CN104819971B - The detection method of mercury in a kind of water - Google Patents
The detection method of mercury in a kind of water Download PDFInfo
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- CN104819971B CN104819971B CN201510262981.1A CN201510262981A CN104819971B CN 104819971 B CN104819971 B CN 104819971B CN 201510262981 A CN201510262981 A CN 201510262981A CN 104819971 B CN104819971 B CN 104819971B
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Abstract
The invention belongs to a kind of detection methods of mercury in the detection technique field of mercury in environment more particularly to water, the described method comprises the following steps：(1) standard curve, the detection of (4) sample are drawn in the processing of sample, the preparation of (2) mercury standard serial solution, (3), and (5) calculate.For the detection method of mercury under preferable experiment condition, sensitivity is higher in water provided by the invention, and detection limit is down to 0.004mg/L, and its analyze speed is fast, stability is good.
Description
Technical field
The invention belongs to a kind of detection methods of mercury in the detection technique field of mercury in environment more particularly to water.
Background technology
With the rapid development of economy, a large amount of untreated waste water, waste residue are discharged into rivers and lake, water body is caused
It is contaminated.It is mainly heavy metal ion through examining its pollutant, for heavy metal ion (mercury Hg2+；Lead Pb2+；Cadmium Cd2+；Copper
Cu2+), particularly mercury, cadmium, lead, copper etc. have significant bio-toxicity.They cannot be degraded by microorganisms in water body, can only
The various chemical forms of generation are mutually converted and migrated.It will retain, accumulate and migrate after environment or the ecosystem is entered, cause
Harm.
Wherein, mercury is the high toxicity of generally existing in environment, has the harmful substance of extreme influence to human health.From physiology
It is said on, the steam of mercury metal and the derivative (such as methyl mercury) of organic mercury are to the brain of the mankind and other relevant physical functions
Many aspects can all generate harmful influence.Inorganic mercury can be changed into methyl mercury, the mercury of this form by the bacterium in environment
Pollution can be passed to or be gathered in more higher leveled organic-biological body by food chain.And the heart of inorganic mercury energy loss victimization class
The organs such as dirty, kidney, stomach, intestines.Water-soluble dimercurion (Hg2+) it is most universal and most steady in various forms of mercury pollution substances
Fixed one kind, it is the major way of water environment and soil pollution.Therefore, the water-soluble Hg in environment2+Detection and monitoring
It is necessary.
The method of detection mercury has 4 kinds, i.e. atomic fluorescence method, cold-vapour atomic absorption method, dithizone spectrophotometry and electricity at present
Feel coupled plasma mass, the factor that cold-vapour atomic absorption method has influence mercuryvapour generation is more, and instrumental response value is not easy
Stablize；Dithizone colorimetric method is cumbersome, toxicity is big, sensitivity is low；Inductively coupled plasma mass spectrometry instrument cost is high；It is former
Sub- fluorescence method has obtained larger application as a kind of detection means relatively effectively, economic, easy, and existing atomic fluorescence method exists
In detection process there are sensitivity it is low the problem of.
The content of the invention
The technical problems to be solved by the invention are：In view of the deficienciess of the prior art, provide a kind of detection sensitivity
The detection method of mercury in high water.
In order to solve the above technical problems, the technical scheme is that：
The detection method of mercury, the described method comprises the following steps in a kind of water：
(1) processing of sample
10mL water samples are taken in micro-wave digestion pipe, add in 0.1mL sulfuric acid, 0.1mL mass concentrations are molten for 5% potassium permanganate
Liquid shakes up, and the micro-wave digestion pipe is placed in microwave dissolver, clears up 1h in 120 DEG C, takes out, be cooled to room temperature, to resolution
It is 10% hydroxylamine hydrochloride solution that liquid, which adds in mass concentration, through shaking potassium permanganate is made just to fade, spare；
(2) preparation of mercury standard serial solution
Take 0 respectively, 1,2,5,7, mercury standard working solution that 10ml concentration is 10 μ g/L in 100ml volumetric flasks, spend from
Sub- water constant volume, shakes up, and stands, to be measured；
(3) standard curve is drawn
It is 10% stannous chloride solution as reducing agent using mass concentration, under the determination condition of the fluorescence mercury vapourmeter of setting
It is measured, the fluorescence intensity of mercury standard serial solution in wavelength is determination step (2) at 253.7nm, using concentration as horizontal seat
Mark, fluorescence intensity draw standard curve for ordinate, and standard curve concentration range is 0~1 μ g/L；
(4) detection of sample
Sample in step (1) is taken in 10ml reaction bulbs, adding mass concentration as 10% stannous chloride solution, it is described
The volume ratio of sample and stannous chloride solution is 4~5:1, under the determination condition of step (3) in determination step (1) sample it is glimmering
Luminous intensity；
(5) calculate
The calculating of mercury content is as follows in sample：
X=(y-a)/(bVSample)
In formula：The concentration of mercury in x-sample；
The fluorescence intensity of y-sample；
A, b-regression coefficient；
VSampleThe sampling volume of-sample.
As an improvement mass concentration described in step (1) is made for 10% hydroxylamine hydrochloride solution using following methods：
Weigh 10g hydroxylamine hydrochlorides, it is soluble in water and be diluted to 100ml, nitrogen or cleaned air 30min are led to the flow velocity of 2.5L/min,
With drive away Trace Mercury to get.
As an improvement mercury standard working solution is prepared using following methods in step (2)：0.5g potassium bichromates are taken, it is molten
In 950ml water, 50ml nitric acid is added, mixing obtains mercury standard fixer；The mercury chloride that 0.1354g is taken to dry, with the mercury
It is moved into after the dissolving of standard fixer in 1000ml volumetric flasks, is settled to scale with the mercury standard fixer, mixing obtains the mercury
Standard reserving solution；Mercury standard reserving solution described in 5ml is taken in 500ml volumetric flasks, 50ml hydrochloric acid is added in, is fixed with the mercury standard
Liquid is diluted to scale, and mixing obtains interstitial fluid in the mercury standard；Interstitial fluid in mercury standard described in 5ml is taken in 500ml volumetric flasks, to add
Enter 50ml hydrochloric acid, scale be diluted to deionized water, mixing to get.
As an improvement mass concentration described in step (3) is made for 10% stannous chloride solution using following methods：
10g is analyzed into pure stannous chloride, 20mL hydrochloric acid is added in the draught cupboard of no mercury pollution, is slowly heated, stannous chloride is molten follow-up
The continuous heating removal of mercury in 3-5 minutes, be then diluted with water to 100mL to get.
As an improvement the determination condition of the fluorescence mercury vapourmeter in the step (3) is as follows：
As a further improvement, the carrier gas flux is 22.5 lattice.
As a further improvement, the gas-liquid volume ratio is 3:1.
As a further improvement, the photomultiplier negative high voltage is 500V.
As a further improvement, the recovery time is 40s.
As an improvement the potassium permanganate, hydroxylamine hydrochloride, stannous chloride, sulfuric acid, potassium bichromate and hydrochloric acid are excellent
Grade is pure.
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：
The detection method of mercury in water provided by the invention, sample are cleared up using Microwave Digestion, and sample decomposition is compared
Completely and digestion time is shorter；It adds in stannous chloride and ion state mercury is reduced into atomic state mercury, mercury steaming can be formed at normal temperatures
Gas, the ultraviolet excitation for the 253.7nm that ground state atom is sent by low pressure mercury lamp and generate resonance fluorescence, focused on by transmissive mirror
In photomultiplier, by opto-electronic conversion and amplify, under the determination condition of setting, fluorescence intensity and the mercury in sample
Content is directly proportional；The present invention, which only need to carry out simple pre-treatment, to be measured on fluorescence mercury vapourmeter, and analyze speed is fast, stablizes
Property it is good, high sensitivity, detection limit are down to 0.004mg/L, it is sufficient to meet testing requirements, suitable for heavy metal in waste water project-
The detection of mercury.
When carrier gas flux too small (i.e. air pressure meter reading be less than 20 lattice), mercury vapour enters that light path is slow, and mercury vapor atoms are also
It is not Fluoresceinated may chemical combination in mercury salt or generate fluorescent quenching and weaken fluorescence intensity so that measurement result is relatively low；Work as load
During throughput excessive (i.e. air pressure meter reading is less than 30 lattice), then mercury vapor atoms are influenced in the fluorescence pond residence time, and easily
Fluorescent quenching is generated with the collisions such as other particles and reducing fluorescence efficiency makes Lower result.
Gas-liquid volume ratio is also very big on testing result influence, and when the space in reaction bulb, then gas liquid ratio is big greatly, fluorescence intensity
Also it is just high but unstable, interference is generated due to space is easily mixed into other gases very much, and when liquid volume increases, in reaction bulb
Space can reduce, gas liquid ratio is also small, and space is small, can influence vapor liquid equilibrium reduce mercury atom gasifying machine meeting, make the fluorescence measured
It is worth relatively low.
When one timing of sample concentration, then fluorescence intensity increases for voltage rise, and sensitivity is also high, but overtension can be to surveying
Determine fluorescence intensity signal value and generate fluctuation, make the precision for measuring result poor.
After adding in reducing agent in sample vibration certain time is needed to can be only achieved reaction balance, generally needed 30-40 seconds, so one
As select the reading duration as 30-40 seconds.
For the detection method of mercury under preferable experiment condition, sensitivity is higher in water provided by the invention, and detection limit is low
Reach 0.004mg/L, and its analyze speed is fast, stability is good.
Description of the drawings
Fig. 1 is canonical plotting of the wavelength for the fluorescence intensity of measure and mercury element concentration at 253.7nm；
Fig. 2 is the relational graph of voltage and fluorescence intensity；
Fig. 3 is the relational graph of time and fluorescence intensity；
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The detection method of mercury, the described method comprises the following steps in a kind of water：
(1) processing of sample
10mL water samples are taken in micro-wave digestion pipe, add in 0.1mL sulfuric acid, 5% liquor potassic permanganates of 0.1mL shake up, will
The micro-wave digestion pipe is placed in microwave dissolver, clears up 1h in 120 DEG C, and taking-up is cooled to room temperature, and quality is added in digestion solution
Concentration is 10% hydroxylamine hydrochloride solution, and (wherein, mass concentration is made for 10% hydroxylamine hydrochloride solution using following methods：It weighs
10g hydroxylamine hydrochlorides, it is soluble in water and be diluted to 100ml, nitrogen or cleaned air 30min are led to the flow velocity of 2.5L/min, to drive
Except Trace Mercury to get) through shake potassium permanganate is made just to fade, it is spare；
(2) preparation of mercury standard serial solution
Take 0 respectively, 1,2,5,7, mercury standard working solution that 10ml concentration is 10 μ g/L in 100ml volumetric flasks, spend from
Sub- water constant volume, shakes up, and stands, to be measured；Wherein, mercury standard working solution is prepared using following methods：0.5g potassium bichromates are taken, are dissolved in
In 950ml water, 50ml nitric acid is added, mixing obtains mercury standard fixer；The mercury chloride that 0.1354g is taken to dry, with the mercury mark
It is moved into after quasi- fixer dissolving in 1000ml volumetric flasks, is settled to scale with the mercury standard fixer, mixing obtains the mercury mark
Quasi- storing solution；Mercury standard reserving solution described in 5ml is taken in 500ml volumetric flasks, 50ml hydrochloric acid is added in, with the mercury standard fixer
Scale is diluted to, mixing obtains interstitial fluid in the mercury standard；Interstitial fluid in mercury standard described in 5ml is taken in 500ml volumetric flasks, to add in
50ml hydrochloric acid is diluted to scale with deionized water, mixing to get.
(3) standard curve is drawn
It is 10% stannous chloride solution as reducing agent using mass concentration, wherein, (mass concentration is molten for 10% stannous chloride
Liquid is made using following methods：10g is analyzed into pure stannous chloride, 20mL hydrochloric acid is added in the draught cupboard of no mercury pollution, slowly
Heating, continue after stannous chloride is molten heat the removal of mercury in 3-5 minute, be then diluted with water to 100mL to get) in setting fluorescence survey
It is measured under the determination condition of mercury instrument, it is strong in the fluorescence that wavelength is determination step (2) mercury standard serial solution at 253.7nm
Degree, using concentration as abscissa, fluorescence intensity draws standard curve for ordinate, and standard curve concentration range is 0~1 μ g/L,
Standard curve is shown in Fig. 1；
It can show that standard curve regression equation is y=21.227x+0.2053, R from Fig. 12=0.999.
The determination condition of fluorescence mercury vapourmeter
| Fluorescence mercury vapourmeter model | YYG-2A |
| Photomultiplier negative high voltage (V) | 450 |
| Carrier gas flux (air pressure meter reading/lattice) | 22.5 |
| Shield gas flow amount (air pressure meter reading/lattice) | 40 |
| Gas-liquid volume ratio | 2:1 |
| Analyze wavelength (nm) | 253.7 |
| Recovery time (s) | 30 |
(4) detection of sample
With pipette, extract 2mL samples, it is injected into reaction bulb from liquid injection port.0.5mL stannous chloride solutions are drawn again,
It is injected from the mouth, fluorescence intensity, fluorescent value 18.4 is measured under the determination condition of step (3)；
(5) result of calculation
The calculating of mercury content is as follows in sample：
X=(y-a)/(bVSample)
In formula：The concentration of mercury in x-sample；
The fluorescence intensity of y-sample；
A, b-regression coefficient；
VSampleThe sampling volume of-sample；
X=(the 18.4-0.2053)/μ g/L of (21.227*2)=0.43.
Said determination condition is constant, only changes carrier gas flux therein, and same concentration (1 μ g/ are measured with different carrier gas fluxes
L sample), fluorescence intensity are shown 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
From table 1 it follows that carrier gas flux, in 15-25 lattice, fluorescence intensity is in rising trend, when carrier gas flux surpasses
When crossing 30 lattice, fluorescence intensity gradually weakens, in order to improve the accuracy of testing result, the carrier gas in determination condition of the invention
Flow elects 20-30 lattice as.
Said determination condition is constant, only changes gas liquid ratio therein, and same concentration (1 μ g/L) is measured with different gas liquid ratios
Sample, fluorescence intensity are shown in Table 2 with the variation of gas liquid ratio
Table 2
From Table 2, it can be seen that gradually smaller with the ratio of gas liquid ratio, fluorescent value gradually increases, in order to improve inspection
The accuracy of result is surveyed, the gas liquid ratio in determination condition of the invention elects 2~4 as:1.
Said determination condition is constant, only changes photomultiplier operating voltage therein, is measured under different voltage same
The sample of one concentration (1 μ g/L), fluorescence intensity are shown in Fig. 2 with the variation of voltage.
From figure 2 it can be seen that the relation between voltage and fluorescence intensity, voltage is bigger, and fluorescence intensity is bigger, inspection
It is higher to survey sensitivity, if but voltage is excessively high, also have damage to multiplier tube, therefore the photoelectricity in the determination condition of the present invention times
Increase pipe operating voltage and elect 450~500V as.
The sample of same concentration (1 μ g/L) is measured under the 10-50s recovery times, with 10ml reaction bulbs, built-in 2ml samples+
The stannous chloride of 1ml mass concentrations 10%, remaining determination condition is constant, with it is different concussion the times be measured, fluorescent value with
The result of variations of concussion time (10-50s) is shown in Fig. 3.
From figure 3, it can be seen that in 10-40s, fluorescent value lengthens with the concussion time and has increased trend, illustrates to add
Enter after reducing agent, it is necessary to certain concussion time can be only achieved reaction balance, therefore, during reduction in determination condition of the invention
Between elect 30~40s as.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (4)
1. the detection method of mercury in a kind of water, which is characterized in that the described method comprises the following steps：
(1) processing of sample
10mL water samples are taken in micro-wave digestion pipe, add in 0.1mL sulfuric acid, 0.1mL mass concentrations are 5% liquor potassic permanganate, are shaken
It is even, the micro-wave digestion pipe is placed in microwave dissolver, 1h is cleared up in 120 DEG C, takes out, be cooled to room temperature, to digestion solution plus
Enter mass concentration for 10% hydroxylamine hydrochloride solution, through shaking potassium permanganate is made just to fade, it is spare；The mass concentration is 10%
Hydroxylamine hydrochloride solution is made using following methods：Weigh 10g hydroxylamine hydrochlorides, it is soluble in water and be diluted to 100ml, with 2.5L/min
Flow velocity lead to nitrogen or cleaned air 30min, with drive away Trace Mercury to get；
(2) preparation of mercury standard serial solution
Take 0 respectively, 1,2,5,7, mercury standard working solution that 10ml concentration is 10 μ g/L in 100ml volumetric flasks, use deionized water
Constant volume shakes up, and stands, to be measured；
(3) standard curve is drawn
It is 10% stannous chloride solution as reducing agent using mass concentration, is carried out under the determination condition of the fluorescence mercury vapourmeter of setting
It measures, it is glimmering using concentration as abscissa in the fluorescence intensity that wavelength is mercury standard serial solution in determination step (2) at 253.7nm
Luminous intensity draws standard curve for ordinate, and standard curve concentration range is 0~1 μ g/L；The measurement strip of the fluorescence mercury vapourmeter
Part is as follows：Photomultiplier negative high voltage 500V；22.5 lattice of air pressure meter reading of carrier gas flux；The air pressure meter reading of shield gas flow amount
40~60 lattice；Gas-liquid volume ratio 3:1；Analyze wavelength 253.7nm；Recovery time 40s；
(4) detection of sample
Sample in step (1) is taken in 10ml reaction bulbs, adding mass concentration as 10% stannous chloride solution, the sample
Volume ratio with stannous chloride solution is 4~5:1, the fluorescence of sample is strong in determination step (1) under the determination condition of step (3)
Degree；
(5) result of calculation
The calculating of mercury content is as follows in sample：
X=(y-a)/(bVSample)
In formula：The concentration of mercury in x-sample；
The fluorescence intensity of y-sample；
A, b-regression coefficient；
VSampleThe sampling volume of-sample.
2. the detection method of mercury in a kind of water as described in claim 1, it is characterised in that:Mercury standard working solution in step (2)
It is prepared using following methods：0.5g potassium bichromates are taken, are dissolved in 950ml water, add 50ml nitric acid, mixing obtains mercury standard and consolidates
Determine liquid；The mercury chloride that 0.1354g is taken to dry is moved into 1000ml volumetric flasks after being dissolved with the mercury standard fixer, with described
Mercury standard fixer is settled to scale, and mixing obtains mercury standard reserving solution；Mercury standard reserving solution described in 5ml is taken in 500ml volumetric flasks
In, 50ml hydrochloric acid is added in, is diluted to scale with the mercury standard fixer, mixing obtains interstitial fluid in mercury standard；Take mercury described in 5ml
Interstitial fluid is in 500ml volumetric flasks in standard, adds in 50ml hydrochloric acid, and scale is diluted to deionized water, mixing to get.
3. the detection method of mercury in a kind of water as described in claim 1, it is characterised in that:Mass concentration described in step (3)
It is made for 10% stannous chloride solution using following methods：By 10g stannous chlorides, 20mL is added in the draught cupboard of no mercury pollution
Hydrochloric acid slowly heats, continue after stannous chloride is molten heat the removal of mercury in 3-5 minutes, be then diluted with water to 100mL to get.
4. the detection method of mercury in a kind of water as described in claim 1, it is characterised in that:The potassium permanganate, hydroxylamine hydrochloride,
Stannous chloride, sulfuric acid, potassium bichromate and hydrochloric acid are top pure grade.
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| CN105606555A (en) * | 2016-03-10 | 2016-05-25 | 山东五洲检测有限公司 | Method for detecting content of mercury ions in water |
| CN106353271A (en) * | 2016-10-25 | 2017-01-25 | 福建紫金矿冶测试技术有限公司 | Mercury detector standard sample selecting and working curve manufacturing method |
| CN111443056B (en) * | 2020-06-03 | 2023-02-28 | 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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| CN101482506B (en) * | 2008-01-10 | 2012-03-28 | 江苏江分电分析仪器有限公司 | Mercury content measuring method and device |
| CN104297173A (en) * | 2013-07-18 | 2015-01-21 | 上海威正测试技术有限公司 | Method for rapid detection of mercury content in ocean sediments |
| CN104297174A (en) * | 2013-07-18 | 2015-01-21 | 上海威正测试技术有限公司 | Method for rapid detection of mercury content in water |
| CN103499558A (en) * | 2013-09-06 | 2014-01-08 | 深圳市中兴环境仪器有限公司 | System and method for determining mercury concentration in water |
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| 冷原子荧光法测定地面水和土壤中的痕量总汞;荆镝等;《中国环境监测》;19960630;第9-11页 * |
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