CN112229941A - Halogen detection method in geological sample - Google Patents
Halogen detection method in geological sample Download PDFInfo
- Publication number
- CN112229941A CN112229941A CN202011056766.3A CN202011056766A CN112229941A CN 112229941 A CN112229941 A CN 112229941A CN 202011056766 A CN202011056766 A CN 202011056766A CN 112229941 A CN112229941 A CN 112229941A
- Authority
- CN
- China
- Prior art keywords
- solution
- fluorine
- chlorine
- detected
- detection method
- 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.)
- Withdrawn
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for detecting halogen in a geological sample, which comprises the steps of firstly treating a sample to be detected by an alkali fusion method to transfer fluorine and chlorine to be detected into a solution, and then detecting by an ion chromatograph. The invention combines the alkali fusion with the ion chromatograph, realizes the simultaneous digestion of a plurality of samples, saves the pretreatment time, realizes the simultaneous determination of F and Cl elements by the high-precision ion chromatography, and has the popularization universality.
Description
Technical Field
The invention relates to the field of geological detection, in particular to a halogen detection method in a geological sample.
Background
Fluorine and chlorine are halogen elements, and are active in chemical property and easy to volatilize. Fluorine and chlorine are used as mineralizers and play an important role in the mineralization process, and Cu, Pb, Zn and Au are easy to react with Cl-The fluorine-rich fluid contributes to the transport and migration of the mineral elements such as W, Sn, Mo, Nb, Ta, etc. as the fluid transports the complex. In recent years, the role of fluorine and chlorine in the mineralization of these elements has attracted attention of a wide range of geologists, but the lack of fluorine is widespreadChlorine analysis techniques, make the geochemical study of F and Cl of these mineralisation systems lacking, the role of F and Cl in the mineralization process is not clear.
The existing halogen element analysis methods are mostly used for analyzing geological samples of plants, foods, crude oil, cement, coal, soil and oceans, and few methods are specially used for analyzing geological samples of rocks. The main analysis methods include direct analysis and indirect analysis, wherein the direct analysis adopts direct sample injection of samples without pretreatment, and the indirect analysis needs pretreatment of the samples and solution sample injection.
The direct analysis mainly includes neutron activation method in early years, X-ray fluorescence spectroscopy (XRF), Atomic Absorption Spectroscopy (AAS), molecular absorption spectroscopy (HR-CS-MAS) developed in the last 10 years, Laser Induced Breakdown Spectroscopy (LIBS), and electron probe (EMP). Neutron activation, XRF, AAS and HR-CS-MAS do not enable simultaneous fluorine and chlorine determination, while LA-ICP-MS can only be used for Cl and Br determination in fluid inclusions, and EMP is only used for fluorine and chlorine analysis of single minerals.
Indirect analyses include colorimetry, Ion Selective Electrode (ISE), inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma emission spectroscopy (ICP-OES), Ion Chromatography (IC). However, these analytical techniques all require pre-treatment to obtain a solution for analysis, such as water immersion, acid digestion, microwave induced combustion, pyrohydrolysis, and the like. When the solution is obtained, the halogen element in the complete geological sample cannot be released, or the problems of too long time consumption and too high cost often occur. Meanwhile, many existing methods can only measure Cl and Br with relatively high atomic mass, and cannot realize quantitative analysis of halogen element F with smaller atomic mass.
Disclosure of Invention
Therefore, the invention provides a method for detecting halogen in a geological sample, aiming at solving the technical problem that the existing detection method cannot quantitatively detect chlorine and fluorine in the geological sample.
Therefore, the invention adopts the following technical scheme:
the invention provides a method for detecting halogen in a geological sample, which comprises the steps of converting fluorine and chlorine elements in a sample to be detected into substances dissolved in water by an alkali fusion method, and then detecting by ion chromatography.
The detection method comprises the following steps:
s1: fully mixing the sample powder to be detected with a sodium hydroxide solution and then evaporating to dryness;
s2: burning the evaporated substance in the S1 at 500-600 ℃ for 30-40 minutes;
s3: taking out the burning product, adding deionized water, and boiling for 10-15 minutes;
s4: adding deionized water into the mixture after the boiling step of S3 for dilution, and shaking up overnight;
s5: centrifuging at 1500rpm-2500rpm for 5-8 min to separate the overnight shaken substance in S4, and diluting the supernatant to obtain a solution to be detected;
s6: preparing standard curves of fluorine and chlorine;
s7: detecting the solution to be detected by using ion chromatography to obtain an ion chromatogram of the solution to be detected, calculating the mass of fluorine and chlorine in the solution to be detected according to a standard curve of the fluorine and chlorine, and then calculating the mass of the fluorine and chlorine in the sample to be detected.
Further, in S5, the concentration of NaOH in the solution to be tested is not more than 0.0375 wt%.
In S1, adding 0.6-1.2 mL of 15 wt-20 wt% sodium hydroxide solution into a sample powder to be detected, wherein the mass of the sample powder to be detected is 0.05-0.1 g;
preferably, the sample powder to be tested has a mass of 0.05g, and 0.6mL of 15 wt% sodium hydroxide solution is added.
Further, the series of fluorine and chlorine standard samples are mixed solutions of NaCl, NaF, and NaOH.
The method for preparing the series of standard samples of fluorine and chlorine comprises the following steps:
firstly, respectively dissolving NaCl and NaF in water to obtain a 1mg/mL NaCl solution and a 1mg/mL NaF solution, and respectively preparing NaF and NaCl mixed standard solutions of 4 mu g/mL, 10 mu g/mL, 40 mu g/mL, 200 mu g/mL and 400 mu g/mL by using a mother solution weighing method;
then respectively putting 0.6mL of 15% NaOH solution and 0.700g of NaCl and NaF mixed standard solution into a 15mL centrifuge tube, weighing by using a balance, and diluting the mixed solution to 14 g;
finally, diluting 0.2mL of clear solution of each concentration obtained in the mixed solution to 4mL in a 5mL centrifuge tube to obtain a series of fluorine and chlorine standard samples, wherein the fluorine and chlorine concentrations in the series of fluorine and chlorine standard samples are the same and are respectively 0.010 mu g/mL, 0.025 mu g/mL, 0.100 mu g/mL, 0.500 mu g/mL and 1 mu g/mL.
The standard curve of fluorine and chlorine in S6 is y ═ k × m + b, wherein y is the ion spectrogram peak area of fluorine or chlorine in the sample, m is the mass of fluorine or chlorine in the sample, k is the slope of the equation, and b is the intercept of the equation.
Preferably, in S1-S4, the container used is a silver crucible.
Further, the silver crucible is cleaned before and after use, and the cleaning treatment is to add dilute hydrochloric acid to boil for 5-10 minutes and then to burn for 1-2 hours at 850 ℃.
The technical scheme of the invention has the following advantages:
(1) the invention combines the alkali fusion with the ion chromatograph, realizes the simultaneous digestion of a plurality of samples, saves the pretreatment time, realizes the simultaneous determination of F and Cl elements by the high-precision ion chromatography, and has the popularization universality.
(2) According to the method, the NaOH solution is used for digesting the sample, so that the problem that the sample is not sufficiently digested is avoided, volatilization of F and Cl is avoided, the alkaline fusion digestion residue is further soaked in water, and F, Cl loss in the experimental process is reduced; the combination of ion chromatography with high precision analysis up to ppb-ppt level makes the method useful for analytical testing of samples of relatively low content.
(3) The first peak in the ion chromatogram due to the experiment is OH-And the second and third peaks are F-And Cl-Peak of (2), with OH-Increase in concentration, F-And Cl-Moving before the peak time of (OH)-The peak of (A) greatly suppresses F-The present invention limits the NaOH concentration in the solution to be measured to not more than 0.0375 wt% so thatTo obtain F-Does not receive OH-The influence of the peak reduces the error of the experiment.
(4) The solution amounts of the sample to be detected and NaOH used in the method are small, compared with the existing alkali fusion digestion method in the early years, the method is simpler to operate, the chemical reagent consumption is less, the blank of the test is reduced, and the cost is greatly reduced.
(5) The silver crucible and the centrifugal tube are used as the equipment, and can be cleaned and reused after being used, so that the material consumption is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an ion chromatogram of a GSP-2 sample according to example 1 of the present invention;
FIG. 2 is a graph comparing fluorine contents and reference values of samples obtained in example 1 and example 2 of the present invention;
FIG. 3 is a graph comparing chlorine contents of samples obtained in example 1 and example 2 of the present invention with reference values.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field.
The rock samples used in the specific embodiment of the invention are respectively:
GSR-1, GSR-2, GSR-3, GSR-7: the source is national geological analysis research center);
BHVO-1, BCR-2, BIR-1, AGV-2, STM-1, G-2, GSP-2, RGM-1: the source is the united states geological exploration (u.s.geological Survey);
JG-1: the source is the Japanese Geological Survey (Geological Survey of Japan).
Example 1
The invention provides a method for detecting halogen in a geological sample, wherein the samples to be detected are JG-1, G-2, RGM-1, AGV-2, BHVO-1 and GSR-1 respectively, and the detection method comprises the following specific steps:
(1) adding dilute hydrochloric acid into a silver crucible, placing the silver crucible on a hot plate, boiling the silver crucible for 10 minutes, and then firing the silver crucible for 2 hours at 850 ℃;
(2) weighing 0.05g of sample powder to be detected in a silver crucible, adding 0.6mL of 15 wt% sodium hydroxide solution, fully mixing, and evaporating to dryness;
(3) firing the silver crucible at 600 ℃ for 30 minutes;
(4) taking out the fired silver crucible, adding deionized water and boiling for 10 minutes;
(5) transferring the liquid and the solid in the silver crucible into a 15mL centrifuge tube, weighing by using a balance, adding deionized water into the solution to dilute to 14g, and shaking up overnight;
(6) centrifuging the centrifuge tube at 2500rpm for 5 minutes, taking 0.2mL of supernatant liquid to dilute to 4mL to obtain a solution to be detected;
(7) respectively dissolving NaCl and NaF in water to obtain a 1mg/mL NaCl solution and a 1mg/mL NaF solution, and respectively preparing NaF and NaCl mixed standard solutions of 4 mu g/mL, 10 mu g/mL, 40 mu g/mL, 200 mu g/mL and 400 mu g/mL by using a mother liquor weighing method;
(8) respectively putting 0.6mL of 15% NaOH solution and 0.700g of NaCl and NaF mixed standard solution into a 15mL centrifuge tube, weighing by using a balance, and diluting the mixed solution to 14 g;
(9) diluting 0.2mL of clear liquid of the obtained mixed solution with each concentration to 4mL in a 5mL centrifuge tube respectively to obtain a series of fluorine and chlorine standard samples, wherein the fluorine and chlorine concentrations in the series of fluorine and chlorine standard samples are the same and are respectively 0.010 mu g/mL, 0.025 mu g/mL, 0.100 mu g/mL, 0.500 mu g/mL and 1 mu g/mL;
(10) detecting a series of standard solutions of fluorine and chlorine by using ion chromatography to prepare standard curves of fluorine and chlorine;
(11) detecting the solution to be detected by using ion chromatography to obtain an ion chromatogram of the solution to be detected, as shown in fig. 1, which is an ion chromatogram of GSP-2, calculating the mass of fluorine and chlorine in the solution to be detected by using a standard curve of fluorine and chlorine, and then calculating the mass of fluorine and chlorine in the sample to be detected.
Example 2
The invention provides a method for detecting halogen in a geological sample, wherein the samples to be detected are JG-1, G-2, RGM-1, AGV-2, BHVO-1 and GSR-1 respectively, and the detection method comprises the following specific steps:
(1) adding dilute hydrochloric acid into a silver crucible, placing the silver crucible on a hot plate, boiling for 5 minutes, and then firing for 1 hour at 850 ℃;
(2) weighing 0.1g of sample powder to be detected in a silver crucible, adding 1.2mL of 20 wt% sodium hydroxide solution, fully mixing, and evaporating to dryness;
(3) firing the silver crucible at 600 ℃ for 30 minutes;
(4) taking out the fired silver crucible, adding deionized water and boiling for 10 minutes;
(5) transferring the liquid and the solid in the silver crucible into a 15mL centrifuge tube, weighing by using a balance, adding deionized water into the solution to dilute to 14g, and shaking up overnight;
(6) centrifuging the centrifugal tube at 1500rpm for 8 minutes, taking 0.1mL of supernatant liquid to dilute to 4mL to obtain a solution to be detected;
(7) and detecting the solution to be detected by using ion chromatography to obtain an ion chromatogram of the solution to be detected, calculating the mass of fluorine and chlorine in the solution to be detected by using the standard curve of fluorine and chlorine obtained in the embodiment 1, and then calculating the mass of fluorine and chlorine in the sample to be detected.
Example 3
The invention provides a method for detecting halogen in a geological sample, wherein the samples to be detected are GSR-2, GSR-3, GSR-7, BCR-2, BIR-1, STM-1 and GSP-2 respectively, and the detection method comprises the following specific steps:
(1) adding dilute hydrochloric acid into a silver crucible, placing the silver crucible on a hot plate, boiling the silver crucible for 10 minutes, and then firing the silver crucible for 2 hours at 850 ℃;
(2) weighing 0.05g of sample powder to be detected in a silver crucible, adding 0.6mL of 15 wt% sodium hydroxide solution, fully mixing, and evaporating to dryness;
(3) firing the silver crucible at 600 ℃ for 30 minutes;
(4) taking out the fired silver crucible, adding deionized water and boiling for 10 minutes;
(5) transferring the liquid and the solid in the silver crucible into a 15mL centrifuge tube, weighing by using a balance, adding deionized water into the solution to dilute to 14g, and shaking up overnight;
(6) centrifuging the centrifuge tube at 2500rpm for 5 minutes, taking 0.2mL of supernatant liquid to dilute to 4mL to obtain a solution to be detected;
(7) and detecting the solution to be detected by using ion chromatography to obtain an ion chromatogram of the solution to be detected, calculating the mass of fluorine and chlorine in the solution to be detected by using the standard curve of fluorine and chlorine obtained in the embodiment 1, and then calculating the mass of fluorine and chlorine in the sample to be detected.
Test example 1
The relationship between the peak area and the fluorine and chlorine mass for a series of fluorine and chlorine standard solutions in example 1 is shown in table 1 below:
TABLE 1 relationship between peak area and fluorine and chlorine mass in a series of fluorine and chlorine standard solutions
| 1 | 2 | 3 | 4 | 5 | |
| F or Cl concentration (μ g/mL) | 0.010 | 0.025 | 0.100 | 0.500 | 1.000 |
| Quality of F or Cl is μ g | 0.040 | 0.100 | 0.400 | 2.000 | 4.000 |
| F-Peak area | 0.137 | 0.344 | 1.352 | 6.699 | 13.723 |
| Cl-Peak area | 0.330 | 0.458 | 1.155 | 4.563 | 9.104 |
The available fluorine standard curve is y-3.4226 m-0.0257, R20.9998; the standard curve of chlorine is that y is 2.2075m +0.2345, R20.9998 where y is fluorine or chlorine of the sampleThe peak area of the ion spectrogram, and m is the mass of fluorine or chlorine in the sample.
Test example 2
The experimental blanks and limits of detection were tested using the method of example 1 using blank samples and the results are shown in table 2 below:
TABLE 2 Experimental blanks and limits of detection
For samples with low F, Cl content, the accuracy of data results will be directly affected by excessively high process blank and detection limit, and as shown in the table above, the method of the present invention has low experimental process blank and detection limit, is suitable for most rock geological samples, and is suitable for wide popularization.
Test example 3
The method of example 1 was used to perform a spiking recovery test using a blank sample and a standard solution, the results of which are shown in table 3 below:
TABLE 3 spiked recovery of fluorine and chlorine in the experiment
As can be seen from the above table, the results show that the recovery rates of F and Cl in the spiked range are 93-103% and 92-103%, respectively, and have good recovery rates, which indicates that F, Cl is less lost and less polluted in the above test process, and the test requirements are met.
Test example 4
The samples of example 1 and example 3 were each tested in duplicate, and the fluorine and chlorine contents of the samples were calculated from the standard curves of test example 1 and compared with the set values, and the results are shown in table 4:
TABLE 4 results of measured values and comparison with standard values for each sample
As can be seen from the above table, the values of fluorine and chlorine in the sample detected by the method provided by the present application substantially match the standard values with little deviation.
Test example 5
Comparing the test results of example 1 and example 2 with the reference values, the results are shown in fig. 1 and fig. 2, as shown in fig. 2, the test results and the reference values of the fluorine content of example 1 and example 2 are basically consistent, as shown in fig. 3, the results of chlorine in example 1 are closer to the reference values, and the results of example 2 are slightly smaller than the reference values, so that the application prefers that the sample powder to be tested has a mass of 0.05g, and 0.6mL of 15 wt% sodium hydroxide solution is added.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (9)
1. The method for detecting the halogen in the geological sample is characterized in that fluorine and chlorine elements in a sample to be detected are converted into substances dissolved in water by an alkali fusion method, and then the detection is carried out by ion chromatography.
2. The detection method according to claim 1, characterized in that it comprises the steps of:
s1: fully mixing the sample powder to be detected with a sodium hydroxide solution and then evaporating to dryness;
s2: burning the evaporated substance in the S1 at 500-600 ℃ for 30-40 minutes;
s3: taking out the burning product, adding deionized water, and boiling for 10-15 minutes;
s4: adding deionized water into the mixture after the boiling step of S3 for dilution, and shaking up overnight;
s5: centrifuging at 1500rpm-2500rpm for 5-8 min to separate the overnight shaken substance in S4, and diluting the supernatant to obtain a solution to be detected;
s6: preparing standard curves of fluorine and chlorine;
s7: detecting the solution to be detected by using ion chromatography to obtain an ion chromatogram of the solution to be detected, calculating the mass of fluorine and chlorine in the solution to be detected according to a standard curve of the fluorine and chlorine, and then calculating the mass of the fluorine and chlorine in the sample to be detected.
3. The detection method according to claim 2, wherein in S5, the concentration of NaOH in the solution to be detected is not more than 0.0375 wt%.
4. The detection method according to claim 2 or 3, wherein in S1, the sample powder to be detected has a mass of 0.05g-0.1g, and 0.6mL-1.2mL of 15 wt% -20 wt% sodium hydroxide solution is added.
5. The detection method according to claim 4, wherein the sample powder to be detected has a mass of 0.05g, and 0.6mL of 15 wt% sodium hydroxide solution is added.
6. The detection method according to claim 1, wherein the series of standard samples of fluorine and chlorine is a mixed solution of NaCl, NaF and NaOH.
7. The detection method according to claim 6, wherein the method for preparing the series of fluorine and chlorine standard samples comprises:
firstly, respectively dissolving NaCl and NaF in water to obtain a 1mg/mL NaCl solution and a 1mg/mL NaF solution, and respectively preparing NaF and NaCl mixed standard solutions of 4 mu g/mL, 10 mu g/mL, 40 mu g/mL, 200 mu g/mL and 400 mu g/mL by using a mother solution weighing method;
then 0.6mL of 15% NaOH solution and 0.700g of NaCl and NaF mixed standard solution are respectively put into a 15mL centrifuge tube and diluted to 14 g;
finally, diluting 0.2mL of clear solution of each concentration obtained in the mixed solution to 4mL in a 5mL centrifuge tube to obtain a series of fluorine and chlorine standard samples, wherein the fluorine and chlorine concentrations in the series of fluorine and chlorine standard samples are the same and are respectively 0.010 mu g/mL, 0.025 mu g/mL, 0.100 mu g/mL, 0.500 mu g/mL and 1 mu g/mL.
8. The detection method according to any one of claims 2 to 7, wherein the container used in S1 to S4 is a silver crucible.
9. The detection method according to claim 8, wherein the silver crucible is cleaned before and after use, and the cleaning treatment is to add dilute hydrochloric acid to boil for 5-10 minutes and then to burn for 1-2 hours at 850 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011056766.3A CN112229941A (en) | 2020-09-29 | 2020-09-29 | Halogen detection method in geological sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011056766.3A CN112229941A (en) | 2020-09-29 | 2020-09-29 | Halogen detection method in geological sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112229941A true CN112229941A (en) | 2021-01-15 |
Family
ID=74120424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011056766.3A Withdrawn CN112229941A (en) | 2020-09-29 | 2020-09-29 | Halogen detection method in geological sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112229941A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115326914A (en) * | 2022-10-11 | 2022-11-11 | 北矿检测技术有限公司 | Method for simultaneously and rapidly measuring chlorine, bromine and iodine by high-temperature hydrolysis combined ICP-MS |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101980010A (en) * | 2010-05-25 | 2011-02-23 | 江西中烟工业有限责任公司 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
| CN102128790A (en) * | 2010-12-06 | 2011-07-20 | 山东电力研究院 | Method for measuring sulfate ions in scaled component of water vapor system in power station |
| CN102590375A (en) * | 2012-01-30 | 2012-07-18 | 云南民族大学 | Method for extracting anions from plant medicine by alkali fusion method performing ion chromatographic detection |
| CN110487932A (en) * | 2019-08-23 | 2019-11-22 | 泽州县和美环保科技有限公司 | The detection method of chlorine in a kind of solid waste |
| CN111089933A (en) * | 2019-12-30 | 2020-05-01 | 安徽皖仪科技股份有限公司 | Method for measuring anions in electroplating sludge |
-
2020
- 2020-09-29 CN CN202011056766.3A patent/CN112229941A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101980010A (en) * | 2010-05-25 | 2011-02-23 | 江西中烟工业有限责任公司 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
| CN102128790A (en) * | 2010-12-06 | 2011-07-20 | 山东电力研究院 | Method for measuring sulfate ions in scaled component of water vapor system in power station |
| CN102590375A (en) * | 2012-01-30 | 2012-07-18 | 云南民族大学 | Method for extracting anions from plant medicine by alkali fusion method performing ion chromatographic detection |
| CN110487932A (en) * | 2019-08-23 | 2019-11-22 | 泽州县和美环保科技有限公司 | The detection method of chlorine in a kind of solid waste |
| CN111089933A (en) * | 2019-12-30 | 2020-05-01 | 安徽皖仪科技股份有限公司 | Method for measuring anions in electroplating sludge |
Non-Patent Citations (2)
| Title |
|---|
| KENJI SHIMIZU等: "Ion Chromatographic Determination of Fluorine and Chlorine in Silicate Rocks Following Alkaline Fusion", 《GEOSTANDARDS AND RESEARCH GEOANALYTICAL》 * |
| 刘燕等: "同时测定粉末地质样品中的氟和氯-碱熔-IC", 《第九届全国成矿理论与找矿方法学术讨论会论文摘要集》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115326914A (en) * | 2022-10-11 | 2022-11-11 | 北矿检测技术有限公司 | Method for simultaneously and rapidly measuring chlorine, bromine and iodine by high-temperature hydrolysis combined ICP-MS |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lanping et al. | A rapid and simple single-stage method for Ca separation from geological and biological samples for isotopic analysis by MC-ICP-MS | |
| Tan et al. | High-sensitivity determination of Cd isotopes in low-Cd geological samples by double spike MC-ICP-MS | |
| Cotta et al. | Classical and new procedures of whole rock dissolution for trace element determination by ICP‐MS | |
| Zhu et al. | An improved method of Cr purification for high precision measurement of Cr isotopes by double spike MC-ICP-MS | |
| Tolu et al. | Selenium speciation analysis at trace level in soils | |
| Merryfield et al. | Simultaneous determination of metals in oil by inductively coupled plasma emission spectrometry | |
| Kennett et al. | Compositional characterization of prehistoric ceramics: a new approach | |
| De Muynck et al. | Development of a new method for Pb isotopic analysis of archaeological artefacts using single-collector ICP-dynamic reaction cell-MS | |
| Yang et al. | On-line determination of silver in sea-water and marine sediment by inductively coupled plasma mass spectrometry | |
| Liu et al. | Optimization of lithium isotope analysis in geological materials by quadrupole ICP-MS | |
| Satyanarayanan et al. | High precision multielement analysis on geological samples by HR-ICP-MS | |
| CN110530960A (en) | A kind of Carbonate Oil gas reservoir pyrite Rb-Sr isotope dating Age Dating | |
| Dellinger et al. | Measurements of rhenium isotopic composition in low-abundance samples | |
| Yoshinaga et al. | Determination of copper, zinc, cadmium and lead in a fish otolith certified reference material by isotope dilution inductively coupled plasma mass spectrometry using off-line solvent extraction | |
| Feng et al. | A simple single-stage extraction method for Mo separation from geological samples for isotopic analysis by MC-ICP-MS | |
| CN112229941A (en) | Halogen detection method in geological sample | |
| Ohta et al. | A precise and accurate analytical method for determination of osmium isotope ratios at the 1–15 pg level by using a MC-ICP-MS equipped with sparging introduction and high-sensitivity discrete dynode-type ion-counting detectors | |
| US10422023B2 (en) | Recovery of rare earth elements by liquid-liquid extraction from fresh water to hypersaline solutions | |
| Tazoe et al. | Determination of cerium isotope ratios in geochemical samples using oxidative extraction technique with chelating resin | |
| Bing et al. | Simultaneous determination of iodine, bromine, selenium and arsenic in geological samples by inductively coupled plasma mass spectrometry | |
| Huang et al. | Determination of silver in geological samples using aerosol dilution ICP-MS after water-bath extraction with inverse aqua regia | |
| Erdman et al. | Sulfur concentration in geochemical reference materials by solution inductively coupled plasma‐mass spectrometry | |
| Nakagawa et al. | Precise isotopic analysis of Mo in seawater using multiple collector-inductively coupled mass spectrometry coupled with a chelating resin column preconcentration method | |
| Tudorache et al. | Barium concentrations and speciation in mineral natural waters of central Romania | |
| Walsh | Determination of boron at trace levels in rocks by inductively coupled plasma spectrometry |
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 | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210115 |