CN108444931A - A kind of method of arsenic content in measurement gold mine - Google Patents
A kind of method of arsenic content in measurement gold mine Download PDFInfo
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- CN108444931A CN108444931A CN201810150559.0A CN201810150559A CN108444931A CN 108444931 A CN108444931 A CN 108444931A CN 201810150559 A CN201810150559 A CN 201810150559A CN 108444931 A CN108444931 A CN 108444931A
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- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 70
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 42
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 40
- 239000010931 gold Substances 0.000 title claims abstract description 40
- 238000005259 measurement Methods 0.000 title abstract description 12
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- XGGLLRJQCZROSE-UHFFFAOYSA-K ammonium iron(iii) sulfate Chemical compound [NH4+].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGGLLRJQCZROSE-UHFFFAOYSA-K 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims description 52
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 claims description 50
- 238000010521 absorption reaction Methods 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 46
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 38
- 239000003153 chemical reaction reagent Substances 0.000 claims description 37
- 239000000523 sample Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 229910052802 copper Inorganic materials 0.000 claims description 27
- 239000010949 copper Substances 0.000 claims description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 25
- 229910000070 arsenic hydride Inorganic materials 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 18
- HBYGBTMNPMMONF-UHFFFAOYSA-N [Ag].C(Cl)(Cl)Cl Chemical compound [Ag].C(Cl)(Cl)Cl HBYGBTMNPMMONF-UHFFFAOYSA-N 0.000 claims description 16
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 11
- 238000002835 absorbance Methods 0.000 claims description 11
- 235000002906 tartaric acid Nutrition 0.000 claims description 11
- 239000011975 tartaric acid Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims description 10
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 8
- 241001411320 Eriogonum inflatum Species 0.000 claims description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 8
- 235000011150 stannous chloride Nutrition 0.000 claims description 8
- 239000001119 stannous chloride Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 6
- 229910017626 NH4Fe(SO4)2 Inorganic materials 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 5
- 239000012488 sample solution Substances 0.000 claims description 5
- 239000000779 smoke Substances 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 2
- VTUTXGYGWPTUIY-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;chloroform Chemical compound ClC(Cl)Cl.OCCN(CCO)CCO VTUTXGYGWPTUIY-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 9
- 238000011161 development Methods 0.000 abstract description 6
- 238000002798 spectrophotometry method Methods 0.000 abstract description 5
- 238000010561 standard procedure Methods 0.000 abstract description 4
- 238000003556 assay Methods 0.000 abstract description 3
- 229920002678 cellulose Polymers 0.000 abstract description 3
- 239000001913 cellulose Substances 0.000 abstract description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 abstract description 3
- 239000013558 reference substance Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 238000012795 verification Methods 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- GLVPUAWFPNGKHO-UHFFFAOYSA-L N.[Fe+2].[O-]S([O-])(=O)=O Chemical compound N.[Fe+2].[O-]S([O-])(=O)=O GLVPUAWFPNGKHO-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940000406 drug candidate Drugs 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003777 experimental drug Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (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 belongs to technical field of analytical chemistry, and in particular to a method of measuring arsenic content in gold mine；This method replaces copper sulphate in national standard method using ammonium ferric sulfate, experimental procedure is optimized simultaneously, it is poor to solve arsenic measurement result precision in national standard method, the low problem of accuracy, it ensure that the accuracy of result, and this method is easy to operate, measurement range is wide, pass through arsenogen cellulose content in determined by ultraviolet spectrophotometry gold mine, testing cost is reduced for bargh, it is really that enterprise achievees the purpose that cost efficiency, it can be widely applied to the test analysis field of arsenic content in gold mine, low-grade arsenic in gold mine industry has been pushed to measure fixed development, also technical support and guarantee are provided for bargh's analysis test.This method is suitble to arsenic content to be 0.05%~0.40% ore assay.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a method of measuring arsenic content in gold mine.
Background technology
Arsenic is a kind of poisonous and hazardous element, it is enriched in nature, in the industrial production the discharge meeting of arsenic-containing waste water
Environment is caused seriously to pollute, especially in terms of metal smelt, arsenic can corrode steel stove and pipeline, therefore, Accurate Determining ore
In arsenic content it is most important to the development of environment and industry.Currently, the common method for measuring low-grade arsenic in gold mine has：
DDTC-Ag salt spectrophotometry, atomic fluorescence spectrometry and inductively coupled plasma emission spectrography.DDTC-Ag salt is divided
Photometry measures arsenic in ore, and the ultraviolet specrophotometer used, the Instrument purchase is at low cost, test is accurate, substantially reduces survey
Cost is tried, has really achieved the purpose that be enterprise's cost efficiency, this method is high in mine popularity rate；Atomic fluorescence spectrophotometry
Method, the Instrument purchase cost is higher, and test precision is not high, and the medicine and reagent used experiment is more demanding, therefore tests
As a result accuracy is not high；Inductively coupled plasma emission spectrography, this method test is accurate, and is suitble to full elemental analysis, fits
It closes multiple elements while measuring, so the instrument is not suitable for individually measuring arsenogen cellulose content, and the Instrument purchase cost is very high, because
This is extremely low in the popularity rate of bargh.Wherein Gold Concentrate under Normal Pressure standard GB/T/T 7739.3-2007 and gold ore national standard
Have 10 years within GB/T 20899.3-2007 to 2018 years and have a surplus, method for testing and analyzing cannot fully meet industry development
Needs, the copper sulphate used in two national standards reacts with potassium iodide, causes arsenic measurement result precision poor, accurate
It spends low, the needs of industry development cannot be met, to affect the application and popularization that the analysis of gold mine middle-low grade arsenic amount measures.Cause
This research and development low cost test analysis method that precision is good and accuracy is high is extremely urgent, and assay field hair from now on
The trend of exhibition.
Invention content
In order to overcome the above problem, the present invention to provide a kind of method measuring arsenic content in gold mine, this method uses sulfuric acid
Iron ammonium replaces copper sulphate in national standard method, while being optimized to experimental procedure, solves arsenic measurement result essence in national standard method
The low problem of density contrast, accuracy, ensure that the accuracy of result, and this method is easy to operate, and measurement range is wide, by ultraviolet
Spectrophotometry measures arsenogen cellulose content in gold mine, reduces testing cost for bargh, is really that enterprise reaches drop
The purpose of this synergy can be widely applied to the test analysis field of arsenic content in gold mine, push low-grade arsenic in gold mine industry
Fixed development is measured, also provides technical support and guarantee for bargh's analysis test.This method be suitble to arsenic content be
0.05%~0.40% ore assay.
The method of arsenic content, is as follows in a kind of measurement gold mine：
It is put Step 1: the gold mine that granularity is 0.038~0.074mm is accurately weighed 0.2000g samples after crushing, drying
Into 250mL beakers, after wetting with water, 10~15mL concentrated nitric acids is added, is placed on electric furnace pan and heats 5~10min, addition 8~
15mL (1+1) sulfuric acid is heated to emitting sulfur trioxide dense smoke, and holding smokes clogging 5~10min of state, removes cooling；
Step 2: being rinsed with water wall of cup, the tartaric acid solution of a concentration of 400g/L of 5~15mL is added, heating is boiled, and making can
Soluble dissolves, and removes, is cooled to room temperature, and moves into 100mL volumetric flasks, is diluted with water to scale, mixing, volume is denoted as V0；
Take volume for V Step 3: dividing1Above-mentioned solution in 125mL arsine gas generators, 5~10mL (1+ are added
1) sulfuric acid, the tartaric acid solution of a concentration of 400g/L of 5~10mL is added after mixing, and it is molten that 2~5mL ammonium ferric sulfates are added after mixing
Liquid, after mixing plus water makes volume reach 40mL, adds the liquor kalii iodide of a concentration of 300g/L of 2~5mL after mixing, after mixing
The stannous chloride solution of a concentration of 400g/L of 2~5mL is added, places 10~15min；
Step 4: pipetting the copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL in graduated absorption tube
In, pass through the mouth bottle stopper in step 3 on arsine gas generator to enter arsenic the other side of absorption tube connecting conduit, conduit
Change in hydrogen generator, 5g arsenic-free zinc granules are added into arsine gas generator, after reacting 40min, removes absorption tube；
Liquid volume in absorption tube is set to be 10.00mL, mixing Step 5: chloroform is added into absorption tube；
Step 6: the solution in step 5 in absorption tube is moved into 1cm cuvettes, with the copper reagent silver of a concentration of 2g/L
Salt chloroform soln is that reference liquid measures absorbance at spectrophotometer wavelength 530nm, finds corresponding from working curve
Arsenic amount；
Step 7: the blank test of gold ore sample is not added according to step 1 to step 6；
Step 8: calculating the mass fraction of arsenic as follows：
In formula：
ω (As) --- the mass fraction of arsenic, %；
m1--- the arsenic amount checked in from working curve, μ g；
m2--- the arsenic amount of the companion sample blank checked in from working curve, μ g；
m0--- the quality of sample, g；
V0--- the volume of sample solution, mL；
V1--- divide the volume for taking test solution, mL；
Analysis result indicates that when mass fraction is less than 0.10%, analysis result is indicated to three small to 2 significant digits
Number.
In the step three, preparation ρ (Fe)=20g/L of ammonium ferric sulfate solution：Weigh 108g [NH4Fe(SO4)2·
2H2O], water and 10mL (1+1) H is added2SO4, after stirring and dissolving, move into 1000mL volumetric flasks, be diluted with water to scale, shake
It is even.
In the step four, the preparation of copper reagent silver salt chloroform soln (2g/L)：Weigh 1g copper reagent silver salt in
In 1000mL reagent bottle, 500mL triethanolamines-chloroform soln (3+97) is added, stirs to dissolve, static 12 hours,
It uses, is stored in brown reagent bottle after filtering.
The drafting of working curve in the step six：
Take the arsenic hydride generator of 7 125mL, be separately added into successively 0mL, l.00mL, 2.00mL, 3.00mL, 4.00mL,
The arsenic standard solution of a concentration of 5ug/mL of 5.00mL and 6.00mL, then add respectively successively into the arsenic hydride generator of 7 125mL
Enter 5~10mL (1+1) sulfuric acid, is separately added into the wine of a concentration of 400g/L of 5~10mL after mixing into 7 arsenic hydride generators again
Stone acid solution, is separately added into 2~5mL ammonium ferric sulfate solutions after mixing into 7 arsenic hydride generators again, to 7 arsenic after mixing
Change in hydrogen generator respectively plus water makes in each arsenic hydride generator liquid volume reach 40mL, again to 7 arsenic hydrides after mixing
It is separately added into the liquor kalii iodide of a concentration of 300g/L of 2~5mL in generator, distinguishes into 7 arsenic hydride generators after mixing
The stannous chloride solution of a concentration of 400g/L of 2~5mL is added, 7 arsenic hydride generators are placed into 10~15min；
The copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL is pipetted respectively in 7 graduated absorption tubes
In, 7 absorption tubes are separately connected 7 conduits, then the other side of 7 conduits is passed through into 7 arsine gas generators respectively
On mouth bottle stopper enter in arsine gas generator, then respectively into 7 arsine gas generators be added 5g arsenic-free zinc granules,
After reacting 40min, 7 absorption tubes are removed；
It is separately added into chloroform of the chloroform for supplementing volatilization into 7 absorption tubes, makes every absorption intraluminal fluid
Body volume is 10.00mL, and the solution in 7 absorption tubes is moved into 7 1cm cuvettes, with a concentration of 2g/L by mixing respectively
Copper reagent silver salt chloroform soln be that reference liquid measures absorbance in spectrophotometer wavelength 530nm at, be horizontal with arsenic amount
Coordinate, absorbance are ordinate drawing curve.
Beneficial effects of the present invention：
Invention provides a kind of method measuring arsenic content in gold mine, and this method replaces traditional test side using ammonium ferric sulfate
Copper sulphate in method, while experimental drug and step are optimized, the operational stability of test analysis is improved, ensure that result
Accuracy, and this method is easy to operate, and measurement range is wide, arsenic in determined by ultraviolet spectrophotometry gold mine, reduces testing cost,
Test accuracy is improved, achievees the purpose that cost efficiency for enterprise, can be widely applied to the test analysis neck of arsenic content in gold mine
Domain has pushed low-grade arsenic in gold mine industry to measure fixed development, also for bargh analysis test provide technical support and
It ensures.
Specific implementation mode
The invention will be further described with reference to embodiments.
The drafting of working curve：
Take the arsenic hydride generator of 7 125mL, be separately added into successively 0mL, l.00mL, 2.00mL, 3.00mL, 4.00mL,
The arsenic standard solution of a concentration of 5ug/mL of 5.00mL and 6.00mL, then add respectively successively into the arsenic hydride generator of 7 125mL
Enter 5mL (1+1) sulfuric acid, the tartaric acid for being separately added into a concentration of 400g/L of 5mL after mixing into 7 arsenic hydride generators again is molten
Liquid, is separately added into 2mL ammonium ferric sulfate solutions after mixing into 7 arsenic hydride generators again, to 7 arsenic hydride generators after mixing
It is middle to add water that liquid volume in each arsenic hydride generator is made to reach 40mL respectively, divide again into 7 arsenic hydride generators after mixing
Not Jia Ru a concentration of 300g/L of 2mL liquor kalii iodide, it is a concentration of into 7 arsenic hydride generators to be separately added into 2mL after mixing
7 arsenic hydride generators are placed 10min by the stannous chloride solution of 400g/L；
The copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL is pipetted respectively in 7 graduated absorption tubes
In, 7 absorption tubes are separately connected 7 conduits, then the other side of 7 conduits is passed through into 7 arsine gas generators respectively
On mouth bottle stopper enter in arsine gas generator, then respectively into 7 arsine gas generators be added 5g arsenic-free zinc granules,
After reacting 40min, 7 absorption tubes are removed；
It is separately added into chloroform of the chloroform for supplementing volatilization into 7 absorption tubes, makes every absorption intraluminal fluid
Body volume is 10.00mL, and the solution in 7 absorption tubes is moved into 7 1cm cuvettes, with a concentration of 2g/L by mixing respectively
Copper reagent silver salt chloroform soln be that reference liquid measures absorbance in spectrophotometer wavelength 530nm at, be horizontal with arsenic amount
Coordinate, absorbance are ordinate drawing curve.
Embodiment 1
The method of arsenic content, is as follows in a kind of measurement gold mine：
Step 1: the gold ore sample 1# that granularity is 0.038~0.074mm is accurately weighed 0.2000g after crushing, drying
Sample is put into 250mL beakers, after wetting with water, 10mL concentrated nitric acids is added, is placed on electric furnace pan and heats 5min, 8mL (1+ are added
1) sulfuric acid is heated to emitting sulfur trioxide dense smoke, and holding smokes clogging state 5min, removes cooling；
Step 2: being rinsed with water wall of cup, the tartaric acid solution of a concentration of 400g/L of 5mL is added, heating is boiled, and solubility is made
Salt dissolves, and removes, is cooled to room temperature, and moves into 100mL volumetric flasks, is diluted with water to scale, mixing, volume is denoted as V0；
Take volume for V Step 3: dividing1Above-mentioned solution in 125mL arsine gas generators, be added 5mL (1+1) sulphur
The tartaric acid solution of a concentration of 400g/L of 5mL is added after mixing for acid, is added 2mL ammonium ferric sulfate solutions after mixing, after mixing plus water
So that volume is reached 40mL, the liquor kalii iodide of a concentration of 300g/L of 2mL is added after mixing, it is a concentration of that 2mL is added after mixing
The stannous chloride solution of 400g/L places 10min；
Step 4: pipetting the copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL in graduated absorption tube
In, pass through the mouth bottle stopper in step 3 on arsine gas generator to enter arsenic the other side of absorption tube connecting conduit, conduit
Change in hydrogen generator, 5g arsenic-free zinc granules are added into arsine gas generator, after reacting 40min, removes absorption tube；
Step 5: the chloroform that chloroform is used to supplement volatilization is added into absorption tube, make liquid bulk in absorption tube
Product is 10.00mL, mixing；
Step 6: the solution in step 5 in absorption tube is moved into 1cm cuvettes, with the copper reagent silver of a concentration of 2g/L
Salt chloroform soln is that reference liquid measures absorbance at spectrophotometer wavelength 530nm, finds corresponding from working curve
Arsenic amount；
Step 7: the blank test of gold ore sample is not added according to step 1 to step 6；
Step 8: calculating the mass fraction of arsenic as follows：
In formula：
ω (As) --- the mass fraction of arsenic, %；
m1--- the arsenic amount checked in from working curve, μ g；
m2--- the arsenic amount of the companion sample blank checked in from working curve, μ g；
m0--- the quality of sample, g；
V0--- the volume of sample solution, mL；
V1--- divide the volume for taking test solution, mL；
Analysis result indicates that when mass fraction is less than 0.10%, analysis result is indicated to three small to 2 significant digits
Number.
In the step three, preparation ρ (Fe)=20g/L of ammonium ferric sulfate solution：Weigh 108g [NH4Fe(SO4)2·
2H2O], water and 10mL (1+1) H is added2SO4, after stirring and dissolving, move into 1000mL volumetric flasks, be diluted with water to scale, shake
It is even.
In the step four, the preparation of copper reagent silver salt chloroform soln (2g/L)：Weigh 1g copper reagent silver salt in
In 1000mL reagent bottle, 500mL triethanolamines-chloroform soln (3+97) is added, stirs to dissolve, static 12 hours,
It uses, is stored in brown reagent bottle after filtering.
Precision Experiment is carried out with gold ore sample, accuracy experiment, verification method are carried out using national standard reference substance
Precision and accuracy, wherein sample 1# according in embodiment 1 measurement method measure 11 times, the results are shown in Table 1, sample compiled
It number replaces the sample 1# in embodiment 1 to measure twice by the national standard reference substance of GBW 07287, the results are shown in Table
2。
1 method precision of table is tested
2 method accuracy of table is tested
Conclusion：From table 1 with table 2 as can be seen that this method precision is good and accuracy is high, this method meets test and wants
It asks.
Embodiment 2
The method of arsenic content, is as follows in a kind of measurement gold mine：
Step 1: the gold ore sample 2# that granularity is 0.038~0.074mm is accurately weighed 0.2000g after crushing, drying
Sample is put into 250mL beakers, after wetting with water, 13mL concentrated nitric acids is added, is placed on electric furnace pan and heats 8min, 10mL (1 is added
+ 1) sulfuric acid is heated to emitting sulfur trioxide dense smoke, and holding smokes clogging state 8min, removes cooling；
Step 2: being rinsed with water wall of cup, the tartaric acid solution of a concentration of 400g/L of 10mL is added, heating is boiled, made solvable
Property salt dissolving, remove, be cooled to room temperature, move into 100mL volumetric flasks in, be diluted with water to scale, mixing, volume is denoted as V0；
Take volume for V Step 3: dividing1Above-mentioned solution in 125mL arsine gas generators, be added 8mL (1+1) sulphur
The tartaric acid solution of a concentration of 400g/L of 8mL is added after mixing for acid, is added 3mL ammonium ferric sulfate solutions after mixing, after mixing plus water
So that volume is reached 40mL, the liquor kalii iodide of a concentration of 300g/L of 3mL is added after mixing, it is a concentration of that 3mL is added after mixing
The stannous chloride solution of 400g/L places 12min；
Step 4: pipetting the copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL in graduated absorption tube
In, pass through the mouth bottle stopper in step 3 on arsine gas generator to enter arsenic the other side of absorption tube connecting conduit, conduit
Change in hydrogen generator, 5g arsenic-free zinc granules are added into arsine gas generator, after reacting 40min, removes absorption tube；
Step 5: the chloroform that chloroform is used in supplement volatilization is added into absorption tube so that absorb intraluminal fluid
Body volume is 10.00mL, mixing；
Step 6: the solution in step 5 in absorption tube is moved into 1cm cuvettes, with the copper reagent silver of a concentration of 2g/L
Salt chloroform soln is that reference liquid measures absorbance at spectrophotometer wavelength 530nm, finds corresponding from working curve
Arsenic amount；
Step 7: the blank test of gold ore sample is not added according to step 1 to step 6；
Step 8: calculating the mass fraction of arsenic as follows：
In formula：
ω (As) --- the mass fraction of arsenic, %；
m1--- the arsenic amount checked in from working curve, μ g；
m2--- the arsenic amount of the companion sample blank checked in from working curve, μ g；
m0--- the quality of sample, g；
V0--- the volume of sample solution, mL；
V1--- divide the volume for taking test solution, mL；
Analysis result indicates that when mass fraction is less than 0.10%, analysis result is indicated to three small to 2 significant digits
Number.
In the step three, preparation ρ (Fe)=20g/L of ammonium ferric sulfate solution：Weigh 108g [NH4Fe(SO4)2·
2H2O], water and 10mL (1+1) H is added2SO4, after stirring and dissolving, move into 1000mL volumetric flasks, be diluted with water to scale, shake
It is even.
In the step four, the preparation of copper reagent silver salt chloroform soln (2g/L)：Weigh 1g copper reagent silver salt in
In 1000mL reagent bottle, 500mL triethanolamines-chloroform soln (3+97) is added, stirs to dissolve, static 12 hours,
It uses, is stored in brown reagent bottle after filtering.
Precision Experiment is carried out with gold ore sample, accuracy experiment, verification method are carried out using national standard reference substance
Precision and accuracy, wherein sample 2# according in embodiment 2 measurement method measure 11 times, the results are shown in Table 3, sample compiled
It number replaces the sample 2# in embodiment 2 to measure twice by the national standard reference substance of GBW 07167, the results are shown in Table
4。
3 method precision of table is tested
4 method accuracy of table is tested
Conclusion：From table 3 with table 4 as can be seen that this method precision is good and accuracy is high, this method meets test and wants
It asks.
Embodiment 3
The method of arsenic content, is as follows in a kind of measurement gold mine：
Step 1: the gold ore sample 3# that granularity is 0.038~0.074mm is accurately weighed 0.2000g after crushing, drying
Sample is put into 250mL beakers, after wetting with water, 15mL concentrated nitric acids is added, is placed on electric furnace pan and heats 10min, 15mL is added
(1+1) sulfuric acid is heated to emitting sulfur trioxide dense smoke, and holding smokes clogging state 10min, removes cooling；
Step 2: being rinsed with water wall of cup, the tartaric acid solution of a concentration of 400g/L of 15mL is added, heating is boiled, made solvable
Property salt dissolving, remove, be cooled to room temperature, move into 100mL volumetric flasks in, be diluted with water to scale, mixing, volume is denoted as V0；
Take volume for V Step 3: dividing1Above-mentioned solution in 125mL arsine gas generators, be added 10mL (1+1)
The tartaric acid solution of a concentration of 400g/L of 10mL is added after mixing for sulfuric acid, is added 5mL ammonium ferric sulfate solutions after mixing, after mixing
Add water that volume is made to reach 40mL, the liquor kalii iodide of a concentration of 300g/L of 5mL is added after mixing, 5mL concentration is added after mixing
For the stannous chloride solution of 400g/L, 15min is placed；
Step 4: pipetting the copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL in graduated absorption tube
In, pass through the mouth bottle stopper in step 3 on arsine gas generator to enter arsenic the other side of absorption tube connecting conduit, conduit
Change in hydrogen generator, 5g arsenic-free zinc granules are added into arsine gas generator, after reacting 40min, removes absorption tube；
Liquid volume in absorption tube is set to be 10.00mL, mixing Step 5: chloroform is added into absorption tube；
Step 6: the solution in step 5 in absorption tube is moved into 1cm cuvettes, with the copper reagent silver of a concentration of 2g/L
Salt chloroform soln is that reference liquid measures absorbance at spectrophotometer wavelength 530nm, finds corresponding from working curve
Arsenic amount；
Step 7: the blank test of gold ore sample is not added according to step 1 to step 6；
Step 8: calculating the mass fraction of arsenic as follows：
In formula：
ω (As) --- the mass fraction of arsenic, %；
m1--- the arsenic amount checked in from working curve, μ g；
m2--- the arsenic amount of the companion sample blank checked in from working curve, μ g；
m0--- the quality of sample, g；
V0--- the volume of sample solution, mL；
V1--- divide the volume for taking test solution, mL；
Analysis result indicates that when mass fraction is less than 0.10%, analysis result is indicated to three small to 2 significant digits
Number.
In the step three, preparation ρ (Fe)=20g/L of ammonium ferric sulfate solution：Weigh 108g [NH4Fe(SO4)2·
2H2O], water and 10mL (1+1) H is added2SO4, after stirring and dissolving, move into 1000mL volumetric flasks, be diluted with water to scale, shake
It is even.
In the step four, the preparation of copper reagent silver salt chloroform soln (2g/L)：Weigh 1g copper reagent silver salt in
In 1000mL reagent bottle, 500mL triethanolamines-chloroform soln (3+97) is added, stirs to dissolve, static 12 hours,
It uses, is stored in brown reagent bottle after filtering.
Analysis result is indicated to 2 significant digits, when mass fraction is less than 0.10%, indicates three decimals.
Precision Experiment is carried out with gold ore sample, accuracy experiment, verification method are carried out using national standard reference substance
Precision and accuracy, wherein sample 3# according in embodiment 3 measurement method measure 11 times, the results are shown in Table 5, sample compiled
It number replaces the sample 3# in embodiment 3 to measure twice by the national standard reference substance of GBW 07231, the results are shown in Table
6。
5 method precision of table is tested
6 method accuracy of table is tested
Conclusion：From table 5 with table 6 as can be seen that this method precision is good and accuracy is high, this method meets test and wants
It asks.
Claims (4)
1. a kind of method measuring arsenic content in gold mine, it is characterised in that be as follows：
It is put into Step 1: the gold mine that granularity is 0.038~0.074mm is accurately weighed 0.2000g samples after crushing, drying
In 250mL beakers, after wetting with water, 10~15mL concentrated nitric acids is added, is placed on electric furnace pan and heats 5~10min, addition 8~
15mL (1+1) sulfuric acid is heated to emitting sulfur trioxide dense smoke, and holding smokes clogging 5~10min of state, removes cooling；
Step 2: being rinsed with water wall of cup, the tartaric acid solution of a concentration of 400g/L of 5~15mL is added, heating is boiled, and solubility is made
Salt dissolves, and removes, is cooled to room temperature, and moves into 100mL volumetric flasks, is diluted with water to scale, mixing, volume is denoted as V0；
Take volume for V Step 3: dividing1Above-mentioned solution in 125mL arsine gas generators, be added 5~10mL (1+1) sulphur
The tartaric acid solution of a concentration of 400g/L of 5~10mL is added after mixing, 2~5mL ammonium ferric sulfate solutions are added after mixing, mix for acid
After even plus water makes volume reach 40mL, and the liquor kalii iodide of a concentration of 300g/L of 2~5mL is added after mixing, 2 are added after mixing
The stannous chloride solution of a concentration of 400g/L of~5mL places 10~15min；
Step 4: the copper reagent silver salt chloroform soln for pipetting a concentration of 2g/L of 10.00mL is incited somebody to action in graduated absorption tube
The other side of absorption tube connecting conduit, conduit passes through the mouth bottle stopper in step 3 on arsine gas generator to enter arsenic hydride gas
In body generator, 5g arsenic-free zinc granules are added into arsine gas generator, after reacting 40min, remove absorption tube；
Liquid volume in absorption tube is set to be 10.00mL, mixing Step 5: chloroform is added into absorption tube；
Step 6: the solution in step 5 in absorption tube is moved into 1cm cuvettes, with the copper reagent silver salt three of a concentration of 2g/L
Chloromethanes solution is that reference liquid measures absorbance at spectrophotometer wavelength 530nm, and corresponding arsenic is found from working curve
Amount；
Step 7: the blank test of gold ore sample is not added according to step 1 to step 6；
Step 8: calculating the mass fraction of arsenic as follows：
In formula：
ω (As) --- the mass fraction of arsenic, %；
m1--- the arsenic amount checked in from working curve, μ g；
m2--- the arsenic amount of the companion sample blank checked in from working curve, μ g；
m0--- the quality of sample, g；
V0--- the volume of sample solution, mL；
V1--- divide the volume for taking test solution, mL；
Analysis result indicates that when mass fraction is less than 0.10%, analysis result is indicated to three decimals to 2 significant digits.
2. according to a kind of method measuring arsenic content in gold mine shown in claim 1, it is characterised in that in the step three,
Preparation ρ (Fe)=20g/L of ammonium ferric sulfate solution：Weigh 108g [NH4Fe(SO4)2·2H2O], water and 10mL (1+1) is added
H2SO4, after stirring and dissolving, move into 1000mL volumetric flasks, be diluted with water to scale, shake up.
3. according to a kind of method measuring arsenic content in gold mine shown in claim 1, it is characterised in that in the step four,
The preparation of copper reagent silver salt chloroform soln (2g/L)：1g copper reagent silver salt is weighed in 1000mL reagent bottles, 500mL is added
Triethanolamine-chloroform soln (3+97), stirs to dissolve, and static 12 hours, is used after filtering, is stored in brown reagent
In bottle.
4. according to a kind of method measuring arsenic content in gold mine shown in claim 1, it is characterised in that in the step six
The drafting of working curve：
Take the arsenic hydride generator of 7 125mL, be separately added into successively 0mL, l.00mL, 2.00mL, 3.00mL, 4.00mL,
The arsenic standard solution of a concentration of 5ug/mL of 5.00mL and 6.00mL, then add respectively successively into the arsenic hydride generator of 7 125mL
Enter 5~10mL (1+1) sulfuric acid, is separately added into the wine of a concentration of 400g/L of 5~10mL after mixing into 7 arsenic hydride generators again
Stone acid solution, is separately added into 2~5mL ammonium ferric sulfate solutions after mixing into 7 arsenic hydride generators again, to 7 arsenic after mixing
Change in hydrogen generator respectively plus water makes in each arsenic hydride generator liquid volume reach 40mL, again to 7 arsenic hydrides after mixing
It is separately added into the liquor kalii iodide of a concentration of 300g/L of 2~5mL in generator, distinguishes into 7 arsenic hydride generators after mixing
The stannous chloride solution of a concentration of 400g/L of 2~5mL is added, 7 arsenic hydride generators are placed into 10~15min；
The copper reagent silver salt chloroform soln of a concentration of 2g/L of 10.00mL is pipetted respectively in 7 graduated absorption tubes, it will
7 absorption tubes are separately connected 7 conduits, then the mouth by the other side of 7 conduits on 7 arsine gas generators respectively
Bottle stopper enters in arsine gas generator, then 5g arsenic-free zinc granules are added into 7 arsine gas generators respectively, reaction
After 40min, 7 absorption tubes are removed；
It is separately added into chloroform of the chloroform for supplementing volatilization into 7 absorption tubes, makes liquid bulk in every absorption tube
Product is 10.00mL, and the solution in 7 absorption tubes is moved into 7 1cm cuvettes, with the copper of a concentration of 2g/L by mixing respectively
Reagent silver salt chloroform soln is that reference liquid measures absorbance at spectrophotometer wavelength 530nm, using arsenic amount as abscissa,
Absorbance is ordinate drawing curve.
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| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102077060A (en) * | 2008-06-04 | 2011-05-25 | G·帕特尔 | A monitoring system based on etching of metals |
| CN107421947A (en) * | 2017-09-25 | 2017-12-01 | 长春黄金研究院 | A kind of method of arsenic content in measure gold mine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102077060A (en) * | 2008-06-04 | 2011-05-25 | G·帕特尔 | A monitoring system based on etching of metals |
| CN107421947A (en) * | 2017-09-25 | 2017-12-01 | 长春黄金研究院 | A kind of method of arsenic content in measure gold mine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
| CN110220856B (en) * | 2019-06-05 | 2021-07-27 | 常州大学 | Method for detecting content of chloride ions in electrodeposition liquid of electrolytic copper foil by flow injection method |
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Application publication date: 20180824 |