CN101221127A - Concurrent measuring method for multiple metallic elements in transformer oil - Google Patents

Concurrent measuring method for multiple metallic elements in transformer oil Download PDF

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Publication number
CN101221127A
CN101221127A CNA2007101396190A CN200710139619A CN101221127A CN 101221127 A CN101221127 A CN 101221127A CN A2007101396190 A CNA2007101396190 A CN A2007101396190A CN 200710139619 A CN200710139619 A CN 200710139619A CN 101221127 A CN101221127 A CN 101221127A
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transformer oil
sample
metallic element
temperature
multiple metallic
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CN101221127B (en
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石景燕
孙心利
李振海
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Hebei Electric Power Co Ltd
Hebei Electric Power Construction Adjustment Test Institute
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Electric Power Research Institute of State Grid Hebei Electric Power Co Ltd
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Abstract

The invention relates to a method for simultaneously determining various metal elements in transformer oil. An analyzing sample of the transformer oil of the invention is weighed quantificationally after a collected oil sample is heated and stirred uniformly; an infrared heating method is adopted for carrying out vaporizing and carbonizing at constant temperature on the analyzing sample of the quantificational transformer oil, a box type high temperature furnace is adopted for carrying out high temperature cineration on the carbonized sample, acid liquid is adopted for carrying out dissolving on the incinerated sample under the lower temperature heating condition, a soluzione leggermente acida is adopted for carrying out diluting and volume fixing on the dissolved sample to be prepared into analyzing liquid. The analyzing liquid accurately determines the content of various metal elements by using a complete spectrum direct reading plasma emission spectrum apparatus. The method of the invention can determine a plurality of elements and has high accuracy, can determine oil mediums with different varieties and content ranges, being capable of accurately showing the change current of the metals in the oil mediums and being convenient for accurately analyzing and finding out hidden troubles in time.

Description

Determination method multiple metallic element time the in a kind of transformer oil
Technical field
Determination method when patent of the present invention relates in a kind of transformer oil multiple metallic element.
Technical background
In recent years, for adapting to the development and national economy needs, country had strengthened the investment of power industry, and increasing high capacity unit puts into operation in succession.Along with the construction of big electrical network, the safety of electrical network is also increasing to influence of society, and in many factors that influences power grid security, because the existence of excess metal impurity and the power equipment operation troubles and the accident that cause take place frequently in various places in recent years in the oil.But the problem that causes owing to metallic impurity in the oil also is not familiar with fully.Relevant metallic impurity cause fault, and the research of the analytical approach of metallic impurity also more and more causes domestic and international numerous researchists' attention in the oil.But at present,, both do not had national standard method, do not had corresponding industry analysis method yet, caused the poor efficiency of crash analysis and expensive thus, can't supervise the operation of equipment safely and effectively yet about the detection of metallic impurity in the transformer oil.
Conventional stratographic analysis result can show whether fault overheated and discharge takes place in the transformer, but can't failure judgement occur in what position or loop actually, if increase the analysis data of metallic element this moment, again in conjunction with electric index, problem has taken place, which kind of fault has taken place in the parts that just can accurately judge what material, greatly reduces the maintenance difficulty, saves the repair time, saves recondition expense.At present, the fault and the accident that cause because of the excessive existence of metallic element in the transformer oil constantly take place, but Determination of Metal Elements had not but both had national standard in the transformer oil, did not have industry standard yet, and this is serious problems that press for solution.
First because in recent years a lot of excessive existence because of metallic element in the transformer oil take place and cause big power equipment operation troubles; Second because do not have the standard method of metallic element in the transformer oil at present and cause the expensive poor efficiency of fault handling, directly influenced the safe operation of electrical network.
Summary of the invention
Technical matters solved by the invention provides the wherein method of metallic element of a kind of pre-service of transformer oil and quantitative measurement.
The present invention adopts following technical scheme:
(1) the transformer oil analytic sample among the present invention is heated for the oil sample of gathering and is quantitatively taken by weighing after shaking up;
(2) the present invention adopts the Infrared Heating method that quantitative transformer oil analytic sample is carried out evaporation at constant temperature and carbonization;
(3) sample after the present invention adopts box high temperature furnace to carbonization carries out the high temperature ashing;
(4) the present invention adopts and to dissolve with the sample of acid solution after to ashing under the low-temperature heat condition;
(5) sample after the present invention adopts dilute acid soln to dissolving dilutes and constant volume, is prepared into analysis solution;
(6) analytical solution is accurately measured the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
Transformer oil analytic sample of the present invention is heated for the oil sample of gathering and is quantitatively taken by weighing after shaking up, promptly heat 15-20min down at 50-60 ℃, taking-up shakes up, the range of weighing of described transformer oil analytic sample is controlled at 10g-20g, and being accurate to 0.001g, sample places the quartz beaker of dried and clean.
Employing Infrared Heating method of the present invention is carried out evaporation at constant temperature and carbonization to quantitative transformer oil analytic sample, and the Infrared Heating step is to adopt the ceramic infrared electric heating plate of controllable temperature to carry out under 260 ℃ ± 10 ℃ temperature, till carbonization.
Of the present invention sample after the carbonization is carried out the high temperature ashing, the high temperature ashing is slowly to be warmed up to 625 ℃ from room temperature, and under 625 ℃ ± 5 ℃, kept 60 minutes, be that the high temperature ashing is to adopt box high temperature furnace slowly to be warmed up to 625 ℃ from room temperature, and under 625 ℃ ± 5 ℃, kept 60 minutes, be beneficial to thorough ashing.
Employing of the present invention is being dissolved with the sample of acid solution after to ashing under the low-temperature heat condition, is the HNO that added earlier 1: 1 with sour heating for dissolving step 34.5-5.5ml, add 1: 1 HCl 13.5-16.5ml again, under 80-110 ℃ of temperature heating for dissolving to solution concentration to 1-3ml, be the HNO that added earlier 1: 1 promptly with sour heating for dissolving 3, add 1: 1 HCl (HNO wherein again 3With the additional proportion of HCl be 1: 3), low-temperature heat is dissolved to the surplus 1-3ml of solution.
The sample of employing dilute acid soln of the present invention after to dissolving dilutes and constant volume, is prepared into analysis solution, and the dilution constant volume is solution quantitatively to be diluted in the volumetric flask of 25ml-50ml with rare nitric acid of 2%;
Analytical solution of the present invention is accurately measured the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
Transformer oil analytic sample of the present invention is handled according to two kinds of situations: first kind of situation is if transformer oil is untapped, clean, new transformer oil, to the transformer oil gathered directly weighing be analytic sample, second kind of situation is if transformer oil was to use, has impurity, just need under 55 ± 5 ℃ temperature, keep 10-15 minute the transformer oil of gathering, shake up weighing again as analytic sample.
The condition that the present invention carries out the full spectrum direct-reading plasma emission spectrometer of multielement simultaneous determination is: echelle grating, the pouring-in detecting device of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.0L/min, secondary air amount 1.0L/min, plasma gas flow rate 1.0L/min, sample size 1.85ml/min, atomizer pressure are 28psi, peristaltic pump rotating speed 130Z/min.
Dilution constant volume of the present invention is with rare nitric acid of 2% solution quantitatively to be diluted in the volumetric flask of 25ml-or 50ml.
Of the present inventionly measure multiple element simultaneously and be meant in, can measure elements such as copper, iron, zinc, aluminium, chromium, manganese, silver, nickel simultaneously with the transformer oil sample solution of once handling.
All vessel in the scheme of the present invention are all used 1: 1 HNO before use 3Soaked 24 hours, with high purity water cleaning, drying for standby.This programme can overcome the pollution in the experimentation to greatest extent, and the metallic element meaning that trace is existed is very big.
Good effect of the present invention is as follows: a large amount of existence of metallic impurity in the oily medium, have a strong impact on the insulating property of equipment, and can cause security incidents such as overheated, oil flow electrification, multipoint earthing, paradoxical discharge, and then quicken oil quality deterioration, have a strong impact on the safe operation of equipment.By measuring the metal ingredient in the oily medium, can grasp the operation variation tendency of oily medium, increase very fast or variation abnormality if find the content of a certain element or several elements, unusual wearing and tearing, corrode, overheated still discharge might appear in which position that can in time judge which parts, in conjunction with chromatogram index and electric index, just can accurately judge unusual concrete position takes place again.
Detect the content of metallic impurity in the oily medium, grasp various change of elements scopes and development trend, not only can judge the quality good or not and the equipment running status of fresh oil, also help and in time take to operate targetedly that the equipment that guarantees to greatest extent is in a safe condition operation.
The present invention is in conjunction with the parts material of transformer and to the influence degree of security of operation, from helping nine kinds of elements such as many-sided screening such as fault judgement, cause investigation and instrumental analysis copper, iron, zinc, chromium, manganese, silver, aluminium.Adopt the Infrared Heating method of domestic initiation to carry out sample carbonization, high temperature ashing, carry out the processing of sample with the method for acid dissolving at last, use the dilute acid soln constant volume then, under optimum optimizing condition, finish the quantitative measurement of metallic element with full spectrum direct-reading plasma emission spectrometer, adopt U.S. constand s-21 standard miscella to carry out the degree of accuracy of this method and the test of accuracy and recovery of standard addition, realize satisfactory results.It is many that the inventive method is measured element, and the accuracy height can be measured the oily medium of variety classes (comprising transformer oil, lubricated wet goods) and different content scope (ppb to ppm all can).The accurate mensuration of element can guarantee the accurate location of fault, can accurately embody the variation tendency of metal in the oily medium, is convenient to accurate analysis, in time scents a hidden danger; Can guarantee the safe and stable operation of equipment.
The development of the inventive method has overcome also that the direct injected method can only be measured oil soluble metal, can only measure particle less than several microns, tenor is difficult for accurately defectives such as mensuration less than 10ppb; The inventive method can not brought other impurity into as thinning agent because of introducing a large amount of aviation kerosenes with the dilute acid soln constant volume of high purity water preparation.
Heating means of the present invention can guarantee the quick thermally equivalent of the transformer oil that is heated, and can not splash, and can not introduce other impurity.The present invention adopts mixed-acid dissolution can measure oil-soluble and non-oil-soluble metallic element simultaneously, can measure the metallic element of variable grain size, different content scope.Adopt full spectrum direct-reading plasma emission spectrometer can realize that the multiple metallic element of different content measures simultaneously.
Nonisulated impurity content in the oil medium is generally smaller, but when abnormal conditions took place, tenor wherein can increase hundred times, the amplitude of variation of impurity content is very big, can be from several ppb to several ppm, and the impurity element kind that may exist in the oily medium is various.The inventive method adopts inductively coupled plasma emission spectrography, and this method is highly sensitive, and accuracy is good, and the interference between the element is few, and the range of linearity of working curve is wide, can measure multiple element simultaneously.
The molten method of ashing acid heats carbonization and high temperature ashing with sample earlier, adds acid again and is dissolved into the mensuration that aqueous solution is carried out spectrometer.The molten method of ashing acid is wider to the accommodation of sample, no matter seriously whether the pollution level of sample, no matter the size of impurity particle how in the sample, the content range of metallic element also can very wide (can regulate by sampling amount), all can obtain satisfied measurement result.
The present invention both had been applicable to new transformer oil, also was applicable to transformer oil used or that using.
Embodiment
The kind of metallic element is different with grain size, and the state that is presented in the fluid is incomplete same.Some presents suspended state, is suspended in the fluid, and the metal of some bulky grain, big proportion will be deposited in the fluid bottom.So, both reduced the viscosity of oily medium, be convenient to weighing, made also that impurity wherein was even 50-60 ℃ of heated sample.Therefore, before the test sampling, at first oil samples is heated to 50-60 ℃ and keep 15-20min, mixing takes by weighing sample then.
Select ceramic infrared electric heating plate to carry out the heating of sample, can keep the temperature difference of whole liquid smaller, easy control of temperature, efficiency of heating surface height approximately needed get final product in 4-6 hour to 10 heating evaporations that restrain samples.It is dried to allow oil samples be evaporated to, and neither the formation burning is splashed and also can not caused the process pollution, reaches quick and complete carbonization at last.
Experimental result shows that ashing temperature measured value plumbous and manganese in the time of 600 ℃ is on the low side, and the measured value of each element can meet the demands in the time of 625 ℃, therefore, according to measurement result and comprehensive many-sided factor, finally selects 625 ℃ of ashing temperature, and the ashing time is 60 minutes.
Use 1: 1 HCl or 1: 1 HNO singlely 3Handle sample, Instrument measuring result's amplitude of variation is bigger, and repeatability is not fine.Adopted 1: 1 HNO of first adding 5ml afterwards 3, adding 1: 1 HCl of 15ml again, the effect of sample dissolution is fine.Not only sample dissolution is complete, and, sample determination repeated satisfactory.In addition, by investigating under the different acidity emissive porwer of each element in the standard solution, wherein acidity be respectively 1%, 2%, 5%, 7% 4 kind of situation, experimental data shows: when acidity was controlled at 2% and 5%, the measurement result of each element was satisfied.Therefore, adopt 2% solution acidity, and the acidity of sample and the acidity of standard solution are consistent.
Embodiment 1: the representational oily medium that will collect is put into constant temperature oven, heats 15-20min down at 50-60 ℃, and taking-up shakes up.Accurately (size according to impurity level content is determined for weighing 10.000g or 20.000g, suitable with the ashing amount that guarantees sample) sample is in the 50ml quartz beaker, be positioned on the ceramic infrared electric heating plate, open ventilation equipment, adjust the temperature to 260 ℃ of heated sample, after sample becomes black solid, continue heating 30min again.Then quartz beaker carefully is positioned in the high temperature furnace, begins to warm to 625 ℃, and keep 60min down, guarantee that ashing is thorough at 625 ℃ from room temperature.
After the ashing, take out cooling.In quartz beaker, add 1: 1 HNO of 5ml 3, add 1: 1 HCl of 15ml again, when regulating electric plate temperature and be 100 ℃ of heated solutions to 1-3ml, cooling, HNO with 2% 3Sample solution is transferred in the 25ml polyethylene volume bottle constant volume.
With instrument parameter and the experiment condition of the solution behind the constant volume, on full spectrum direct-reading plasma emission spectrometer, carry out various Determination of Metal Elements according to the best.The optimum determining spectral line of each element is as shown in the table.
The optimum determining spectral line of each element
Measure element Aluminium Al Chromium Cr Copper Cu Iron Fe Plumbous Pb
Best spectral line nm 396.152 283.563 324.754 259.940 220.353
Measure element Manganese Mn Nickel Silver Ag Zinc Zn
Best spectral line nm 257.610 221.647 328.068 213.856
Embodiment 2: transformer oil analytic sample of the present invention is heated for the oil sample of gathering and is quantitatively taken by weighing after shaking up, and promptly at 50 ℃ of heating 15min down, taking-up shakes up, and the range of weighing of described transformer oil analytic sample is controlled at 15g;
The present invention adopts the Infrared Heating method that quantitative transformer oil analytic sample is carried out evaporation at constant temperature and carbonization, and the Infrared Heating step is to adopt the ceramic infrared electric heating plate of controllable temperature to carry out under 250 ℃ temperature, till carbonization;
The sample of the present invention after to carbonization carries out the high temperature ashing, and the high temperature ashing is slowly to be warmed up to 625 ℃ from room temperature, and keeps 60 minutes down at 625 ℃;
The present invention adopts is dissolving with the sample of acid solution after to ashing under the low-temperature heat condition, is 1: 1 HNO of adding earlier with sour heating for dissolving step 35ml adds 1: 1 HCl15ml again, under 95 ℃ of temperature heating for dissolving to solution concentration to 3ml;
Sample after the present invention adopts dilute acid soln to dissolving dilutes and constant volume, is prepared into analysis solution, and the dilution constant volume is solution quantitatively to be diluted in the volumetric flask of 50ml with rare nitric acid of 2%;
Analytical solution of the present invention is accurately measured the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
Transformer oil analytic sample of the present invention is handled according to two kinds of situations: first kind of situation is if transformer oil is untapped, clean, new transformer oil, to the transformer oil gathered directly weighing be analytic sample, second kind of situation is if transformer oil was to use, has impurity, just need keep 10 minutes down the transformer oil of gathering, shake up weighing again as analytic sample at 55 ℃.
The condition that the present invention carries out the full spectrum direct-reading plasma emission spectrometer of multielement simultaneous determination is: echelle grating, the pouring-in detecting device of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.0L/min, secondary air amount 1.0L/min, plasma gas flow rate 1.0L/min, sample size 1.85ml/min, atomizer pressure are 28psi, peristaltic pump rotating speed 130Z/min.
Embodiment 3: transformer oil analytic sample of the present invention is heated for the oil sample of gathering and is quantitatively taken by weighing after shaking up, and promptly at 55 ℃ of heating 17min down, taking-up shakes up, and the range of weighing of described transformer oil analytic sample is controlled at 10g;
The present invention adopts the Infrared Heating method that quantitative transformer oil analytic sample is carried out evaporation at constant temperature and carbonization, and the Infrared Heating step is to adopt the ceramic infrared electric heating plate of controllable temperature to carry out under 260 ℃ ± 10 ℃ temperature, till carbonization;
The sample of the present invention after to carbonization carries out the high temperature ashing, and the high temperature ashing is slowly to be warmed up to 625 ℃ from room temperature, and keeps 60 minutes down at 625 ℃;
The present invention adopts is dissolving with the sample of acid solution after to ashing under the low-temperature heat condition, is 1: 1 HNO of adding earlier with sour heating for dissolving step 35.5ml, add 1: 1 HCl 16.5ml again, under 110 ℃ of temperature heating for dissolving to solution concentration to 2ml;
Sample after the present invention adopts dilute acid soln to dissolving dilutes and constant volume, is prepared into analysis solution, and the dilution constant volume is solution quantitatively to be diluted in the volumetric flask of 50ml with rare nitric acid of 2%;
Analytical solution of the present invention is accurately measured the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
Transformer oil analytic sample of the present invention is handled according to two kinds of situations: first kind of situation is if transformer oil is untapped, clean, new transformer oil, to the transformer oil gathered directly weighing be analytic sample, second kind of situation is if transformer oil was to use, has impurity, just need under 50 ℃ temperature, keep 13 minutes the transformer oil of gathering, shake up weighing again as analytic sample.
The condition that the present invention carries out the full spectrum direct-reading plasma emission spectrometer of multielement simultaneous determination is: echelle grating, the pouring-in detecting device of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.0L/min, secondary air amount 1.0L/min, plasma gas flow rate 1.0L/min, sample size 1.85ml/min, atomizer pressure are 28psi, peristaltic pump rotating speed 130Z/min.
Embodiment 4: transformer oil analytic sample of the present invention is heated for the oil sample of gathering and is quantitatively taken by weighing after shaking up, and promptly at 60 ℃ of heating 20min down, taking-up shakes up, and the range of weighing of described transformer oil analytic sample is controlled at 20g;
The present invention adopts the Infrared Heating method that quantitative transformer oil analytic sample is carried out evaporation at constant temperature and carbonization, and the Infrared Heating step is to adopt the ceramic infrared electric heating plate of controllable temperature to carry out under 270 ℃ temperature, till carbonization;
The sample of the present invention after to carbonization carries out the high temperature ashing, and the high temperature ashing is slowly to be warmed up to 625 ℃ from room temperature, and keeps 60 minutes down at 625 ℃;
The present invention adopts is dissolving with the sample of acid solution after to ashing under the low-temperature heat condition, is 1: 1 HNO of adding earlier with sour heating for dissolving step 34.5ml, add 1: 1 HCl 13.5ml again, under 80 ℃ of temperature heating for dissolving to solution concentration to 1ml;
Sample after the present invention adopts dilute acid soln to dissolving dilutes and constant volume, is prepared into analysis solution, and the dilution constant volume is solution quantitatively to be diluted in the volumetric flask of 25ml with rare nitric acid of 2%;
Analytical solution of the present invention is accurately measured the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
Transformer oil analytic sample of the present invention is handled according to two kinds of situations: first kind of situation is if transformer oil is untapped, clean, new transformer oil, to the transformer oil gathered directly weighing be analytic sample, second kind of situation is if transformer oil was to use, has impurity, just need under 60 ℃ temperature, keep 15 minutes the transformer oil of gathering, shake up weighing again as analytic sample.
The condition that the present invention carries out the full spectrum direct-reading plasma emission spectrometer of multielement simultaneous determination is: echelle grating, the pouring-in detecting device of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.0L/min, secondary air amount 1.0L/min, plasma gas flow rate 1.0L/min, sample size 1.85ml/min, atomizer pressure are 28psi, peristaltic pump rotating speed 130Z/min.

Claims (9)

1. determination method multiple metallic element time the in the transformer oil is characterized in that:
(1) the transformer oil analytic sample among the present invention is heated for the oil sample of gathering and is quantitatively taken by weighing after shaking up;
(2) the present invention adopts the Infrared Heating method that quantitative transformer oil analytic sample is carried out evaporation at constant temperature and carbonization;
(3) sample after the present invention adopts box high temperature furnace to carbonization carries out the high temperature ashing;
(4) the present invention adopts and to dissolve with the sample of acid solution after to ashing under the low-temperature heat condition;
(5) sample after the present invention adopts dilute acid soln to dissolving dilutes and constant volume, is prepared into analysis solution;
(6) analytical solution is accurately measured the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
2. determination method multiple metallic element time the in a kind of transformer oil according to claim 1, it is characterized in that described transformer oil analytic sample is heated for the oil sample of gathering quantitatively takes by weighing after shaking up, promptly heat 15-20min down at 50-60 ℃, taking-up shakes up, and the range of weighing of described transformer oil analytic sample is controlled at 10g-20g.
3. determination method multiple metallic element time the in a kind of transformer oil according to claim 1 and 2, it is characterized in that described employing Infrared Heating method carries out evaporation at constant temperature and carbonization to quantitative transformer oil analytic sample, the Infrared Heating step is to adopt the ceramic infrared electric heating plate of controllable temperature to carry out under 260 ℃ ± 10 ℃ temperature, till carbonization.
4. determination method multiple metallic element time the in a kind of transformer oil according to claim 1 and 2, it is characterized in that described sample after the carbonization being carried out the high temperature ashing, the high temperature ashing is slowly to be warmed up to 625 ℃ from room temperature, and keeps 60 minutes down at 625 ℃ ± 5 ℃.
5. determination method multiple metallic element time the in a kind of transformer oil according to claim 1, it is characterized in that described employing dissolving with the sample of acid solution after to ashing under the low-temperature heat condition, is the HNO that added earlier 1: 1 with sour heating for dissolving step 34.5-5.5ml, add 1: 1 HCl 13.5-16.5ml again, under 80-110 ℃ of temperature heating for dissolving to solution concentration to 1-3ml.
6. determination method multiple metallic element time the in a kind of transformer oil according to claim 1, it is characterized in that the sample after described employing dilute acid soln is to dissolving dilutes and constant volume, be prepared into analysis solution, the dilution constant volume is with rare nitric acid of 2% solution quantitatively to be diluted in the volumetric flask of 25ml-50ml.
7. determination method multiple metallic element time the in a kind of transformer oil according to claim 1 and 2 is characterized in that described analytical solution accurately measures the content of multiple metallic element with full spectrum direct-reading plasma emission spectrometer.
8. determination method multiple metallic element time the in a kind of transformer oil according to claim 1 and 2, it is characterized in that described transformer oil analytic sample handles according to two kinds of situations: first kind of situation is if transformer oil is untapped, clean, new transformer oil, to the transformer oil gathered directly weighing be analytic sample, second kind of situation is if transformer oil was to use, has impurity, just need under 55 ± 5 ℃ temperature, keep 10-15 minute the transformer oil of gathering, shake up weighing again as analytic sample.
9. determination method multiple metallic element time the in a kind of transformer oil according to claim 1 and 2, the condition that it is characterized in that carrying out the full spectrum direct-reading plasma emission spectrometer of multielement simultaneous determination is: echelle grating, the pouring-in detecting device of CID electric charge, radio-frequency generator operating power 1150W, the ICP frequency is 27.12MHZ, carrier gas (atomization gas) flow 1.0L/min, secondary air amount 1.0L/min, plasma gas flow rate 1.0L/min, sample size 1.85ml/min, atomizer pressure is 28psi, peristaltic pump rotating speed 130Z/min.
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CN104880341A (en) * 2014-02-28 2015-09-02 中国科学院寒区旱区环境与工程研究所 Sample pre-treatment method for determining total concentration of trace elements in polar ice and snow
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