Agilent Fpd Detector Manual

[Quincey Homer]

Thisis a basic HPLC comprising an iso pump, manual injection, column compartment and UV detector. This base model HPLC has been built with simple analysis in mind, where an isocratic method and UV detection is sufficient. It would be ideal for analysis of simple compounds (such as caffeine, for example), either as a standalone system in a QC lab, or as a secondary system in a larger research or production lab. Manual injection is ideal for a smaller number of samples where an autosampler would be excessive.

Externally, it is clear that this system has seen previous use, and there are some marks on the casings. Internally the system is clean and has been fully refurbished by a qualified HPLC engineer. Click here to find out more about our refurbished HPLC services

The eDAQ C4D can be connected to the Agilent 7100 CE instrument, providing contactless conductivity detection for the instrument.Both the C4D headstage and UV detector can be connected to the capillary at the same time, enabling both types of detection to be performed with a single sample injection.

The data from both C4D and UV-Visible detectors can be recorded and displayed in real time. You can use either the eDAQ PowerChrom software or Agilent ChemStation software. Use the ET120 C4D Headstage and select either the:

You should ensure that the C4D headstage and its flat grey cable are at least 1 cm away from the capillary as it loops inside the cartridge. This is to prevent the high voltage inside the capillary from shorting through the headstage and its cable, which are both electrically grounded.

You must also have the Application firmware installed on the C4D hardware unit. The user can switch the firmware themselves, between Serial and Application firmware, using the ER8x5 Converter and Updater Software (download from here and find instructions in the video and manuals).

Set up the hardware and PowerChrom software as detailed in the manuals. Connect the headstage to the capillary. You should connect the modified EC071 Trigger cable, from the CE instrument to the I2C connector at the back of the ER8x5 unit, so that the Agilent ChemStation software sends a message to PowerChrom software to trigger start recording.

Selecting C4D Settings The C4D settings (amplitude, frequency and headstage gain) should be selected in the PowerChrom software. Do not use the C4D Configurator Software when the ER815 and ER825 are configured with applications firmware, or when using the ER225.

You must have the Serial firmware installed on the C4D hardware unit. The user can switch the firmware themselves, between Serial and Application firmware, using the ER8x5 Converter and Updater Software (download from here and find instructions in the video and manuals).

You should refer to the Agilent 7100 Capillary Electrophoresis System User Manual, which can be downloaded from here. The Agilent 7100 Capillary Electrophoresis System has a 20-bit AD converter built in. It enables voltage conversions ranging from 0 V to 1 V.

Selecting C4D Settings The C4D Configurator software allows the setting up of the C4D settings (amplitude, frequency and headstage gain) of ER815 and ER825 C4D Detector when they are configured with the serial firmware. It provides a simple alternative to the use of direct serial commands. Download the C4D Configurator software from the Software Downloads. The procedure for using this software is shown in a video and has been written up as a pdf manual.

A novel, rapid and efficient manual shaking and ultrasound-assisted surfactant-enhanced emulsification microextraction (M-UASEME) combined with gas chromatography-flame photometric detection (GC-FPD) was developed for the extraction and determination of eight organophosphorus pesticides (OPPs) in tap water and honey samples. The main parameters that affected the extraction efficiency were investigated and optimized. Under the optimum conditions, the relative standard deviation (RSD, n = 6) ranged from 2.4 to 9.3%. Limits of detection (LOD) were varied between 0.005 and 0.05 g L-1. Good linearity was obtained in a range of 0.5-50.0 g L-1 for all analytes with the correlation coefficients (r) > 0.9964. Finally, the developed method was successfully applied to determine the eight pesticide residues in real samples. The recoveries of the target analytes in samples were between 82.4 and 96.7%.

The traditional liquid-liquid extraction (LLE) method has been in use for many years and taken an important role in the field of sample preparation. However, from the practical point of view, LLE suffered from several inherent drawbacks, such as time consuming, unsatisfactory enrichment factors and the use of large volume of hazardous organic solvents.11 Ramos, L.; J. Chromatogr. A 2012, 1221, 84.

In this work, we developed a novel manual shaking and ultrasound-assisted surfactant-enhanced emulsification microextraction (M-UASEME) for the determination of eight organophosphorus pesticides (OPPs) in tap water and honey samples. Various parameters such as the kind and volume of the extraction solvent, the type and concentration of the surfactant, ultrasound time, salt addition and the extraction temperature were evaluated and optimized. The developed M-UASEME method overcomes several drawbacks of the former liquid-phase microextraction methods, while it maintains their advantages.

All pesticide standards (ethoprophos, fenitrothion, malathion, chlorpyrifos, isocarbophos, methidathion, profenofos, and triazophos) were obtained from Agricultural Environmental Protection Institution (Tianjin, China). The stock standard solutions of each analyte were prepared in acetone at a concentration of 1 g L-1. The standard working solutions (1 mg L-1) were daily achieved by appropriate dilution of the stock standard solutions with ultra-high purity water. Both the stock standard solutions and standard working solutions were stored in dark at 4 C.

All reagents used in this application were of HPLC grade unless otherwise mentioned and all dilutions were carried out using ultra-high purity water (resistivity of 18.2 MΩ cm). Ultra-high purity water was purified by a Milli-Q purification system (Millipore, Bedford, MA, USA). Extraction solvents chlorobenzene, 1,2-dichlorobenzene, and carbon tetrachloride were obtained from Sinopharm Chemical Reagent Co. Ltd (Tianjin, China). Sodium dodecyl sulfate (SDS), cethyltrimethyl ammonium bromide (CTAB), Tween 20, Triton X-100 and Triton X-114 were purchased from Beijing Chemical Reagents Company (Beijing, China).

The chromatographic analysis was carried out on an Agilent 6890N gas chromatograph (GC) equipped with a flame photometric detector (FPD) system (Agilent Technologies, Palo Alto, CA, USA). Chromatographic separation was accomplished on an HP-5 (5% phenyl, 95% methylpolysiloxane, 30 m 0.25 mm i.d. 0.25 m) capillary column, obtained from J&W Scientific (Folsom, CA, USA). The injection port was made in the splitless mode at 270 C with splitless time of 0.5 min. Nitrogen was used as the carrier gas at a flow rate of 1.0 mL min-1. The detector temperature was set at 250 C and it was fed with 75 mL min-1 of hydrogen (> 99.999%), 100 mL min-1 of purified compressed air and 25 mL min-1 of nitrogen (> 99.999%) as auxiliary gas. The temperature-programmed mode was as follows: the initial oven temperature was set at 100 C and then ascended to 220 C at the rate of 20 C min-1, held for 1 min and followed by a 30 C min-1 ramp to 280 C, held for 2 min. The total GC run time was 11 min. The identification of the analytes was confirmed by the retention time.

Honey (Bai Hua, 2010) was obtained from the local supermarket. 0.5 g (dry weight) of the honey sample was accurately weighted and diluted with ultra-high purity water to form a 50 g L-1 honey solution.

For the M-UASEME, 5.0 mL aqueous samples were placed in a 10 mL screw cap glass centrifuge tube. 15.0 L of chlorobenzene as extraction solvent and 5.0 L of 200 mmol L-1 Triton X-100 as emulsifier (the concentration of Triton X-100 in sample solution was 0.2 mmol L-1) were added into the test tube. The mixture was gently shaken three times (about two seconds) by hand, and a cloudy solution was formed. Then the cloudy solution was immersed into an ultrasonic water bath for extraction. The extractions were performed at 40 kHz of ultrasound frequency and 300 W (KQ 300DB, 300 W, 0-40 kHz, Kunshan Ultrasonic Instrument, Kunshan, China) for 10 s at 23 C. In the whole extraction step, the OPPs were extracted into the fine droplets of chlorobenzene. Then the emulsion was disrupted by centrifugation (RJ-TDL-40B, 0-5000 rpm, Ruijiang Instrument, Wuxi, China). In order to avoid the influence of temperature changes during the centrifugation process, the test tube was wrapped up by absorbent cotton and was stuffed into a 50 mL plastic centrifuge tube. The plastic centrifuge tube was centrifuged at the speed of 3800 rpm for 5 min and the extraction solvent was sedimented at the bottom of the test tube. After that, the sedimented phase was withdrawn by a 10.0 L microsyringe (Gao Ge, Shanghai, China) and 1.0 L of collected organic solvent was injected into the GC system for analysis.

In order to achieve high extraction recoveries and enrichment factors (EFs), various parameters which could probably influence the extraction were investigated and optimized. The optimization was carried out on an aqueous solution containing 5.0 g L-1 of each analyte and the parameters were performed by modifying one at a time while keeping the remaining constant. The enrichment factors (EFs), which were defined as the ratio between the concentration of analyte in the sediment phase and the initial concentration of analyte in the sample, were used to evaluate the extraction efficiency.

The selection of an appropriate extraction solvent is critical for the establishment of an efficient M-UASEME process. The extraction solvent has to meet the following requirements: it should have a higher density than water, good chromatographic behavior, a low solubility in water, high extraction capability for the target analytes and could form a stable emulsification system under ultrasound energy. Therefore, three organic solvents including chlorobenzene, 1,2-dichlorobenzene, and carbon tetrachloride were examined as possible extraction solvents for M-UASEME. The experiment was performed by using 15.0 L of each extraction solvent with Triton X-100 as an emulsifier. Figure 1 shows the effect of these extraction solvents on the EFs. As can be seen in Figure 1, when chlorobenzene was used, the highest value of EFs could be achieved. This can be explained by the fact that, chlorobenzene has the closer polarities with the target analytes than the others and these properties could be favorable for the extraction efficiency. Therefore, chlorobenzene was selected.

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