CN109765288A - A kind of quantitative analysis method of rare earth element Interwell tracer - Google Patents
A kind of quantitative analysis method of rare earth element Interwell tracer Download PDFInfo
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Abstract
The invention discloses a kind of quantitative analysis methods of rare earth element Interwell tracer, belong to rare earth element Interwell tracer measurement field.The quantitative analysis method of rare earth element Interwell tracer of the present invention, including filter, pre- resolution, micro-wave digestion, catch up with acid cut appearance, drafting standard curve, measuring and etc..The method of the present invention is sufficiently to be cleared up organic matter using pre- resolution-microwave procedure digestion procedure, it removes matrix bring " carbon effect ", simultaneously using collision pool technology and online Internal standard correction methods further remove between other oxides and rare earth element it is equal interfere, to reach the stability of detection, precision and accuracy.
Description
Technical field
The invention belongs to rare earth element Interwell tracers to measure field, and in particular to a kind of rare earth element Interwell tracer
Quantitative analysis method.
Background technique
Inter-well tracer test technology is to inject tracer in oil well, and then around, producing well detects its output situation, and
Tracer curve is drawn, to obtain oil reservoir and oil well information.In recent years, trace matter detection inter-well tracer test monitoring technology,
Stablize especially with the chemical substance of rare earth element, and be not widely present in the Nature, is that one kind can find the good of oil sources
Good tracer, many oil field mining sites are used widely at home.Therefore, a kind of Interwell tracer (yttrium, scandium, group of the lanthanides etc. are studied
16 kinds of rare earth elements, except promethium) accurate quantitative analysis method it is crucial for inter-well tracer test monitoring technology, and very
A ring.
Since the sample of rare earth tracer is using underground water as matrix, and with a certain amount of organic matter, ingredient is very complicated.
Traditional analysis method such as X-ray fluorescence spectra (XRF), inductively coupled plasma spectrometry (ICP-AES) are difficult to solve base
The problem of soma is disturbed.Although icp ms (ICP-MS) can solve Matrix effects problem, such sample
For product often with certain organic matter is contained, carbon effect and carbon accumulation can be generated by directly being measured using ICP-MS, influence detection
Precision and accuracy, especially Sc element.It is flat by the way that other organic matters (such as methanol) progress carbon is added there are also method
Weighing apparatus is to reduce Matrix effects, although the problem of can solve Matrix Match, without eliminating carbon accumulation problem.Because of carbon in sample
Excessive concentration prevent plasma from the carbon in fully oxidized sample, cause carbon particle to be deposited at interception taper hole, significantly
Influence the stability of test.Meanwhile the content of organics in different samples be it is indefinite, for the additional amount of Carbon balance reagent
Be not it is fixed, additional amount and sample have substantial connection also just not have versatility.
Summary of the invention
The problem of for existing method, the purpose of the present invention is more complicated, the examples for oil field water constituent between well
If impurity is more, the features such as salinity is high, and organic matter is more, a kind of accurate quantitative analysis method of rare earth element Interwell tracer is provided.
In order to achieve the above object, the technical solution of the present invention is as follows:
A kind of quantitative analysis method of rare earth element Interwell tracer, comprising the following steps:
(1) filter: sample to be tested is filtered through middling speed quantitative filter paper, filters the grains of sand, is removed upper oil phase, is isolated limpid
Oil field water；
(2) pre- resolution: accurately pipetting the above-mentioned filtered oil field water of 5mL, and 10mL concentrated nitric acid is added, pre- to clear up；
(3) micro-wave digestion: adding 5ml concentrated nitric acid and 3ml hydrogen peroxide into the oil field water after above-mentioned pre- resolution, carries out micro-
Wave resolution；
(4) it catches up with acid cut to hold: after the completion of resolution, acid being caught up with to be mixed to 1-2mL with 2% dust technology transfer constant volume at 180 DEG C,
It is to be measured；
(5) draw standard curve: prepare contain rare earth element to be measured series of standards working solution, take rhodium internal standard and
The helium crash mode of icp ms removes interference, draws standard curve；
(6) it measures: taking the helium of rhodium internal standard and icp ms to collide mould test solution in step (3)
Formula removal interference, the data measured import standard curve, obtain rare earth element content.
Pre- resolution parameter on the basis of above scheme, in the step (2) are as follows: 120 DEG C -150 DEG C of temperature；Time 1
~1.5h.
Micro-wave digestion program on the basis of above scheme, in the step (3) are as follows: 0 DEG C -110 DEG C, climb 10min,
Keep 10min；110 DEG C -150 DEG C, climb 5min, keeps 10min；150 DEG C -180 DEG C, climb 10min, keeps 50min；Microwave
Power is 1000W~1500W.
On the basis of above scheme, the running parameter of icp ms in the step (5) are as follows:
Analytical model is KED mode；Online Rh internal standard adding manner；Collision gas flow: 3mL/min；Nebulizer flow:
1.02L/min；Secondary air amount: 1.2L/min；Plasma flow amount: 18L/min；RF power: 1600W.
On the basis of above scheme, the concentration ladder of the series of standards working solution of rare earth element in the step (5)
Degree is 0ng/mL, 0.05ng/mL, 0.10ng/mL, 0.50ng/mL, 1.00ng/mL, 2.00ng/mL, 5.0ng/mL.
On the basis of above scheme, the rare earth element be Ce140, Dy164, Er166, Eu153, Gd158, Ho165,
At least one of La139, Lu175, Nd142, Pr141, Sc45, Sm152, Tb159, Tm169, Y89, Yb174.
The advantages of technical solution of the present invention:
The present invention take filtering, step by step resolution etc. modes can eliminate the grains of sand and organic matter etc. interference.
And organic matter close for mass number between rare earth element to be measured clears up the CO not exclusively generated2Scandium element is determined
Situations such as amount analysis generates interference takes rhodium internal standard and the helium crash mode of icp ms to remove dry
It disturbs, each element detection limit can reach 0.05ppb or more, reach the more accurate purpose of each element detection data.
The method of the present invention is sufficiently to be cleared up organic matter using pre- resolution-microwave procedure digestion procedure, removes matrix
Bring " carbon effect ", can completely remove the interference problem of carbon enhanced sensitivity and carbon accumulation because of caused by carbon content height.Benefit simultaneously
With collision pool technology and online Internal standard correction methods further remove between other oxides and rare earth element it is equal interfere, to reach detection
Stability, precision and accuracy.Method is easy, the measurement of most samples suitable for real work.
Detailed description of the invention
Fig. 1 is Ce140 elemental standards gradient matched curve figure；
Fig. 2 is Dy164 elemental standards gradient matched curve figure；
Fig. 3 is Er166 elemental standards gradient matched curve figure；
Fig. 4 is Eu153 elemental standards gradient matched curve figure；
Fig. 5 is Gd158 elemental standards gradient matched curve figure；
Fig. 6 is Ho165 elemental standards gradient matched curve figure；
Fig. 7 is La139 elemental standards gradient matched curve figure；
Fig. 8 is Lu175 elemental standards gradient matched curve figure；
Fig. 9 is Nd142 elemental standards gradient matched curve figure；
Figure 10 is Pr141 elemental standards gradient matched curve figure；
Figure 11 is Sc45 elemental standards gradient matched curve figure；
Figure 12 is Sm152 elemental standards gradient matched curve figure；
Figure 13 is Tb159 elemental standards gradient matched curve figure；
Figure 14 is Tm169 elemental standards gradient matched curve figure；
Figure 15 is Y89 elemental standards gradient matched curve figure；
Figure 16 is Yb174 elemental standards gradient matched curve figure.
Specific embodiment
Term as used in the present invention generally has those of ordinary skill in the art usual unless otherwise specified
The meaning of understanding.
Combined with specific embodiments below, and referring to the data further detailed description present invention.Following embodiment only be
It illustrates the present invention, rather than limits the scope of the invention in any way.
Embodiment
A kind of quantitative analysis method of rare earth element Interwell tracer
1. filtering
Sample is filtered through middling speed quantitative filter paper, filters the impurity such as the grains of sand, and the organic matters such as removal upper oil phase are isolated about
10mL limpid oil field water.
2. pre- resolution
5mL filtrate is accurately pipetted from above-mentioned filtrate into digestion tube, and 10mL concentrated nitric acid is added, is placed in pre- resolution instrument,
120 DEG C -150 DEG C, 1~1.5h is cleared up in advance.
3. micro-wave digestion
5ml concentrated nitric acid and 3ml hydrogen peroxide are added into the oil field water after pre- resolution, is placed in microwave dissolver.Resolution
Program: 0 DEG C -110 DEG C, climb 10min, keeps 10min；110 DEG C -150 DEG C, climb 5min, keeps 10min；150℃-180
DEG C, climb 10min, keeps 50min, and microwave power is 1000W~1500W.
4. catching up with acid, the dilute constant volume of acid
After resolution, digestion tube is placed in and is caught up in sour instrument, is caught up with acid to 1-2mL at 180 DEG C, with 2% dust technology
Constant volume is shifted, is mixed, it is to be measured.
5. the configuration of internal standard solution and standard curve
Series of standards solution gradient and Rh inner mark solution are configured with 2% nitric acid constant volume, takes rhodium internal standard and inductive coupling
The helium crash mode of plasma mass spectrograph removes interference, draws standard curve.
Optical viewer vacuum degree situation before measurement, the instrumental response value with helium purge collision cell to rhodium internal standard element are steady
It is fixed.
The running parameter of the icp ms are as follows:
Analytical model is KED mode；Online Rh internal standard adding manner；Collision gas flow: 3mL/min；Nebulizer flow:
1.02L/min；Secondary air amount: 1.2L/min；Plasma flow amount: 18L/min；RF power: 1600W.
Wherein the inner mark solution concentration and rare earth element concentration of standard solution gradient are as shown in table 1:
1 inner mark solution concentration of table and rare earth element concentration of standard solution gradient
6. measurement
Standard blank is done with 2% dust technology, respectively 5 Plays solution concentration of analytical procedure, according to the line of intensity and concentration
Matched curve is drawn in sexual intercourse.
Rhodium internal standard and the helium crash mode of icp ms is taken to remove test solution in step (3) dry
It disturbs, the data measured import standard curve, and each rare earth element content in sample is calculated.
Each element normal gradients matched curve figure is respectively as shown in Fig. 1~16:
By Fig. 1~16 it is found that each rare earth element matched curve is good, detection limit can reach 0.05ppb or more.
For the precision and accuracy for further investigating method, mark-on reclaims test, gained recycling are carried out to each element
Rate is between 80%-120.
Influence of the different operating parameter to detection precision
The scheme of pre- resolutions different from the method for the present invention, micro-wave digestion and instrument analytical model is respectively adopted, measurement disappears in advance
Influence of the variation of solution, micro-wave digestion and instrument analytical model parameter to the method for the present invention result, as shown in table 2, except institute in table 2
Outside the parameter of column, other parameters are identical as the parameter of the method for the present invention.
2 different parameters of table change the influence to the method for the present invention result (sampling amount is all 5mL)
Pass through the data of upper table 2, it can be seen that in the case that the additional amount and digestion time of reagent are inadequate, testing result
The rate of recovery and precision do not reach requirement, illustrate that the organic matter in sample is not cleared up completely, the CO of generation2To members such as Sc
Element interferes.With the increase of nitric acid and hydrogen peroxide use, interference is further eliminated using the crash mode of ICP-MS,
The more satisfactory rate of recovery and precision are reached.If continuing the amount of increasing nitric acid and hydrogen peroxide, phase can may be also obtained
With as a result, but will lead to the extension for catching up with the sour time using excessive acid, influence experiment efficiency, and acidity is excessively high can be to instrument
Device generates irreversible influence.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.
Claims (6)
1. a kind of quantitative analysis method of rare earth element Interwell tracer, it is characterised in that: the following steps are included:
(1) filter: sample to be tested is filtered through middling speed quantitative filter paper, filters the grains of sand, is removed upper oil phase, is isolated limpid oil field
Water；
(2) pre- resolution: accurately pipetting the above-mentioned filtered oil field water of 5mL, and 10mL concentrated nitric acid is added, pre- to clear up；
(3) micro-wave digestion: adding 5ml concentrated nitric acid and 3ml hydrogen peroxide into the oil field water after above-mentioned pre- resolution, carries out microwave and disappears
Solution；
(4) it catches up with acid cut to hold: after the completion of resolution, acid being caught up with to be mixed to 1-2mL with 2% dust technology transfer constant volume at 180 DEG C, to
It surveys；
(5) it draws standard curve: preparing the series of standards working solution for containing rare earth element to be measured, take rhodium internal standard and inductance
The helium crash mode of couple plasma mass spectrometer removes interference, draws standard curve；
(6) it measures: taking the helium crash mode of rhodium internal standard and icp ms to go test solution in step (3)
Except interference, the data measured import standard curve, obtain rare earth element content.
2. the quantitative analysis method of rare earth element Interwell tracer according to claim 1, it is characterised in that: the step
(2) the pre- resolution parameter in are as follows: 120 DEG C -150 DEG C of temperature；1~1.5h of time.
3. the quantitative analysis method of rare earth element Interwell tracer according to claim 1, it is characterised in that: the step
(3) the micro-wave digestion program in are as follows: 0 DEG C -110 DEG C, climb 10min, keeps 10min；110 DEG C -150 DEG C, climb 5min, keeps
10min；150 DEG C -180 DEG C, climb 10min, keeps 50min；Microwave power is 1000W~1500W.
4. the quantitative analysis method of rare earth element Interwell tracer according to claim 1, it is characterised in that: the step
(5) running parameter of icp ms in are as follows: analytical model is KED mode；Online Rh internal standard adding manner；
Collision gas flow: 3mL/min；Nebulizer flow: 1.02L/min；Secondary air amount: 1.2L/min；Plasma flow amount:
18L/min；RF power: 1600W.
5. the quantitative analysis method of rare earth element Interwell tracer according to claim 1, it is characterised in that: the step
(5) in the concentration gradient of the series of standards working solution of rare earth element be 0ng/mL, 0.05ng/mL, 0.10ng/mL,
0.50ng/mL、1.00ng/mL、2.00ng/mL、5.0ng/mL。
6. the quantitative analysis method of any one rare earth element Interwell tracer according to claim 1~5, it is characterised in that:
The rare earth element be Ce140, Dy164, Er166, Eu153, Gd158, Ho165, La139, Lu175, Nd142, Pr141,
At least one of Sc45, Sm152, Tb159, Tm169, Y89, Yb174.
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Cited By (2)
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| CN110749642A (en) * | 2019-10-29 | 2020-02-04 | 中广核工程有限公司 | Tracer element concentration detection method for steam generator humidity measurement test |
| CN113376244A (en) * | 2021-07-21 | 2021-09-10 | 青岛大地新能源技术研究院 | Detection method of thickened oil water-soluble tracer |
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| CN110749642A (en) * | 2019-10-29 | 2020-02-04 | 中广核工程有限公司 | Tracer element concentration detection method for steam generator humidity measurement test |
| CN113376244A (en) * | 2021-07-21 | 2021-09-10 | 青岛大地新能源技术研究院 | Detection method of thickened oil water-soluble tracer |
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