CN109297920B - Cold atom absorption device and method for measuring total arsenic and total antimony - Google Patents
Cold atom absorption device and method for measuring total arsenic and total antimony Download PDFInfo
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- CN109297920B CN109297920B CN201811443196.6A CN201811443196A CN109297920B CN 109297920 B CN109297920 B CN 109297920B CN 201811443196 A CN201811443196 A CN 201811443196A CN 109297920 B CN109297920 B CN 109297920B
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 69
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 35
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 35
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000003814 drug Substances 0.000 claims abstract description 34
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 32
- 230000003287 optical effect Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000007664 blowing Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea group Chemical group NC(=S)N UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000070 arsenic hydride Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 9
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 238000004801 process automation Methods 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
Abstract
The invention discloses a cold atom absorption device for measuring total arsenic and total antimony, which comprises a sample feeding pipeline, a peristaltic pump, a blow-off pipe, an air pump and an atom absorption optical component. The outside of the blow-off pipe is provided with a heating device, one end of the peristaltic pump is connected with the sample injection pipeline, the other end of the peristaltic pump is connected with the bottom of the blow-off pipe, the upper part of the blow-off pipe is connected with an air pump through a pipeline, and the air pump is connected with the atomic absorption optical component. The middle part of the blow-off pipe is connected with a sample introduction pipeline through a pipeline, and the sample introduction pipeline is provided with an emptying pipeline. The invention also discloses a cold atom absorption method for measuring total arsenic and total antimony. The invention has the advantages that: rational in infrastructure, analysis process automation degree is high, and the analytic process is quick, high-efficient, and the medicament that needs is few, and the degree of accuracy is high.
Description
Technical Field
The invention relates to the technical field of water quality analysis, in particular to a cold atom absorption device and method for measuring total arsenic and total antimony.
Background
The existing total arsenic and total antimony analysis methods are both spectrophotometry, and the analysis process of the total arsenic is as follows: the sample is required to be pumped into a blowing support pipe, an acid reagent is added for digestion, the reaction is carried out under the action of sodium borohydride to generate arsine gas, the gas is blown to a quartz mixing pipe with a sand core by an air pump, the gas and a color developing agent are subjected to color development reaction at a certain temperature, and the absorbance of the gas is measured at a certain wavelength to convert a concentration value. The analysis process of the total antimony is as follows: pumping the sample into a water path, adding a hydrochloric acid solution and a thiourea reagent, fully reducing, adding potassium iodide and a color developing agent for color development reaction, and absorbing and colorimetric the reactant at a certain wavelength so as to calculate the concentration value of the sample. However, the spectrophotometry analysis of the two parameters has a common disadvantage that a large amount of medicament is needed, the testing time is long, the process is complicated, and the accuracy of the spectrophotometry is not high enough.
Disclosure of Invention
In view of the above problems, the present invention provides a cold atom absorption apparatus and method for measuring total arsenic and total antimony with fast and accurate analysis process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a cold atom absorption device for measuring total arsenic and total antimony comprises a sample introduction pipeline, a peristaltic pump, a blow-off pipe, an air pump and an atom absorption optical component. The outside of the blow-off pipe is provided with a heating device, one end of the peristaltic pump is connected with the sample injection pipeline, the other end of the peristaltic pump is connected with the bottom of the blow-off pipe, the upper part of the blow-off pipe is connected with an air pump through a pipeline, and the air pump is connected with the atomic absorption optical component. The middle part of the blow-off pipe is connected with a sample introduction pipeline through a pipeline, and the sample introduction pipeline is provided with an emptying pipeline.
Furthermore, the sample introduction pipeline comprises a plurality of three-way valves, and each three-way valve comprises a normally-open end, a common end and a normally-closed end.
Further, the sample injection pipeline comprises three-way valves Q0, Q1, Q2, Q3, Q4, Q5 and Q6. Wherein, Q0's normal open end is connected the pure water pipe, the end that closes normally connects water sample pipe, the common port links to each other with Q1's normal open end, Q1's normal close end is connected the mark liquid pipe, the end that closes normally of Q2 is connected to the common port, Q2's common port is connected the end that opens normally of Q4, the end that opens normally is connected with Q3's normal open end, the evacuation pipeline is connected to Q3's normal close end, Q5 common port is connected to Q4's common port, R1 medicament pipe is connected to the end that closes normally, Q5's common port is connected Q6 common port, the end that closes normally is connected R2 medicament pipe, the peristaltic pump is connected to Q6's common port, the end that closes normally is connected R3.
Furthermore, a three-way valve QE is arranged at the joint of the middle part of the blow-off pipe and the sample feeding pipeline, the public end of the QE is connected with the public end of the Q3, the normally closed end is connected with the middle part of the blow-off pipe, and the normally open end is connected with the emptying pipeline.
Furthermore, a three-way valve QF is arranged at the joint of the air pump and the atomic optical absorption component, the common end of the QF is connected with the air pump, and the atomic optical absorption component comprises a total arsenic absorption part, a total antimony absorption part and a T-shaped three-way valve. The total arsenic absorption part and the total antimony absorption part are respectively provided with an air inlet and an air outlet, the air inlet of the total arsenic absorption part and the air inlet of the total antimony absorption part are respectively connected with the normally closed end and the normally open end of the QF, the air outlets of the total arsenic absorption part and the total antimony absorption part are respectively connected with two valve ports of the T-shaped tee joint, and the other valve port of the T-shaped tee joint is connected with an absorption liquid pipe.
Furthermore, a water sample detector is arranged at the joint of the sample feeding pipeline and the peristaltic pump.
The invention also discloses a cold atom absorption method for measuring total arsenic and total antimony, which adopts the cold atom absorption device for measuring total arsenic and total antimony and comprises the following steps:
step 1: starting the instrument, pumping a water sample into the stripping pipe from the bottom of the stripping pipe through a peristaltic pump, and discharging redundant samples from the upper end of the stripping pipe;
step 2: slowly rotating a peristaltic pump to pump a quantitative R1 medicament into the stripping tube and fully mixing the quantitative R1 medicament with a water sample, starting a heating device, and heating and digesting the sample in the blowing tube, wherein the R1 medicament is a sulfuric acid solution;
and step 3: slowly rotating a peristaltic pump to pump a quantitative R2 medicament into the air stripping tube and fully mixing the quantitative R2 medicament with a sample in the air stripping tube, wherein the R2 medicament is a thiourea solution;
and 4, step 4: slowly rotating the peristaltic pump, intermittently and quantitatively adding the R3 medicament into the stripping tube, and simultaneously starting the air pump to blow the AsH3 gas generated in the stripping tube into the atomic absorption optical component for atomic absorption, wherein the R3 medicament is a mixed solution of sodium borohydride and sodium hydroxide;
and 5: after the blowing is finished, calculating the peak area in the absorption process to obtain the total arsenic or total antimony content of the sample;
step 6: and slowly rotating the peristaltic pump, pumping pure water into the pipeline for cleaning, and completely blowing the gas in the pipeline out of the pipeline through the gas pump to be completely absorbed in the absorption liquid.
The invention has the following beneficial effects: the invention has the advantages of reasonable structure, high automation degree of the analysis process, simple, rapid and efficient analysis process, less required medicament and high accuracy.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Description of the main component symbols: 1. a sample introduction pipeline; 101. a pure water pipe; 102. a water sample pipe; 103. a marking liquid pipe; 104. r1 vial; 105. r2 vial; 106. r3 vial; 2. a peristaltic pump; 3. blowing off the pipe; 4. an air pump; 5-atom absorbing optical members; 51. a total arsenic absorbing section; 52. a total antimony absorbing portion; 53. t-shaped tee joints; 6. heating the aluminum piece; 7. a water sample detector.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
As shown in figure 1, a cold atom absorption device for measuring total arsenic and total antimony comprises a sample introduction pipeline 1, a peristaltic pump 2, a blow-off pipe 3, an air pump 4 and an atom absorption optical component 5.
The sample introduction pipeline 1 comprises a plurality of three-way valves, and each three-way valve comprises a normally open end (NO), a common end (COM) and a normally closed end (NC). The sample introduction pipeline 1 comprises three-way valves Q0, Q1, Q2, Q3, Q4, Q5 and Q6. Wherein, the normal open end of Q0 connects pure water pipe 101, and the normal close end connects water sample pipe 102, and the common port links to each other with the normal open end of Q1, and the normal close end of Q1 connects the mark liquid pipe 103, and the normal close end of Q2 is connected to the common port, and the normal open end of Q4 is connected to the common port of Q2, and the normal open end is connected with the normal open end of Q3, and the normal close end of Q3 is connected W1 evacuation pipeline. The common end of Q4 is connected with the common end of Q5, the normally closed end is connected with the R1 medicament tube 104, the common end of Q5 is connected with the common end of Q6, and the normally closed end is connected with the R2 medicament tube 105. The common end of Q6 is connected with peristaltic pump 2, and the junction of Q6 and peristaltic pump 2 is equipped with water sample detector 7, and the bottom of blowing off pipe 3 is connected to the other end of peristaltic pump 2, and R3 medicament pipe 106 is connected to Q6 normally closed end.
The outer side of the blow-off pipe 3 is provided with a heating aluminum piece 6, the upper part of the blow-off pipe 3 is connected with an air pump 4 through a pipeline, and the air pump 4 is connected with an atomic absorption optical component 5. The joint of the air pump 4 and the atomic optical absorption component 5 is provided with a three-way valve QF, and the common end of the QF is connected with the air pump 4. The atomic optical absorption member 5 includes a total arsenic absorption portion 51, a total antimony absorption portion 52, and a T-junction 53. The total arsenic absorbing section 51 and the total antimony absorbing section 52 are provided with an air inlet and an air outlet, respectively. The inlet of the total arsenic absorbing portion 51 is connected to the normally closed end of QF, and the inlet of the total antimony absorbing portion 52 is connected to the normally open end of QF. The outlets of the total arsenic absorption part 51 and the total antimony absorption part 52 are respectively connected with two valve ports of a T-shaped tee 53, and the other valve port of the T-shaped tee 53 is connected with an absorption liquid pipe (not shown in the figure).
The common end of Q3 is connected with the middle part of the blow-off pipe 3, a three-way valve QE is arranged at the joint, the common end of QE is connected with the common end of Q3, the normally closed end is connected with the middle part of the blow-off pipe 3, and the normally open end is connected with the W2 emptying pipeline.
The invention also discloses a cold atom absorption method for measuring total arsenic and total antimony, which adopts the cold atom absorption device for measuring total arsenic and total antimony and comprises the following steps:
step 1: starting the instrument, pumping a water sample into the stripping tube 3 from the bottom of the stripping tube 3 through the peristaltic pump 2, and discharging redundant samples from the upper end of the stripping tube 3;
step 2: slowly rotating the peristaltic pump 2 to pump a quantitative R1 medicament into the stripping tube 3 and fully mixing the quantitative R1 medicament with a water sample, starting the heating aluminum piece 6 to heat and digest the sample in the stripping tube 3, wherein the R1 medicament is a sulfuric acid solution;
and step 3: slowly rotating the peristaltic pump 2 to pump a quantitative R2 medicament into the air stripping tube 3 and fully mixing the quantitative R2 medicament with a sample in the air stripping tube 3, wherein the R2 medicament is thiourea solution;
and 4, step 4: slowly rotating the peristaltic pump 2, intermittently and quantitatively adding the R3 medicament into the stripping tube 3, and simultaneously starting the air pump 4 to blow the AsH3 gas generated in the stripping tube 3 into the atomic absorption optical component 5 for atomic absorption, wherein the R3 medicament is a mixed solution of sodium borohydride and sodium hydroxide;
and 5: after the blowing is finished, calculating the peak area in the absorption process to obtain the total arsenic or total antimony content of the sample;
step 6: and slowly rotating the peristaltic pump 2, pumping pure water into the pipeline for cleaning, and completely blowing the gas in the pipeline out of the pipeline through the air pump 4 to be completely absorbed in the absorption liquid.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A cold atom absorption method for measuring total arsenic and total antimony is characterized in that: the cold atom absorption device for measuring total arsenic and total antimony is adopted, the cold atom absorption device for measuring total arsenic and total antimony comprises a sample introduction pipeline, a peristaltic pump, an air blowing-off pipe, an air pump and an atom absorption optical component, a heating device is arranged on the outer side of the air blowing-off pipe, one end of the peristaltic pump is connected with the sample introduction pipeline, the other end of the peristaltic pump is connected with the bottom of the air blowing-off pipe, the upper part of the air blowing-off pipe is connected with the air pump through a pipeline, the air pump is connected with the atom absorption optical component, the middle part of the air blowing-off pipe is connected with the sample introduction pipeline through a pipeline, and a drain pipeline is arranged on the sample introduction; the cold atom absorption method for measuring total arsenic and total antimony comprises the following steps:
step 1: starting the instrument, pumping a water sample into the stripping pipe from the bottom of the stripping pipe through a peristaltic pump, and discharging redundant samples from the upper end of the stripping pipe;
step 2: slowly rotating a peristaltic pump to pump a quantitative R1 medicament into the stripping tube and fully mixing the quantitative R1 medicament with a water sample, starting a heating device, and heating and digesting the sample in the blowing tube, wherein the R1 medicament is a sulfuric acid solution;
and step 3: slowly rotating a peristaltic pump to pump a quantitative R2 medicament into the air stripping tube and fully mixing the quantitative R2 medicament with a sample in the air stripping tube, wherein the R2 medicament is a thiourea solution;
and 4, step 4: slowly rotating the peristaltic pump, intermittently and quantitatively adding the R3 medicament into the stripping tube, and simultaneously starting the air pump to blow the AsH3 gas generated in the stripping tube into the atomic absorption optical component for atomic absorption, wherein the R3 medicament is a mixed solution of sodium borohydride and sodium hydroxide;
and 5: after the blowing is finished, calculating the peak area in the absorption process to obtain the total arsenic or total antimony content of the sample;
step 6: and slowly rotating the peristaltic pump, pumping pure water into the pipeline for cleaning, and completely blowing the gas in the pipeline out of the pipeline through the gas pump to be completely absorbed in the absorption liquid.
2. The method of claim 1, wherein the cold atomic absorption method comprises the following steps: the sample introduction pipeline comprises a plurality of three-way valves, and each three-way valve comprises a normally open end, a public end and a normally closed end.
3. The method of claim 2, wherein the cold atomic absorption method comprises the following steps: the sample introduction pipeline comprises three-way valves Q0, Q1, Q2, Q3, Q4, Q5 and Q6, wherein a normally open end of Q0 is connected with a pure water pipe, a normally closed end is connected with a water sample pipe, a common end is connected with a normally open end of Q1, a normally closed end of Q1 is connected with a standard liquid pipe, a common end is connected with a normally closed end of Q2, a common end of Q2 is connected with a normally open end of Q4, a normally open end is connected with a normally open end of Q3, a normally closed end of Q3 is connected with an emptying pipeline, a common end of Q4 is connected with a Q5 common end, a normally closed end is connected with an R1 medicament pipe, a common end of Q5 is connected with a Q6 common end, a normally closed end is connected with an R2 medicament pipe, a common end of Q6 is connected with a pump, and a normally closed end.
4. A method of measuring cold atomic absorption of total arsenic and total antimony as claimed in claim 3, wherein: and a three-way valve QE is arranged at the joint of the middle part of the blow-off pipe and the sample feeding pipeline, the public end of the QE is connected with the public end of the Q3, the normally closed end is connected with the middle part of the blow-off pipe, and the normally open end is connected with the emptying pipeline.
5. The method of claim 1, wherein the cold atomic absorption method comprises the following steps: the atomic optical absorption component comprises a total arsenic absorption part, a total antimony absorption part and a T-shaped tee joint, wherein the total arsenic absorption part and the total antimony absorption part are respectively provided with an air inlet and an air outlet, the air inlet of the total arsenic absorption part and the air inlet of the total antimony absorption part are respectively connected with a normally closed end and a normally open end of the QF, the air outlets of the total arsenic absorption part and the total antimony absorption part are respectively connected with two valve ports of the T-shaped tee joint, and the other valve port of the T-shaped tee joint is connected with an absorption liquid pipe.
6. The method of claim 1, wherein the cold atomic absorption method comprises the following steps: and a water sample detector is arranged at the joint of the sample introduction pipeline and the peristaltic pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811443196.6A CN109297920B (en) | 2018-11-29 | 2018-11-29 | Cold atom absorption device and method for measuring total arsenic and total antimony |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811443196.6A CN109297920B (en) | 2018-11-29 | 2018-11-29 | Cold atom absorption device and method for measuring total arsenic and total antimony |
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| Publication Number | Publication Date |
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| CN109297920A CN109297920A (en) | 2019-02-01 |
| CN109297920B true CN109297920B (en) | 2021-05-11 |
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|---|---|---|---|---|
| US4294127A (en) * | 1979-06-15 | 1981-10-13 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Automatic sample feeder for flameless atomic absorption spectrometer |
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| CN107290553A (en) * | 2015-07-15 | 2017-10-24 | 厦门市吉龙德环境工程有限公司 | Dissolvable sulfide analysis method in a kind of water sample |
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2018
- 2018-11-29 CN CN201811443196.6A patent/CN109297920B/en active Active
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|---|---|---|---|---|
| US4294127A (en) * | 1979-06-15 | 1981-10-13 | Bodenseewerk Perkin-Elmer & Co., Gmbh | Automatic sample feeder for flameless atomic absorption spectrometer |
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| CN102262087A (en) * | 2011-04-27 | 2011-11-30 | 杭州慕迪科技有限公司 | On-line monitoring device for total arsenic in water quality |
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| Title |
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| Optimization of instrument conditions for the analysis for mercury, arsenic, antimony and selenium by atomic absorption spectroscopy;Elisabeth Mohammed et al;《MethodsX》;20180729;第825页第1段-第828页第1段，附图1 * |
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