Method for determining manganese and titanium content in ferrophosphorus through microwave digestion ICP-AES method
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A technology of ICP-AES and microwave digestion, which is applied in the field of analytical chemistry, can solve the problems of complex melting process, inability to measure, and long time consumption, and achieve the effect of avoiding environmental pollution, no impact on accuracy, and simple and fast operation
Inactive Publication Date: 2019-08-27
HANDAN IRON & STEEL GROUP +1
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[0003] At present, the ferrophosphorus analysis method is carried out according to a series of ferrous metallurgical industry standards or commodity inspection standards. The ferrous metallurgical industry standards include YB / T4531, YB / T4532 and YB / T4533, but the determination of titanium content is not included; / T3319.1-2012 Import and Export of Ferrophosphorus Part 1: Determination of Phosphorus, Manganese, Silicon, Titanium, Vanadium, Chromium Content by Inductively Coupled Plasma Atomic Emission Spectrometry", but the commodity inspection standard adopts conventional acid dissolution sample preparation, fusion sample The process is complicated and the detection time is long
Chinese patent application 200710099813.0 discloses a method for the determination of phosphorus and manganese in ferrophosphorus. This method uses a photometric method to measure manganese, but manganese and titanium cannot be measured at the same time, and the photometric method is complicated to operate and cannot achieve rapid determination. Purpose; Chinese patent application 200810229712.5 discloses a method for measuring titanium content in low-carbon ferrophosphorus, and Chinese patent application 201710469835.5 discloses a method for the determination of impurity elements in low-titanium ferrophosphorus for high-grade silicon steel by ICP-AES. Although this method is determined by inductively coupled plasma atomic emission spectrometry, it does not include the determination of manganese, and the conventional acid heating method is used to dissolve the sample, which takes a long time and consumes a large amount of acid, which does not meet the concept of green environmental protection.
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Embodiment 1
[0022] The present embodiment is a kind of microwave digestion ICP-AES method for the determination of manganese and titanium content in ferrophosphorus, including microwave assisted digestion and dissolution, preparation of standard solution, drawing of standard curve, and determination of ferrophosphorus sample;
[0023] (1) Microwave-assisted digestion and dissolution of samples: Accurately weigh 0.2000g of ferrophosphorus standard sample (GBW(E)010420) into a microwave digestion tank, add 5mL of pure water, nitric acid with a concentration of 1.42g / mL and nitric acid with a concentration of 1.19g / mL Add 5 mL of hydrochloric acid each, then add 2 mL of hydrofluoric acid with a concentration of 1.15 g / mL, shake gently, and wait until there is no reaction, then tighten the lid of the digestion tank, and perform microwave digestion according to the procedures in Table 1; , add 2mL saturated boric acid solution, cool the test solution, transfer it to a volumetric flask and make ...
Embodiment 2
[0038] The present embodiment is a kind of microwave digestion ICP-AES method for the determination of manganese and titanium content in ferrophosphorus, including microwave assisted digestion and dissolution, preparation of standard solution, drawing of standard curve, and determination of ferrophosphorus sample;
[0039] (1) Microwave-assisted digestion and dissolution of samples: Accurately weigh 0.1000g of ferrophosphorus standard sample (ZBT384)
[0040] Yu Microwave
[0041] In the digestion tank, add 5mL of pure water, 5mL of 1.42g / mL nitric acid and 1.19g / mL hydrochloric acid each, then add 1mL of 1.15g / mL hydrofluoric acid, shake gently, and wait for After the reaction, tighten the lid of the digestion tank, and carry out microwave digestion according to the procedure in Table 5; after the digestion is completed, add 2 mL of saturated boric acid solution, cool the test solution, transfer it to a volumetric flask and make it to volume;
[0042] Table 5 Microwave diges...
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Abstract
The invention discloses a method for determining manganese and titanium content in ferrophosphorus through a microwave digestion ICP-AES method. The method comprises the steps of microwave sample digestion, standard solution preparation, standard curve drawing and sample determination; and the steps are as follows: adding nitric acid, hydrochloric acid and hydrofluoric acid to perform microwave digestion after wetting a ferrophosphorus sample by water, and adding a boric acid solution after the microwave digestion is accomplished; manufacturing a matrix solution through high-purity iron and reference monopotassium phosphate reagent digested sample, adding single element standard solutions of manganese and titanium to prepare a series of mixed standard solutions in different concentrations;selecting the optimal analysis wavelengths of the manganese and titanium, and determining the emission intensity of the manganese and titanium elements in the blank solution and the series of mixed standard solutions by utilizing an inductively coupled plasma atomic emission spectrometer, and drawing a series of standard curves; and determining the spectral line intensities of the manganese and titanium in a ferrophosphorus sample to-be-determined solution by utilizing the inductively coupled plasma atomic emission spectrometer, and finding out the concentrations of the manganese and titaniumand ferrophosphorus samples from the standard curve. The method disclosed by the invention is low in cost, simple in operation and strong in practicability.
Description
technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a microwave digestion ICP-AES method for determining the manganese and titanium contents in ferrophosphorus. Background technique [0002] Ferrophosphorus, as a phosphorus additive in steelmaking and casting, is widely used in rolls, automobile cylinder liners, engine rollers and large castings to increase the corrosion resistance and wear resistance of mechanical parts; ferrophosphorus can also be used to make grenades, The shells of shells, etc., are brittle, and can obtain a large number of shrapnel after explosion, which improves the killing efficiency. In the import and export trade, phosphorus, silicon, manganese, titanium, carbon, sulfur and other components have been required to be tested. [0003] At present, the ferrophosphorus analysis method is carried out according to a series of ferrous metallurgical industry standards or commodity inspecti...
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