Determination of lysine content based on an in situ pretreatment and headspace gas chromatographic measurement technique.

This work reports on a simple method for the determination of lysine content by an in situ sample pretreatment and headspace gas chromatographic measurement (HS-GC) technique, based on carbon dioxide (CO2) formation from the pretreatment reaction (between lysine and ninhydrin solution) in a closed vial. It was observed that complete lysine conversion to CO2 could be achieved within 60 min at 60 °C in a phosphate buffer medium (pH = 4.0), with a minimum molar ratio of ninhydrin/lysine of 16. The results showed that the method had a good precision (RSD < 5.23%) and accuracy (within 6.80%), compared to the results measured by a reference method (ninhydrin spectroscopic method). Due to the feature of in situ sample pretreatment and headspace measurement, the present method becomes very simple and particularly suitable to be used for batch sample analysis in lysine-related research and applications. Graphical abstract The flow path of the reaction and HS-GC measurement for the lysine analysis.

Determination of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution by reaction-based headspace gas chromatography.

We report on a headspace gas chromatographic method for determining the content of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution. It was based on quantitatively converting 3-chloro-1,2-propanediol to formaldehyde by periodate oxidation in a closed headspace sample vial at a room temperature for 10 min, and then to methanol by borohydride reduction at 90°C for 40 min followed by the headspace gas chromatographic measurement. The results showed that the present method has an excellent measurement precision (relative standard deviation < 2.60%) and accuracy (recoveries from 96.4-102%) in 3-chloro-1,2-propanediol analysis. The limit of quantitation was 0.031 mg/mL. It is simple and suitable for determining the 3-chloro-1,2-propanediol content in polyamideamine epichlorohydrin resin solution.

Determination of the softening point of rosin by a simple and automated headspace gas chromatographic technique.

We report a simple and automated headspace gas chromatographic technique for the determination of the softening point of rosin. A lumpy solid of rosin is added into a headspace vial, then an automated stepwise temperature ramping and headspace sampling was performed at each temperature stage and gas chromatography measurement. By plotting the gas chromatography signal for an impurity in rosin versus the temperature, a transition point (corresponding to the rosin softening point) was determined. The results show that the present method has a good precision (<0.76%), and good accuracy (the relative differences compared to the ring and ball method was <4.0%). The present method is simple, accurate, and automated. It is practical and suitable for testing the softening of rosin and derivatives in mills.

Efficient Determination of Specific Surface Area of Shale Samples Using a Tracer-Based Headspace Gas Chromatographic Technique.

This paper reports on a novel method for determining the specific surface area (SSA) of shale via headspace gas chromatography (HS-GC). The method is based on the water adsorption on the surface of shale sample after achieving phase equilibrium at an elevated temperature (i.e., heating at 125 °C for 48 h). A mathematical model shows that the SSA can be determined from the signal of the vapor water released during HS-GC analysis. The results obtained by this method correlated well (R2 = 0.992) with data obtained by the reference BET method. Because the phase equilibrium step for multiple samples can be conducted simultaneously, and because the phase re-equilibrium step is much faster in the HS-GC measurement, the present method is more efficient for batch sample testing.

Method for improving accuracy in full evaporation headspace analysis.

We report a new headspace analytical method in which multiple headspace extraction is incorporated with the full evaporation technique. The pressure uncertainty caused by the solid content change in the samples has a great impact to the measurement accuracy in the conventional full evaporation headspace analysis. The results (using ethanol solution as the model sample) showed that the present technique is effective to minimize such a problem. The proposed full evaporation multiple headspace extraction analysis technique is also automated and practical, and which could greatly broaden the applications of the full-evaporation-based headspace analysis.

Determination of Porosity in Shale by Double Headspace Extraction GC Analysis.

This paper reports on a novel method for the rapid determination of the shale porosity by double headspace extraction gas chromatography (DHE-GC). Ground core samples of shale were placed into headspace vials and DHE-GC measurements of released methane gas were performed at a given time interval. A linear correlation between shale porosity and the ratio of consecutive GC signals was established both theoretically and experimentally by comparing with the results from the standard helium pycnometry method. The results showed that (a) the porosity of ground core samples of shale can be measured within 30 min; (b) the new method is not significantly affected by particle size of the sample; (c) the uncertainties of measured porosities of nine shale samples by the present method range from 0.31 to 0.46 p.u.; and (d) the results obtained by the DHE-GC method are in a good agreement with those from the standard helium pycnometry method. In short, the new DHE-GC method is simple, rapid, and accurate, making it a valuable tool for shale gas-related research and applications.

[A Method for Determination of Migratable Fluorescent Whitening Agents in Paper Products by Dual-Wavelength UV Spectroscopy].

The current national standard method GB/T 27741-2011, i.e., "quantitative determination of migratable fluorescent whitening agents-UV spectroscopy", overestimates the migratable fluorescent whitening agents (FWA) in the paper based products because of the spectral interference of the leached lignin from the cellulose fibers. To minimize such interference, a spectroscopic method based on dual-wavelength (305 and 348 nm) measurement was proposed. It was observed that the dual-wavelength spectroscopy can effectively subtract the spectral absorption contributed by the leached lignin in the extraction medium, thus more accurately determination of migratable FWA can be performed. The results showed that the present method has a relative standard deviation of 2.17%, the quantitative detection limit of 16.9 mg x kg(-1), and recovery of 98%-103%. Compared with the current alternative standard-HPLC method, the present method possesses advantages of low operation and maintenance costs, simple, and practical in application. Therefore, it is more suitable for the rapid determination of migratable FWA in the product quality control in the production process and sample examination in the commercial market.

[A triple-wavelength visible spectroscopic method for determination of iron content in lignocellulosic materials].

The present paper described a triple-wavelength visible spectroscopic method for the determination of iron content in lignocellulosic materials. After the sample was pretreated with acidic hydrolysis method under selected conditions, the color agent, 1, 10-phenanthroline monohydrate, was added in the filtrate and then measured by a triple-wavelength spectroscopic method at wavelengths of 416, 510 and 700 nm, from which the iron contents of the sample can be calculated. The results showed that this method can efficiently deduct the influences of acidic soluble lignin and furfural compounds generated during the sample pretreatment and baseline drift caused by the tiny particles in the filtrates. It not only has a good measurement precision but also is accurate, in which the relative differences of the results obtained by the present method and ICP-OES method is less than 5%. The method is simple and practical, and suitable for industrial applications.

[Rapid determination of silicon content in black liquor of straw fibrous material].

The present paper reports a novel method for the determination of silicon content in straw fibrous material black liquor based on alpha-Si--Mo heteropoly acid spectrophotometry. The selected conditions were as follows: detection wavelength 360 nm, pH 4.0, and reaction time 10 min. It was found that the acidic soluble lignin in the sample liquor was the major interference species in the silicon content determination. The interference of acidic soluble lignin can be eliminated by hydrogen peroxide-nitric acid digestion method. The present method is not only simple, rapid, stable and less interferential, but also of good measurement precision and accuracy, with the relative standard deviations of 0.9%, and recoveries of 99.0%-102%. It is suitable for use in high silicon content of black liquor routine rapid analyses.

Determination of methanol partition coefficient in octanol/water system by a three-phase ratio variation headspace gas chromatographic method.

Determining the methanol partition coefficient (Kow) in octanol/water system is important to assess the risk of its impact to humans and the environment. In this paper, we report a novel method for the determination of the Kow of methanol with headspace gas chromatography (HS-GC), using a three-phase equilibrium-based phase ratio variation approach. Three headspace vials with different phase ratios [(1) 0.2 mL of water plus 3 mL of octanol, (2) 1 mL of water plus 3 mL of octanol and (3) 1 mL of water plus 10 mL of octanol] were used in the experiment. After pre-standing at 25 °C for > 10 h and equilibrating in the headspace oven at a temperature of interest for additional 25 min, the methanol signals of the vapor phase (i.e., the headspace) in these vials were measured by HS-GC, from which the Kow of methanol can be calculated based on the established equations. The results showed that the method has good precision (within 0.06 log unit in standard deviation) and acceptable accuracy (with method error within 0.5 log unit). A correlation between the Kow of methanol and temperature extrapolated the Kow values in a temperature range of interest. The present method represents a simple and in-situ approach for the determination of the Kow of methanol and is also suitable to be applied to other volatile compounds.