CN103364258A - Method for measuring metal content in gas mud - Google Patents

Abstract

The invention discloses a method for measuring the metal content in gas mud, which comprises the following steps of: collecting a gas mud sample, drying and grinding, and uniformly mixing by a nylon sieve for further use; weighing 0.1-0.2g of the sieved sample, and putting the sample in a polytetrafluoroethylene digestion tube; adding a specific acid system into the digestion tube, wherein the total volume of the solvent sample does not exceed 20ml; digesting the solvent sample by use of microwaves; putting the digestion tube in a digestion tank and heating to 100 DEG C at a certain speed; keeping for 20 minutes; after the digestion is over, cooling to the room temperature; opening the digestion tank, filtering digestion liquid in the digestion tube and transferring into a volumetric flask; adding 10ml of a saturated boric acid solution; washing the digestion tube with distilled water; putting the washing liquid into the volumetric flask; fixing the volume and shaking uniformly to obtain to-be-measured liquid; analyzing the metal content in the to-be-measured liquid by use of a plasma emission spectrum analyzer, and converting into the metal content in the gas mud. The method disclosed by the invention is convenient for measuring on the metal content in the gas mud, and effectively improves the accuracy of the metal content measurement.

Description

The assay method of tenor in the gas mud

Technical field

The present invention relates to the assay method of tenor in a kind of gas mud.

Background technology

The solid waste that produces in the Production Process for Steel Enterprise mainly contains grain slag, slag, slag, dirt mud, flyash and waste refractory materials etc., and wherein the dirt mud drum is drawn together dedusting ash, gas mud, OG mud etc.Gas mud in the dirt mud is the product that particulate that the raw material dust taken out of with blast furnace gas in the blast furnace ironmaking process and high-temperature region vigorous reaction produce obtains through wet dedusting, and it mainly is comprised of breeze, coke powder, flux, dust etc.The gas mud amount is large, wide, wherein contains various metals, comprises poisonous and harmful heavy metallic such as lead, cadmium, arsenic etc., also the metal of bag expansion recoverable such as iron, nickel, zinc etc.From the environmental protection angle, detect Heavy Metals content in the gas mud, can deposit disposal according to the respective country standard, otherwise with polluted underground water and surface water environment; From the resource recycling angle, understand the content of beary metal that recovery value is arranged in the gas mud, can be follow-up difference recycling data supporting is provided, turn waste into wealth.

At present in the gas mud tenor all less than Accurate Determining method targetedly, the complicacy of gas mud matrix, the existence that particularly has the difficulties such as part coke powder, dedusting ash to clear up matrix has restricted the Accurate Determining of classic method to tenor.Traditional unlimited heated type Wet complex operation, length consuming time, analyst's working strength is large, and clears up weak effect; The solid waste leaching method is just simulated the content that metal leaches in the solid waste stacking process, can not accurately detect tenor wherein.And micro-wave digestion is as a kind of novel, efficient Specimen eliminating technology, have quick, easy, pollute less, decompose and wait advantage fully, become sample and decomposed one of indispensable method, it is widely used in fields such as biology, food, medicine, environment, but the research that is applied to metallurgy industry solid waste heavy metal element also seldom.

Summary of the invention

Technical matters to be solved by this invention provides the assay method of tenor in a kind of gas mud; this method adopts simple and efficient pre-treating method to cooperate the conventional sense means to measure that tenor becomes possibility in the gas mud; Effective Raise tenor accuracy, precision and the sensitivity measured, provide reliable data supporting for formulating environmental protection and resource recycling scheme.

For solving the problems of the technologies described above, the assay method of tenor comprises the steps: in the gas mud of the present invention

Step 1, sample preparation, with the gas mud sample oven dry under 105 ± 5 ℃ that gathers, the sample of oven dry is milled with attrition mill, and makes sample pass through 100 order nylon mesh, and mixing is for subsequent use;

Step 2, claim sample, accurately take by weighing sample after 0.1000g～0.2000g sieves in the teflon digestion tube of clean dried;

Step 3, interpolation acid system add 4 mL HNO3,4mLHCl, 2mLH2SO4 and 2mLHF in the teflon digestion tube, the solvent samples cumulative volume is no more than 20mL behind the adding acid system;

Step 4, adopt microwave that solvent samples is cleared up, the teflon digestion tube is placed in the counteracting tank and be warming up to 100 ℃ with 10 ℃/minute speed, then kept 20 minutes;

Step 5, digestion solution shift, after clearing up end, be cooled to room temperature, open counteracting tank, digestion solution filtration in the teflon digestion tube is transferred in the 100ml plastics volumetric flask, add the saturated BAS of 10ml in the plastics volumetric flask, with distilled water washing teflon digestion tube, cleansing solution is incorporated in the plastics volumetric flask, constant volume, shake up, obtain liquid to be measured;

Step 6, tenor are measured, and the using plasma emission spectrometric analyzer is analyzed tenor in the liquid to be measured, and converting obtains tenor in the gas mud.

Because the assay method of tenor has adopted technique scheme in the gas mud of the present invention, namely gather the oven dry of gas mud sample, mill, and for subsequent use by 100 order nylon mesh mixings, take by weighing 0.1～0.2g and sieve rear sample in the teflon digestion tube of clean dried, in digestion tube, add specific acid system, the solvent samples cumulative volume is no more than 20ml after adding acid system, adopt microwave that solvent samples is cleared up, the teflon digestion tube placed in the counteracting tank and be warming up to 100 ℃ with 10 ℃/minute speed, then kept 20 minutes, clear up end after, be cooled to room temperature, open counteracting tank, digestion solution filtration in the digestion tube is transferred in the 100ml plastics volumetric flask, adds the saturated BAS of 10ml, wash digestion tube with distilled water, in cleansing solution and the people's plastics volumetric flask, constant volume shakes up, and obtains liquid to be measured, the using plasma emission spectrometric analyzer is analyzed tenor in the liquid to be measured, converts to obtain tenor in the gas mud.This method adopts simple and efficient pre-treating method to cooperate the conventional sense means to measure that tenor becomes possibility in the gas mud; Effective Raise tenor accuracy, precision and the sensitivity measured, provide reliable data supporting for formulating environmental protection and resource recycling scheme.

Embodiment

The assay method of tenor comprises the steps: in the gas mud of the present invention

Step 1, sample preparation, with the gas mud sample oven dry under 105 ± 5 ℃ that gathers, the sample of oven dry is milled with attrition mill, and makes sample pass through 100 order nylon mesh, and mixing is for subsequent use;

Step 2, claim sample, accurately take by weighing sample after 0.1000g～0.2000g sieves in the teflon digestion tube of clean dried; Can add the wetting sample of a small amount of deionized water in this step;

Step 3, interpolation acid system add 4 mL HNO3,4mLHCl, 2mLH2SO4 and 2mLHF in the teflon digestion tube, the solvent samples cumulative volume is no more than 20mL behind the adding acid system;

Step 4, adopt microwave that solvent samples is cleared up, the teflon digestion tube is placed in the counteracting tank and be warming up to 100 ℃ with 10 ℃/minute speed, then kept 20 minutes;

Step 5, digestion solution shift, after clearing up end, be cooled to room temperature, open counteracting tank, digestion solution filtration in the teflon digestion tube is transferred in the 100ml plastics volumetric flask, add the saturated BAS of 10ml in the plastics volumetric flask, with distilled water washing teflon digestion tube, cleansing solution is incorporated in the plastics volumetric flask, constant volume, shake up, obtain liquid to be measured;

Step 6, tenor are measured, and the using plasma emission spectrometric analyzer is analyzed tenor in the liquid to be measured, and converting obtains tenor in the gas mud.

The said determination step is carried out in the process, can adopt the gross control measure of routine analysis, does whole process and clears up blank, standard discovery test and recovery testu, with the accuracy of guaranteeing to measure.

Gas mud is the accessory substance of ironmaking processes, and every day, generation was very large.The content of metal all has vital impact to environmental protection and resource recycling in the Accurate Determining gas mud.

This method adopts microwave dissolver that gas mud is cleared up, select specific acid system, according to the increasing temperature and pressure program of setting, in airtight counteracting tank, clear up the gas mud sample of collection, clear up finish after, use the plasma emission spectrometry instrument to analyze tenor in the digestion solution.This method is so that adopt simple and efficient pre-treating method to cooperate the conventional sense means to measure that tenor becomes possibility in the gas mud.Accuracy, precision, sensitivity that tenor is measured all can fully be satisfied need of production.This method is used for the mensuration of metallurgy industry gas mud tenor, provides data supporting for formulating environmental protection and resource recycling scheme, and stronger using value is arranged.

This method adopts microwave directly to release energy to the sample that gathers, and has avoided the loss of energy in the assay method of traditional heat conduction, thermal convection, has improved the service efficiency of energy.Clear up with heating plate, electric furnace and to compare, clear up and can fast 4～100 times finish.Simultaneously sample clear up can carry out more accurately, thorough, in clearing up program, can avoid the use of perchloric acid, adopt HNO3 during micro-wave digestion, based on the cause of counteracting tank internal pressure, can produce higher temperature and be cleared up preferably the result, to replace the use of perchloric acid.This method adopts the counteracting tank airtight microwave digestion, can assist reaction by improving temperature/pressure, make reactant under specified temp fast decoupled occur, and reduces and decomposes the required time, increase work efficiency, and traditional assay method this be impossible.Adopt volatile element such as As in this method gas mud, Hg etc. can be retained in the digestion solution, and the deviation that causes measurement result and to the pollution of environment prevents from volatilizing.Also make simultaneously operating personnel avoid contacting acid mist and harmful gas, such as hydrofluorite.The micro-wave digestion instrument that this method adopts can be by the automatic adjusting of magnetron, the transmission of quantitative control microwave energy, control decomposition condition and the automatic control of realization to reacting with this, mistake and the error of having avoided manual operation to produce guarantee to clear up collimation and the repeatability of reaction.

Adopt this method to select the representative gas mud in ironmaking zone to carry out six parallel laboratory tests.Carry out simultaneously blank mark-on experiment, obtain the sample parallel laboratory test result of table 1, the recovery experiment result of table 2 and the sample mark-on experimental result of table three; Can see from table 1, table 2 and table 3, the relative standard deviation of each ultimate analysis is in 4.57%～9.97% scope, and blank recovery of standard addition is in 90.0%～110% scope, and the sample recovery of standard addition is in 85%～110% scope.The preci-sion and accuracy index that this method tenor is measured satisfies the basic demand that environmental monitoring station's solid sample is analyzed.

  

Table 1. sample parallel laboratory test result

Element	Analysis result (mg/l)	Mark-on concentration (mg/l)	The recovery (%)
				Iron	2.02	2.00	101
Zinc	1.80	2.00	90.0
				Plumbous	0.031	0.03	103
Chromium	0.055	0.05	110
				Cadmium	0.067	0.07	95.7
Nickel	0.0398	0.04	99.5

Table 2. recovery experiment result

Table 3. sample mark-on experimental result

  

Claims (1)

1. the assay method of tenor in the gas mud is characterized in that this method comprises the steps:

Step 1, sample preparation, with the gas mud sample oven dry under 105 ± 5 ℃ that gathers, the sample of oven dry is milled with attrition mill, and makes sample pass through 100 order nylon mesh, and mixing is for subsequent use;

Step 2, claim sample, accurately take by weighing sample after 0.1000g～0.2000g sieves in the teflon digestion tube of clean dried;

Step 3, interpolation acid system add 4mL HNO3,4mLHCl, 2mLH2SO4 and 2mLHF in the teflon digestion tube, the solvent samples cumulative volume is no more than 20mL behind the adding acid system;

Step 4, adopt microwave that solvent samples is cleared up, the teflon digestion tube is placed in the counteracting tank and be warming up to 100 ℃ with 10 ℃/minute speed, then kept 20 minutes;

Step 5, digestion solution shift, after clearing up end, be cooled to room temperature, open counteracting tank, digestion solution filtration in the teflon digestion tube is transferred in the 100ml plastics volumetric flask, add the saturated BAS of 10ml in the plastics volumetric flask, with distilled water washing teflon digestion tube, cleansing solution is incorporated in the plastics volumetric flask, constant volume, shake up, obtain liquid to be measured;

Step 6, tenor are measured, and the using plasma emission spectrometric analyzer is analyzed tenor in the liquid to be measured, and converting obtains tenor in the gas mud.