Time-Resolved Laser-Induced Breakdown Spectrometry for the Rapid Determination of Beryllium in Beryllium-Copper Alloys

1986 ◽  
Vol 40 (4) ◽  
pp. 491-494 ◽  
Author(s):  
John A. Millard ◽  
Robert H. Dalling ◽  
Leon J. Radziemski

Time-resolved laser-induced breakdown spectrometry has been combined with the long spark technique and applied to the rapid determination of beryllium in beryllium-copper alloys. A calibration curve was developed which related the beryllium concentration in a solid copper matrix to the Be(I) 234.9-nm to Cu(II) 235.7-nm intensity ratio. The beryllium concentrations ranged from 0.001 to 0.22%. For the lowest concentration the relative standard deviation of replicate samples was 7%, implying a detection limit of 0.0002% (2 ppm) at a signal-to-noise ratio of 3. The excitation temperature was determined from Boltzmann plots on Cu(I) and Cu(II), assuming local thermodynamic equilibrium. The values from the two spectra agreed well, and averaged to 13,850 K at 1 μS into the plasma lifetime.

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 35
Author(s):  
Jason Hoisington ◽  
Jason S. Herrington

A canister-based sampling method along with preconcentrator-Gas chromatography-Mass Spectrometry (GC-MS) analysis was applied to ethylene oxide (EtO or EO) and 75 other volatile organic compounds (VOCs) in ambient air. Ambient air can contain a large variety of VOCs, and thorough analysis requires non-discriminatory sampling and a chromatographic method capable of resolving a complex mixture. Canister collection of whole air samples allows for the collection of a wide range of volatile compounds, while the simultaneous analysis of ethylene oxide and other VOCs allows for faster throughput than separate methods. The method presented is based on US EPA Method TO-15A and allows for the detection of EtO from 18 to 2500 pptv. The method has an average accuracy of 104% and precision of 13% relative standard deviation (RSD), with an instrument run time of 32 min. In addition, a link between canister cleanliness and ethylene oxide growth is observed, and potential mechanisms and cleaning strategies are addressed.


1992 ◽  
Vol 46 (9) ◽  
pp. 1382-1387 ◽  
Author(s):  
J. A. Aguilera ◽  
C. Aragón ◽  
J. Campos

Laser-induced breakdown spectroscopy has been used to determine carbon content in steel. The plasma was formed by focusing a Nd:YAG laser on the sample surface. With the use of time-resolved spectroscopy and generation of the plasma in nitrogen atmosphere, a precision of 1.6% and a detection limit of 65 ppm have been obtained. These values are similar to those of other accurate conventional techniques. Matrix effects for the studied steels are reduced to a small slope difference between the calibration curves for stainless and nonstainless steels.


2015 ◽  
Vol 69 (5) ◽  
Author(s):  
Qing-Qing Guan ◽  
Xiao-Dian Huang ◽  
Yan-Hua Zeng ◽  
Chao-Hai Wei ◽  
Ping Ning ◽  
...  

AbstractThis paper reports a headspace analysis technique for the determination of products, i.e., cyclohexanone (CE) and cyclohexanol (CL), of phenol hydrogenation in a supercritical water reaction system (SWRS) with water removal by hydrate formation. An addition of anhydrous calcium chloride leads to water absorption resulting in crystal water; thus, the samples can be quantitatively measured without the influence of water. After achieving equilibrium at 150­°C and maintaining it for 5 min, the obtained results showed a relative standard deviation of less than 5.3 % and the recovery ranged from 93 % to 104 %. The presented method is simple and accurate for the analysis of CL, CE and phenol in samples from phenol conversion in SWRS.


Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2930 ◽  
Author(s):  
Tingting Shen ◽  
Wenwen Kong ◽  
Fei Liu ◽  
Zhenghui Chen ◽  
Jingdong Yao ◽  
...  

Quick access to cadmium (Cd) contamination in lettuce is important to supervise the leafy vegetable growth environment and market. This study aims to apply laser-induced breakdown spectroscopy (LIBS) technology for fast determination of Cd content and diagnosis of the Cd contamination degree in lettuce. Emission lines Cd II 214.44 nm, Cd II 226.50 nm, and Cd I 228.80 nm were selected to establish the univariate analysis model. Multivariate analysis including partial least squares (PLS) regression, was used to establish Cd content calibration models, and PLS model based on 22 variables selected by genetic algorithm (GA) obtained the best performance with correlation coefficient in the prediction set Rp2 = 0.9716, limit of detection (LOD) = 1.7 mg/kg. K-Nearest Neighbors (KNN) and random forest (RF) were used to analyze Cd contamination degree, and RF model obtained the correct classification rate of 100% in prediction set. The preliminary results indicate LIBS coupled with chemometrics could be used as a fast, efficient and low-cost method to assess Cd contamination in the vegetable industry.


2013 ◽  
Vol 295-298 ◽  
pp. 950-953 ◽  
Author(s):  
Dong Yuan ◽  
Da You Fu ◽  
Wen Yuan Tan

A rapid spectrophotometric method for flow injection determination of sulfite in tan wastewater is described. The proposed method was based on the addition reaction of sulfite with fuchsin in Na2B4O7-NaOH medium. The optimum conditions allow a linear calibration range of 0.01-1.20 μg ml-1 SO32-. The detection limit is 0.0023μg ml-1 (S/N=3), and the relative standard deviation for night replicate measurements is 1.1% for 0.5μg ml-1 of sulfite. The sampling rate is 60 samples h-1. The procedure has been applied to the determination of sulfite in tan wastewater. The results were in good agreement with those obtained by pararosaniline method.


2021 ◽  
Author(s):  
Tao Lin ◽  
Xinglian Chen ◽  
Li Wang ◽  
Haixian Fang ◽  
Maoxuan Li ◽  
...  

Abstract The simultaneous determination method of 8 amide pesticides by multi-walled carbon nanotubes (MWCNs) cleanup, combined with QuEChERS method and ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry has been developed and successfully applied in complex matrix such as green onions, celery, leeks, citrus, lychees, avocado. The matric effect of MWCNs is optimized and compared with QuEChERS materials. The results show that MWCNs can effectively reduce the matrix effect in sample extraction. The mass spectrometry is optimized, through their chemical structure skeletons, the ESI+ and ESI- mode are simultaneously scanned in the method. The coefficient (r) is greater than 0.9990, the limit of quantification ranges from 0.03 to 0.80 μg/kg, the recovery rate ranges from 71.2% to 120%, and the relative standard deviation (RSD) ranges from 3.8% to 9.4%. The method is fast, simple, sensitive, and has good purification effect. It is suitable for the rapid determination of amide pesticides in complex matrix agri-food.


2002 ◽  
Vol 85 (3) ◽  
pp. 712-718
Author(s):  
Mohammad Farid Hussain ◽  
Anil Kumar Sangahi ◽  
Iqbal Ahmad ◽  
Bal Krishan Puri

Abstract Lead is quantitatively adsorbed as the lead N-methylethylxanthocarbamate (MEXC)–benzyldimethyltetradecylammonium (BDTA) ion pair complex on microcrystalline naphthalene in the pH range 4.0–11.0. The metal is desorbed with HCl and determined by differential pulse polarography. Alternatively lead can be quantitatively adsorbed on the adsorbent (MEXC–BDTA–naphthalene) packed in a column at a flow rate of 1–2 mL/min and determined similarly. Dissolved oxygen is removed by adding a few milliliters of 4% NaBH4 solution. The detection limit is 0.12 μg/mL at the minimum instrumental settings (signal-to-noise ratio, 2). Linearity was obtained over the concentration range 0.3–20.0 μg/mL with a correlation factor of 0.9998 and a relative standard deviation of ± 0.98%. Various parameters, such as the effect of pH, volume of aqueous phase, flow rate, and the interference of a large number of metal ions and anions, were studied in detail to optimize the conditions for the trace determination of lead in various standard alloys, standard biological materials, and environmental samples.


1999 ◽  
Vol 82 (3) ◽  
pp. 614-619 ◽  
Author(s):  
Steven M Plakas ◽  
Kathleen R El Said ◽  
F Aladar Bencsath ◽  
Steven M Musser ◽  
Calvin C Walker

Abstract Rapid methods are described for determination of flumequine (FLU) residues in muscle and plasma of farm-raised channel catfish (Ictalurus punctatus). FLU residues were extracted from tissues with an acidified methanol solution, and extracts were cleaned up on C18 solid-phase extraction cartridges. FLU concentrations were determined by liquid chromatography (LC)using a C18 analytical column and fluorescence detection (excitation, 325 nm; emission, 360 nm). Mean recoveries of FLU from fortified muscle were 87–94% at 5 levels ranging from 10 to 160 ppb (5 replicates per level). FLU recoveries from fortified plasma were 92–97% at 5 levels ranging from 20 to 320 ppb. Limits of detection (signal-to-noise ratio, 3:1)for the method as described were 3 and 6 ppb for muscle and plasma, respectively. Relative standard deviations (RSDs) for recoveries were ≤12%. Live catfish were dosed with 14C-labeled or unlabeled FLU to generate incurred residues. Recoveries of 14C residues throughout extraction and cleanup were 90 and 94% for muscle and plasma, respectively. RSDs for incurred FLU at 2 levels in muscle and plasma ranged from 2 to 6%. The identity of FLU in incurred tissues was confirmed by LC/mass spectrometry.


2013 ◽  
Vol 448-453 ◽  
pp. 359-362
Author(s):  
Mo Jie Sun ◽  
Ling Zhang ◽  
Ruo Kun Jia

Chloral alkali at room temperature Can be quickly converted into chloroform completely, Application of this principle, By Purge and Trap GC/MS method , Determination of the alkali content of chloroform in water before and after the difference, Inverse to get the water content of chloral. NaOH were added to different volumetric flask. It is flask with standard solutions in different concentrations. Aside a certain amount of determination, error is larger. NaOH was injected directly into the injector. This was the method. It completely transformed in Purge and Trap, greatly reduces human error. The linear range is 0.5-20ug/L, the minimum detection limit can reach 0.05ug/L, the relative standard deviation is less than 2.3%, the average recovery was 97.5%. This method is simple and quick,the results are accurate and reliable, which is able to meet the drinking water source in the analytical needs of chloral.


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