CN101788495A - Method for measuring arsenic by iodine solution absorption method - Google Patents
Method for measuring arsenic by iodine solution absorption method Download PDFInfo
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- CN101788495A CN101788495A CN201010103727A CN201010103727A CN101788495A CN 101788495 A CN101788495 A CN 101788495A CN 201010103727 A CN201010103727 A CN 201010103727A CN 201010103727 A CN201010103727 A CN 201010103727A CN 101788495 A CN101788495 A CN 101788495A
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Abstract
The invention discloses an accurate and reliable method for measuring arsenic by an iodine solution absorption method, which solves the problem that the traditional method produces poisonous waste liquor. In a H2SO4 medium greater than 3.6N, Zn reacts with an acid to produce nascent activated hydrogen; in the presence of KI and acidic SnCl2, As<5+> is reduced into As<3+>, and the trivalent arsenic reacts with the nascent activated hydrogen to produce hydrogen arsenide gas; and the hydrogen arsenide gas is absorbed by an iodine solution and is oxidized into quinquevalent arsenic. In a 0.25 equivalent sulfuric acid medium, the quinquevalent arsenic reacts with ammonium molybdate to produce yellow heteromolybdoarsenic acid. The heteromolybdoarsenic acid is reduced into arsenic molybdenum blue by hydrazine sulfatefor for colorimetric determination. The method for measuring arsenic by iodine solution absorption and the colorimetric determination of the arsenic molybdenum blue is more suitable for the analysis of As in raw materials for copper smelting and semi-finished products of matte anode copper; moreover, the use of poisonous and hazardous reagents is avoided, and environment pollution is reduced.
Description
Technical field
The present invention relates to the analytical approach of arsenic element in copper concentrate, anode copper, the matte.
Background technology
Prior art uses the toluene method of extraction to measure the arsenic of raw material and intermediate material all the time, uses the content of arsenic in DDTC-Ag Their Determination by Spectrophotometry blister copper, the anode copper.But this method needs to use virose chemical reagent (toluene, methenyl choloride) throughout the year, virose reagent causes very big influence to health of operators in the analytic process, and annual poisonous toluene waste liquid 36000ml, the methenyl choloride waste liquid 12000ml of producing.Though through relevant department approval, waste liquid is by burying processing, will cause to a certain degree pollution to environment.
The assay method of micro amount of arsenic need be used atomic fluorescence spectrometer in the aluminium ingot, does carrier gas with argon gas, measures the gaseous state arsonium.Belong to instrumental analysis.The mensuration of arsenic is the amino-acid compound that rapid analysis method is used in the water, the pH value correctives.
Summary of the invention
The object of the present invention is to provide a kind of method of the absorptionmetric determination of iodine solution accurately and reliably arsenic, solve the problem of the generation of the existing poisonous waste liquid of method.
The method of iodine solution absorptionmetric determination arsenic of the present invention, step is as follows: in containing 250 milliliters of conical beakers of arsenic test solution, 50 milliliters of adding distil waters, add 15ml sulfuric acid, add reductive agent potassium iodide 2-7ml, mixing adds reductive agent stannous chloride 0.5-3ml, shakes up, be reduced to yellow the disappearance, add screening agent tartrate 5-7ml, shake up, place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 40-50 minute; Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drip 2 reductive agent sodium sulphites, shake yellow is taken off, add developer ammonium molybdate 0.6-1 milliliter, shake up, add reductive agent four 1-5 milliliters, shake up, be diluted with water to scale, shake up in boiling water bath and heated 10-20 minute, take off cooling, with 1 centimetre of cuvette, with the reagent blank is reference, measures absorbance in spectrophotometer 680-840nm place; Absorption liquid is selected from a kind of in iodine solution or the bromine water, and reductive agent four is selected from a kind of in sulfuric acid diammonium, ascorbic acid or the stannous chloride.
The consumption of potassium iodide is preferably 5ml, and the consumption of stannous chloride is preferably 0.5ml, and tartaric consumption is preferably 5ml, and the consumption of developer ammonium molybdate is preferably 0.6 milliliter, and the consumption of reductive agent four is preferably 3 milliliters.
The present invention is achieved in that greater than 3.6N H
2SO
4In the medium, Zn produces nascent state activation hydrogen with the acid effect, at KI and acid SnCl
2Exist down, make As
5+Be reduced into As
3+, the activation hydrogen of trivalent arsenic and nascent state generates arsine gas, is absorbed by iodine solution, and be oxidized to pentavalent arsenic, in 0.25 equivalent sulfuric acid medium, pentavalent arsenic and ammonium molybdate generate yellow arsenic molybdenum heteropolyacid, with the sulfuric acid diammonium it are reduced into the arsenic molybdenum blue and carry out colorimetric estimation.
Arsenic is the harmful element in the copper smelting process, expects that from former each flow process of smelting all has strict demand and control to the content of arsenic.The inventive method iodine solution absorbs with the arsenic molybdenum blue colorimetric method measures arsenic, is more suitable for the analysis of As in raw material that copper smelts and semi-manufacture matte, the anode copper, and has avoided the use of poisonous and harmful reagent, has reduced environmental pollution.
Degree reaching former analytical approach aspect the accuracy of analytical approach, the precision has satisfied our factory raw material and half-finished content range, satisfies to produce actually, and to energy-saving and cost-reducing, occupational health safety, environmental protection have positive effect.
Economic benefit: according to market price measuring and calculating, adopt iodine solution absorptionmetric determination arsenic to measure arsenic than toluene extraction, each sample can be saved 1.54 yuan of reagent expenses.
579 * 1.54=890 unit
Environmental benefit:
1. toluene in use damages chemical examination worker health, makes that the people feels to feel sick, dizziness, and central nervous system is played anesthetic action, contacts the infringement that a certain amount of benzene can cause neurasthenia syndrome and hemopoietic system for a long time.
2. toluene waste liquid toxicity is very big, and is if arbitrarily stack, volatile; Surrounding environment is polluted.
3. though,, also will cause to a certain degree pollution to burying the soil because of the soil can't decompose, regenerate it through burying.
Embodiment
The following examples can further specify the present invention, but do not limit the present invention in any way.
The collocation method of reagent is as follows:
Sulfuric acid (1+1); Measure 100ml distilled water and under constantly stirring, add the 100ml concentrated sulphuric acid.
Potassium iodide (300g/l): take by weighing potassium iodide 300g in 600ml distilled water, dissolving fully the back with distilled water diluting to 100ml.Stannous chloride (200g/l): take by weighing the 20g stannous chloride and be dissolved in the 20ml concentrated hydrochloric acid, dissolving fully the back with distilled water diluting to 100ml.
Tartrate (500g/l): take by weighing 50g tartrate and be dissolved in the 100ml distilled water.
Iodine solution (2g/l): take by weighing 2g iodine, the 4g potassium iodide is dissolved in the 1000ml distilled water.
Sodium sulphite (100g/l): take by weighing the 10g sodium sulphite and be dissolved in the 100ml distilled water.
Ammonium molybdate (23g/l): take by weighing the 23g ammonium molybdate and be dissolved in (in 276ml sulfuric acid+400ml water), be diluted with water to 1000ml.
Sulfuric acid hydrazine (3g/l): take by weighing 0.3g sulfuric acid hydrazine and be dissolved in the 100ml distilled water.
In 250 milliliters of conical beakers that contain the arsenic test solution, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, 300g/l potassium iodide 5ml, and mixing adds 200g/l stannous chloride solution 0.5ml, shakes up, and is reduced to yellow the disappearance, adds 500g/l tartrate 5ml, shakes up.Place 10min, add arsenic-free zinc granule 4 grams, have the gas conduit and the conduit other end rapidly beyond the Great Wall and inserted in 25 milliliters of color comparison tubes that fill 10ml iodine solution (2g/l) in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 100g/l sodium sulfite solutions, shake yellow is taken off, add 0.6 milliliter of 23g/l ammonium molybdate solution, shake up, add 3 milliliters of 3g/l hydrazine sulfate solution, shake up, be diluted with water to scale, shake up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.
Embodiment 1
Get the copper concentrate sample, accurately take by weighing 0.5000 gram sample, in 100 ml beakers, add 15 milliliters of (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds stannous chloride solution 0.5ml, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.
The mean value of arsenic content is 0.15% in 10 working samples, standard deviation 0.010, and the coefficient of variation is 6.67%.
Reference examples 1
Take by weighing 5 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 5ml, 10ml, 15ml, 20ml, 25ml (1+1) sulfuric acid respectively, add liquor kalii iodide 5ml, mixing adds 0.5ml stannous chloride solution, shakes up, be reduced to yellow the disappearance, tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of hydrazine sulfate solution, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table one:
Table one acidity of sulfuric acid is to generating the influence of arsine gas
| The amount (ml) that adds (1+1) sulfuric acid | ??5 | ??10 | ??15 | ??20 | ??25 |
| The absorbance of arsenic | ??0.176 | ??0.189 | ??0.249 | ??0.248 | ??0.245 |
As can be seen when (1+1) sulfuric acid during greater than 15ml, absorbance tends towards stability by table one, and the present invention adopts 15ml addition effect best.
Embodiment 2-embodiment 6
Take by weighing 5 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, add 3ml, 4ml, 5ml, 6ml, 7ml liquor kalii iodide respectively, mixing adds stannous chloride solution 0.5ml, shakes up, be reduced to yellow the disappearance, tartarize 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table two
Table two potassium iodide is to generating the influence of arsine gas
| Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| The amount (ml) that adds (300g/l) potassium iodide | ??3 | ??4 | ??5 | ??6 | ??7 |
| Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| The absorbance of arsenic | ??0.170 | ??0.227 | ??0.381 | ??0.376 | ??0.375 |
As can be seen when potassium iodide is 5ml, absorbance is the highest by table two, and the present invention adopts 5ml addition effect best.
Embodiment 7-embodiment 9, reference examples 2-reference examples 3
Take by weighing 5 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, mixing adds 0.5ml, 1ml, 2ml, 4ml, 5ml stannous chloride solution respectively, shakes up, be reduced to yellow the disappearance, tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.
Its experiment the results are shown in Table three
Table three stannous chloride consumption is to generating the influence of arsine gas
| Embodiment 7 | Embodiment 8 | Embodiment 9 | Reference examples 2 | Reference examples 3 | |
| Add (200g/l) stannous chloride (ml) | ??0.5 | ??1 | ??2 | ??4 | ??5 |
| The absorbance of arsenic | ??0.409 | ??0.345 | ??0.331 | ??0.249 | ??0.241 |
By table three as can be seen when the consumption of stannous chloride is 0.5ml, the absorbance maximum that records, so the present invention adopts 0.5ml addition effect best.
Embodiment 10-embodiment 11, reference examples 4
Take by weighing 3 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, mixing adds 0.5ml stannous chloride solution, shakes up, be reduced to yellow the disappearance, add 3ml, 5ml, 7ml tartaric acid solution respectively, shake up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table four
Table four tartrate consumption is to generating the influence of arsine gas
| Reference examples 4 | Embodiment 10 | Embodiment 11 | |
| Add (500g/l) tartrate (ml) | ??3 | ??5 | ??7 |
| The absorbance of arsenic | ??0.280 | ??0.340 | ??0.337 |
As can be seen when tartaric consumption during greater than 5ml, the absorbance that records tends towards stability, so the present invention adopts 5ml addition effect best by table four.
Embodiment 12-embodiment 13, reference examples 5-reference examples 6
Take by weighing 4 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 20,30,40,50 minutes respectively.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table five
Table five soak time is to generating the influence of arsine gas
| Reference examples 5 | Reference examples 6 | Embodiment 12 | Embodiment 13 | |
| Soak time (minute) | ??20 | ??30 | ??40 | ??50 |
| The absorbance of arsenic | ??0.113 | ??0.129 | ??0.140 | ??0.139 |
Can absorb during greater than 40 minutes fully when soak time as can be seen by table five, so the present invention adopts, and to absorb 45 minutes effects best.
Embodiment 14-embodiment 15, reference examples 7-reference examples 9
Take by weighing 5 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, add 0.6ml, 1ml, 2.5ml, 4ml, 5ml ammonium molybdate solution respectively, shake up, add 3 milliliters of sulfuric acid hydrazine solutions, shake up, be diluted with water to scale, shake up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table six
Table six developer and acidity are to generating the influence of arsenic molybdenum blue
| Embodiment 14 | Embodiment 15 | Reference examples 7 | Reference examples 8 | Reference examples 9 | |
| The amount (ml) that adds (23g/l) ammonium molybdate | ??0.6 | ??1 | ??2.5 | ??4 | ??5 |
| The absorbance of arsenic | ??0.172 | ??0.156 | ??0.101 | ??0.024 | ??/ |
As can be seen when the consumption of ammonium molybdate during greater than 0.6ml, the absorbance that records begins to reduce, so the present invention adopts 0.6ml addition effect best by table six.
Embodiment 16-embodiment 18,
Take by weighing 3 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shake yellow is taken off, add 0.6 milliliter of ammonium molybdate solution, shake up, add 1ml, 3ml, 5ml sulfuric acid hydrazine solution respectively, shake up, be diluted with water to scale, shake up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table seven
Table seven reductive agent consumption is to generating the influence of arsenic molybdenum blue
| Embodiment 16 | Embodiment 17 | Embodiment 18 | |
| The amount (ml) that adds (0.3%) sulfuric acid hydrazine | ??1 | ??3 | ??5 |
| The absorbance of arsenic | ??0.173 | ??0.186 | ??0.185 |
As can be seen when the consumption of sulfuric acid hydrazine during greater than 3ml, the absorbance that records tends towards stability, so the present invention adopts 3ml addition effect best by table seven.
Embodiment 19-embodiment 21, reference examples 10-reference examples 12
Take by weighing 6 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Respectively at heating in the boiling water bath 1,3,5,10,15,20 minute, take off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table eight
The table eight water-bath time is to generating the influence of arsenic molybdenum blue
| Reference examples 10 | Reference examples 11 | Reference examples 12 | Embodiment 19 | Embodiment 20 | Embodiment 21 | |
| The water-bath time (minute) | ??1 | ??3 | ??5 | ??10 | ??15 | ??20 |
| The absorbance of arsenic | ??0.039 | ??0.090 | ??0.102 | ??0.124 | ??0.138 | ??0.135 |
By table eight as can be seen when the water-bath time is 15 minutes, the absorbance maximum that records, so the present invention adopts 15 minutes effects best.
Embodiment 22-embodiment 27, reference examples 13
Take by weighing 2 parts on the different 0.5000g samples of high low content, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance respectively at spectrophotometer 680nm, 693nm, 700nm, 720nm, 750nm, 840nm, 866nm place.Its experiment the results are shown in Table nine
Table nine wavelength is to the influence of arsenic molybdenum blue absorbance
| Embodiment 22 | Embodiment 23 | Embodiment 24 | Embodiment 25 | Embodiment 26 | Embodiment 27 | Reference examples 13 | |
| Wavelength (nm) | ??680 | ??693 | ??700 | ??720 | ??750 | ??840 | ??866 |
| Embodiment 22 | Embodiment 23 | Embodiment 24 | Embodiment 25 | Embodiment 26 | Embodiment 27 | Reference examples 13 | |
| The absorbance of 1# sample arsenic | ??0.597 | ??0.625 | ??0.64 | ??0.692 | ??0.819 | ??1.262 | ??1.0681 |
| The absorbance of 2# sample arsenic | ??0.077 | ??0.080 | ??0.082 | ??0.089 | ??0.104 | ??0.162 | ??0.135 |
By table nine as can be seen wavelength at 840nm, the absorbance maximum that records, but consider to take into account the high, normal, basic content of sample, so the present invention adopts 720nm place measurement effect best.
Embodiment 28-embodiment 30
Take by weighing 3 parts on 0.5000g sample, place 100 ml beakers respectively, add 15ml (1+1) sulfuric acid, 5 milliliters of nitric acid cover the table ware, and 100-200 ℃ of dissolving steamed to just emitting the sulfuric acid cigarette, takes off cooling.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Move in the 100ml volumetric flask.Divide and get an amount of test solution in 250 milliliters of conical beakers, 50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shake yellow is taken off, add 0.6 milliliter of ammonium molybdate solution, shake up, add 3 milliliters of sulfuric acid hydrazine solutions respectively, 100g/l ascorbic acid solution 1ml, 10% stannous chloride solution 0.5ml shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Its experiment the results are shown in Table ten:
Three kinds of reductive agent contrasts of table ten
| Embodiment 28 | Embodiment 29 | Embodiment 30 | |
| The reductive agent title | The sulfuric acid hydrazine | Ascorbic acid | Stannous chloride |
| The absorbance of arsenic | ??0.185 | ??0.179 | ??0.175 |
Embodiment 31 accurately takes by weighing four parts on 3.0000 certain sample of gram, in 500 milliliters of conical beakers, adds (1+1) nitric acid 40ml, covers the table ware, and 100-200 ℃ is heated to dissolving fully, moves in the 500ml volumetric flask.Divide respectively and get the 10ml test solution in 100 ml beakers, in wherein adding certain arsenic titer respectively in three parts of test solutions, add 15 milliliters of (1+1) sulfuric acid, cover the table ware, 100-200 ℃ of steaming taken off cooling to just emitting the sulfuric acid cigarette.Washing table ware and wall of cup do not cover the table ware, and 100-200 ℃ is heated to and just emits the sulfuric acid cigarette again, takes off cooling.Wash in 250 milliliters of conical beakers.50 milliliters of adding distil waters add 15ml (1+1) sulfuric acid, liquor kalii iodide 5ml, and mixing adds 0.5ml stannous chloride solution, shakes up, and is reduced to yellow the disappearance, and tartarize solution 5ml shakes up.Place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 45 minutes.Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drips 2 sodium sulfite solutions, shakes yellow is taken off, and adds 0.6 milliliter of ammonium molybdate solution, shakes up, and adds 3 milliliters of sulfuric acid hydrazine solutions, shakes up, and is diluted with water to scale, shakes up.Heating is 15 minutes in boiling water bath, takes off cooling.With 1 centimetre of cuvette, be reference with the reagent blank, measure absorbance in spectrophotometer 720nm place.Analysis result sees Table 11.
Table ten mark-on reclaims experiment
Test as can be seen by mark-on that this method has high accuracy, can satisfy the microanalysis of arsenic fully.
Claims (2)
1. the method for an iodine solution absorptionmetric determination arsenic, it is characterized in that: in containing 250 milliliters of conical beakers of arsenic test solution, 50 milliliters of adding distil waters, add 15ml sulfuric acid, add reductive agent potassium iodide 2-7ml, mixing adds reductive agent stannous chloride 0.5-3ml, shakes up, be reduced to yellow the disappearance, add screening agent tartrate 5-7ml, shake up, place 10min, add arsenic-free zinc granule 4 grams, fill in rapidly and have gas conduit and the conduit other end has inserted in 25 milliliters of color comparison tubes that fill the 10ml absorption liquid in advance, the jam-pack bottle stopper absorbs 40-50 minute; Take off color comparison tube, clean catheter tip with distilled water, solution is incorporated in the color comparison tube, drip 2 reductive agent sodium sulphites, shake yellow is taken off, add developer ammonium molybdate 0.6-1 milliliter, shake up, add reductive agent four 1-5 milliliters, shake up, be diluted with water to scale, shake up in boiling water bath and heated 10-20 minute, take off cooling, with 1 centimetre of cuvette, with the reagent blank is reference, measures absorbance in spectrophotometer 680-840nm place; Absorption liquid is selected from a kind of in iodine solution or the bromine water, and reductive agent four is selected from a kind of in sulfuric acid diammonium, ascorbic acid or the stannous chloride.
2. the method for iodine solution absorptionmetric determination arsenic according to claim 1, it is characterized in that: the consumption of described potassium iodide is 5ml, and the consumption of stannous chloride is 0.5ml, and tartaric consumption is 5ml, the consumption of developer ammonium molybdate is 0.6 milliliter, and the consumption of reductive agent four is 3 milliliters.
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| ITRM20110349A1 (en) * | 2011-07-04 | 2013-01-05 | Pompeo Moscetta | PROCEDURE AND APPARATUS FOR DETERMINATION OF ARSENIC IN LIQUID SAMPLES. |
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| US5330917A (en) * | 1989-02-02 | 1994-07-19 | Hybrivet Systems, Inc. | Test swab device and method of detecting lead, mercury, arsenic, and bismuth |
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| ITRM20110349A1 (en) * | 2011-07-04 | 2013-01-05 | Pompeo Moscetta | PROCEDURE AND APPARATUS FOR DETERMINATION OF ARSENIC IN LIQUID SAMPLES. |
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| CN114216948A (en) * | 2021-11-01 | 2022-03-22 | 佛山科学技术学院 | Electrochemical method for detecting arsenic ions in solution |
| CN114216948B (en) * | 2021-11-01 | 2023-09-26 | 佛山科学技术学院 | Electrochemical method for detecting arsenic ions in solution |
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