CN108037237A - The method of Zn content in EDTA volumetric determination zinc ores - Google Patents
The method of Zn content in EDTA volumetric determination zinc ores Download PDFInfo
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Abstract
The method of Zn content in EDTA volumetric determination zinc ores, by zinc ore sample hydrochloric acid, nitric acid and sulfuric acid dissolution, the coexistence elements such as iron of precipitation separation, manganese, lead, the interference of the elements such as screening agent masking iron, aluminium, silicon, copper is added in filtrate, in ethyl sodium solution, glassy yellow is titrated to EDTA standard solution, the content of Zn is calculated according to the dosage of the EDTA of consumption.The simple inexpensive, detection of agents useful for same of the present invention it is time-consuming it is short, cost is low, testing result is accurate.
Description
Technical field
The invention belongs to the sample ore analysis method technical field of industry such as dig up mine, smelt, and in particular to zinc contains in zinc ore
The assay method of amount.
Background technology
The zinc ore in China is generally with lead symbiosis, therefore referred to as Pb-Zn deposits, the place of production spread all over the country, accurate to analyze zinc in zinc ore
Content, is conducive to the selecting to zinc ore, reduces the consumption of the energy, improves productivity effect.At present in zinc ore zinc detection side
Method has flame atomic absorption spectrophotometer detection method and EDT volumetric methods.Flame atomic absorption spectrophotometer detection method is used
Aqua regia dissolution sample, with the zinc titer of authorized by state be configured to respectively 0.00ml, 1.00ml, 2.00ml, 4.00ml,
6.00ml, 8.00ml, 10.00ml standard series, the portable lamp of flame atomic absorption spectrophotometer is arranged to zinc lamp, in wavelength
To be measured at 213.8mm.Since the concentration of flame atomic absorption spectrophotometer detection is relatively low, the sample measured can only
Measured after dilution, evaluated error, and the purchase instrument of Flame Atomic Absorption Spectrometry spectrophotometer can be increased so during diluted
Device is of high cost.And existing EDTA volumetric methods, molten sample time are slow, agents useful for same is more, of high cost, and analysis result accuracy is also paid no attention to
Think.
The content of the invention
Present invention aims to solve the deficiencies of the prior art, and provides a kind of a kind of simple inexpensive, detection of agents useful for same it is time-consuming it is short,
The method that cost is low, testing result accurately uses Zn content in EDTA volumetric determination zinc ores.
The purpose of the present invention is achieved through the following technical solutions：
The method of Zn content, comprises the following steps that in EDTA volumetric determination zinc ores：
(1) reagent and preparation：Preparation ascorbic acid, anhydrous sodium acetate, analysis pure hydrochloric acid, the pure glacial acetic acid of analysis, analysis are pure
Nitric acid, analytical pure sulfuric acid, the xylenol orange of concentration 5g/L, volume ratio 1:1 hydrochloric acid, volume ratio 1:1 sulfuric acid, volume ratio 1:1
Ammonium hydroxide, acetic acid-sodium acetate buffer solution, the ammonium fluoride of concentration 400g/L, the sal-ammoniac of 12 ﹪ of mass concentration；
(2) preparation of EDTA standard solution：Weigh 112gEDTA disodium salts to be dissolved in a small amount of water, be diluted with water to 10L,
The EDTA standard solution of concentration 0.03mol/L is configured to, is demarcated after placing three days；
(3) demarcate：The metallic zinc of 99.999 ﹪ of 1g purity ＞ is weighed, is placed in 300ml beakers, adds 10ml volume ratios
1:1 hydrochloric acid, cap upper surface ware, dissolution in low temperature zinc, after the completion of being dissolved to zinc, removes flushing table ware, is cooled to room temperature and is diluted to
500ml, draws 50ml in the triangular flask of three 250ml, adds 2 drop xylenol orange indicator, with volume ratio 1 respectively:1 hydrochloric acid
Or ammonium hydroxide is adjusted to solution and just becomes yellow, add 25ml acetic acid-sodium acetate buffer solution, titrated with EDTA standard solution to be calibrated
It is terminal to glassy yellow, while makees blank test；Calculate titer of the EDTA to zinc:
In formula, TEDTA/Zn- EDTA standard solution is to the titer of zinc, g/ml；
TZnThe titer of-metallic zinc, g/ml；
VZnThe volume for the standard zinc drawn during-calibration, ml；
VEDTAThe volume of EDTA, ml are consumed during-calibration；
V0- blank test consumes the volume of EDTA, ml；
When the very poor value of calibration result three times is not more than 0.000005g/ml, its average value is taken, is otherwise re-scaled；
(4) ammonia washing lotion is prepared：10g sal-ammoniacs is soluble in water, add 70-80ml ammonium hydroxide, be diluted with water to 1L；
(5) preparation of sample：1h will be dried at 105 DEG C in advance by the zinc ore sample of 200 mesh sieves, then be placed in drying
It is cooled to room temperature in device；
(6) analytical procedure：0.1~0.5g zinc ores sample is weighed in the beaker of 300ml, adds a small amount of water to moisten, is added
10ml analyzes pure hydrochloric acid, and capping table ware dissolution in low temperature 3~5 minutes, the addition pure nitric acid of 5ml analyses is complete to sample decomposition, steams extremely
It is closely dry to remove, table ware and wall of cup are purged with water, adds sal-ammoniac 50ml, it is 50ml to boil to volume, adds ammonium hydroxide 25ml, boils
2min, is filtered in the triangular flask of 500ml while hot, is washed beaker 3 times with the ammonia washing lotion of heat, is precipitated 4~6 times, adds in filtrate
Enter 2 drop xylenol orange, with volume ratio 1:1 sulfuric acid is adjusted to colourless, adds ammonium fluoride 1ml, the ascorbic acid of mass concentration 30% few
Perhaps, 2 drop xylenol orange, adds acetic acid-sodium acetate buffer solution 20ml, and it is eventually to be titrated to glassy yellow with EDTA standard titration solutions
Point；
(7) Calculation results：
In formula, the mass content of zinc in Zn ﹪-zinc ore；
TEDTA/Zn- EDTA standard solution is to the titer of zinc, g/ml；
VEDTAThe volume of EDTA, ml are consumed during-titration；
M-sample size, g；
The arithmetic mean of instantaneous value for taking two parts of parallel analysis results is final analysis result, and the absolute difference of parallel analysis result is not
More than defined tolerance.
In the determination step of the method for the present invention, add concentrated nitric acid to sample decompose it is complete when, for hardly possible decompose sample,
Plus 2~5ml concentrated sulfuric acids, in addition continue to be heated to wet salt shape；For carbon containing higher sample, 1ml perchloric acid is added.
The present invention is by zinc ore sample hydrochloric acid, nitric acid and the coexistence elements such as sulfuric acid dissolution, iron of precipitation separation, manganese, lead.Filter
The interference of the elements such as screening agent masking iron, aluminium, silicon, copper is added in liquid.In acetic acid-sodium acetate solution, with EDTA standard solution
Glassy yellow is titrated to, the content of Zn is calculated according to the dosage of the EDTA of consumption.
Present invention improves over existing EDT volumetric methods, detection time is shortened, reduces reagent dosage, reduce experiment
Reagent cost, analysis result accuracy are also improved significantly.The method of the present invention is suitable for low cadmium (≤0.1%), low lead (≤
3%), Zn content be 5~60% zinc ore in Zn content measure.
Embodiment
Elaborate with reference to specific embodiment to the method for the present invention.
The method of Zn content, method comprise the following steps that in EDTA volumetric determination zinc ores：
(1) reagent and preparation：Preparation ascorbic acid, anhydrous sodium acetate, analysis pure hydrochloric acid, the pure glacial acetic acid of analysis, analysis are pure
Sulfuric acid, the xylenol orange of concentration 5g/L, volume ratio 1:1 hydrochloric acid, volume ratio 1:1 sulfuric acid, volume ratio 1:1 ammonium hydroxide, second
Acid-sodium acetate buffer solution, the ammonium fluoride of concentration 400g/L, the sal-ammoniac of 12 ﹪ of mass concentration；
(2) preparation of EDTA standard solution：Weigh 112gEDTA disodium salts to be dissolved in a small amount of water, be diluted with water to 10L,
The EDTA standard solution of concentration 0.03mol/L is configured to, is demarcated after placing three days；
(3) demarcate：The metallic zinc of 99.999 ﹪ of 1g purity ＞ is weighed, is placed in 300ml beakers, adds 10ml volume ratios
1:1 hydrochloric acid, cap upper surface ware, dissolution in low temperature zinc, after the completion of being dissolved to zinc, removes flushing table ware, is cooled to room temperature and is diluted to
500ml, draws 50ml in the triangular flask of three 250ml, adds 2 drop xylenol orange indicator, with volume ratio 1 respectively:1 hydrochloric acid
Or ammonium hydroxide is adjusted to solution and just becomes yellow, add 25ml acetic acid-sodium acetate buffer solution, titrated with EDTA standard solution to be calibrated
It is terminal to glassy yellow, while makees blank test；Calculate titer of the EDTA to zinc:
In formula, TEDTA/Zn- EDTA standard solution is to the titer of zinc, g/ml；
TZnThe titer of-metallic zinc, g/ml；
VZnThe volume for the standard zinc drawn during-calibration, ml；
VEDTAThe volume of EDTA, ml are consumed during-calibration；
V0- blank test consumes the volume of EDTA, ml；
When the very poor value of calibration result three times is not more than 0.000005g/ml, its average value is taken, is otherwise re-scaled；
(4) ammonia washing lotion is prepared：10g sal-ammoniacs is soluble in water, add 70-80ml ammonium hydroxide, be diluted with water to 1L；
(5) preparation of sample：1h will be dried at 105 DEG C in advance by the zinc ore sample of 200 mesh sieves, then be placed in drying
It is cooled to room temperature in device；
(6) analytical procedure：0.1~0.5g zinc ores sample is weighed in the beaker of 300ml, adds a small amount of water to moisten, is added few
Water moistening is measured, adds 10ml analysis pure hydrochloric acids, capping table ware dissolution in low temperature 3~5 minutes, adds 5ml and analyze pure nitric acid to sample
Decompose completely, steam to closely dry and remove, purge table ware and wall of cup with water, add sal-ammoniac 50ml, it is 50ml to boil to volume, adds ammonia
Water 25ml, boils 2min, filters while hot in the triangular flask of 500ml, washes beaker 3 times with the ammonia washing lotion of heat, precipitates 4~6 times,
2 drop paranitrophenols are added in filtrate, with volume ratio 1:1 sulfuric acid be adjusted to it is colourless, add mass concentration 30% ammonium fluoride 1ml,
Ascorbic acid is a little, and 2 drop xylenol orange, add PH5~6 acetic acid-sodium acetate buffer solution 20ml, useTZn=0.002g/ml；CEDTA =0.03mol/LEDTA standard titration solutions to be titrated to glassy yellow be terminal；
In above-mentioned analytical procedure, by zinc ore sample hydrochloric acid, nitric acid and sulfuric acid dissolution, precipitable separation iron, manganese, lead etc.
Coexistence elements.
(7) Calculation results：
In formula, the mass content of zinc in Zn ﹪-zinc ore；
TEDTA/Zn- EDTA standard solution is to the titer of zinc, g/ml；
VEDTAThe volume of EDTA, ml are consumed during-titration；
M-sample size, g；
The arithmetic mean of instantaneous value for taking two parts of parallel analysis results is final analysis result, and the absolute difference of parallel analysis result is not
More than tolerance as defined in following table：
| Zn content W% | Tolerance % |
| ＜ 15.00 | 0.15 |
| 15.00~30.00 | 0.20 |
| 30.00~45.00 | 0.30 |
| 45.00~60.00 | 0.35 |
| ﹥ 60.00 | 0.40 |
Embodiment：Zinc ore sampling grinding is passed through 200 mesh hole sizers, sample dries 1h at 105 DEG C in advance, is placed in drier
It is cooled to room temperature.0.2003g samples are weighed in the beaker of 300ml, add a small amount of water to moisten, add 10ml analyses pure hydrochloric acid (no
Dilution), capping table ware dissolution in low temperature 3~5 minutes, adding the pure nitric acid (not diluting) of 5ml analyses, (hardly possible is decomposed completely to sample decomposition
Sample add 2~5ml concentrated sulfuric acids, continue to be heated to wet salt shape；If sample is carbon containing higher, 1ml perchloric acid can be added), steam near
It is dry.Remove, purge table ware and wall of cup with water, add 12% sal-ammoniac 50ml, boil to volume about 50ml, add ammonium hydroxide 25ml,
2min is boiled, is filtered while hot in the triangular flask of 500ml, beaker is washed 3 times with the ammonia washing lotion of heat, precipitates 4~6 times, in filtrate
It is middle to add 2 drop paranitrophenols, with volumetric concentration 1:1 sulfuric acid is adjusted to colourless, adds 30% ammonium fluoride 1ml, and ascorbic acid is a little,
2 drop xylenol orange, add buffer solution 20ml, it is terminal to be titrated to glassy yellow with EDTA standard solution.Measurement result see the table below, zinc
Content is 50.53%.
Using the method for the present invention, the standard quality control sample of two authorized by state is selected to carry out microtest, result of the test
It is as follows：
Five samples of selection carry out the experiment of the rate of recovery, and result of the test is as follows：
Tests prove that using the method for the present invention, the precision of testing result is high, and recovery of standard addition is high, can preferably answer
Rapid and accurate determination for Zn content in zinc ore and zinc essence stone.
Claims (2)
- The method of Zn content in 1.EDTA volumetric determination zinc ores, it is characterised in that comprise the following steps that：(1) reagent and preparation：Prepare ascorbic acid, anhydrous sodium acetate, analysis pure hydrochloric acid, the pure glacial acetic acid of analysis, analysis bright sulfur Acid, analyzes pure nitric acid, the xylenol orange of concentration 5g/L, volume ratio 1:1 hydrochloric acid, volume ratio 1:1 sulfuric acid, volume ratio 1:1 Ammonium hydroxide, acetic acid-sodium acetate buffer solution, the ammonium fluoride of concentration 400g/L, the sal-ammoniac of 12 ﹪ of mass concentration；(2) preparation of EDTA standard solution：Weigh 112gEDTA disodium salts to be dissolved in a small amount of water, be diluted with water to 10L, prepare Into the EDTA standard solution of concentration 0.03mol/L, demarcated after placing three days；(3) demarcate：The metallic zinc of 99.999 ﹪ of 1g purity ＞ is weighed, is placed in 300ml beakers, adds 10ml volume ratios 1:1 Hydrochloric acid, cap upper surface ware, dissolution in low temperature zinc, after the completion of being dissolved to zinc, removes flushing table ware, is cooled to room temperature and is diluted to 500ml, point Not Xi Qu 50ml in the triangular flask of three 250ml, add 2 drop xylenol orange indicator, with volume ratio 1:1 hydrochloric acid or ammonium hydroxide tune Just become yellow to solution, add 25ml acetic acid-sodium acetate buffer solution, glassy yellow is titrated to EDTA standard solution to be calibrated For terminal, while make blank test；Calculate titer of the EDTA to zinc:<mrow> <msub> <mi>T</mi> <mrow> <mi>E</mi> <mi>D</mi> <mi>T</mi> <mi>A</mi> <mo>/</mo> <mi>Z</mi> <mi>n</mi> </mrow> </msub> <mo>=</mo> <mfrac> <mrow> <mo>(</mo> <msub> <mi>T</mi> <msub> <mi>Z</mi> <mi>n</mi> </msub> </msub> <mo>&times;</mo> <msub> <mi>V</mi> <msub> <mi>Z</mi> <mi>n</mi> </msub> </msub> <mo>)</mo> </mrow> <mrow> <mo>(</mo> <msub> <mi>V</mi> <mrow> <mi>E</mi> <mi>D</mi> <mi>T</mi> <mi>A</mi> </mrow> </msub> <mo>-</mo> <msub> <mi>V</mi> <mn>0</mn> </msub> <mo>)</mo> </mrow> </mfrac> </mrow>In formula, TEDTA/Zn- EDTA standard solution is to the titer of zinc, g/ml；TZnThe titer of-metallic zinc, g/ml；VZnThe volume for the standard zinc drawn during-calibration, ml；VEDTAThe volume of EDTA, ml are consumed during-calibration；V0- blank test consumes the volume of EDTA, ml；When the very poor value of calibration result three times is not more than 0.000005g/ml, its average value is taken, is otherwise re-scaled；(4) ammonia washing lotion is prepared：10g sal-ammoniacs is soluble in water, add 70-80ml ammonium hydroxide, be diluted with water to 1L；(5) preparation of sample：1h will be dried at 105 DEG C in advance by the zinc ore sample of 200 mesh sieves, then be placed in drier It is cooled to room temperature；(6) analytical procedure：0.1~0.5g zinc ores sample is weighed in the beaker of 300ml, adds a small amount of water to moisten, adds 10ml Pure hydrochloric acid is analyzed, capping table ware dissolution in low temperature 3~5 minutes, the addition pure nitric acid of 5ml analyses is complete to sample decomposition, steams near and does Remove, purge table ware and wall of cup with water, add sal-ammoniac 50ml, it is 50ml to boil to volume, adds ammonium hydroxide 25ml, boils 2min, Filter while hot in the triangular flask of 500ml, wash beaker 3 times with the ammonia washing lotion of heat, precipitate 4~6 times, 2 drops are added in filtrate Xylenol orange, with volume ratio 1:1 sulfuric acid is adjusted to colourless, adds ammonium fluoride 1ml, the ascorbic acid of mass concentration 30% a little, 2 drops Xylenol orange, adds acetic acid-sodium acetate buffer solution 20ml, and it is terminal to be titrated to glassy yellow with EDTA standard titration solutions；(7) Calculation results：<mrow> <mi>Z</mi> <mi>n</mi> <mi>%</mi> <mo>=</mo> <mfrac> <mrow> <msub> <mi>T</mi> <mrow> <mi>E</mi> <mi>D</mi> <mi>T</mi> <mi>A</mi> <mo>/</mo> <mi>Z</mi> <mi>n</mi> </mrow> </msub> <mo>&times;</mo> <msub> <mi>V</mi> <mrow> <mi>E</mi> <mi>D</mi> <mi>T</mi> <mi>A</mi> </mrow> </msub> </mrow> <mi>m</mi> </mfrac> <mo>&times;</mo> <mn>100</mn> <mi>%</mi> <mo>;</mo> </mrow>In formula, the mass content of zinc in Zn ﹪-zinc ore；TEDTA/Zn- EDTA standard solution is to the titer of zinc, g/ml；VEDTAThe volume of EDTA, ml are consumed during-titration；M-sample size, g；The arithmetic mean of instantaneous value for taking two parts of parallel analysis results is final analysis result, and the absolute difference of parallel analysis result is not more than Defined tolerance.
- 2. the method for Zn content in EDTA volumetric determinations zinc ore according to claim 1, it is characterised in that measuring In step, when addition concentrated nitric acid to sample decomposes complete, for the sample of hardly possible decomposition, in addition add 2~5ml concentrated sulfuric acids, continue to add Heat is to wet salt shape；For carbon containing higher sample, 1ml perchloric acid is added.
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Cited By (3)
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| CN109030710A (en) * | 2018-05-31 | 2018-12-18 | 长春黄金研究院有限公司 | A method of being simple and efficient Zn content in the complicated sample ore of measurement |
| CN111220600A (en) * | 2019-09-02 | 2020-06-02 | 新兴铸管股份有限公司 | Method for measuring zinc content in zinc-aluminum alloy |
| CN111830194A (en) * | 2020-05-22 | 2020-10-27 | 西北矿冶研究院 | Chemical analysis method for zinc in high-manganese and high-zinc material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109030710A (en) * | 2018-05-31 | 2018-12-18 | 长春黄金研究院有限公司 | A method of being simple and efficient Zn content in the complicated sample ore of measurement |
| CN111220600A (en) * | 2019-09-02 | 2020-06-02 | 新兴铸管股份有限公司 | Method for measuring zinc content in zinc-aluminum alloy |
| CN111830194A (en) * | 2020-05-22 | 2020-10-27 | 西北矿冶研究院 | Chemical analysis method for zinc in high-manganese and high-zinc material |
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Application publication date: 20180515 |