CN109115590A - A kind of method that micro-wave digestion-inductively coupled plasma emission spectrography measures calcium, magnesium, iron, copper in Industrial Boiler water - Google Patents
A kind of method that micro-wave digestion-inductively coupled plasma emission spectrography measures calcium, magnesium, iron, copper in Industrial Boiler water Download PDFInfo
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- CN109115590A CN109115590A CN201811018308.3A CN201811018308A CN109115590A CN 109115590 A CN109115590 A CN 109115590A CN 201811018308 A CN201811018308 A CN 201811018308A CN 109115590 A CN109115590 A CN 109115590A
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Abstract
The present invention proposes a kind of method that micro-wave digestion-inductively coupled plasma emission spectrography measures calcium, magnesium, iron, copper in Industrial Boiler water, the present invention is optimized using micro-wave digestion as pretreatment technology and to time used in micro-wave digestion sample and temperature, select suitable analytical line, reduce time of measuring, the accuracy of measurement is improved again, reagent blank background can be reduced, sample cross contamination is avoided；In combination with inductively coupled plasma emission spectrography, have precision height, analysis speed fast, matrix effect is small, detection limit is low, and environmental-friendly, a variety of advantages such as measurement, effectively increase working efficiency while realizing multielement in water quality.
Description
Technical field
The present invention relates to analysis of chemical elements fields, and in particular to a kind of micro-wave digestion-inductively coupled plasma body transmitting
Calcium, magnesium, iron, Cupper determination method in spectrographic determination Industrial Boiler water.
Background technique
The water quality of boiler feed water has vital effect for the safety of boiler, energy-saving run.In boiler feed water
Calcium, magnesium are the important elements for leading to boiler fouling, and the iron, copper in boiler feed water are the important elements for leading to boiler corrosion.If water
Matter is not up to standard, boiler not only can fouling, influence heating surface heat transfer, increase thermal resistance, cause the waste of fuel, and metal can be made to send out
Raw underdeposit corrosion, causes boiler Water-cooled boiler wall to overheat, and leads to bulge or booster, and serious person even causes halt production, pot
Furnace is scrapped, and the safe and economical operation of heat power equipment has been seriously endangered.Therefore, the formation to prevent boiler scale and corrosion, it is necessary to
The content of calcium, magnesium, iron, copper in boiler feed water is detected, the management to boiler feed water is reinforced.
Currently, laboratory mostly uses greatly spectrophotometry and compleximetry to detect calcium, magnesium, iron, the copper in water,
But these classical measuring methods need separately to measure each element, measurement while can not achieve multielement, not only cumbersome,
Time-consuming, more organic reagent is used in low efficiency and experimentation, brings pollution to environment, to experimental implementation person with
Carry out certain harm.The factor for influencing inorganic elements measurement result accuracy mainly includes the instrument in Sample Pretreatment Technique and later period
Device detection, therefore the instrument testing conditions of suitable pre-treating method and optimization are selected, for improving the accuracy and effect of detection
Rate has a very important significance.
Summary of the invention
In order to solve the defects of prior art with deficiency, the present invention provides a kind of micro-wave digestion-inductively coupled plasmas
The method of calcium, magnesium, iron, copper in body emission spectrographic determination boiler feed water is efficient one kind, high-precision, highly sensitive, stability
Detection method that is good, environmental-friendly, can quickly analyzing multiple element.
The technical solution is as follows:
Calcium in a kind of micro-wave digestion of the present invention-inductively coupled plasma emission spectrography measurement Industrial Boiler water, magnesium,
The method of iron, copper, includes the following steps:
(1) 100mL boiler feed water water sample is measured, 1.5mL concentrated nitric acid is added immediately, water sample is made to be acidified to pH value 1.Work as water
When suspended matter is more in sample, store in vinyon bottle after using middling speed quantitative filter paper to filter as sample；
(2) it takes the sample 10mL prepared in step (1) to be placed in polytetrafluoroethylene (PTFE) counteracting tank, it is real to carry out micro-wave digestion
It tests, after program operation, taking-up counteracting tank is deflated, opened after temperature in tank and equilibrium at room temperature in cooling in ventilating kitchen
Lid removes digestion solution in tank and swings decontamination solution top tank structure into 50mL volumetric flask at least twice with experimental water, collect all solution
And it is diluted with water to volumetric flask groove, it is to be measured；
(3) it functions as follows condition with inductive coupling plasma emission spectrograph to be measured water sample, operating condition
And elemental analysis line is as follows: radio-frequency power 1100W, and atomization gas flow is 0.7L/min, secondary air amount 0.5L/min, sees
Examine height be 15mm, pump speed 70r/min, duplicate reading 3 times, the calcium, magnesium, iron, copper elemental analysis line be calcium
393.37nm, magnesium 279.55nm, iron 238.20nm, copper 327.39nm；
(4) use experimental water that boiler feed water water sample is replaced to detect by above-mentioned steps are synchronous with sample using as blank assay.
As above-mentioned technical proposal preferential, the boiler feed water water sample includes boiler feedwater sample, boiler water sample, pot
Furnace return water sample, the setting of micro-wave digestion program are as follows: the microwave digestion temperature of boiler feedwater sample is 170 DEG C, and the retention time is
10min；The microwave digestion temperature of boiler water sample is 185 DEG C, retention time 15min；The micro-wave digestion of boiler blow-down water sample
180 DEG C of temperature, retention time 12min, the retention time is the duration after reaching digestion condition.
The present invention is by this pre-treating method of micro-wave digestion and inductively coupled plasma emission spectrography (ICP-AES) phase
In conjunction with Microwave Digestion can be in closed container through heating sample dissolution only with less acid, while can reduce examination
Agent blank background, avoids sample cross contamination.ICP-AES has fast compared with high precision, analysis speed, and matrix effect is small, detection
Low, the features such as measuring while can be realized multielement in water quality is limited, is greatly improved work efficiency.Micro-wave digestion pretreatment process
In temperature and the retention time be two important parameters, be related to the order of accuarcy of subsequent measurements, digestion condition is excessively high, counteracting tank
Easily damaged, digestion condition is too low, and resolution is incomplete；Retention time is too long, and Specimen eliminating is complete, but wastes time, and is unfavorable for fast
Speed analysis；Retention time is too short, and Specimen eliminating is incomplete, and measurement result is relatively low.The present invention selects reasonable microwave digestion temperature
The accuracy of detection is improved with the retention time and reduces the time used in pre-treatment.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is influence schematic diagram of the digestion condition to concentration of element to be measured in water supply；
Fig. 2 is influence schematic diagram of the digestion condition to concentration of element to be measured in boiler water；
Fig. 3 is influence schematic diagram of the digestion condition to concentration of element to be measured in return water；
Fig. 4 is influence schematic diagram of the retention time to concentration of element to be measured in water supply；
Fig. 5 is influence schematic diagram of the retention time to concentration of element to be measured in boiler water；
Fig. 6 is influence schematic diagram of the retention time to concentration of element to be measured in return water.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is described in further detail.
By the present invention propose calcium in micro-wave digestion-inductively coupled plasma emission spectrography measurement Industrial Boiler water,
The method of magnesium, iron, copper, to the 1# boiler feedwater of the steam boiler of certain model WNS4-1.0-Y, 2# boiler water, 3# boiler blow-down water
It is measured respectively:
A. the instrument used in continuous mode and reagent are as follows: Optima 7000DV type inductively coupled plasma body
Emission spectrometer (PE company of the U.S.)；TOPEX microwave dissolver (Shanghai Yi Yao instrument Science and Technology Ltd.), 1000mg/L's
Calcium, magnesium, iron, copper standard solution, the dust technology of volume fraction 5% and the concentrated nitric acid of ρ=1.42g/ml, all experiment reagents are equal
For excellent pure grade, experimental water meets GB/T6682 " water for analytical laboratory use-Specification and test methods " primary standard, all vessel
It is rinsed 3 times with secondary distilled water again after being impregnated for 24 hours with the dust technology of volume fraction 5%.The single standard solution is configured to
Hybrid standard stock solution is diluted with volume fraction for 5% dust technology step by step using when；
B. include the following steps:
(1) 100mL boiler feed water water sample is measured respectively, and 1.5mL concentrated nitric acid is added, so that water sample is acidified to pH value is about 1, when
When Suspended Substance in Water Sample is more, stored in vinyon bottle after being filtered with middling speed quantitative filter paper, the boiler feed water water sample packet
Include 1# boiler feedwater sample, 2# boiler water sample, 3# boiler blow-down water sample；
(2) each 10mL of sample 1-3# prepared in step (1) is taken, is placed in polytetrafluoroethylene (PTFE) counteracting tank, according to certain
Program carries out micro-wave digestion experiment, and after program operation, taking-up counteracting tank is in cooling in ventilating kitchen, to temperature in tank and room
It after temperature balance, deflates, uncap, remove digestion solution in tank and swing decontamination solution top tank structure twice with experimental water into 50mL volumetric flask,
It collects all solution and is diluted with water to groove, it is to be measured.Micro-wave digestion experimental arrangement is the microwave digestion temperature of boiler feedwater sample
It is 170 DEG C, retention time 10min；The microwave digestion temperature of boiler water sample is 185 DEG C, retention time 15min；Boiler
180 DEG C, retention time 12min of the microwave digestion temperature of return water sample, the retention time is holding after reaching digestion condition
The continuous time.
(3) condition is functioned as follows with inductively coupled plasma emission spectrography to be measured the water sample after resolution,
Operating condition and elemental analysis line are as follows: radio-frequency power 1100W, and atomization gas flow is 0.7L/min, and secondary air amount is
0.5L/min, height of observation 15mm, pump speed 70r/min, duplicate reading 3 times, the calcium, magnesium, iron, copper elemental analysis line
For calcium 393.37nm, magnesium 279.55nm, iron 238.20nm, copper 327.39nm；The working principle of ICP-AES is to utilize argon plasma
The high temperature that body generates makes sample be decomposed to form the atom and ion of excitation state completely, since the atom and ion of excitation state are unstable
Fixed, outer-shell electron can be from excitation state to low energy level transition, therefore launches characteristic spectral line.After grating beam splitting, inspection is utilized
The intensity of device detection characteristic spectral line is surveyed, to measure the content of element to be measured in sample.
(4) use experimental water that water sample is replaced to detect by above-mentioned steps are synchronous using as blank assay.
It is essentially selection instrument since calcium, magnesium, iron, the content of four kinds of metallic elements of copper are relatively low in boiler feed water
Recommend the first sensitivity line of element, i.e., for highly sensitive line as analytical line, every kind of element can a plurality of characteristic spectrum of simultaneous selection
For line as analytical line, the response intensity of different wave length is different, also different to different element anti-interference abilities.In analysis test
Before, 2 spectral lines are selected as analytical line to element to be measured and are tested, spectrum comparison is carried out by test mixed standard solution,
From emissive porwer, co-existing element interference situation, peak shape, stability, detection limit, etc. selected, choose response intensity value
The spectral line high, small by co-existing element interference, peak shape is good, stability is strong, detection limit is low as analytical line, be shown in by analytical line selection result
Following table.
The selection of the elemental analysis line to be measured of table 1
Temperature and two parameters of retention time when micro-wave digestion have important influence to the result of micro-wave digestion, the present invention
The water supply of steam boiler of model WNS6-1.25-Y.Q, boiler water, return water are chosen respectively in advance as research object, 3 kinds of water
Sample carries out mark-on processing respectively, the 100mg/L mixed standard solution of 2mL is separately added into 50mL water sample, using unitary variant
Method is studied, and is optimized respectively to two parameters of microwave digestion temperature and retention time in micro-wave digestion pre-treating method
It discusses.
Micro-wave digestion uses temperature programming, and 10min is interior to reach certain setting temperature from room temperature, and is kept for certain time.
Test has investigated the retention time respectively as 20min, and water supply, boiler water, return water are 120 DEG C, 140 in the microwave digestion temperature of setting
DEG C, 170 DEG C, 180 DEG C, 185 DEG C, under the conditions of 190 DEG C, the concentration of calcium, magnesium, iron, copper that ICP-AES is measured.The result is shown in Figure 1~figure
3.It can be seen from the figure that digestion condition-concentration relationship variation tendency of three kinds of water samples is consistent, i.e., with digestion condition
Rising, the concentration of element to be measured also rises with it, and when temperature reaches certain value, concentration of element to be measured variation is unobvious.It gives
When the digestion condition of water reaches 170 DEG C, the concentration value of element to be measured reaches maximum in sample；The digestion condition of return water reaches 180
DEG C when, the concentration of element to be measured reaches maximum in sample；When the digestion condition of boiler water reaches 185 DEG C, element to be measured in sample
Concentration reach maximum.Three kinds of water samples when temperature is increased to 190 DEG C, due to hypertonia in counteracting tank, open by counteracting tank
Beginning pressure release.This is because concentrated nitric acid can be chemically reacted with the impurity in water, organic matter, inorganic matter, suspended matter, precipitating, with
Gradually rising for temperature, react to positive balance direction carry out, effectively remove impurities in water, organic matter, inorganic matter, suspension
Object, precipitating, so that sample matrices tend to simply, concentration of element to be measured is gradually risen in water；When temperature reaches certain value, complete
Resolution, the concentration of element to be measured in water reach balance.It salt content in boiler water, impurity and is introduced by water treatment organic
Object, inorganic matter are high compared with water supply and return water content, and boiler water is to prevent fouling and corrosion and maintain certain basicity, hydrogen-oxygen in water
Root can form the magnesium hydroxide, iron hydroxide, Kocide SD for being insoluble in water with element to be measured, and be slightly soluble in the hydroxide of water
Calcium, thus organic matter, inorganic matter, the content of indissoluble substance are most in boiler water；Water supply is due to by resins exchange or reverse osmosis
It handles, is practically free of impurity in water supply；Return water contains a certain amount of iron in water sample due to passing through water return pipeline.Therefore boiler
Digestion condition highest required for water, digestion condition required for water supply is minimum, and return water is placed in the middle.
Retention time is too long, and Specimen eliminating is complete, but wastes time, and is unfavorable for quickly analyzing；Retention time is too short, sample
Not exclusively, measurement result is relatively low for resolution.Test investigated respectively the retention time 5min, 8min, 10min, 12min, 15min,
Under the conditions of 18min, inductively coupled plasma atomic emission spectrometry (ICP-AES) measure water supply, boiler water, calcium in return water,
The concentration of magnesium, iron, copper, is as a result shown in Fig. 4~Fig. 6.It can be seen from the figure that the change of the retention time-concentration relationship of three kinds of water samples
Change trend is consistent, i.e., as the increase of retention time, the concentration of element to be measured also rise with it, reaches one when the retention time
When definite value, concentration of element variation to be measured is unobvious.When the retention time of water supply reaches 10min, concentration of element value to be measured is maximum；It returns
When the retention time of water reaches 12min, concentration of element value to be measured is maximum；When the retention time of boiler water reaches 15min, member to be measured
Plain concentration value is maximum.This is because resolution reaction is more and more thorough with the increase of retention time, matrix composition gradually tends to be single
One, the concentration of element to be measured increases therewith.Water supply, return water, the matrix composition of boiler water are gradually complicated, organic matter, nothing in water sample
Time required for the ingredients such as machine object and concentrated nitric acid react gradually increases, therefore boiler water retention time longest, the holding of water supply
Time is most short, and return water is placed in the middle.
Measure the calibration curve and detection limit of the present embodiment
With volume fraction be 5% dust technology dilute hybrid standard stock solution, be configured to mass concentration be 0,0.05,
0.10, the serial mixed standard solution of 0.50,1.0,2.0mg/L, measures its spectral intensity.It is cross with elemental mass concentration to be measured
Coordinate, emissive porwer are ordinate, draw standard curve.Then matrix blank solution is carried out METHOD FOR CONTINUOUS DETERMINATION 10 times, with 10 times
3 times of measurement result standard deviation are used as detection limit, 5 times of Determination Limits as this method of detection limit.The line of element to be measured
Property range, standard deviation, detection limit, Determination Limit are shown in Table 2.
The range of linearity of the element to be measured of table 2, regression equation, standard deviation, detection limit, Determination Limit
Measure the precision of the present embodiment
By detection method of the present invention, 7 parallel determinations are carried out respectively, precision of the invention is detected, are tied
Fruit such as table 3.The relative standard deviation (RSD) of each element to be measured is 0.38%~9.32%.
3 precision measurement result (n=7) of table
Measure the rate of recovery of the present embodiment
The mark-on reclaims test that sample is carried out according to experimental method, calculates its recovery of standard addition.The rate of recovery=(measurement is total
Amount-measured value) ÷ additional amount × 100%.The results are shown in Table 4, the recovery of standard addition of each element to be measured 95%~103% it
Between, as a result it is satisfied with.
4 recovery of standard addition measurement result of table
The present embodiment and absorption process measurement result compare
After being measured to 1# water supply, 2# boiler water, 3# return water water sample according to experimental method, and Atomic absorption is used simultaneously
Method (AAS) tests 3 samples and carries out result comparison, analyzes result such as table 5.As can be seen from Table 5, the present embodiment measurement result
It is almost the same with AAS measurement result.
5 sample analysis result of table and result control
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (2)
1. a kind of micro-wave digestion-inductively coupled plasma emission spectrography measurement Industrial Boiler water in calcium, magnesium, iron, copper
Method, which comprises the steps of:
(1) 100mL boiler feed water water sample is measured, 1.5mL concentrated nitric acid is added immediately, so that water sample is acidified to pH value 1, when in water sample
When suspended matter is more, store in vinyon bottle after using middling speed quantitative filter paper to filter as sample；
(2) it takes the sample 10mL prepared in step (1) to be placed in polytetrafluoroethylene (PTFE) counteracting tank, carries out micro-wave digestion experiment, to
After program is run, takes out counteracting tank and deflate, uncap after temperature in tank and equilibrium at room temperature in cooling in ventilating kitchen, remove
Digestion solution swings decontamination solution top tank structure at least twice with experimental water into 50mL volumetric flask in tank, collects all solution and adds water
It is diluted to groove, it is to be measured；
(3) it functions as follows condition with inductive coupling plasma emission spectrograph to be measured water sample, operating condition and member
Plain analytical line is as follows: radio-frequency power 1100W, and atomization gas flow is 0.7L/min, secondary air amount 0.5L/min, and observation is high
Degree be 15mm, pump speed 70r/min, duplicate reading 3 times；The calcium, magnesium, iron, copper elemental analysis line be calcium 393.37nm, magnesium
279.55nm, iron 238.20nm, copper 327.39nm；
(4) use experimental water that boiler feed water water sample is replaced to detect by above-mentioned steps are synchronous with sample using as blank assay.
2. a kind of micro-wave digestion as described in claim 1-inductively coupled plasma emission spectrography measurement Industrial Boiler is used
The method of calcium, magnesium, iron, copper in water, which is characterized in that the boiler feed water water sample include boiler feedwater sample, boiler water sample,
Boiler blow-down water sample, the setting of micro-wave digestion program are as follows: the microwave digestion temperature of boiler feedwater sample is 170 DEG C, the retention time
For 10min；The microwave digestion temperature of boiler water sample is 185 DEG C, retention time 15min；The microwave of boiler blow-down water sample disappears
180 DEG C of temperature of solution, retention time 12min, the retention time is the duration after reaching digestion condition.
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| CN113109323A (en) * | 2021-04-15 | 2021-07-13 | 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) | Method for determining main heavy metal elements in marine sediments |
| CN113324978A (en) * | 2021-06-01 | 2021-08-31 | 天津市食品安全检测技术研究院 | Method for detecting calcium and iron in health food |
| CN114324309A (en) * | 2022-01-04 | 2022-04-12 | 新余钢铁股份有限公司 | ICP (inductively coupled plasma) measuring method for synchronously testing total hardness, phosphate radical and iron in industrial water |
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| CN113109323A (en) * | 2021-04-15 | 2021-07-13 | 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) | Method for determining main heavy metal elements in marine sediments |
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| CN114324309A (en) * | 2022-01-04 | 2022-04-12 | 新余钢铁股份有限公司 | ICP (inductively coupled plasma) measuring method for synchronously testing total hardness, phosphate radical and iron in industrial water |
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Application publication date: 20190101 |