CN111398400A - Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry - Google Patents

Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry Download PDF

Info

Publication number
CN111398400A
CN111398400A CN202010244580.4A CN202010244580A CN111398400A CN 111398400 A CN111398400 A CN 111398400A CN 202010244580 A CN202010244580 A CN 202010244580A CN 111398400 A CN111398400 A CN 111398400A
Authority
CN
China
Prior art keywords
inductively coupled
coupled plasma
selenium
plasma mass
tellurium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010244580.4A
Other languages
Chinese (zh)
Other versions
CN111398400B (en
Inventor
阳国运
何雨珊
潘倩妮
覃盛
张文捷
刘梓楠
黄献珠
齐永辉
黄庆柒
唐裴颖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangxi Geology & Mineral Test Research Center
Original Assignee
Guangxi Geology & Mineral Test Research Center
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangxi Geology & Mineral Test Research Center filed Critical Guangxi Geology & Mineral Test Research Center
Priority to CN202010244580.4A priority Critical patent/CN111398400B/en
Publication of CN111398400A publication Critical patent/CN111398400A/en
Application granted granted Critical
Publication of CN111398400B publication Critical patent/CN111398400B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses a method for determining Se and Te by an alkali fusion inductively coupled plasma mass spectrometry, which comprises the steps of weighing a soil sample to be determined, melting and decomposing the soil sample by sodium peroxide, adding tartaric acid into the solution to form complex anions of tungsten, molybdenum, tin and the like, adding 732 type cation exchange resin, and adsorbing most of sodium, iron, aluminum, zinc and the like in the solution onto the resin to obtain a solution to be determined; measuring the mass spectrum counting of selenium and tellurium on an inductively coupled plasma mass spectrometer in a KED mode, simultaneously measuring a working curve, substituting the obtained emission intensity meter value into the working curve, and calculating the content of selenium and tellurium in the liquid to be measured. According to the method, the hydrogen is used as the reaction gas of the collision pool, the interference of polyatomic ions such as double argon, argon and chlorine is eliminated, the signal-to-back ratio is improved by 5-10 times, the selenium detection limit is 0.005 microgram/g, the tellurium detection limit is 0.002 microgram/g, and the problems that the current polyatomic ions such as double argon or chlorine argon and zinc oxide have the interference on selenium and tellurium, the signal-to-back ratio is low, and the detection limit cannot meet the detection requirement are solved.

Description

Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry
Technical Field
The invention relates to the technical field of soil trace element determination, in particular to a method for determining Se and Te by an alkali fusion inductively coupled plasma mass spectrometry.
Background
Soil is the most fundamental and important natural resource for human survival development, and surface soil has been commonly contaminated to varying degrees as human production activities have gone through considerable periods of time, especially with the rapid development of modern industries. Therefore, the method is an important basic work for measuring the contents of the constant and secondary elements and the trace elements in the soil, and has important significance for monitoring the ecological environment, researching regional resources, regulating and controlling agricultural economy and planning sustainable development of national economy.
At present, selenium and tellurium in soil and water system sediments are generally detected by dissolving ores with (acid, hydrofluoric acid and perchloric acid) or (nitric acid and perchloric acid), heating until concentrated perchloric acid is emitted, taking off the ores, cooling, reducing hexavalent selenium and tellurium by using 1+1 hydrochloric acid, adding ferric salt, and then respectively detecting selenium and tellurium by using an atomic fluorescence method. Because the inductively coupled plasma mass spectrometry has the characteristics of simultaneous determination of single elements, high sensitivity and high detection speed, in recent years, workers try to determine tellurium in soil and water system sediments by using the inductively coupled plasma mass spectrometry, but excessive treatment is not carried out on the interference of tellurium, and the accuracy of results is difficult to ensure by complex samples. For selenium, the detection limit is difficult to meet the detection requirement due to the interference of polyatomic ions such as double argon, chlorine argon, zinc oxide and the like.
For example, the Chinese patent discloses a method for simultaneously measuring iodine, boron, tin and germanium elements in soil, which comprises the steps of raw material pretreatment, determination liquid preparation, working curve drawing and determination of the content of each element in the soil. The raw material pretreatment is to use sodium peroxide for pretreatment, a citric acid solution and cationic resin are added into a pretreated sample to prepare a determination solution, and the obtained determination solution is determined by adopting an inductively coupled plasma mass spectrometry. The method can simultaneously measure a plurality of elements of iodine, boron, tin and germanium in the soil, has high working efficiency and simple operation, utilizes the inductively coupled plasma mass spectrometry to measure, and has the advantages of higher sensitivity, lower detection limit, stronger anti-interference capability, higher accuracy and the like compared with the atomic fluorescence spectrometry. The detection limits of the elements are respectively 0.005 mu g/g of selenium and 0.002 mu g/g of tellurium after determination, which is superior to the detection limit of the atomic fluorescence spectrometry. Zhangjie et al disclose the resin exchange separation-inductively coupled plasma mass spectrometry for determining W, Mo, Sn, Ge, Se and Te in Pb-Zn ore, wherein the detection limits of Se and Te are 0.05 μ g/g and 0.03 μ g/g, respectively. Because the content of selenium and tellurium in soil is low, the interference of polyatomic ions such as double argon or chlorine argon and zinc oxide on selenium and tellurium cannot be eliminated by the conventional method, the detection limit is high, and a small amount of selenium and tellurium elements in soil cannot be accurately determined.
Disclosure of Invention
The method can completely dissolve selenium and tellurium by adopting alkali fusion, not only remove a large amount of salt through resin adsorption, but also eliminate the interference of zinc, and then eliminate the interference of double-argon polyatomic ions through a KED mode (taking hydrogen as reaction gas and having the flow rate of 6.2m L/min), so that the method ensures that the selenium and the tellurium can be completely dissolved by adopting the alkali fusion, and the interference of double-argon polyatomic ions is eliminated, thereby ensuring that the selenium and the tellurium can be completely dissolved by adopting the KED mode78The signal-to-back ratio of Se is improved by 5 to 10 times, and most metal ions are removed by resin adsorption,126the interference on Te is obviously reduced, the actual detection limit is obviously reduced, and therefore, the selenium in soil and water system sediments can be simultaneously measuredTellurium, the result is accurate and efficient.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry comprises the following steps:
(1) weighing 0.4000g of soil sample to be detected in a corundum crucible, and adding 2.0g of Na2O2After uniformly stirring, placing the corundum crucible on a fire-resistant plate heated to 450-;
(2) stirring and taking 4m L samples to be tested into a polytetrafluoroethylene crucible, adding 2.5m L tartaric acid solution, shaking up, adding 2-3g cationic resin, shaking up, placing on an oscillator to vibrate for 15-20min, adding 8m L water, shaking up, and then placing on the oscillator to vibrate for 15-20min to obtain a determination solution;
(3) setting working parameters on an inductively coupled plasma mass spectrometer, pumping a measured liquid into an atomizer, introducing ammonia water and an ethanol solution into a tee joint by taking argon as a carrier gas, introducing an atomizing gas into plasma flame to excite ionization, introducing hydrogen into the plasma flame in a KED mode, wherein the KED mode is used for introducing hydrogen as a reaction gas, the flow rate is 6.2m L/min, measuring the mass spectrum counting of selenium and tellurium, simultaneously measuring a working curve, substituting the obtained emission intensity meter value into the working curve, and calculating the content of selenium and tellurium in the liquid to be measured.
Further, the operating parameters of the inductively coupled plasma mass spectrometer are that the power is 1500W, the plasma gas flow is 14L/min, the auxiliary gas flow is 0.8L/min, the atomizer flow rate is 1.1L/min, the sample injection flushing time is 16s, the scanning mode is peak jump, the residence time is 0.15s, the single element integration time is 6s, the sampling rate is higher than the sampling rate, and the sampling rate is higher than the sampling rate,
Figure BDA0002433653140000031
A sampling cone with the diameter of 1.1mm,
Figure BDA0002433653140000032
0.7mm of cut, and the detected isotope is78Se、126Te、185Re。
Further, the collision cell reaction gas is hydrogen, and the flow rate is 6.2m L/min.
Further, the concentration of the tartaric acid solution was 0.8%.
Further, the concentration of the ammonia water is 0.8%, the concentration of the ethanol is 5%, and the ammonia water is pumped in by a peristaltic pump in a three-way mode.
Further, the internal standard solution is Re internal standard solution with the concentration of 0.5 mu g/m L.
Further, the drawing method of the working curve comprises the following steps: 2.0g Na was added to a series of Teflon beakers2O2Adding water of about 50m L, adding an internal standard solution of 5.00m L, adding a series of selenium and tellurium standard solutions, adding water to about 90m L, stirring uniformly to obtain a sample to be detected, pretreating the sample according to the step (2), measuring the mass spectrum counting of selenium and tellurium on an inductively coupled plasma mass spectrometer according to the step (3), and drawing a working curve according to the mass spectrum counting.
Further, the cation exchange resin is 732 type cation exchange resin.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the method can completely dissolve selenium and tellurium by adopting alkali fusion, not only removes a large amount of salt through resin adsorption, but also eliminates the interference of zinc, and then eliminates the interference of double-argon polyatomic ions through a KED mode (taking hydrogen as reaction gas and having the flow rate of 6.2m L/min), thereby further leading the double-argon polyatomic ions to be in a state of being dissolved in water78The signal-to-back ratio of Se is improved by 5 to 10 times, and most metal ions are removed by resin adsorption,126the interference on Te is obviously reduced, wherein the detection limit of selenium is 0.005 mu g/g, the detection limit of tellurium is 0.002 mu g/g, and the detection limit is obviously reduced, so that the selenium and tellurium in soil and water system sediments can be simultaneously measured, and the result is accurate and the efficiency is high. Solves the problem that the prior polyatomic ions such as double argon or chlorine argon and zinc oxide and the like interfere selenium and telluriumThe signal-to-back ratio is low, and the detection limit cannot meet the detection requirement.
2. The method adds ammonia water and ethanol in the determination process, has sensitization effect, can double the sensitivity, and meets the determination requirement of low-content selenium and tellurium in the current soil.
3. The method has the advantages of higher sensitivity, lower detection limit, stronger anti-interference capability, higher accuracy and the like, and can simultaneously determine the low-content selenium and tellurium in the soil.
Drawings
FIG. 1 is a standard working curve diagram of elemental selenium;
FIG. 2 is a standard operating curve of tellurium.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
The experimental methods used are conventional methods unless otherwise specified, and the materials, reagents and the like used in the following examples are commercially available, and only reagents and ultrapure water which are confirmed to be superior pure are used in the analysis.
Example 1
A method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry comprises the following steps:
(1) weighing 0.4000g of soil sample to be detected in a corundum crucible, and adding 2.0g of Na2O2After uniformly stirring, placing the corundum crucible on a fire-resistant plate heated to 500 ℃, baking for about 5 minutes until sodium peroxide is in a scorched state, transferring the corundum crucible into a muffle furnace heated to 500 ℃, heating to 750 ℃, preserving heat and melting for 8min, taking out the crucible, cooling, placing the crucible into a beaker, adding 80m L hot water, adding 0.5 mu g/m L of 5.00m L Re internal standard solution, stirring uniformly by using a plastic rod, and taking out the crucible to obtain a sample to be detected;
(2) stirring and taking 4m L samples to be tested into a 30ml polytetrafluoroethylene crucible, adding 2.5m L tartaric acid solution (the concentration is 0.8%), shaking uniformly, adding 3g 732 type cation exchange resin, shaking uniformly, placing on an oscillator to oscillate for 20min, adding 8m L water, shaking uniformly, and then placing on the oscillator to oscillate for 15min to obtain a test solution;
(3) setting working parameters on an inductively coupled plasma mass spectrometer that the power is 1500W, the plasma gas flow is 14L/min, the auxiliary gas flow is 0.8L/min, the atomizer flow rate is 1.1L/min, the sample injection pump flow rate is 30rpm, the sample injection flushing time is 16s, the scanning mode is peak jump, the residence time is 0.15s, the single element integration time is 6s, the sampling time is four times,
Figure BDA0002433653140000041
A sampling cone with the diameter of 1.1mm,
Figure BDA0002433653140000042
0.7mm of cut, and the detected isotope is78Se、126Te、185Re. liquid to be measured is pumped into the atomizer, argon is used as carrier gas, 0.8% ammonia water and 5% ethanol solution are introduced through the tee, the atomized gas is introduced into plasma flame to excite ionization, mass spectrum counting of selenium and tellurium is measured in KED mode (reaction gas is hydrogen gas, flow is 6.2m L/min), simultaneously, measurement of working curve is carried out, the obtained emission intensity meter value is substituted into the working curve, and the selenium and tellurium content in the liquid to be measured is calculated.
Drawing a working curve: 2.0g Na was added to a series of Teflon beakers2O2Adding water of about 50m L, adding an internal standard solution of 5.00m L, adding a series of selenium and tellurium standard solutions, adding water to about 90m L, stirring uniformly to obtain a sample to be detected, pretreating the sample according to the step (2), measuring the mass spectrum counting of selenium and tellurium on an inductively coupled plasma mass spectrometer according to the step (3) as shown in tables 1 and 2, and drawing a working curve according to the mass spectrum counting as shown in fig. 1 and 2.
Table 1: configuration of selenium element working curve
Concentration (ug/L) Emission intensity count value
0.00 13
0.10 74
0.50 336
1.00 649
5.00 3276
10.0 6487
20.0 13092
Table 2: configuration of tellurium element working curve
Concentration (ug/L) Emission intensity count value
0.00 2
0.05 97
0.25 456
0.50 951
2.50 4525
5.00 8927
10.0 17662
In order to verify the accuracy of the method, a plurality of standard samples with known selenium and tellurium contents are taken, the determination solution is prepared by the same method as the steps (1) and (2), then inductively coupled plasma mass spectrometry is added, mass spectrometry counting of selenium and tellurium is measured in a KED mode (reaction gas is hydrogen, the flow is 6.2m L/min), the determination results are substituted into the standard curves of each element, then the contents of selenium and tellurium are respectively calculated, and the determination results are shown in the following table 3.
Table 3: standard value and measured value of selenium and tellurium national standard substance
Figure BDA0002433653140000061
Note: when the content detection limit is more than 3 times, the element accuracy meets the requirement that the absolute value of delta log C is less than or equal to 0.05.
The detection limit of each element in the blank solution was measured by a 3-fold signal-to-noise ratio method, and the results are shown in table 4.
Table 4: limit of selenium and tellurium detection
Figure BDA0002433653140000062
Figure BDA0002433653140000071
From the results, the detection limit of selenium and tellurium in the invention is 0.005 mug/g and 0.002 mug/g, and the sensitivity is obviously higher than that of the existing detection method.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.

Claims (7)

1. A method for measuring Se and Te by alkali fusion inductively coupled plasma mass spectrometry is characterized by comprising the following steps:
(1) weighing 0.4000g of soil sample to be detected in a corundum crucible, and adding 2.0g of Na2O2After uniformly stirring, placing the corundum crucible on a fire-resistant plate heated to 450-;
(2) stirring and taking 4m L samples to be tested into a polytetrafluoroethylene crucible, adding 2.5m L tartaric acid solution, shaking up, adding 2-3g of cation exchange resin, shaking up, placing on an oscillator to vibrate for 15-20min, adding 8m L water, shaking up, and then placing on the oscillator to vibrate for 15-20min to obtain a test solution;
(3) setting working parameters on an inductively coupled plasma mass spectrometer, pumping a measured liquid into an atomizer, introducing ammonia water and an ethanol solution into a tee joint by taking argon as a carrier gas, introducing an atomizing gas into plasma flame to excite ionization, measuring the mass spectrum counting of selenium and tellurium by using a KED mode, introducing hydrogen as a reaction gas in the KED mode, measuring a working curve, substituting the obtained emission intensity meter value into the working curve, and calculating the content of selenium and tellurium in the liquid to be measured.
2. The method for determining Se and Te by using the alkali fusion inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the inductively coupled plasma mass spectrometry has the operating parameters of 1500W of power, 14L/min of plasma gas flow, 0.8L/min of auxiliary gas flow, 1.1L/min of atomizer flow rate, 16s of sample introduction and flushing time, peak jump in a scanning mode, 0.15s of residence time, 6s of single element integration time, 1.1mm of ø sampling cone, 0.7mm of ø truncation, and isotope detection78Se、126Te、185Re。
3. The method for determining Se and Te by using the alkali fusion inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: the concentration of the tartaric acid solution is 0.8%.
4. The method for determining Se and Te by using the alkali fusion inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: the concentration of the ammonia water is 0.8%, the concentration of the ethanol is 5%, and the ammonia water is pumped in by a peristaltic pump in a three-way mode.
5. The method for determining Se and Te by using the alkali fusion inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the internal standard solution is Re internal standard solution with a concentration of 0.5 μ g/m L.
6. The method for determining Se and Te by using the alkali fusion inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: the drawing method of the working curve comprises the following steps: 2.0g Na was added to a series of Teflon beakers2O2Adding about 50m L of water, adding 5.00m L of internal standard solution, and adding a series of selenium and telluriumAdding water into the standard solution to about 90m L, stirring uniformly to obtain a sample to be detected, pretreating the sample according to the step (2), measuring the mass spectrum counting of selenium and tellurium according to the step (3) on an inductively coupled plasma mass spectrometer, and drawing a working curve according to the mass spectrum counting.
7. The method for determining Se and Te by using the alkali fusion inductively coupled plasma mass spectrometry as claimed in claim 1, wherein the method comprises the following steps: the cation exchange resin is 732 type cation exchange resin.
CN202010244580.4A 2020-03-31 2020-03-31 Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry Active CN111398400B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010244580.4A CN111398400B (en) 2020-03-31 2020-03-31 Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010244580.4A CN111398400B (en) 2020-03-31 2020-03-31 Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry

Publications (2)

Publication Number Publication Date
CN111398400A true CN111398400A (en) 2020-07-10
CN111398400B CN111398400B (en) 2022-11-15

Family

ID=71436815

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010244580.4A Active CN111398400B (en) 2020-03-31 2020-03-31 Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry

Country Status (1)

Country Link
CN (1) CN111398400B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113376142A (en) * 2021-06-21 2021-09-10 江西农业大学 Vegetable selenium-rich element detection method based on PRLIBS technology

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758927A (en) * 2016-02-26 2016-07-13 广西壮族自治区地质矿产测试研究中心 Method for simultaneously measuring iodine, boron, tin and germanium elements in soil
CN108828052A (en) * 2018-08-02 2018-11-16 青海省核工业地质局核地质研究所((青海省核工业地质局检测试验中心)) The method of tin amount in alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758927A (en) * 2016-02-26 2016-07-13 广西壮族自治区地质矿产测试研究中心 Method for simultaneously measuring iodine, boron, tin and germanium elements in soil
CN108828052A (en) * 2018-08-02 2018-11-16 青海省核工业地质局核地质研究所((青海省核工业地质局检测试验中心)) The method of tin amount in alkali fusion-inductively coupled plasma mass spectrometry measurement tin ore

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
廖文榕: "电感耦合等离子体质谱(ICP-MS)法测定化妆品中的总硒量", 《海峡药学》 *
李冰等: "电感耦合等离子体质谱法同时测定地质样品中痕量碘溴硒砷的研究 Ⅱ.土壤及沉积物标准物质分析", 《岩矿测试》 *
韩丽荣等: "乙醇增强-电感耦合等离子体质谱法直接测定地质样品中碲", 《岩矿测试》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113376142A (en) * 2021-06-21 2021-09-10 江西农业大学 Vegetable selenium-rich element detection method based on PRLIBS technology
CN113376142B (en) * 2021-06-21 2023-12-22 江西农业大学 Vegetable selenium-rich element detection method based on PRLIBS technology

Also Published As

Publication number Publication date
CN111398400B (en) 2022-11-15

Similar Documents

Publication Publication Date Title
CN102998303B (en) Applied microwave clears up the detection method that-ICP-AES measures Niobium in Steel, tantalum content
CN103196880B (en) Method for determining content of arsenic in iron ore by using hydride generation-atomic fluorescence spectroscopy
Liu et al. Dielectric barrier discharge-plasma induced vaporization and its application to the determination of mercury by atomic fluorescence spectrometry
Li et al. Determination of mercury by intermittent flow electrochemical cold vapor generation coupled to atomic fluorescence spectrometry
Li et al. Significant signal enhancement of dielectric barrier discharge plasma induced vapor generation by using non-ionic surfactants for determination of mercury and cadmium by atomic fluorescence spectrometry
CN105319202A (en) Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method
Yang et al. Efficient generation of volatile species for cadmium analysis in seafood and rice samples by a modified chemical vapor generation system coupled with atomic fluorescence spectrometry
CN110672707A (en) Method for measuring boron, arsenic, bromine and tungsten in geochemical sample by ICP-MS
CN102269733A (en) Detection method for content of trace selenium in low alloy steel
CN102928364A (en) Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid
Wen et al. Chemical vapor generation from an ionic liquid using a solid reductant: determination of Hg, As and Sb by atomic fluorescence spectrometry
CN111398400B (en) Method for determining Se and Te by alkali fusion inductively coupled plasma mass spectrometry
Lin et al. Review of high-precision Sr isotope analyses of low-Sr geological samples
CN103076384A (en) Method for testing Boron element in tobacco
CN105784828B (en) The measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of buccal cigarette
Dongxing et al. On-line electrolytic dissolution of solid metal samples and determination of copper in aluminium alloys by flame atomic absorption spectrometry
CN105606436A (en) Method for quickly measuring content of five rare earth elements in edible packing material
CN105758929B (en) The measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of matrix cigarette
CN103760218B (en) A kind of method of trace B impurity in Quick Measurement polysilicon
Zhang et al. Determination of Pb in geological materials by heat extraction slurry sampling ET-AAS
Hu et al. Voltammetric determination of cadmium (II) using a chemically modified electrode
Sun et al. Simultaneous determination of trace cadmium and mercury in Chinese herbal medicine by non-dispersive atomic fluorescence spectrometry using intermittent flow vapor generator
CN111398399A (en) Method for determining silver by inductively coupled plasma mass spectrometry
CN113777095A (en) Method for detecting content of potassium and sodium in molybdenum trioxide for high-solubility catalyst
CN103575799A (en) Method for measuring impurity elements in electrolytic manganese dioxide for battery

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant