CN105784532A - Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate - Google Patents
Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate Download PDFInfo
- Publication number
- CN105784532A CN105784532A CN201610233785.6A CN201610233785A CN105784532A CN 105784532 A CN105784532 A CN 105784532A CN 201610233785 A CN201610233785 A CN 201610233785A CN 105784532 A CN105784532 A CN 105784532A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- calcium oxide
- solution
- beaker
- oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate, and belongs to the technical field of metallurgical analysis methods.The continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate is short in analysis time, accurate in determination and low in detection cost.The method comprises the first step of sample preparation, the second step of primary sedimentation, the third step of secondary sedimentation, the fourth step of determination preparation, the fifth step of determination of the content of calcium oxide, the sixth step of determination of the total content of calcium oxide and magnesium oxide, the seventh step of determination of the content of rare earth oxide, and the eighth step of calculation of the content of rare earth oxide, calcium oxide and magnesium oxide.The method is easy to master, high in result accuracy and capable of being applied and popularized in production.Adopted equipment is simple, has the advantage of being accurate and is applicable to continuous and rapid determination of rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate.
Description
Technical field
Present invention relates particularly to a kind of rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, belong to metallurgical analysis method and technology field.
Background technology
Rare earth has the title of industry " gold " to have the new material that the physical characteristics such as excellent photoelectromagnetic can be different, various in style with other materials component property due to it, and its most significant function is exactly the quality and the performance that increase substantially other products.Such as increase substantially the tactical qualities for manufacturing tank, aircraft, the steel of guided missile, aluminium alloy, magnesium alloy, titanium alloy.And rare earth is many high-tech lubricants such as electronics, laser, nuclear industry, superconduction equally.Rare earth science and technology is once for military affairs, necessarily bring rising to of military science and technology, and rare earth is in metallurgical industry, and petrochemical industry, the aspect such as glass ceramics is also widely applied.
Measure rare earth ore concentrate middle rare earth, calcium oxide, method of magnesium oxide and generally use inductively coupled plasma method, need to use platinum crucible to melt, need to control salt amount, simultaneously need to Matrix Match, said method needs operator to have higher operating experience simultaneously, simultaneously need to outfit main equipment, cost of determination is high.
Summary of the invention
Therefore, it is an object of the invention to provide a kind of analysis time short, measure accurately, rare earth ore concentrate middle rare earth that testing cost is low, calcium oxide, magnesian method for continuously measuring, it is characterised in that said method comprising the steps of:
Step one: sample prepares
Rare earth ore concentrate sample is put in crucible with sodium hydroxide and sodium peroxide and mixs homogeneously, melted in high temperature furnace, from high temperature furnace, take out crucible, cooling；
Step 2: first time precipitation
Put in the beaker filling triethanolamine and sodium carbonate after step one cooling and boil leaching, wash crucible, filter with quantitative filter paper after cooling, wash beaker with sodium carbonate liquor, wash precipitation with sodium carbonate liquor；
Step 3: second time precipitation
Precipitation step 2 obtained moves in the beaker that step 2 uses together with quantitative filter paper, add nitric acid and perchloric acid, cap upper surface ware is put on electric furnace heating evaporation, takes off cooling after solution reaction calmness, continues heating heating to dry, walls of beaker and surface plate is purged with nitric acid (1+1), instill hydrogen peroxide after adding water, after boiling, take off cooling, filter with quantitative Medium speed filter paper, wash beaker and precipitation with nitric acid, residue is removed；
Step 4: preparation of determine
The filtrate that step 3 obtains adds ammonium chloride, it is neutralized to PH=8 with ammonia after boiling, instills hydrogen peroxide, add ammonia, boil, precipitation filters with quantitative Medium speed filter paper after declining, and filtrate is filled in volumetric flask, is diluted to volumetric flask scale constant volume, point taking two parts of test solutions puts in beaker, the a content for measuring calcium oxide, another part is used for measuring calcium oxide and magnesian total content, and precipitation and quantitatively Medium speed filter paper are for measuring the content of rare earth oxide；
Step 5: the mensuration of the content of calcium oxide
It is firstly added triethanolamine being used for measuring in the test solution of calcium oxide content, is then sequentially added into water, oxammonium hydrochloride., potassium hydroxide solution, instill calcein, be titrated to fluorescence green with EDTA standard solution and disappear, record EDTA standard solution consumption VCa；
Step 6: the mensuration of calcium oxide and magnesian total content
It is firstly added triethanolamine being used for measuring in the calcium oxide test solution with magnesian total content, then water, oxammonium hydrochloride., ammonia ammonium chloride solution it are sequentially added into, instilling C.I. 14645., being titrated to test solution with EDTA standard solution is pure blue, records EDTA standard solution consumption V(Mg+Ca)；
Step 7: rare earth oxide content measures
The precipitation and the quantitative Medium speed filter paper that obtain step 4 are put in beaker, add water, filter paper is smashed, it is subsequently adding oxalic acid, takes off after boiling, be incubated half an hour at 60 70 degree, filter with quantitative filter paper after standing a period of time, wash beaker and precipitation with oxalic acid solution, precipitation is put in crucible jointly together with quantitative filter paper, after low temperature dry ashing process, calcination, cooling, weigh quality m1；
Step 8: rare earth oxide, calcium oxide, content of magnesia calculating.
Further, described step one particularly as follows:
Weighing sample 0.5000g to be placed in the corundum crucible filling the 1-2 gram of sodium hydroxide removing moisture content, then add 2-3 gram of sodium peroxide, mixing, lid layer sodium peroxide is covered on surface again, 700 degree melted 10 minutes in Muffle furnace, takes out crucible, cooling from Muffle furnace.
Further, described step 2 particularly as follows:
Put in the 400mL beaker filling 150mL triethanolamine (1+10) and 2 grams of sodium carbonate after step one cooling and boil leaching, wash crucible, by the solution in beaker heated and boiled 1-2 minute, filter with quantitative filter paper after cooling, wash beaker 3-4 time with sodium carbonate (1+100) solution, wash precipitation 4-5 time.
Further, described step 3 particularly as follows:
Precipitation step 2 obtained moves in the beaker that step 2 uses together with quantitative filter paper, add 20mL nitric acid (67%), add 5mL perchloric acid (69%), cap upper surface ware is put on electric furnace and heats, it is evaporated to nitrogen dioxide to disperse completely, perchloric acid is smoldered in a large number, beaker is taken off after solution reaction calmness, cooling, continue heating to dry, walls of beaker and surface plate is purged with 10mL nitric acid (1+1), add 80mL hot water, then 0.1mL hydrogen peroxide (35%) is added, boil 1-2 minute, cool down after taking off, filter with quantitative Medium speed filter paper, beaker is washed 3-4 time with nitric acid (1+100), wash precipitation 7-8 time, residue is removed.
Further, described step 4 particularly as follows:
The filtrate that step 3 obtains adds ammonium chloride 3 grams, it is neutralized to PH=8 with ammonia (1+1) after boiling, precipitate appearance in a large number, instill 0.1mL hydrogen peroxide (30%), add 20mL ammonia (1+1), boil 2 minutes, precipitation filters with quantitative Medium speed filter paper after declining, filtrate is filled in 250mL volumetric flask, after solution cooling, it is diluted to volumetric flask scale constant volume, divides and take 50mL solution two parts in two 250mL beakers as two points of test solutions uses, the a content for measuring calcium oxide, another part is used for measuring calcium oxide and magnesian total content.
Further, described step 5 particularly as follows:
It is being used for measuring in the test solution of calcium oxide content, it is firstly added 50mL triethanolamine (12%), then 50mL water it is sequentially added into, add oxammonium hydrochloride., add 40mL potassium hydroxide solution (20%), instill calcein, be titrated to fluorescence green with EDTA standard solution and disappear, record EDTA standard solution consumption VCa。
Further, described step 6 particularly as follows:
It is being used for measuring in the calcium oxide test solution with magnesian total content, it is firstly added 50mL triethanolamine (12%), then 50mL water it is sequentially added into, add oxammonium hydrochloride., add 10mL ammonia-ammonium chloride solution, instilling chromium black T indicator, being titrated to test solution with EDTA standard solution is pure blue, records EDTA standard solution consumption V(Mg+Ca)。
Further, described step 7 particularly as follows:
The precipitation and the quantitative Medium speed filter paper that obtain step 4 are put in beaker, add boiling water 50mL, filter paper is smashed, it is subsequently adding oxalic acid (1+25) 100mL, take off after boiling, it is incubated half an hour at 60 70 degree, filter with quantitative filter paper after standing two hours, with oxalic acid (1+100) solution washing beaker, precipitate 10 times with oxalic acid (1+100) solution washing, precipitation is put in porcelain crucible jointly together with quantitative filter paper, puts in Muffle furnace and weigh quality m after 850 DEG C of ashing, calcination 40 minutes, coolings1。
Further, in described method, step 8 is pressed formula one, formula two and is calculated calcium oxide content W (CaO) and content of magnesia W (MgO) respectively, calculates rare earth oxide content W(RExOy with formula three):
W (CaO) %=C (V-V01) M (CaO) 100/mK × 100(formula one)
In formula: M (CaO): the molal weight (g/mol) of calcium oxide
M: sample mass (g)
K: sample separatory ratio (50/250=1/5)
C:EDTA concentration of standard solution (mol/L)
V: sample consumes the volume (mL) of EDTA standard solution
V01: the volume (mL) of blank solution consumption EDTA standard solution during titration calcium oxide content
W (MgO) %=C (V(Mg+Ca)-VCa-(V02-V01) M (MgO) 100/mK × 1000(formula two)
In formula: M (CaO): the molal weight (g/mol) of calcium oxide
M: sample mass (g)
K: sample separatory ratio
C:EDTA concentration of standard solution (mol/L)
V(Mg+Ca): the volume (mL) of the consumed EDTA standard solution of calcium and magnesium resultant
V02: the volume (mL) of blank solution consumption EDTA standard solution when titration calcium oxide and magnesian total content；
W(RExOy) (%)=(m1-m0) × 100/m(formula three)
In formula: W: rare earth oxide content
m1: the final quality weighed in rare earth oxide quality and step 7；
m0: the rare earth oxide quality of blank sample；
M: the rare earth ore concentrate quality used in sample mass and step one；
The beneficial effects of the present invention is: a kind of rare earth ore concentrate middle rare earth of the present invention, calcium oxide, magnesian method for continuously measuring, after sample dissolution, it is made directly rare-earth precipitation to measure, solution after filtration carries out calcium oxide, magnesian mensuration, measures rare earth oxide, calcium oxide, magnesian content by once testing simultaneously.Method is prone to grasp and result precision height, it is possible to popularization and application aborning.Use equipment is simple, has feature accurately, it is adaptable to rare earth ore concentrate middle rare earth, calcium oxide, magnesian Fast Continuous Determination.
Accompanying drawing explanation
Fig. 1 is the flow chart of the present invention a kind of rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is illustrated:
The method step of this detailed description of the invention is as shown in Figure 1, select three kinds of samples, respectively rare-earth tailing, is numbered 1, rare-earth original ore, label 2, rare earth ore concentrate is numbered 3, carries out sample according to sampling iron ore standard and produces, and per sample (p.s.) is 4 groups of contrast experiments by following method respectively, the basic process of assay method is: by sample alkali fusion, separates the interference elements such as ferrum, aluminum, manganese in triethanolamine solution.After removing silicon dioxide, with elements such as ammonia precipitation process separating calcium, magnesium, rare earth uses oxalic acid precipitation in the slightly acidic solution of PH=2.Calcination becomes rare earth oxide to weigh.Filtrate is at PH > 12 time add appropriate calcein, with EDTA standard solution titration, measure calcium oxide, add appropriate C.I. 14645. when PH=10, with EDTA standard solution titration, measure calcium oxide+magnesian resultant.Concrete operation method is:
Weighing sample 0.5000g to be placed in the corundum crucible filling the 1-2 gram of sodium hydroxide removing moisture content, then add 2-3 gram of sodium peroxide, mixing, lid layer sodium peroxide is covered on surface again, 700 degree melted 10 minutes in Muffle furnace, takes out crucible, cooling from Muffle furnace.Put into after cooling in the 400mL beaker filling 150mL triethanolamine (1+10) and 2 grams of sodium carbonate and boil leaching, wash crucible, by the solution in beaker heated and boiled 1-2 minute, filter with quantitative filter paper after cooling, wash beaker 3-4 time with sodium carbonate (1+100) solution, wash precipitation 4-5 time.The precipitation obtained is moved in the original beaker used together with quantitative filter paper, add 20mL nitric acid (67%), add 5mL perchloric acid (69%), cap upper surface ware is put on electric furnace and heats, it is evaporated to nitrogen dioxide to disperse completely, perchloric acid is smoldered in a large number, when smoldering, solution occurs that brown or black should add 2mL nitric acid (67%) in time, beaker is taken off after solution reaction calmness, cooling, continue heating to dry, walls of beaker and surface plate is purged with 10mL nitric acid (1+1), add 80mL hot water, then 0.1mL hydrogen peroxide (35%) is added, boil 1-2 minute, cool down after taking off, filter with quantitative Medium speed filter paper, beaker is washed 3-4 time with nitric acid (1+100), wash precipitation 7-8 time, residue is removed.The filtrate obtained adds ammonium chloride 3 grams, it is neutralized to PH=8 with ammonia (1+1) after boiling, precipitate appearance in a large number, instill 0.1mL hydrogen peroxide (30%), add 20mL ammonia (1+1), boil 2 minutes, precipitation filters with quantitative Medium speed filter paper after declining, filtrate is filled in 250mL volumetric flask, after solution cooling, it is diluted to volumetric flask scale constant volume, divides and take 50mL solution two parts in two 250mL beakers as two points of test solutions uses, the a content for measuring calcium oxide, another part is used for measuring calcium oxide and magnesian total content.
It is being used for measuring in the test solution of calcium oxide content, it is firstly added 50mL triethanolamine (12%), first adds triethanolamine, it is to first the interference element such as ferrum and aluminum be sheltered, then 50mL water it is sequentially added into, add the oxammonium hydrochloride. playing further masking action, add 40mL potassium hydroxide solution (20%), potassium hydroxide solution plays the effect of buffer solution, pH value is 12, instilling calcein indicator, calcein indicator manufacture method is: 1g calcein and the finely ground mixing of sodium chloride after 100g drying, is placed in port grinding bottle standby.It is titrated to fluorescence green with EDTA standard solution to disappear, EDTA standard solution C(EDTA)=0.01783mol/L, record EDTA standard solution consumption VCa。
It is being used for measuring in the calcium oxide test solution with magnesian total content, it is firstly added 50mL triethanolamine (12%), then 50mL water it is sequentially added into, adding oxammonium hydrochloride., add 10mL ammonia-ammonium chloride solution, ammonia-ammonium chloride solution plays the effect of buffer solution, pH value is 10, ammonia-ammonium chloride buffer solution (PH=10) preparation method is: be dissolved in 200mL water by 67g ammonium chloride, adds 570mL strong aqua ammonia, is diluted to 1000mL with water.Instilling chromium black T indicator, chromium black T indicator preparation method is: the finely ground mixing of sodium chloride after being dried with 100g by 1g C.I. 14645., is placed in port grinding bottle standby.Being titrated to test solution with EDTA standard solution is pure blue, records EDTA standard solution consumption V(Mg+Ca)。
The precipitation of acquisition and quantitative Medium speed filter paper are put in beaker, add boiling water 50mL, filter paper is smashed, is subsequently adding oxalic acid (1+25) 100mL, takes off after boiling, it is incubated half an hour at 60 70 degree, filter with quantitative filter paper after standing two hours, with oxalic acid (1+100) solution washing beaker, precipitate 10 times with oxalic acid (1+100) solution washing, precipitation is put in porcelain crucible jointly together with quantitative filter paper, puts in Muffle furnace and weigh quality m after 850 DEG C of ashing, calcination 40 minutes, coolings1。
Calculate calcium oxide content W (CaO) and content of magnesia W (MgO) by formula one, formula two respectively, calculate rare earth oxide content W(RExOy with formula three):
W (CaO) %=C (V-V01) M (CaO) 100/mK × 100(formula one)
In formula: M (CaO): the molal weight (g/mol) of calcium oxide
M: sample mass (g)
K: sample separatory ratio (50/250=1/5)
C:EDTA concentration of standard solution (mol/L)
V: sample consumes the volume (mL) of EDTA standard solution
V01: the volume (mL) of blank solution consumption EDTA standard solution, i.e. blank value during titration calcium oxide content；
W (MgO) %=C (V(Mg+Ca)-VCa-(V02-V01) M (MgO) 100/mK × 1000(formula two)
In formula: M (CaO): the molal weight (g/mol) of calcium oxide
M: sample mass (g)
K: sample separatory ratio
C:EDTA concentration of standard solution (mol/L)
V(Mg+Ca): the volume (mL) of the consumed EDTA standard solution of calcium and magnesium resultant
V02: the volume (mL) of blank solution consumption EDTA standard solution when titration calcium oxide and magnesian total content.
W(RExOy) (%)=(m1-m0) × 100/m(formula three)
In formula: W: rare earth oxide content
m1: rare earth oxide quality i.e. the final quality weighed；
m0: the rare earth oxide quality of blank sample；
M: the rare earth ore concentrate quality that namely sample mass uses；
Wherein the preparation method of blank sample is: in the corundum crucible filling the 1-2 gram of sodium hydroxide removing moisture content, then add 2-3 gram of sodium peroxide, mixing, lid layer sodium peroxide is covered on surface again, 700 degree melted 10 minutes in Muffle furnace, take out crucible, cooling from Muffle furnace.Put into after cooling in the 400mL beaker filling 150mL triethanolamine (1+10) and 2 grams of sodium carbonate and boil leaching, wash crucible, by the solution in beaker heated and boiled 1-2 minute, filter with quantitative filter paper after cooling, wash beaker 3-4 time with sodium carbonate (1+100) solution, wash precipitation 4-5 time.The precipitation obtained is moved in the original beaker used together with quantitative filter paper, add 20mL nitric acid (67%), add 5mL perchloric acid (69%), cap upper surface ware is put on electric furnace and heats, it is evaporated to nitrogen dioxide to disperse completely, perchloric acid is smoldered in a large number, when smoldering, solution occurs that brown or black should add 2mL nitric acid (67%) in time, beaker is taken off after solution reaction calmness, cooling, continue heating to dry, walls of beaker and surface plate is purged with 10mL nitric acid (1+1), add 80mL hot water, then 0.1mL hydrogen peroxide (35%) is added, boil 1-2 minute, cool down after taking off, filter with quantitative Medium speed filter paper, beaker is washed 3-4 time with nitric acid (1+100), wash precipitation 7-8 time, residue is removed.The filtrate obtained adds ammonium chloride 3 grams, it is neutralized to PH=8 with ammonia (1+1) after boiling, precipitate appearance in a large number, instill 0.1mL hydrogen peroxide (30%), add 20mL ammonia (1+1), boil 2 minutes, precipitation filters with quantitative Medium speed filter paper after declining, filtrate is filled in 250mL volumetric flask, after solution cooling, it is diluted to volumetric flask scale constant volume, divide and take 50mL solution two parts in two 250mL beakers as two points of test solutions uses, the a content for measuring blank sample calcium oxide, another part is used for measuring blank sample calcium oxide and magnesian total content.
It is being used for measuring in the test solution of blank sample calcium oxide content, it is firstly added 50mL triethanolamine (12%), first adds triethanolamine, it is to first the interference element such as ferrum and aluminum be sheltered, then 50mL water it is sequentially added into, add the oxammonium hydrochloride. playing further masking action, add 40mL potassium hydroxide solution (20%), potassium hydroxide solution plays the effect of buffer solution, pH value is 12, instill calcein indicator, calcein indicator manufacture method is: 1g calcein and the finely ground mixing of sodium chloride after 100g drying, it is placed in port grinding bottle standby.It is titrated to fluorescence green with EDTA standard solution to disappear, EDTA standard solution C(EDTA)=0.01783mol/L, record EDTA standard solution consumption V01。
It is being used for measuring in the blank sample calcium oxide test solution with magnesian total content, it is firstly added 50mL triethanolamine (12%), then 50mL water it is sequentially added into, adding oxammonium hydrochloride., add 10mL ammonia-ammonium chloride solution, ammonia-ammonium chloride solution plays the effect of buffer solution, pH value is 10, ammonia-ammonium chloride buffer solution (PH=10) preparation method is: be dissolved in 200mL water by 67g ammonium chloride, adds 570mL strong aqua ammonia, is diluted to 1000mL with water.Instilling chromium black T indicator, chromium black T indicator preparation method is: the finely ground mixing of sodium chloride after being dried with 100g by 1g C.I. 14645., is placed in port grinding bottle standby.Being titrated to test solution with EDTA standard solution is pure blue, records EDTA standard solution consumption V02。
The precipitation of acquisition and quantitative Medium speed filter paper are put in beaker, add boiling water 50mL, filter paper is smashed, it is subsequently adding oxalic acid (1+25) 100mL, take off after boiling, it is incubated half an hour at 60 70 degree, filter with quantitative filter paper after standing two hours, with oxalic acid (1+100) solution washing beaker, precipitate 10 times with oxalic acid (1+100) solution washing, precipitation is put in porcelain crucible jointly together with quantitative filter paper, puts into the rare earth oxide quality m weighing blank sample in Muffle furnace after 850 DEG C of ashing, calcination 40 minutes, coolings0。
Three kinds of samples measure calcium oxide, content of magnesia result as shown in table 1,
Table 1
The result measuring rare earth oxide content of three kinds of samples is as shown in table 2,
Table 2
Be can be seen that by table 1, table 2, for sample three kinds different, each group rare earth oxide of contrast experiment, calcium oxide, content of magnesia measurement result relatively, illustrating that the method precision of the present invention is fine, the method for the present invention can also be generalized to rare-earth tailing and rare-earth original ore use simultaneously.
This method measures the accuracy of calcium oxide content to utilize the baotite R-715 of known standard value, baotite R-716, tri-kinds of rare earth ore concentrates of baotite R-717 to verify, measurement result is as shown in table 3, checking this method measures the accuracy of rare earth oxide content, and measurement result is as shown in table 4
Table 3
| The name of an article | Extreme difference | Tolerance | Measured value W (CaO) % | Standard value W (CaO) % |
| Baotite R-716 | -0.06 | 0.50 | 21.40 | 21.46 |
| Baotite R-715 | +0.03 | 0.35 | 5.20 | 5.17 |
| Baotite R-717 | 0 | 0.50 | 21.80 | 21.80 |
Table 4
| The name of an article | Extreme difference | Tolerance | Measured value W(RExOy) (%) | Standard value W(RExOy) (%) |
| Baotite R-716 | -0.09 | 0.40 | 7.20 | 7.29 |
| Baotite R-715 | +0.03 | 0.40 | 3.40 | 3.37 |
| Baotite R-717 | -0.06 | 0.40 | 13.00 | 13.06 |
Baotite R-717 i.e. certain rare earth ore concentrate utilizing known standard value verifies that this method measures the accuracy of content of magnesia, and measurement result is as shown in table 5,
Table 5
| The name of an article | Extreme difference | Tolerance | Measured value W (MgO) % | Standard value W (MgO) % |
| Rare earth ore concentrate | 0.03 | 0.10 | 1.10 | 1.07 |
| Baotite R-717 | -0.06 | 0.10 | 1.00 | 1.06 |
By table 3, table 4, table 5 it can be seen that rare earth oxide, calcium oxide, content of magnesia measured value and known standard value closely, it was demonstrated that the accuracy of the present invention is significantly high.
The above is the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from principle of the present invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. a rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that said method comprising the steps of:
Step one: sample prepares
Rare earth ore concentrate sample is put in crucible with sodium hydroxide and sodium peroxide and mixs homogeneously, melted in high temperature furnace, from high temperature furnace, take out crucible, cooling；
Step 2: first time precipitation
Put in the beaker filling triethanolamine and sodium carbonate after step one cooling and boil leaching, wash crucible, filter with quantitative filter paper after cooling, wash beaker with sodium carbonate liquor, wash precipitation with sodium carbonate liquor；
Step 3: second time precipitation
Precipitation step 2 obtained moves in the beaker that step 2 uses together with quantitative filter paper, add nitric acid and perchloric acid, cap upper surface ware is put on electric furnace heating evaporation, takes off cooling after solution reaction calmness, continues heating heating to dry, walls of beaker and surface plate is purged with nitric acid (1+1), instill hydrogen peroxide after adding water, after boiling, take off cooling, filter with quantitative Medium speed filter paper, wash beaker and precipitation with nitric acid, residue is removed；
Step 4: preparation of determine
The filtrate that step 3 obtains adds ammonium chloride, it is neutralized to PH=8 with ammonia after boiling, instills hydrogen peroxide, add ammonia, boil, precipitation filters with quantitative Medium speed filter paper after declining, and filtrate is filled in volumetric flask, is diluted to volumetric flask scale constant volume, point taking two parts of test solutions puts in beaker, the a content for measuring calcium oxide, another part is used for measuring calcium oxide and magnesian total content, and precipitation and quantitatively Medium speed filter paper are for measuring the content of rare earth oxide；
Step 5: the mensuration of the content of calcium oxide
It is firstly added triethanolamine being used for measuring in the test solution of calcium oxide content, is then sequentially added into water, oxammonium hydrochloride., potassium hydroxide solution, instill calcein, be titrated to fluorescence green with EDTA standard solution and disappear, record EDTA standard solution consumption VCa；
Step 6: the mensuration of calcium oxide and magnesian total content
It is firstly added triethanolamine being used for measuring in the calcium oxide test solution with magnesian total content, then water, oxammonium hydrochloride., ammonia ammonium chloride solution it are sequentially added into, instilling C.I. 14645., being titrated to test solution with EDTA standard solution is pure blue, records EDTA standard solution consumption V(Mg+Ca)；
Step 7: rare earth oxide content measures
The precipitation and the quantitative Medium speed filter paper that obtain step 4 are put in beaker, add water, filter paper is smashed, it is subsequently adding oxalic acid, takes off after boiling, be incubated half an hour at 60 70 degree, filter with quantitative filter paper after standing a period of time, wash beaker and precipitation with oxalic acid solution, precipitation is put in crucible jointly together with quantitative filter paper, after low temperature dry ashing process, calcination, cooling, weigh quality m1；
Step 8: rare earth oxide, calcium oxide, content of magnesia calculating.
2. as claimed in claim 1 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step one particularly as follows:
Weighing sample 0.5000g to be placed in the corundum crucible filling the 1-2 gram of sodium hydroxide removing moisture content, then add 2-3 gram of sodium peroxide, mixing, lid layer sodium peroxide is covered on surface again, 700 degree melted 10 minutes in Muffle furnace, takes out crucible, cooling from Muffle furnace.
3. as claimed in claim 2 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step 2 particularly as follows:
Put in the 400mL beaker filling 150mL triethanolamine (1+10) and 2 grams of sodium carbonate after step one cooling and boil leaching, wash crucible, by the solution in beaker heated and boiled 1-2 minute, filter with quantitative filter paper after cooling, wash beaker 3-4 time with sodium carbonate (1+100) solution, wash precipitation 4-5 time.
4. as claimed in claim 3 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step 3 particularly as follows:
Precipitation step 2 obtained moves in the beaker that step 2 uses together with quantitative filter paper, add 20mL nitric acid (67%), add 5mL perchloric acid (69%), cap upper surface ware is put on electric furnace and heats, it is evaporated to nitrogen dioxide to disperse completely, perchloric acid is smoldered in a large number, beaker is taken off after solution reaction calmness, cooling, continue heating to dry, walls of beaker and surface plate is purged with 10mL nitric acid (1+1), add 80mL hot water, then 0.1mL hydrogen peroxide (35%) is added, boil 1-2 minute, cool down after taking off, filter with quantitative Medium speed filter paper, beaker is washed 3-4 time with nitric acid (1+100), wash precipitation 7-8 time, residue is removed.
5. as claimed in claim 4 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step 4 particularly as follows:
The filtrate that step 3 obtains adds ammonium chloride 3 grams, it is neutralized to PH=8 with ammonia (1+1) after boiling, precipitate appearance in a large number, instill 0.1mL hydrogen peroxide (30%), add 20mL ammonia (1+1), boil 2 minutes, precipitation filters with quantitative Medium speed filter paper after declining, filtrate is filled in 250mL volumetric flask, after solution cooling, it is diluted to volumetric flask scale constant volume, divides and take 50mL solution two parts in two 250mL beakers as two points of test solutions uses, the a content for measuring calcium oxide, another part is used for measuring calcium oxide and magnesian total content.
6. as claimed in claim 5 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step 5 particularly as follows:
It is being used for measuring in the test solution of calcium oxide content, it is firstly added 50mL triethanolamine (12%), then 50mL water it is sequentially added into, add oxammonium hydrochloride., add 40mL potassium hydroxide solution (20%), instill calcein, be titrated to fluorescence green with EDTA standard solution and disappear, record EDTA standard solution consumption VCa。
7. as claimed in claim 5 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step 6 particularly as follows:
It is being used for measuring in the calcium oxide test solution with magnesian total content, it is firstly added 50mL triethanolamine (12%), then 50mL water it is sequentially added into, add oxammonium hydrochloride., add 10mL ammonia-ammonium chloride solution, instilling chromium black T indicator, being titrated to test solution with EDTA standard solution is pure blue, records EDTA standard solution consumption V(Mg+Ca)。
8. as claimed in claim 5 rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring, it is characterised in that described step 7 particularly as follows:
The precipitation and the quantitative Medium speed filter paper that obtain step 4 are put in beaker, add boiling water 50mL, filter paper is smashed, it is subsequently adding oxalic acid (1+25) 100mL, take off after boiling, it is incubated half an hour at 60 70 degree, filter with quantitative filter paper after standing two hours, with oxalic acid (1+100) solution washing beaker, precipitate 10 times with oxalic acid (1+100) solution washing, precipitation is put in porcelain crucible jointly together with quantitative filter paper, puts in Muffle furnace and weigh quality m after 850 DEG C of ashing, calcination 40 minutes, coolings1。
9. rare earth ore concentrate middle rare earth, calcium oxide, magnesian method for continuously measuring as claimed in claim 1, it is characterized in that, in described method, step 8 is pressed formula one, formula two and is calculated calcium oxide content W (CaO) and content of magnesia W (MgO) respectively, calculates rare earth oxide content W(RExOy with formula three):
W (CaO) %=C (V-V01) M (CaO) 100/mK × 100 formula one
In formula: M (CaO): the molal weight of calcium oxide
M: sample mass
K: sample separatory ratio
C:EDTA concentration of standard solution
V: sample consumes the volume of EDTA standard solution
V01: the volume of blank solution consumption EDTA standard solution during titration calcium oxide content
W (MgO) %=C (V(Mg+Ca)-VCa-(V02-V01) M (MgO) 100/mK × 1000 formula two
In formula: M (MgO): magnesian molal weight
M: sample mass
K: sample separatory ratio
C:EDTA concentration of standard solution
V(Mg+Ca): the volume of the consumed EDTA standard solution of calcium and magnesium resultant
V02: the volume of blank solution consumption EDTA standard solution when titration calcium oxide and magnesian total content；
W(RExOy) (%)=(m1-m0) × 100/m formula three
In formula: W: rare earth oxide content
m1: the final quality weighed in rare earth oxide quality and step 7；
m0: the rare earth oxide quality of blank sample；
M: the rare earth ore concentrate quality used in sample mass and step one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610233785.6A CN105784532A (en) | 2016-04-15 | 2016-04-15 | Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610233785.6A CN105784532A (en) | 2016-04-15 | 2016-04-15 | Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105784532A true CN105784532A (en) | 2016-07-20 |
Family
ID=56397606
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610233785.6A Pending CN105784532A (en) | 2016-04-15 | 2016-04-15 | Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105784532A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404763A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in desulfurizing agent |
| CN106404993A (en) * | 2016-08-29 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Measuring method of magnesium oxide in magnesium refractory material |
| CN106404992A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in lime |
| CN107655784A (en) * | 2017-09-13 | 2018-02-02 | 广西大学 | A kind of method of granule sludge calcification in measure paper waste |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4676891B2 (en) * | 2006-01-27 | 2011-04-27 | 新日本製鐵株式会社 | Method for measuring magnesium oxide content and calcium oxide content in oxide materials using infrared absorption spectroscopy |
| JP5446993B2 (en) * | 2010-02-26 | 2014-03-19 | Ｊｆｅスチール株式会社 | Granular component estimation method |
| CN104569129A (en) * | 2014-12-29 | 2015-04-29 | 内蒙古包钢钢联股份有限公司 | Method for determining content of single rear earth oxide in steel |
| CN104792784A (en) * | 2015-05-20 | 2015-07-22 | 内蒙古包钢钢联股份有限公司 | Continuous determination method for content of calcium oxide and magnesium oxide in blast furnace slag |
| CN104977385A (en) * | 2015-06-12 | 2015-10-14 | 内蒙古包钢钢联股份有限公司 | Method for continuous determination of calcium oxide and magnesium oxide content of limestone and dolomite |
| CN105158405A (en) * | 2015-08-21 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for continuously determining content of calcium oxide and magnesium oxide in bentonite |
-
2016
- 2016-04-15 CN CN201610233785.6A patent/CN105784532A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4676891B2 (en) * | 2006-01-27 | 2011-04-27 | 新日本製鐵株式会社 | Method for measuring magnesium oxide content and calcium oxide content in oxide materials using infrared absorption spectroscopy |
| JP5446993B2 (en) * | 2010-02-26 | 2014-03-19 | Ｊｆｅスチール株式会社 | Granular component estimation method |
| CN104569129A (en) * | 2014-12-29 | 2015-04-29 | 内蒙古包钢钢联股份有限公司 | Method for determining content of single rear earth oxide in steel |
| CN104792784A (en) * | 2015-05-20 | 2015-07-22 | 内蒙古包钢钢联股份有限公司 | Continuous determination method for content of calcium oxide and magnesium oxide in blast furnace slag |
| CN104977385A (en) * | 2015-06-12 | 2015-10-14 | 内蒙古包钢钢联股份有限公司 | Method for continuous determination of calcium oxide and magnesium oxide content of limestone and dolomite |
| CN105158405A (en) * | 2015-08-21 | 2015-12-16 | 内蒙古包钢钢联股份有限公司 | Method for continuously determining content of calcium oxide and magnesium oxide in bentonite |
Non-Patent Citations (2)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局: "《中华人民共和国国家标准 GB/T 18114-2010 稀土精矿化学分析方法》", 14 January 2011, 中国标准出版社 * |
| 周凯红等: "EDTA滴定法测定稀土矿石中氧化钙", 《冶金分析》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404763A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in desulfurizing agent |
| CN106404992A (en) * | 2016-08-26 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium oxide and magnesium oxide in lime |
| CN106404993A (en) * | 2016-08-29 | 2017-02-15 | 内蒙古包钢钢联股份有限公司 | Measuring method of magnesium oxide in magnesium refractory material |
| CN107655784A (en) * | 2017-09-13 | 2018-02-02 | 广西大学 | A kind of method of granule sludge calcification in measure paper waste |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105784532A (en) | Continuous determination method for rare earth oxide, calcium oxide and magnesium oxide in rare earth ore concentrate | |
| CN102253030B (en) | Method for determining impurity content in high-titanium slag | |
| CN103175824A (en) | Method for measuring content of silicon and phosphorus in ferromanganese iron by inductively coupled plasma spectrum emission instrument | |
| KR20120085296A (en) | Method for analyzing and detecting calcium element in ore | |
| CN107462690B (en) | Soil detection method and application thereof | |
| CN104297246B (en) | Method for measuring magnesium content in aluminum magnesium alloy powder | |
| CN102042982A (en) | Method for testing content of boron trioxide in glass containing zinc and lead | |
| CN105738559A (en) | Method for measuring calcium oxide and magnesium oxide content of tundish covering agent | |
| CN104819908A (en) | Continuous measuring method of calcium and barium content in silicon-calcium-barium and silicon-aluminum-calcium-barium alloy | |
| CN103529165A (en) | Method for directly determining aluminum content in vanadium-aluminum alloy | |
| CN104820061A (en) | Measuring method of calcium content in silicon-calcium-barium alloy | |
| CN105911051A (en) | Continuous determination method for calcium oxide and magnesium oxide in rare earth ore concentrate | |
| CN103115920A (en) | Method for measuring iron/calcium ratio in iron-calcium core-spun yarn | |
| CN105738362A (en) | Method for measuring contents of calcium oxide and magnesia in iron ore | |
| CN111830106A (en) | Method for measuring content of fluorine ions in serpentine | |
| CN105606762A (en) | Measuring method for content of calcium oxide and magnesium oxide in open-hearth furnace slag, converter slag and electric furnace slag | |
| CN105651931A (en) | Method for measuring content of calcium oxide and magnesium oxide in refined slag | |
| CN104422685A (en) | Method for determining content of metal aluminum in ladle slag modifying agent | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN105806826A (en) | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method | |
| CN105911049A (en) | Method for determining calcium oxide in rare earth concentrate | |
| CN112379036A (en) | Method for measuring content of nickel, cobalt and manganese in ternary material and method for calculating content of single element | |
| CN101660995A (en) | Method of measuring total content of rare earth in rare earth chrome-manganese-silicon inoculant | |
| CN106053718B (en) | A kind of rare earth ore concentrate middle rare earth, calcium oxide, magnesia, barium monoxide method for continuously measuring | |
| CN103940944A (en) | Method for detecting content of calcium oxide in limestone by using DBC (Dibromochloro)-arsenazo indicator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160720 |