CN104819971A - Detection method for mercury in water - Google Patents
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- CN104819971A CN104819971A CN201510262981.1A CN201510262981A CN104819971A CN 104819971 A CN104819971 A CN 104819971A CN 201510262981 A CN201510262981 A CN 201510262981A CN 104819971 A CN104819971 A CN 104819971A
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Abstract
The invention belongs to the technical field of detection of mercury in the environment and particularly relates to a detection method for mercury in water. The detection method comprises the following steps: (1) sample treatment; (2) preparation of standard series of mercury solution; (3) drawing of a standard curve; (4) sample detection; and (5) calculation. The detection method provided by the invention has the advantages that under the better experimental condition, the sensitivity is high, the detection limit reaches 0.004mg/L as low as possible, the analysis speed is high and the stability is good.
Description
Technical field
The invention belongs to the detection technique field of mercury in environment, particularly relate to the detection method of mercury in a kind of water.
Background technology
Along with the fast development of economy, a large amount of undressed waste water, waste residue are discharged in rivers and lake, cause water body to be polluted.Through checking its pollutant mainly heavy metal ion, for heavy metal ion (mercury Hg
2+; Plumbous Pb
2+; Cadmium Cd
2+; Copper Cu
2+), particularly mercury, cadmium, lead, copper etc. have significant bio-toxicity.They can not be degraded by microorganisms in water body, various chemical form can only occur and mutually transform and move.Will retain, accumulate and move after entered environment or the ecosystem, work the mischief.
Wherein, mercury is ubiquitous high toxicity in environment, human health is had to the objectionable impurities of extreme influence.From physiology, the steam of mercury metal and a lot of aspects of organomercurial derivant (as methyl mercury) to the brain of the mankind and other relevant physical function all can produce injurious effects.Inorganic mercury can be become methyl mercury by the Bacterial Transformation in environment, and the mercury pollution of this form can pass to or be gathered in more higher leveled organic-biological body by food chain.And the organ such as heart, kidney, stomach, intestines of inorganic mercury energy loss victimization class.Water miscible dimercurion (Hg
2+) be in various forms of mercury pollution material the most generally and the most stable one, it is the major way of water environment and soil pollution.Therefore, the water miscible Hg in environment
2+detection and monitoring be necessary.
The method of current detection mercury has 4 kinds, i.e. atomic fluorescence method, cold-vapour atomic absorption method, dithizone spectrophotometric method and inductively coupled plasma mass spectrometry, and cold-vapour atomic absorption method exists the many factors affecting mercuryvapour and occur, and instrumental response value is not easily stablized; Dithizone colorimetric method complex operation, toxicity are large, sensitivity is low; Inductively coupled plasma mass spectrometry instrument cost is high; Atomic fluorescence method as a kind of comparatively effectively, economic, easy detection means obtains larger application, in testing process, there is the low problem of sensitivity in existing atomic fluorescence method.
Summary of the invention
Technical matters to be solved by this invention is: the deficiency existed for prior art, provides the detection method of mercury in the water that a kind of detection sensitivity is high.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A detection method for mercury in water, said method comprising the steps of:
(1) process of sample
Get 10mL water sample in micro-wave digestion pipe, add 0.1mL sulfuric acid, 0.1mL mass concentration is 5% liquor potassic permanganate, shakes up, and described micro-wave digestion pipe is placed in microwave dissolver, 1h is cleared up in 120 DEG C, take out, be cooled to room temperature, adding mass concentration to digestion solution is 10% hydroxylamine hydrochloride solution, through shake, potassium permanganate is just faded, for subsequent use;
(2) preparation of mercury standard serial solution
Get 0 respectively, 1,2,5,7,10ml concentration be the mercury standard working solution of 10 μ g/L in 100ml volumetric flask, use deionized water constant volume, shake up, leave standstill, to be measured;
(3) drawing standard curve
Be that 10% stannous chloride solution is as reductive agent using mass concentration, measure under the condition determination of the fluorescence mercury vapor analyzer of setting, the fluorescence intensity of mercury standard serial solution in wavelength is 253.7nm place determination step (2), take concentration as horizontal ordinate, fluorescence intensity is ordinate drawing standard curve, and typical curve concentration range is 0 ~ 1 μ g/L;
(4) detection of sample
Get sample in step (1) in 10ml reaction bulb, adding mass concentration is again 10% stannous chloride solution, the volume ratio of described sample and stannous chloride solution is 4 ~ 5:1, the fluorescence intensity of the middle sample of determination step (1) under the condition determination of step (3);
(5) calculate
Being calculated as follows of mercury content in sample:
X=(y-a)/(bV
sample)
In formula: the concentration of mercury in x-sample;
The fluorescence intensity of y-sample;
A, b-regression coefficient;
V
samplethe sampling volume of-sample.
Improve as one, mass concentration described in step (1) is that 10% hydroxylamine hydrochloride solution adopts following methods to obtain: take 10g oxammonium hydrochloride, soluble in water and be diluted to 100ml, leads to nitrogen or cleaned air 30min with the flow velocity of 2.5L/min, to drive away Trace Mercury, to obtain final product.
Improve as one, in step (2), mercury standard working solution adopts following methods preparation: get 0.5g potassium dichromate, be dissolved in 950ml water, then add 50ml nitric acid, and mixing, obtains mercury standard immobile liquid; Get the mercuric chloride of 0.1354g drying, move in 1000ml volumetric flask after dissolving with described mercury standard immobile liquid, be settled to scale with described mercury standard immobile liquid, mixing, obtains described mercury standard reserving solution; Get mercury standard reserving solution described in 5ml in 500ml volumetric flask, add 50ml hydrochloric acid, be diluted to scale with described mercury standard immobile liquid, mixing, obtains described mercury standard intermediate liquid; Get mercury standard intermediate liquid described in 5ml, in 500ml volumetric flask, to add 50ml hydrochloric acid, be diluted to scale with deionized water, mixing, to obtain final product.
Improve as one, mass concentration described in step (3) is that 10% stannous chloride solution adopts following methods to obtain: 10g is analyzed pure stannous chloride, adding 20mL hydrochloric acid without in the fuming cupboard of mercury pollution, slowly heat, the stannous chloride molten rear continuation heating removal of mercury in 3-5 minute, then be diluted with water to 100mL, obtain final product.
Improve as one, the condition determination of the fluorescence mercury vapor analyzer in described step (3) is as follows:
As improving further, described carrier gas flux is 22.5 lattice.
As improving further, described gas-liquid volume ratio is 3:1.
As improving further, described photomultiplier negative high voltage is 500V.
As improving further, the described recovery time is 40s.
Improve as one, it is pure that described potassium permanganate, oxammonium hydrochloride, stannous chloride, sulfuric acid, potassium dichromate and hydrochloric acid are top grade.
Owing to have employed technique scheme, the invention has the beneficial effects as follows:
The detection method of mercury in water provided by the invention, sample adopts Microwave Digestion to clear up, and sample decomposes relatively completely and digestion time is shorter; Add stannous chloride and ion state mercury is reduced into atomic state mercury, mercury vapour can be formed at normal temperatures, the ultraviolet excitation of the 253.7nm that its ground state atom is sent by low pressure mercury lamp and produce resonance fluorescence, photomultiplier is focused on by transmissive mirror, to amplify through opto-electronic conversion, under the condition determination of setting, its fluorescence intensity is directly proportional to the mercury content in sample; The present invention only need carry out simple pre-treatment and just can measure on fluorescence mercury vapor analyzer, and its analysis speed is fast, good stability, and highly sensitive, detectability is low reaches 0.004mg/L, is enough to meet testing requirement, is applicable to the detection of heavy metal in waste water project-mercury.
When carrier gas flux too small (namely rain glass reading is less than 20 lattice), it is slow that mercury vapour enters light path, and mercury vapor atoms is also not Fluoresceinated just may be mercury salt or produce fluorescent quenching and fluorescence intensity is weakened by chemical combination, makes measurement result on the low side; When carrier gas flux excessive (namely rain glass reading is less than 30 lattice), then affect mercury vapor atoms in the fluorescence pond residence time, and easily and other particles etc. collide and produce fluorescent quenching and reduce fluorescence efficiency and make Lower result.
Gas-liquid volume ratio is also very large on testing result impact, when the space in reaction bulb is large, then gas liquid ratio is large, fluorescence intensity is also just high, but unstable, produce interference because space is too easily mixed into other gases, and when liquid volume increases, space in reaction bulb can reduce, gas liquid ratio is also little, and space is little, can affect vapor liquid equilibrium and reduce the meeting of mercury atom gasifying machine, makes the fluorescent value that records on the low side.
When sample concentration one timing, voltage raises then fluorescence intensity and increases, and its sensitivity is also high, but overtension can produce fluctuation to mensuration fluorescence intensity signal value, makes the precision recording result poor.
Need vibration certain hour just can reach molecular balance after adding reductive agent in sample, generally need 30-40 second, select the reading duration to be 30-40 second so general.
In water provided by the invention, the detection method of mercury is under preferably experiment condition, and its sensitivity is higher, and detectability is low reaches 0.004mg/L, and its analysis speed is fast, good stability.
Accompanying drawing explanation
Fig. 1 is wavelength is the fluorescence intensity of 253.7nm place mensuration and the canonical plotting of mercury element concentration;
Fig. 2 is the graph of a relation of voltage and fluorescence intensity;
Fig. 3 is the graph of a relation of time and fluorescence intensity;
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
A detection method for mercury in water, said method comprising the steps of:
(1) process of sample
Get 10mL water sample in micro-wave digestion pipe, add 0.1mL sulfuric acid, 0.1mL 5% liquor potassic permanganate, shake up, described micro-wave digestion pipe is placed in microwave dissolver, 1h is cleared up in 120 DEG C, taking-up is cooled to room temperature, adding mass concentration to digestion solution is 10% hydroxylamine hydrochloride solution, (wherein, mass concentration is that 10% hydroxylamine hydrochloride solution adopts following methods to obtain: take 10g oxammonium hydrochloride, soluble in water and be diluted to 100ml, nitrogen or cleaned air 30min is led to the flow velocity of 2.5L/min, to drive away Trace Mercury, obtain) through shake, potassium permanganate is just faded, for subsequent use,
(2) preparation of mercury standard serial solution
Get 0 respectively, 1,2,5,7,10ml concentration be the mercury standard working solution of 10 μ g/L in 100ml volumetric flask, use deionized water constant volume, shake up, leave standstill, to be measured; Wherein, mercury standard working solution adopts following methods preparation: get 0.5g potassium dichromate, be dissolved in 950ml water, then add 50ml nitric acid, and mixing, obtains mercury standard immobile liquid; Get the mercuric chloride of 0.1354g drying, move in 1000ml volumetric flask after dissolving with described mercury standard immobile liquid, be settled to scale with described mercury standard immobile liquid, mixing, obtains described mercury standard reserving solution; Get mercury standard reserving solution described in 5ml in 500ml volumetric flask, add 50ml hydrochloric acid, be diluted to scale with described mercury standard immobile liquid, mixing, obtains described mercury standard intermediate liquid; Get mercury standard intermediate liquid described in 5ml, in 500ml volumetric flask, to add 50ml hydrochloric acid, be diluted to scale with deionized water, mixing, to obtain final product.
(3) drawing standard curve
Be that 10% stannous chloride solution is as reductive agent using mass concentration, wherein, (mass concentration is that 10% stannous chloride solution adopts following methods to obtain: 10g is analyzed pure stannous chloride, adding 20mL hydrochloric acid without in the fuming cupboard of mercury pollution, slowly heat, the stannous chloride molten rear continuation heating removal of mercury in 3-5 minute, then 100mL is diluted with water to, obtain) measure under the condition determination of the fluorescence mercury vapor analyzer of setting, in the fluorescence intensity that wavelength is 253.7nm place determination step (2) mercury standard serial solution, take concentration as horizontal ordinate, fluorescence intensity is ordinate drawing standard curve, typical curve concentration range is 0 ~ 1 μ g/L, its typical curve is shown in Fig. 1,
Can show that typical curve regression equation is y=21.227x+0.2053, R from Fig. 1
2=0.999.
The condition determination of fluorescence mercury vapor analyzer
| Fluorescence mercury vapor analyzer model | YYG-2A |
| Photomultiplier negative high voltage (V) | 450 |
| Carrier gas flux (rain glass reading/lattice) | 22.5 |
| Shield gas flow amount (rain glass reading/lattice) | 40 |
| Gas-liquid volume ratio | 2:1 |
| Analytical wavelengths (nm) | 253.7 |
| Recovery time (s) | 30 |
(4) detection of sample
With pipette, extract 2mL sample, it is injected reaction bulb from liquid injection port.Draw 0.5mL stannous chloride solution again, also inject from this mouth, under the condition determination of step (3), measure fluorescence intensity, its fluorescent value is 18.4;
(5) result of calculation
Being calculated as follows of mercury content in sample:
X=(y-a)/(bV
sample)
In formula: the concentration of mercury in x-sample;
The fluorescence intensity of y-sample;
A, b-regression coefficient;
V
samplethe sampling volume of-sample;
x＝(18.4-0.2053)/(21.227*2)＝0.43μg/L。
Said determination condition is constant, and only change carrier gas flux wherein, measure the sample of same concentration (1 μ g/L) with different carrier gas flux, its fluorescence intensity is in table 1
| Carrier gas flux (lattice) | 15 | 20 | 25 | 30 | 35 | 40 |
| Fluorescent value | 17 | 21 | 21.5 | 19.5 | 16.5 | 16 |
Table 1
As can be seen from Table 1, carrier gas flux is when 15-25 lattice, and its fluorescence intensity is in rising trend, when carrier gas flux is more than 30 lattice, its fluorescence intensity weakens gradually, and in order to improve the accuracy of testing result, the carrier gas flux in condition determination of the present invention elects 20-30 lattice as.
Said determination condition is constant, only changes gas liquid ratio wherein, measures the sample of same concentration (1 μ g/L) with different gas liquid ratio, its fluorescence intensity with the change of gas liquid ratio in table 2
Table 2
As can be seen from Table 2, along with the ratio of gas liquid ratio is less gradually, its fluorescent value increases gradually, and in order to improve the accuracy of testing result, the gas liquid ratio in condition determination of the present invention elects 2 ~ 4:1 as.
Said determination condition is constant, and only change photomultiplier operating voltage wherein, under different voltage, measure the sample of same concentration (1 μ g/L), its fluorescence intensity is shown in Fig. 2 with the change of voltage.
As can be seen from Figure 2, the relation between voltage and fluorescence intensity, voltage is larger, its fluorescence intensity is larger, and its detection sensitivity is higher, but if voltage is too high, also have infringement to multiplier tube, the photomultiplier operating voltage therefore in condition determination of the present invention elects 450 ~ 500V as.
The sample of same concentration (1 μ g/L) is measured under the 10-50s recovery time, use 10ml reaction bulb, the stannous chloride of in-built 2ml sample+1ml mass concentration 10%, all the other condition determinations are constant, measure with the difference concussion time, its fluorescent value is shown in Fig. 3 with the result of variations of concussion time (10-50s).
As can be seen from Figure 3, in 10-40s, fluorescent value lengthens with the concussion time and has the trend of increase, after explanation adds reductive agent, need certain concussion time just can reach molecular balance, therefore, the recovery time in condition determination of the present invention elects 30 ~ 40s as.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the detection method of mercury in water, is characterized in that, said method comprising the steps of:
(1) process of sample
Get 10mL water sample in micro-wave digestion pipe, add 0.1mL sulfuric acid, 0.1mL mass concentration is 5% liquor potassic permanganate, shakes up, and described micro-wave digestion pipe is placed in microwave dissolver, 1h is cleared up in 120 DEG C, take out, be cooled to room temperature, adding mass concentration to digestion solution is 10% hydroxylamine hydrochloride solution, through shake, potassium permanganate is just faded, for subsequent use;
(2) preparation of mercury standard serial solution
Get 0 respectively, 1,2,5,7,10ml concentration be the mercury standard working solution of 10 μ g/L in 100ml volumetric flask, use deionized water constant volume, shake up, leave standstill, to be measured;
(3) drawing standard curve
Be that 10% stannous chloride solution is as reductive agent using mass concentration, measure under the condition determination of the fluorescence mercury vapor analyzer of setting, the fluorescence intensity of mercury standard serial solution in wavelength is 253.7nm place determination step (2), take concentration as horizontal ordinate, fluorescence intensity is ordinate drawing standard curve, and typical curve concentration range is 0 ~ 1 μ g/L;
(4) detection of sample
Get sample in step (1) in 10ml reaction bulb, adding mass concentration is again 10% stannous chloride solution, the volume ratio of described sample and stannous chloride solution is 4 ~ 5:1, the fluorescence intensity of the middle sample of determination step (1) under the condition determination of step (3);
(5) result of calculation
Being calculated as follows of mercury content in sample:
X=(y-a)/(bV
sample)
In formula: the concentration of mercury in x-sample;
The fluorescence intensity of y-sample;
A, b-regression coefficient;
V
samplethe sampling volume of-sample.
2. the detection method of mercury in a kind of water as claimed in claim 1, it is characterized in that: mass concentration described in step (1) is that 10% hydroxylamine hydrochloride solution adopts following methods to obtain: take 10g oxammonium hydrochloride, soluble in water and be diluted to 100ml, nitrogen or cleaned air 30min is led to the flow velocity of 2.5L/min, to drive away Trace Mercury, to obtain final product.
3. the detection method of mercury in a kind of water as claimed in claim 1, it is characterized in that: in step (2), mercury standard working solution adopts following methods preparation: get 0.5g potassium dichromate, be dissolved in 950ml water, then add 50ml nitric acid, mixing, obtains mercury standard immobile liquid; Get the mercuric chloride of 0.1354g drying, move in 1000ml volumetric flask after dissolving with described mercury standard immobile liquid, be settled to scale with described mercury standard immobile liquid, mixing, obtains described mercury standard reserving solution; Get mercury standard reserving solution described in 5ml in 500ml volumetric flask, add 50ml hydrochloric acid, be diluted to scale with described mercury standard immobile liquid, mixing, obtains described mercury standard intermediate liquid; Get mercury standard intermediate liquid described in 5ml, in 500ml volumetric flask, to add 50ml hydrochloric acid, be diluted to scale with deionized water, mixing, to obtain final product.
4. the detection method of mercury in a kind of water as claimed in claim 1, it is characterized in that: mass concentration described in step (3) is that 10% stannous chloride solution adopts following methods to obtain: by 10g stannous chloride, adding 20mL hydrochloric acid without in the fuming cupboard of mercury pollution, slowly heat, the stannous chloride molten rear continuation heating removal of mercury in 3-5 minute, then be diluted with water to 100mL, obtain final product.
5. the detection method of mercury in a kind of water as claimed in claim 1, is characterized in that: the condition determination of the fluorescence mercury vapor analyzer in described step (3) is as follows:
6. the detection method of mercury in a kind of water as claimed in claim 5, is characterized in that: the rain glass reading of described carrier gas flux is 22.5 lattice.
7. the detection method of mercury in a kind of water as claimed in claim 5, is characterized in that: described gas-liquid volume ratio is 3:1.
8. the detection method of mercury in a kind of water as claimed in claim 5, is characterized in that: described photomultiplier negative high voltage is 500V.
9. the detection method of mercury in a kind of water as claimed in claim 5, is characterized in that: the described recovery time is 40s.
10. the detection method of mercury in a kind of water as claimed in claim 1, is characterized in that: it is pure that described potassium permanganate, oxammonium hydrochloride, stannous chloride, sulfuric acid, potassium dichromate and hydrochloric acid are top grade.
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| CN111443056A (en) * | 2020-06-03 | 2020-07-24 | 广西中检检测技术服务有限公司 | Method for measuring mercury content in copper concentrate |
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| CN111443056A (en) * | 2020-06-03 | 2020-07-24 | 广西中检检测技术服务有限公司 | Method for measuring mercury content in copper concentrate |
| CN111735782A (en) * | 2020-06-12 | 2020-10-02 | 贵州省分析测试研究院 | System and method for determining transfer of heavy metal in sediment through atmospheric sedimentation |
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