Method for simultaneously determining content of phosphorus, magnesium, iron, aluminum, silicon, calcium, titanium, manganese and strontium in phosphorite by adopting ICP-AES
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An ICP-AES, iron-aluminum-silicon technology, applied in the field of analysis and testing, can solve problems such as large measurement errors and spectral line intensity changes, and achieve the effects of accurate results, strong anti-interference ability, and wide linear range
Inactive Publication Date: 2017-01-04
YUNNAN PHOSPHATE CHEM GROUP CORP
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Since the viscosity, specific gravity and surface tension of the solution affect the atomization process, droplet size, aerosol transmission and solvent evaporation during the ICP-AES measurement process, if the standard solution and the sample solution to be tested are in the matrix There are differences in the composition of elements, total salinity, acidity, etc., which will cause obvious changes in the intensity of spectral lines during the measurement, resulting in large measurement errors
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[0019] The ICP-AES method is a method for simultaneously determining the content of phosphorus, magnesium, iron, aluminum, silicon, calcium, titanium, manganese, and strontium in phosphate rock. The equipment and instruments used: iCAP7400 full-spectrum direct-reading plasma emission spectrometer; hydrofluoric acid-resistant atomizer; Analymate-V4D high-frequency sample dissolution machine ,Specific steps are as follows:
[0020] a. Accurately weigh 0.1000g of phosphate rock sample and put it in a platinum crucible, add 1.2g of lithium metaborate and mix well, add 10 drops of lithium bromide solution, place it on a high-frequency sample dissolution machine, and pre-oxidize at 700°C for 2 minutes to fully oxidize the reduced product , then raise the temperature to 1050°C, and after melting for 2 minutes, take out the platinum crucible with crucible pliers, and immediately pour the red hot molten beads directly into a 400mL polytetrafluoroethylene beaker filled with 100mL nitric ...
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Abstract
The invention relates to the technical field of analysis test, and in particular relates to a method for simultaneously determining content of phosphorus, magnesium, iron, aluminum, silicon, calcium, titanium, manganese and strontium in phosphorite by adopting inductively coupled plasma atomic emission spectrometry (ICP-AES). Specifically, lithium metaborate is a non-oxidant solvent with a high melt point, has high decomposition capacity for a majority of test samples, and can effectively decompose rocks and minerals difficult to dissolve. The method comprises the following steps: placing a phosphorite test sample into a platinum crucible, adding the lithium metaborate solvent and a lithium bromide releasing agent, melting and decomposing the phosphorite sample by using a high-frequency sample melting machine, pouring in a polytetrafluoroethylene beaker with 10 percent nitric acid at a high temperature by virtue of a magnetic stirrer, after the primary sample melting acidification sizing, performing matrix matching by adopting a national grade-I phosphorite, establishing a standard curve by adopting a Yttrium internal standard method, and determining the content of phosphorus pentoxide, magnesium oxide, iron oxide, aluminum oxide, silicon dioxide, calcium oxide, titanium oxide, manganese oxide and strontium oxide in the phosphorite by adopting the ICP-AES. The method has the advantages of rapidness, convenience and accuracy, and is particularly suitable for batch determining the phosphorite samples.
Description
technical field [0001] The invention relates to an ICP-AES method for simultaneously measuring the content of phosphorus, magnesium, iron, aluminum, silicon, calcium, titanium, manganese, manganese and strontium in phosphate rock, belonging to the technical field of analysis and testing. Background technique [0002] The analysis of multiple elements in phosphate rock generally adopts traditional chemical methods, that is, GB / T1870~1881-1995 phosphate rock and phosphate concentrate sampling and sample preparation and chemical analysis methods can only detect a single element, and the operation is lengthy. Sample pretreatment is generally divided into alkali-soluble and acid-soluble, and a large amount of waste liquid is generated at the same time, which can no longer meet the requirements of large-scale rapid analysis. [0003] ICP-AES spectral analysis requires complete dissolution of phosphorus, magnesium, iron, aluminum, silicon, calcium, titanium, manganese, and strontiu...
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