the traditional FETmethod in methanol testing. This technique has been successfully applied to the determination of methanol in oxygen delignification (OD) effluents and pulp washing filtrate.
Based on the above method for methanol, we conducted series of investigations on themethanol formation during OD processes of wheat straw, southern pine, and eucalyptus pulpwith high and low kappa number, respectively, from which a modified first-order kineticmodel was developed and it is suitable to describe the methanol formation in these processes.Combined the kinetic model for lignin removal with the variation of pulp viscosity, weproposed the methanol control strategies at these processes. For the processes of wheat strawand eucalyptus pulp, their kinetic parameters are uniform. The reaction conditions of ODprocess have no influence on the linear relationship between the amounts of methanol and thekappa number of pulps. For southern pine pulp, the improvement of the reaction efficiencycould also significantly reduce the methanol amount (>50%) generated in the process.
Based on phase reaction conversion headspace analysis, a batch testing method for theresidual hydrogen peroxide (with potassium permanganate) and oxalate (with potassiumiodate), respectively, in bleaching effluents were developed. Moreover, an indirect detectionmethod for formaldehyde in the tissue paper and microcapsules latex, using sodiumborohydride as reducing agent in both cases, was also developed. The results showed thatthese methods could meet the testing requirements in these sample analyses, in which theaccuracies of the method were better than95%and LOQ for H_2O_2, C_2O_4~-, CH_2O, and CH_2Owere2.8,13,7.7, and5.7ppm respectively. It was found that using42.5%phosphoric acid asa pretreatment reaction medium could completely dissolve the paper fibers, thus the methanolentrapped in paper products could be released and quantitatively measured by the HS-GCmethod mentioned above.
Based on the tracing headspace analysis technique, the viscosity of a concentrated fluidsample at high temperature was determined, in which a two-phase unsteady-state model wasderived. The tracing headspace analysis technique was also used for measuring the averageparticle size of nano-particles of a polymer latex, according to the solid adsorptionequilibrium constant of volatile components from a three-phase steady-state model.
Based on high pressure SFV-FET, a detection method was established for measuring theproportional coefficients between analytes’ concentration in gas phase and GC signal. It wasapplied to the study of the air emission of methanol from paper products. A similar approach(coupled with a multiple headspace extraction technique) was also used for in-situ detectionof oxygen formation during the degradation of hydrogen peroxide.
为了保证顶空分析技术的进样准确性、提高检测灵敏度，通过对顶空分析的制样平衡、高温平衡、加压平衡、放压平衡四种平衡态下的物料衡算、压力衡算、并综合温度效应，建立了静态顶空分析技术的进样理论基础及灵敏度分析体系。研究了相平衡体系和SFV-FET、SPV-FET、SNV-FET四种典型顶空分析技术中溶质全挥发率、检测灵敏度与溶剂饱和蒸汽压、温度、气液分配系数、定量环体积之间的关系，并给出了提高检测灵敏度的方式。建立了顶空加压过程的非平衡态动态模型，并利用空气中的氧气做示踪剂建立了一种检测样品体积或密度的示踪检测方法。
以全挥发理论的灵敏度分析结果为出发点，为了提高极难挥发的被检测物质的检测灵敏度、解决水相样品高温HS-GC-MS检测的困难，开发了溶剂全固化-溶质全挥发顶空分析技术。该技术成功避免了溶剂高温下大量挥发对气相中被检测物质的稀释，降低了放压过程中气相体积膨胀系数，并消除了被检测物质气液平衡系数对全挥发率的影响（样品最大允许进样量仅与全固化试剂用量相关），极大地提高了检测的灵敏度（2～6个数量级）；同时，避免了溶剂对气相色谱柱分离、检测器的影响，使得水相样品进行高温HS-GC-MS分析成为可能。并建立了氧脱木素废液及纸浆洗涤滤液中低浓度甲醇的检测方法，相比传统全挥发技术该方法的定量限（60ppb）提高了约1800倍。
结合上述建立的低浓度甲醇检测方法，分别研究了麦草浆、南方松硫酸盐浆、高卡伯值桉木浆及低卡伯值桉木浆在氧脱木素过程中的甲醇生成规律，建立了适合描述四种浆料甲醇生成的修正一级动力学模型，并结合木素脱除的动力学模型及纸浆黏度的变化给出了四种纸浆氧脱木素过程中甲醇生成量的控制方案。研究发现：麦草浆和两种桉木浆的甲醇生成动力学参数具有一致性，且其甲醇生成量与卡伯值之间的线性关系不受氧脱木素条件影响；而对于南方松木浆的氧脱木素过程，提高反应温度和用碱量不仅可在更短时间内达到目标卡伯值（并保证了纸浆的黏度）、更可显著降低氧脱木素过程中甲醇的生成量（>50%）。
在相反应转化顶空分析应用中，分别基于高锰酸钾、碘酸钾在酸性体系下的反应特性，建立了漂白废液中残余过氧化氢和草酸根含量的高灵敏度、批量检测方法；并依托硼氢化钠在碱性条件下的高选择性，建立了纸巾和微胶囊乳液中甲醛含量的间接检测方法。结果表明，在本研究确定的反应条件下，四种方法均能满足实际样品的定量限要求（H_2O_22.8ppm，C_2O_4~-13ppm，CH_2O7.7ppm，CH_2O5.7ppm），且具有很好的选择性（有效屏蔽了干扰组分）、准确性（RSD>95%）和可靠性（回收率95%～105%）。另外，还利用样品的破坏性预处理方式，以42.5%磷酸为反应介质通过对反应和检测条件的优化建立了纸浆中甲醇含量的检测方法，经验证该方法具有很高的检测限（66ppm）、准确性（RSD>96.5%）、及可靠性（回收率93%～102%）。
利用示踪顶空分析技术，分别结合顶空的两相非稳态平衡和三相稳态分配平衡建立了高温高浓流体粘度及纳米微乳液颗粒平均粒径、挥发性组分的液-固吸附平衡常数的检测模型。证实了使用两相非稳态平衡示踪检测模型对高温（110℃）高浓（固形物53%～75%）黑液粘度的适用性；并将三相稳态检测模型应用于纳米级聚苯乙烯微乳液的粒径分析中（采用甲苯作示踪技术），结果表明利用该方法检测纳米颗粒平均粒径的方法是完全可行的，并最终确定了甲苯的液-固体系吸附平衡常数（2651cm-1）。
采用高压-溶剂全挥发顶空分析技术建立了气相中挥发性组分浓度与GC检测信号之间比例系数的检测方法，并将其应用于纸品中甲醇向空气的脱附研究中；建立了纸品中甲醇释放的动力学模型，确定了纸品在不同存放密度及环境温度下达到国家室内甲醇限量标准所需的时间、给出了相应的通风条件建议。利用多次顶空抽提技术建立了原位检测过氧化氢漂白过程中氧气生成动态变化的研究方案，并结合具体条件给出了不同体系下氧气生成量与反应条件的关系。
As a vapor-phase extraction technique, static headspace gas chromatography (HS-GC) isan indirect detection technology with high accuracy, sensitivity and automaticity. HSextraction is not only successful in eliminating the effects of solvent and non-volatilecomponents in sample matrix on GC analysis or the possible damage to instrument system,but also greatly simplifies the steps of sample pretreatment, saves time, and avoids the analyteloss during sample preparation. It is very suitable for the determination of analytes in processsamples with high complexity of matrices, such as raw materials, waste effluents, andproducts in pulp and paper industry. However, as a relatively new technology, there is still agreat potential to explore some new theories and techniques for the headspace based analysis,from which the quantification for many difficult industrial samples can be performed byHS-GC.
In order to improving the accuracy and detection sensitivity in headspace analysis, wehave established some new theories of headspace sampling based on mass balance, pressurebalance, and pressure and temperature effects at the equilibrium states. The relations ofanalyte evaporation rate and detection sensitivity with the solvent saturated vapor pressure,temperature, gas-liquid partition coefficient, and sample loop volume have been investigatedfor the typical headspace analysis’ techniques, i.e., phase equilibrium, solvent fullvaporization-full evaporation technique (FET), solvent partial vaporization-FET,non-volatile solvent-FET. Several methodologies have developed for improving the detectionsensitivity in headspace analysis. Moreover, a tracing (using oxygen in sample vial air)detection method that is able to measure the sample’ density/volume has been established.
In order to improve detection sensitivity for trace amount of volatile analytes andovercome the water-vapor problem met in HS-GC-MS analysis for aqueous samples, asolvent full solidification full evaporation technique (SFS-FET) has been developed. Thistechnique can avoid the dilution of solvent vaporization on analytes in vapor, reduce theexpansion coefficient of gas phase in headspace vial during venting, and eliminate the effectof gas-liquid coefficient of analytes on its evaporation rate. The SFS-FET could not onlygreatly increase the detection sensitivity (from2to6orders of magnitude), but also avoid theimpacts of solvent on GC detector and its column separation, which makes it possible toconduct a HS-GC-MS analysis at high temperature for aqueous samples. The limits ofquantification in the new method were60ppb, which is1800times low of the traditional FETmethod in methanol testing. This technique has been successfully applied to the determination of methanol in oxygen delignification (OD) effluents and pulp washing filtrate.
Based on the above method for methanol, we conducted series of investigations on themethanol formation during OD processes of wheat straw, southern pine, and eucalyptus pulpwith high and low kappa number, respectively, from which a modified first-order kineticmodel was developed and it is suitable to describe the methanol formation in these processes.Combined the kinetic model for lignin removal with the variation of pulp viscosity, weproposed the methanol control strategies at these processes. For the processes of wheat strawand eucalyptus pulp, their kinetic parameters are uniform. The reaction conditions of ODprocess have no influence on the linear relationship between the amounts of methanol and thekappa number of pulps. For southern pine pulp, the improvement of the reaction efficiencycould also significantly reduce the methanol amount (>50%) generated in the process.
Based on phase reaction conversion headspace analysis, a batch testing method for theresidual hydrogen peroxide (with potassium permanganate) and oxalate (with potassiumiodate), respectively, in bleaching effluents were developed. Moreover, an indirect detectionmethod for formaldehyde in the tissue paper and microcapsules latex, using sodiumborohydride as reducing agent in both cases, was also developed. The results showed thatthese methods could meet the testing requirements in these sample analyses, in which theaccuracies of the method were better than95%and LOQ for H_2O_2, C_2O_4~-, CH_2O, and CH_2Owere2.8,13,7.7, and5.7ppm respectively. It was found that using42.5%phosphoric acid asa pretreatment reaction medium could completely dissolve the paper fibers, thus the methanolentrapped in paper products could be released and quantitatively measured by the HS-GCmethod mentioned above.
Based on the tracing headspace analysis technique, the viscosity of a concentrated fluidsample at high temperature was determined, in which a two-phase unsteady-state model wasderived. The tracing headspace analysis technique was also used for measuring the averageparticle size of nano-particles of a polymer latex, according to the solid adsorptionequilibrium constant of volatile components from a three-phase steady-state model.
Based on high pressure SFV-FET, a detection method was established for measuring theproportional coefficients between analytes’ concentration in gas phase and GC signal. It wasapplied to the study of the air emission of methanol from paper products. A similar approach(coupled with a multiple headspace extraction technique) was also used for in-situ detectionof oxygen formation during the degradation of hydrogen peroxide.
引文
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