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The aim of the journal «Analysis and Testing Technology and Instruments» is to offer a platform for the publication of new technologies, new theories, new methods and new achievements in the field of analytical chemistry. It follows the guiding principles of combining technical work with academic study and applied science with basic research, and highlights on innovation.
2023, 29(3): 231-244.
doi: 10.16495/j.1006-3757.2023.03.001
Abstract
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Abstract:
Ion mobility spectrometry (IMS) utilizes the difference in ion mobility K (collision cross section) to realize the separation and determination of different ions, which has the advantages of fast analysis speed and high sensitivity. And it coupling with mass spectrometry (IM-MS) was widely used in the fields of proteomics, metabolomics, medicine, etc. With the increasing complexity of the analyzed objects, higher demands are put on the resolution of the IMS. Traveling wave ion mobility spectrometry (TWIMS) uses a time-domain continuous traveling wave electric field to realize ion transport and separation. The analytical path length of the TWIMS is not limited by the amplitude of the travelling wave voltage, theoretically the path can be extended indefinitely to improve the resolution. Currently, the resolution of TWIMS can reach up to 1 860, which is advantageous for the analysis of complex samples with the multiple isomers. The principle of TWIMS and the influencing factors of resolution were introduced, the characteristics, performance and applications of TWIMS instruments with different structures were further discussed, and finally the future development directions of TWIMS were prospected.
Ion mobility spectrometry (IMS) utilizes the difference in ion mobility K (collision cross section) to realize the separation and determination of different ions, which has the advantages of fast analysis speed and high sensitivity. And it coupling with mass spectrometry (IM-MS) was widely used in the fields of proteomics, metabolomics, medicine, etc. With the increasing complexity of the analyzed objects, higher demands are put on the resolution of the IMS. Traveling wave ion mobility spectrometry (TWIMS) uses a time-domain continuous traveling wave electric field to realize ion transport and separation. The analytical path length of the TWIMS is not limited by the amplitude of the travelling wave voltage, theoretically the path can be extended indefinitely to improve the resolution. Currently, the resolution of TWIMS can reach up to 1 860, which is advantageous for the analysis of complex samples with the multiple isomers. The principle of TWIMS and the influencing factors of resolution were introduced, the characteristics, performance and applications of TWIMS instruments with different structures were further discussed, and finally the future development directions of TWIMS were prospected.
2023, 29(3): 245-260.
doi: 10.16495/j.1006-3757.2023.03.002
Abstract:
The in situ, micro-area and high-resolution spatial distribution characteristics of elements in the samples are of practical and important research significance. In biological samples, the in situ spatial distribution characteristics of elements can be used as indicators of physiological processes, reveal metabolic pathways, and reflect the ways in which environmental characteristics affect organisms. In geological samples, the in situ spatial distribution characteristics of elements can be used as a basis for mineral evaluation and an important indicator for studying the process of environmental geochemical changes. At present, several commonly used techniques for measuring the in situ distribution characteristics of elements in micro-areas include: micro X-ray fluorescence spectrometry (μXRF), synchrotron radiation technology (SR), electron microscopy-energy dispersive spectrometry (EM-EDS), electron probe technology (EP), laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS), laser induced breakdown plasma emission spectroscopy (LIBS), etc. Based on the principle of testing samples, these technologies differ in many aspects such as non-destructive testing, quantitative testing, suitable sample type and size, complexity of pre-treatment methods, detection limits and resolution, and so on. The current mainstream of the micro-area in situ element distribution detection techniques were introduced and summarized, the advantages and disadvantages of various techniques and their applicable sample types and application ranges were analyzed and compared. The selection of standard samples, data calibration and processing and visualization into maps were discussed for the first time, which provides a technical reference for related scientific research and analysis work.
The in situ, micro-area and high-resolution spatial distribution characteristics of elements in the samples are of practical and important research significance. In biological samples, the in situ spatial distribution characteristics of elements can be used as indicators of physiological processes, reveal metabolic pathways, and reflect the ways in which environmental characteristics affect organisms. In geological samples, the in situ spatial distribution characteristics of elements can be used as a basis for mineral evaluation and an important indicator for studying the process of environmental geochemical changes. At present, several commonly used techniques for measuring the in situ distribution characteristics of elements in micro-areas include: micro X-ray fluorescence spectrometry (μXRF), synchrotron radiation technology (SR), electron microscopy-energy dispersive spectrometry (EM-EDS), electron probe technology (EP), laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS), laser induced breakdown plasma emission spectroscopy (LIBS), etc. Based on the principle of testing samples, these technologies differ in many aspects such as non-destructive testing, quantitative testing, suitable sample type and size, complexity of pre-treatment methods, detection limits and resolution, and so on. The current mainstream of the micro-area in situ element distribution detection techniques were introduced and summarized, the advantages and disadvantages of various techniques and their applicable sample types and application ranges were analyzed and compared. The selection of standard samples, data calibration and processing and visualization into maps were discussed for the first time, which provides a technical reference for related scientific research and analysis work.
2023, 29(3): 261-271.
doi: 10.16495/j.1006-3757.2023.03.003
Abstract:
The conventional laboratory detection methods have become increasingly mature in the field of drug detection. The existing laboratory analysis methods can no longer meet the needs of on-site rapid drug detection, and it is urgent to develop portable drug detection technology and equipment. In some rapid detection methods, the application of portable devices has become widespread and is being continuously studied in depth. As a device with rapid identification for target substances, sensors can quickly identify suspicious items in drug detection. With the changes in the types of drugs and the continuous updating and iteration of drug types, the detection requirements for sensors have increased, so that different types and functions of sensors have emerged. In view of the sensor with easy operation, low cost and rapid analysis, the application of portable drug sensors are bound to become an important part of field detection, especially in the field of on-site detection. In recent years, with the demand-oriented research and the deepening of research content, some new drug detection technologies, materials and equipment have been successfully developed. With the feedback of measured information and the continuous optimization of equipment, the portable detection equipment for drugs will become a powerful means to fight against drug crimes.
The conventional laboratory detection methods have become increasingly mature in the field of drug detection. The existing laboratory analysis methods can no longer meet the needs of on-site rapid drug detection, and it is urgent to develop portable drug detection technology and equipment. In some rapid detection methods, the application of portable devices has become widespread and is being continuously studied in depth. As a device with rapid identification for target substances, sensors can quickly identify suspicious items in drug detection. With the changes in the types of drugs and the continuous updating and iteration of drug types, the detection requirements for sensors have increased, so that different types and functions of sensors have emerged. In view of the sensor with easy operation, low cost and rapid analysis, the application of portable drug sensors are bound to become an important part of field detection, especially in the field of on-site detection. In recent years, with the demand-oriented research and the deepening of research content, some new drug detection technologies, materials and equipment have been successfully developed. With the feedback of measured information and the continuous optimization of equipment, the portable detection equipment for drugs will become a powerful means to fight against drug crimes.
2023, 29(3): 272-279.
doi: 10.16495/j.1006-3757.2023.03.004
Abstract:
Ultraviolet photochemical vapor generation (UV-PVG) is a newly green sample introduction technology. It has been successfully used as an interface to combine spectroscopy and mass spectrometry to detect target elements. The method is simple and efficient, with low reagent usage, and can be used for on-site detection. And the UV-PVG also broadens the range of elements of chemical vapor generation, which can be applied not only to hydride generating elements such as As、Hg、Sb、Pb, etc., but also to transition metal elements including Cd, Fe, Co, Ni, Os, and non-metallic elements such as I, Br. The mechanism application scope, advantages and disadvantages, and development trend of UV-PVG were discussed.
Ultraviolet photochemical vapor generation (UV-PVG) is a newly green sample introduction technology. It has been successfully used as an interface to combine spectroscopy and mass spectrometry to detect target elements. The method is simple and efficient, with low reagent usage, and can be used for on-site detection. And the UV-PVG also broadens the range of elements of chemical vapor generation, which can be applied not only to hydride generating elements such as As、Hg、Sb、Pb, etc., but also to transition metal elements including Cd, Fe, Co, Ni, Os, and non-metallic elements such as I, Br. The mechanism application scope, advantages and disadvantages, and development trend of UV-PVG were discussed.
2023, 29(3): 280-285.
doi: 10.16495/j.1006-3757.2023.03.005
Abstract:
The chiral membrane of amylose-tris-(3, 5-dimethylphenylcarbamate)-polyethersulfone was prepared by phase conversion method using the amylose-tris-(3, 5-dimethylphenylcarbamate) as the material. The chiral membrane chromatographic separation of propranolol hydrochloride and metoprolol were studied by using the self-made chiral membrane chromatographic device combined with a high performance liquid chromatograph. The effects of injection volume, flow rate and membrane size on the separation of membrane were studied. Under the optimal conditions, the separation factors (α) and resolution (Rs) with water as mobile phase were 3.00 and 0.95 for propranolol hydrochloride, 1.65 and 0.46 for metoprolol, respectively. The study opens up a new way for the isolation and analysis of chiral compounds.
The chiral membrane of amylose-tris-(3, 5-dimethylphenylcarbamate)-polyethersulfone was prepared by phase conversion method using the amylose-tris-(3, 5-dimethylphenylcarbamate) as the material. The chiral membrane chromatographic separation of propranolol hydrochloride and metoprolol were studied by using the self-made chiral membrane chromatographic device combined with a high performance liquid chromatograph. The effects of injection volume, flow rate and membrane size on the separation of membrane were studied. Under the optimal conditions, the separation factors (α) and resolution (Rs) with water as mobile phase were 3.00 and 0.95 for propranolol hydrochloride, 1.65 and 0.46 for metoprolol, respectively. The study opens up a new way for the isolation and analysis of chiral compounds.
2023, 29(3): 286-291.
doi: 10.16495/j.1006-3757.2023.03.006
Abstract:
The method for the determination of dissociative mercury contents in the characteristic Mongolian medicine Shibawei Ouqu pills was established, and the technical support for the limited detection of dissociative mercury in the quality standard of Shibawei Ouqu pills was provided. The dissociative mercury is easily soluble in nitric acid, while processed products are insoluble in nitric acid. Then, the content of dissociative mercury in Shibawei Ouqu pills was determined by atomic fluorescence spectrometry using nitric acid as the solvent. The dissociative mercury showed a good linear relationship in the range of 0.1~2.0 μg/L. The regression equation was Y=1 467.197 6X+3.391 5, and the correlation coefficient R2 was 0.999 59, the average recovery was 95.0%, and relative standard deviation (RSD) was 4.436% (n=6). The average content of dissociative mercury in Shibawei Ouqu pills was 0.671 mg/g. The method is simple, accurate and reliable, and can be used for the limited determination of dissociative mercury in the study of quality standard improvement of Shibawei Ouqu pills.
The method for the determination of dissociative mercury contents in the characteristic Mongolian medicine Shibawei Ouqu pills was established, and the technical support for the limited detection of dissociative mercury in the quality standard of Shibawei Ouqu pills was provided. The dissociative mercury is easily soluble in nitric acid, while processed products are insoluble in nitric acid. Then, the content of dissociative mercury in Shibawei Ouqu pills was determined by atomic fluorescence spectrometry using nitric acid as the solvent. The dissociative mercury showed a good linear relationship in the range of 0.1~2.0 μg/L. The regression equation was Y=1 467.197 6X+3.391 5, and the correlation coefficient R2 was 0.999 59, the average recovery was 95.0%, and relative standard deviation (RSD) was 4.436% (n=6). The average content of dissociative mercury in Shibawei Ouqu pills was 0.671 mg/g. The method is simple, accurate and reliable, and can be used for the limited determination of dissociative mercury in the study of quality standard improvement of Shibawei Ouqu pills.
2023, 29(3): 292-298.
doi: 10.16495/j.1006-3757.2023.03.007
Abstract:
A three-dimensional porous nickel molybdenum sulfide nanoflowers supported on carbon nanotubes (CNT) composite materials (NiMoS@CNT) was prepared. The morphology and structure of the synthesized materials were characterized by scanning electron microscopy and X-ray diffraction. The cyclic voltammetry and chronoamperometry were used to study the electrochemical catalytic performance of the prepared materials. Based on the excellent electrocatalytic performance of NiMoS@CNT for hydrogen peroxide, a sandwich electrochemical sensor for detecting brain natriuretic peptide (BNP) was constructed. Under the optimal conditions, the current response intensity and the logarithm of mass concentration of brain natriuretic peptide was linear in the range of 0.20~20 ng/mL. The immunosensor has a high sensitivity, selectivity and stability, and can be used for the detection of BNP in actual samples.
A three-dimensional porous nickel molybdenum sulfide nanoflowers supported on carbon nanotubes (CNT) composite materials (NiMoS@CNT) was prepared. The morphology and structure of the synthesized materials were characterized by scanning electron microscopy and X-ray diffraction. The cyclic voltammetry and chronoamperometry were used to study the electrochemical catalytic performance of the prepared materials. Based on the excellent electrocatalytic performance of NiMoS@CNT for hydrogen peroxide, a sandwich electrochemical sensor for detecting brain natriuretic peptide (BNP) was constructed. Under the optimal conditions, the current response intensity and the logarithm of mass concentration of brain natriuretic peptide was linear in the range of 0.20~20 ng/mL. The immunosensor has a high sensitivity, selectivity and stability, and can be used for the detection of BNP in actual samples.
2023, 29(3): 299-303.
doi: 10.16495/j.1006-3757.2023.03.008
Abstract:
A method was developed to determine the residues of 2-chloroethanol in gelatin hollow capsules using headspace gas chromatography-electron capture detector method. The physical properties of gelatin disappeared when the gelatin hollow capsule solution was salting out with NaCl solution. The content of 2-chloroethanol in gelatin hollow capsule solution was analyzed by headspace gas chromatography-electron capture detector method. The results showed that 2-chloroethanol had a good linear relationship in the range of 10~35 μg/g, with an r value of 0.999 4. The limits of quantitation and limits of detection were 10 and 5 μg/g, respectively. The recoveries ranged from 92.1%~102.2%, the relative standard deviation (RSD) were all less than 10%. The samples were tested by the method. The method is simple, accurate and sensitive and effective in solving the matrix effect of gelatin hollow capsules, and can be used for the quantitative analysis of 2-chloroethanol in commercially available gelatin hollow capsules.
A method was developed to determine the residues of 2-chloroethanol in gelatin hollow capsules using headspace gas chromatography-electron capture detector method. The physical properties of gelatin disappeared when the gelatin hollow capsule solution was salting out with NaCl solution. The content of 2-chloroethanol in gelatin hollow capsule solution was analyzed by headspace gas chromatography-electron capture detector method. The results showed that 2-chloroethanol had a good linear relationship in the range of 10~35 μg/g, with an r value of 0.999 4. The limits of quantitation and limits of detection were 10 and 5 μg/g, respectively. The recoveries ranged from 92.1%~102.2%, the relative standard deviation (RSD) were all less than 10%. The samples were tested by the method. The method is simple, accurate and sensitive and effective in solving the matrix effect of gelatin hollow capsules, and can be used for the quantitative analysis of 2-chloroethanol in commercially available gelatin hollow capsules.
2023, 29(3): 304-308.
doi: 10.16495/j.1006-3757.2023.03.009
Abstract:
The Fourier transform infrared spectrometer (FTIR) is difficult to achieve good results in industrial field applications due to the limitations of its own volume, weight, and shock resistance. On the basis of fully utilizing the respective optical characteristics of the cube-corner mirror and the planar mirror, a self-compensating double-pendulum interferometer was designed to solve the problem of the stability of the interferometer. Through the electrical analysis and modeling of the scanning mechanism, the relationship between the controller and the scanning speed was established, and the corresponding control algorithm was realized by using high-speed digital signal processing (DSP) technology, which can control the speed error in the range of ±0.2%. The test of the instrument performance and the test of the standard sample showed that the instrument has a high signal-to-noise ratio and stability, which can meet the needs of industrial applications.
The Fourier transform infrared spectrometer (FTIR) is difficult to achieve good results in industrial field applications due to the limitations of its own volume, weight, and shock resistance. On the basis of fully utilizing the respective optical characteristics of the cube-corner mirror and the planar mirror, a self-compensating double-pendulum interferometer was designed to solve the problem of the stability of the interferometer. Through the electrical analysis and modeling of the scanning mechanism, the relationship between the controller and the scanning speed was established, and the corresponding control algorithm was realized by using high-speed digital signal processing (DSP) technology, which can control the speed error in the range of ±0.2%. The test of the instrument performance and the test of the standard sample showed that the instrument has a high signal-to-noise ratio and stability, which can meet the needs of industrial applications.
2023, 29(3): 309-312.
doi: 10.16495/j.1006-3757.2023.03.010
Abstract:
The lignocellulosic materials exist in large quantities on the earth and come from a wide range of sources. The treatment of lignocellulosic waste allows for the recycling of waste, and avoids environmental problems. Due to the thick cell walls of lignocellulosic materials and the cell walls contains crystalline structures, pretreatment is required before transmission electron microscopic observation. The sample pretreatment methods of lignocellulosic materials were described in detail, including sampling, fixation, washing, dehydration, resin embedding and penetration, slicing and dyeing, so as to provide a reference for the preparation of the kind of materials.
The lignocellulosic materials exist in large quantities on the earth and come from a wide range of sources. The treatment of lignocellulosic waste allows for the recycling of waste, and avoids environmental problems. Due to the thick cell walls of lignocellulosic materials and the cell walls contains crystalline structures, pretreatment is required before transmission electron microscopic observation. The sample pretreatment methods of lignocellulosic materials were described in detail, including sampling, fixation, washing, dehydration, resin embedding and penetration, slicing and dyeing, so as to provide a reference for the preparation of the kind of materials.
2023, 29(3): 313-320.
doi: 10.16495/j.1006-3757.2023.03.011
Abstract:
When the fluorescent samples were analyzed using a windowed X-ray energy dispersive spectrometer (EDS) equipped with a scanning electron microscope, due to the excitation of the electron beam, the stimulated fluorescence by sample stimulation will seriously interfere with the analysis of the characteristic X-rays by the EDS energy spectroscopy probe, which leads to qualitative and quantitative difficulties. The new windowless EDS combined with the method of single particle small region acquisition can successfully achieve normal EDS spectral analysis of fluorescent samples because of its excellent low-energy-end signal acquisition and analysis capability. Without the adsorption of the traditional ultra-thin window, the windowless EDS can analyze lithium metal. By optimizing the accelerating voltage and the protective effect of the passivation film on the sample surface, the interference of background noise and sample contamination were overcome, and the detection of elemental lithium was successfully realized.
When the fluorescent samples were analyzed using a windowed X-ray energy dispersive spectrometer (EDS) equipped with a scanning electron microscope, due to the excitation of the electron beam, the stimulated fluorescence by sample stimulation will seriously interfere with the analysis of the characteristic X-rays by the EDS energy spectroscopy probe, which leads to qualitative and quantitative difficulties. The new windowless EDS combined with the method of single particle small region acquisition can successfully achieve normal EDS spectral analysis of fluorescent samples because of its excellent low-energy-end signal acquisition and analysis capability. Without the adsorption of the traditional ultra-thin window, the windowless EDS can analyze lithium metal. By optimizing the accelerating voltage and the protective effect of the passivation film on the sample surface, the interference of background noise and sample contamination were overcome, and the detection of elemental lithium was successfully realized.
2023, 29(3): 321-327.
doi: 10.16495/j.1006-3757.2023.03.012
Abstract:
In order to improve the reliability of detection data of cadmium and lead elements in rice, the content of cadmium and lead in rice were detected according to GB 5009.12—2017 "Determination of Lead in Food" and GB 5009.15—2014 "Determination of Cadmium in Food", and the various error analysis were carried out for the measuring system analysis (MSA) with the atomic absorption spectrophotometer as measuring equipment. The results showed that the Xbar control charts in the stability analysis of two elements have points beyond the upper and lower control limits, and the stability did not meet the requirements. The bias and linear P values were greater than 0.05, which meant that there were no significant bias and linear error. The results of Reproducibility & Repeatability (R&R) were 54.03% and 36.38%, respectively, both greater than 30%, and the measurement errors were beyond the acceptable range. The stability reached the statistical controlled state after the fault investigation of human, machine, material, method, environment, measurement and other aspects, and the R&R were reduced to 9.66% and 8.95%, respectively, both less than 10%, the measurement system was acceptable. The use of MSA method to reduce various types of measurement errors from many aspects, can effectively guarantee the reliability of the detection data of cadmium and lead contents in rice.
In order to improve the reliability of detection data of cadmium and lead elements in rice, the content of cadmium and lead in rice were detected according to GB 5009.12—2017 "Determination of Lead in Food" and GB 5009.15—2014 "Determination of Cadmium in Food", and the various error analysis were carried out for the measuring system analysis (MSA) with the atomic absorption spectrophotometer as measuring equipment. The results showed that the Xbar control charts in the stability analysis of two elements have points beyond the upper and lower control limits, and the stability did not meet the requirements. The bias and linear P values were greater than 0.05, which meant that there were no significant bias and linear error. The results of Reproducibility & Repeatability (R&R) were 54.03% and 36.38%, respectively, both greater than 30%, and the measurement errors were beyond the acceptable range. The stability reached the statistical controlled state after the fault investigation of human, machine, material, method, environment, measurement and other aspects, and the R&R were reduced to 9.66% and 8.95%, respectively, both less than 10%, the measurement system was acceptable. The use of MSA method to reduce various types of measurement errors from many aspects, can effectively guarantee the reliability of the detection data of cadmium and lead contents in rice.
2023, 29(3): 328-333.
doi: 10.16495/j.1006-3757.2023.03.013
Abstract:
A complete set of inductively coupled plasma mass spectrometry (ICP-MS) was established to determined 15 trace elements including copper, cobalt, silver, lead, antimony, beryllium, chromium, indium, yttrium, cadmium, manganese, titanium, tantalum, lanthanum and cerium in magnesium alloys by simple matrix matching method and internal standard method. The test results showed that the detection limits of each element were in the range of 0.003 9~1.6 μg/L. The recoveries were 95.1%~109.2%. The precision was 0.2%~2.3%. The method is simple, fast and efficient, and can meet the market demand for the detection of trace elements in magnesium alloys.
A complete set of inductively coupled plasma mass spectrometry (ICP-MS) was established to determined 15 trace elements including copper, cobalt, silver, lead, antimony, beryllium, chromium, indium, yttrium, cadmium, manganese, titanium, tantalum, lanthanum and cerium in magnesium alloys by simple matrix matching method and internal standard method. The test results showed that the detection limits of each element were in the range of 0.003 9~1.6 μg/L. The recoveries were 95.1%~109.2%. The precision was 0.2%~2.3%. The method is simple, fast and efficient, and can meet the market demand for the detection of trace elements in magnesium alloys.
2023, 29(3): 334-338.
doi: 10.16495/j.1006-3757.2023.03.014
Abstract:
Private third-party testing service is rapidly developing and has become an important part of scientific research and quality control in China. Combined with customer visits, the development background of private testing service was expounded, as well as the current situation and problems of customer service was described, and the future customer service was envisioned, with a view to providing a reference for the quality customer service of private third-party testing institutions.
Private third-party testing service is rapidly developing and has become an important part of scientific research and quality control in China. Combined with customer visits, the development background of private testing service was expounded, as well as the current situation and problems of customer service was described, and the future customer service was envisioned, with a view to providing a reference for the quality customer service of private third-party testing institutions.
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Supervisor: Chinese Academy of Sciences
Sponsor: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences
Honorary Editor-in-Chief: Yu WeiLe
Editor-in-Chief: SHI Yanping
Publisher: “Analysis and Testing Technology and Instruments” Editorial Department
Address: 18 Tianshui Zhong Rd., Lanzhou 730000, China.
Postcode: 730000
Tel: 86-0931-4968280
FAX: 0931-8277088
Email: fxcs@licp.cas.cn
CN 62-1123/O6
ISSN 1006-3757
Postal Code: 54-90
Price: RMB 15/issue,RMB 60/year
