CN102288605A - Method for rapidly determining iron content in concentrated sulphuric acid - Google Patents
Method for rapidly determining iron content in concentrated sulphuric acid Download PDFInfo
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- CN102288605A CN102288605A CN 201110245975 CN201110245975A CN102288605A CN 102288605 A CN102288605 A CN 102288605A CN 201110245975 CN201110245975 CN 201110245975 CN 201110245975 A CN201110245975 A CN 201110245975A CN 102288605 A CN102288605 A CN 102288605A
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- Prior art keywords
- sulphuric acid
- iron
- volume
- solution
- concentrated sulphuric
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 235000011149 sulphuric acid Nutrition 0.000 title claims abstract description 22
- 239000001117 sulphuric acid Substances 0.000 title claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 25
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000012086 standard solution Substances 0.000 claims abstract description 23
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000003556 assay Methods 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000006467 substitution reaction Methods 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- 239000003086 colorant Substances 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for rapidly determining iron content in concentrated sulphuric acid, comprising the following steps of: firstly absorbing 20-25ml analytically pure sulphuric acid, diluting the sulphuric acid into four times of the original volume according to volume ratio, then cooling and pouring the sulphuric acid into a 100ml measuring flask by virtue of a constant volume process, absorbing 25ml of the diluted sulphuric acid into a colorimetric cylinder, and adding 1-3ml of analytically pure nitric acid solution 1+1 and 3-6ml of ammonium thiocyanate solution with the weight concentration of 10-20%, plugging a cover of the colorimetric cylinder, and shaking well; meanwhile, carrying out a blank test in another colorimetric cylinder, adding iron (III) standard solution into the blank colorimetric cylinder to cause the colours in the two colorimetric cylinders to be the same, writing down volume the consumed iron standard solution, and substituting the volume into a formula to calculate the iron content in the concentrated sulphuric acid. The method disclosed by the invention is simple and feasible and has short determination time.
Description
Technical field
The present invention relates to the assay method of impurity in the chemicals, be specifically related to the assay method of lead-acid accumulator with iron content in the analytical pure sulfuric acid.
Background technology
Lead-acid accumulator requires very strict to its impurity content, general producer all uses and analyzes other sulfuric acid preparation electrolytic solution of pure level.In the sulfuric acid quality index, iron content is a very important index, all will measure (therefore the concentrated sulphuric acid mainly is meant iron (III) ion determination because strong oxidizing property contains iron (II) ion hardly) before use.At present, in GB GB/T 625-2007, its analytical approach is a colorimetric behind the employing evaporate to dryness, the defective that exists is: the time consuming time is long, and produce a large amount of acid mists in the process of evaporate to dryness, the ventilation effect of ventilating kitchen is required than higher, run into emergency case such as power failure and adopt this method can't carry out at all, the normal appearance can not in time be quoted the situation that influences production because of analysis result.
Summary of the invention
Purpose of the present invention just provides iron content rapid assay methods in a kind of concentrated sulphuric acid, and this method is simple, and minute is short.
The object of the present invention is achieved like this:
Iron content rapid assay methods in the concentrated sulphuric acid, comprise the following steps: to draw earlier the 20-25mL analytical pure sulfuric acid, be diluted to original four times by volume, cooling then, constant volume is in 100 mL volumetric flasks, volume 25mL after the absorption dilution is in color comparison tube, add again that 1-3mL analyzes pure salpeter solution: 1+1 and the 3-6mL weight concentration is the 10-20% ammonium thiocyanate solution, the lid of jam-pack color comparison tube, shake up, simultaneously in the another color comparison tube, do blank test, in blank color comparison tube, add iron (III) standard solution, make in two color comparison tubes color identical, write down consume the volume number of iron standard solution, calculate the iron content in the concentrated sulphuric acid in the substitution formula.
Described iron (III) standard solution is 0.01mg/ mL.
The concentrated sulphuric acid is after dilution, its solution is used the nitric acid acidifying again, because the thiocyanate ion must could be followed iron (III) ion forming complex under certain acidity, utilize sulphur cryanide ion and iron (III) ion to form this character of sanguine coordination compound then, carry out colorimetric estimation.
Comparatively speaking the method for stipulating among this method and the GB/T 625-2007 all is visual colorimetry, and the result is accurately and reliably the same, and advantage is: do not need to use well heater, also can test under situation about having a power failure; Can not produce a large amount of acid mists, can operate yet in simple and crude laboratory; And operating process weak point consuming time.
Embodiment:
Embodiment 1
The reagent preparation
Salpeter solution (analyzing pure): 1+1,
Ammonium thiocyanate solution (analyzing pure): the 15%(weight concentration),
Iron (III) standard solution: 0.01mg/ mL.
Draw and analyze pure (density is 1.84 Ke ∕ ml) concentrated sulphuric acid 22mL, put into the beaker that fills 50 mL pure water, be placed in the chilled water, be transferred to after the cooling in the 100mL volumetric flask, constant volume is to scale, draw 25mL in the 50mL color comparison tube, add 1 mL salpeter solution, 5mL ammonium thiocyanate solution, jam-pack color comparison tube, shake up, leave standstill.In another color comparison tube, add 1 mL salpeter solution simultaneously, the 5mL ammonium thiocyanate solution, it is concordant to both liquid levels to add entry, with 1 mL pipette, extract ferric iron standard solution, add in the blank contrast pipe, color is the same to two color comparison tubes, writes down ferric iron volume that standard solution consumes.
Result's expression and calculating
Iron content is calculated as follows in massfraction X:
In the formula: C is iron (III) concentration of standard solution, the mg/ml of unit
V is consumed volume, unit/ml by iron (III) standard solution
Calculate that the iron-holder mass percent is 0.00003% in the concentrated sulphuric acid.
Embodiment 2
The reagent preparation
Salpeter solution (analyzing pure): 1+1,
Ammonium thiocyanate solution (analyzing pure): the 20%(weight concentration),
Iron (III) standard solution: 0.01mg/ mL.
Draw and analyze pure (density is 1.84 Ke ∕ ml) concentrated sulphuric acid 22mL, put into the beaker that fills 50 mL pure water, be placed in the chilled water, be transferred to after the cooling in the 100mL volumetric flask, constant volume is to scale, draw 25mL in the 50mL color comparison tube, add the 2mL salpeter solution, 4 mL ammonium thiocyanate solutions, jam-pack color comparison tube, shake up, leave standstill.In another color comparison tube (blank contrast), add the 2mL salpeter solution simultaneously, 4 mL ammonium thiocyanate solutions, it is concordant to both liquid levels to add entry, with 1 mL pipette, extract ferric iron standard solution, add in the blank contrast pipe, color is the same to two color comparison tubes, writes down ferric iron volume that standard solution consumes.
Result's expression and calculating
Iron content is calculated as follows in massfraction X:
In the formula: C is iron (III) concentration of standard solution, the mg/ml of unit
V is consumed volume, unit/ml by iron (III) standard solution
Calculate that the iron-holder mass percent is 0.00003% in the concentrated sulphuric acid.
Embodiment 3
The reagent preparation
Salpeter solution (analyzing pure): 1+1,
Ammonium thiocyanate solution (analyzing pure): the 10%(weight concentration),
Iron (III) standard solution: 0.01mg/ mL.
Draw and analyze pure (density is 1.84 Ke ∕ ml) concentrated sulphuric acid 22mL, put into the beaker that fills 50 mL pure water, be placed in the chilled water, be transferred to after the cooling in the 100mL volumetric flask, constant volume is to scale, draw 25mL in the 50mL color comparison tube, add the 1mL salpeter solution, 6 mL ammonium thiocyanate solutions, jam-pack color comparison tube, shake up, leave standstill.In another color comparison tube (blank contrast), add the 1mL salpeter solution simultaneously, 6 mL ammonium thiocyanate solutions, it is concordant to both liquid levels to add entry, with 1 mL pipette, extract ferric iron standard solution, add in the blank contrast pipe, color is the same to two color comparison tubes, writes down ferric iron volume that standard solution consumes.
Result's expression and calculating
Iron content is calculated as follows in massfraction X:
In the formula: C is iron (III) concentration of standard solution, the mg/ml of unit
V is consumed volume, unit/ml by iron (III) standard solution
Calculate that the iron-holder mass percent is 0.00003% in the concentrated sulphuric acid.
Claims (2)
1. iron content rapid assay methods in the concentrated sulphuric acid, it is characterized in that comprising the following steps: drawing earlier the 20-25mL analytical pure sulfuric acid, be diluted to original four times by volume, cooling then, constant volume is in 100 mL volumetric flasks, volume 25mL after the absorption dilution is in color comparison tube, add again that 1-3mL analyzes pure salpeter solution: 1+1 and the 3-6mL weight concentration is the 10-20% ammonium thiocyanate solution, the lid of jam-pack color comparison tube, shake up, simultaneously in the another color comparison tube, do blank test, in blank color comparison tube, add iron (III) standard solution, make in two color comparison tubes color identical, write down consume the volume number of iron standard solution, calculate the iron content in the concentrated sulphuric acid in the substitution formula.
2. iron content rapid assay methods in a kind of concentrated sulphuric acid as claimed in claim 1 is characterized in that: iron (III) standard solution is 0.01mg/ mL.
Priority Applications (1)
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| CN 201110245975 CN102288605A (en) | 2011-08-25 | 2011-08-25 | Method for rapidly determining iron content in concentrated sulphuric acid |
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| CN 201110245975 CN102288605A (en) | 2011-08-25 | 2011-08-25 | Method for rapidly determining iron content in concentrated sulphuric acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590202A (en) * | 2012-02-17 | 2012-07-18 | 天津市捷威动力工业有限公司 | Measuring method of iron |
| CN102967600A (en) * | 2012-11-26 | 2013-03-13 | 宜宾海丝特纤维有限责任公司 | Method for detecting content of ion in sodium hydroxide solution in viscose |
| CN103712977A (en) * | 2012-09-29 | 2014-04-09 | 天能电池(芜湖)有限公司 | Detection method for lead paste ingredient of negative plate of lead-acid storage battery |
| CN104792717A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting iron content in metallic ores |
| CN107290491A (en) * | 2017-08-02 | 2017-10-24 | 广州检验检测认证集团有限公司 | The method that a kind of endpoint device and judgement based on polyfluortetraethylene pipe deep hole Wet clear up terminal |
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| CN101821008A (en) * | 2007-08-14 | 2010-09-01 | 通用电气公司 | Goods, apparatus and method |
| CN102004084A (en) * | 2010-11-17 | 2011-04-06 | 武汉理工大学 | Method for measuring contents of ferrous ions and iron ions in glass |
| CN102353642A (en) * | 2011-07-14 | 2012-02-15 | 东北大学 | Determination method for cobalt content in high-copper high-iron cobalt ores |
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2011
- 2011-08-25 CN CN 201110245975 patent/CN102288605A/en active Pending
Patent Citations (5)
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| CN101062767A (en) * | 2007-04-16 | 2007-10-31 | 邓金玲 | Environment protection method of handling industrial abandoned phosphorized liquid |
| CN101821008A (en) * | 2007-08-14 | 2010-09-01 | 通用电气公司 | Goods, apparatus and method |
| CN101614727A (en) * | 2008-06-25 | 2009-12-30 | 河南新天地药业有限公司 | D-(-)-to hydroxyl-α (3-methoxyl-1-methyl-3-oxo-propenyl) aminoacetic acid potassium detection technique |
| CN102004084A (en) * | 2010-11-17 | 2011-04-06 | 武汉理工大学 | Method for measuring contents of ferrous ions and iron ions in glass |
| CN102353642A (en) * | 2011-07-14 | 2012-02-15 | 东北大学 | Determination method for cobalt content in high-copper high-iron cobalt ores |
Non-Patent Citations (1)
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| 《化学世界》 19821231 刘栋梁 硫代硫酸钠中铁的快速测定 , * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590202A (en) * | 2012-02-17 | 2012-07-18 | 天津市捷威动力工业有限公司 | Measuring method of iron |
| CN102590202B (en) * | 2012-02-17 | 2014-06-04 | 天津市捷威动力工业有限公司 | Measuring method of iron |
| CN103712977A (en) * | 2012-09-29 | 2014-04-09 | 天能电池(芜湖)有限公司 | Detection method for lead paste ingredient of negative plate of lead-acid storage battery |
| CN102967600A (en) * | 2012-11-26 | 2013-03-13 | 宜宾海丝特纤维有限责任公司 | Method for detecting content of ion in sodium hydroxide solution in viscose |
| CN104792717A (en) * | 2015-05-05 | 2015-07-22 | 梧州市产品质量检验所 | Method of detecting iron content in metallic ores |
| CN107290491A (en) * | 2017-08-02 | 2017-10-24 | 广州检验检测认证集团有限公司 | The method that a kind of endpoint device and judgement based on polyfluortetraethylene pipe deep hole Wet clear up terminal |
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Application publication date: 20111221 |