CN105136778A

CN105136778A - Method for simultaneously determining macroelements in ocean sediments through ICP-OES

Info

Publication number: CN105136778A
Application number: CN201510540184.5A
Authority: CN
Inventors: 殷学博; 曾志刚; 陈帅; 王晓媛; 张玉祥
Original assignee: Institute of Oceanology of CAS
Current assignee: Institute of Oceanology of CAS
Priority date: 2015-08-28
Filing date: 2015-08-28
Publication date: 2015-12-09

Abstract

The invention relates to the field of geochemical analysis, in particular to a method for simultaneously determining macroelements in ocean sediments through an ICP-OES. The sample ocean sediments are added into an antiseptic efficient sample dissolution tank, sodium hydroxide and pure water are added, decomposition is performed for 12-24 h on the condition of the low temperature of 240-280 DEG C to form the aqueous alkali environment similar to the molten state, ocean sediment silicate in the sample is effectively molten, and finally an alkaline oxide on the aqueous alkali condition is obtained through decomposition, double decomposition is performed on the condition of hydrochloric acid after cooling is performed, and metal chloride is formed through complete dissolution, silicon is evenly distributed into the solution in the siliceous state, and then the macroelements in the sample are determined through the ICP-OES. According to the method, ocean sediments can be decomposed on the rapid, simple, low-temperature and closed alkaline condition, meanwhile, the method can also be applied to low temperature and alkali fusion of silicate samples, research and application of determining elements such as SiO2 on the closed, low-temperature and alkali fusion conditions are started, and the method has the wide application prospect in geological industry analysis.

Description

A kind of method of macroelement in ICP-OES Simultaneously test oceanic sediment

Technical field

The present invention relates to geochemical analysis field, specifically a kind of method of macroelement in ICP-OES Simultaneously test oceanic sediment.

Background technology

Macroelement has consequence in Marine Geology scientific research, their behavioural characteristics at geologic process are illustrated according to feature, inquire into migration of elements mode, chemical reaction process, instruction geologic function etc., therefore the test of macroelement is particularly important, at present, macroelement method of testing relative maturity, general employing wet chemical, gravimetric method, spectrophotometer method, the macroelement that ICP-OES and XRF etc. complete in geological sample measures, wherein occupy leading position with ICP-OES and XRF method, ICP-OES method amount of samples is few, but in the mensuration of silicon dioxide, there is certain limitation, mainly be subject to the restriction of sample-smelting method, be difficult to the solubility solution obtaining applicable ICP-OES test, as adopted conventional alkali fusion, be subject to the restriction of container, the quantity of batch processing is simultaneously on the low side, once several, tens samples, there is certain risk and operation uncertainty, high-temperature fusion also easily brings external contamination simultaneously, the method that general employing animal gel method combines with ICP-OES, measure the macroelement in geological sample, treatment effeciency is slow, at substantial is artificial.XRF method is relatively simple, but processing speed is comparatively slow, once can process several sample, equally also consume more manpower, and amount of samples is large in addition, seems unable to do what one wishes to some precious sample determinations.Just based on the effect of macroelement in geological research, analyze the relative merits of its assay method.

Summary of the invention

The object of the invention is the method providing macroelement in a kind of ICP-OES Simultaneously test oceanic sediment.

For achieving the above object, the technical solution used in the present invention is:

A kind of method of macroelement in ICP-OES Simultaneously test oceanic sediment, sample oceanic sediment is added in anticorrosion efficient sample-dissolving tank, add excessive NaOH and 1ml pure water again, under the cryogenic conditions of 240-280 DEG C, clear up 12-24 hour, form approximate molten state aqueous slkali environment, to oceanic sediment silicate efficient melting in sample, finally be decomposed into the basic anhydride under aqueous slkali condition, after cooling, under hydrochloric acid condition, double decomposition, dissolve completely, form metal chloride, silicon is then uniformly distributed in the solution with the form of silicic acid, visible solution is limpid, bright, without residue, dissolve completely, then by the macroelement in ICP-OES working sample.

Described double decomposition forms metal chloride, and silicon is then uniformly distributed in the solution with the form of silicic acid, then by the SiO in ICP-OES working sample ₂, Al ₂o ₃, Fe ₂o ₃, MgO, CaO, K ₂o, TiO ₂macroelement.Employing has two inner arc, the anticorrosion efficient digestion tank (second buckles) that leakproofness is strong.

The present invention has advantage:

The present invention adopts airtight alkali fusion to measure the method for macroelement in marine sediment samples, and after cooling, dissolving with hydrochloric acid sample, changes into acid solution, adopts the macroelement of ICP-OES Accurate Determining except Na.The inventive method is simple to operate, have employed anticorrosion efficient molten counteracting tank, has safe and reliable, can resistance to 300 degree of high temperature; Simple to operate, within one second, fasten, complete the fastening of tank body instantaneously, operating efficiency improves 5-10 doubly in this respect; Tank body is airtight, and have employed two inner arc design, under high temperature, condition of high voltage, inner bag tank body seals, and does not leak, ensure that pressure and the temperature of airtight alkali fusion; Batch operation, once can complete tens, even processes while up to a hundred samples, improves efficiency, save manpower and material resources; Sample requirements is little, once enters to need 100mg sample, greatly saves the use amount of sample, is applicable to very much the mensuration in the fields such as ocean, the two poles of the earth and celestial body geology.

Present invention employs anticorrosion efficient sample-dissolving tank method, achieve fast, marine bottom sediment under simple, low temperature, airtight alkali condition clears up, also may be used on low temperature, the alkali fusion of silicate sample simultaneously, open airtight, low temperature, alkali fusion mensuration SiO ₂deng element research and apply, have broad application prospects in geology industry analysis.Simultaneously also for low temperature, airtight purifying technique provide higher reference value.

Accompanying drawing explanation

The anticorrosion efficient digestion tank schematic diagram that Fig. 1 provides for the embodiment of the present invention.

Embodiment

Table 1 is hemipelagic sediment test data result table

Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.

Embodiment 1

1. accurately take GBW07314 hemipelagic sediment standard substance 100mg in polytetrafluoroethylliner liner, and do 5 Duplicate Samples;

2. add the Powdered NaOH of excessive 5-10 times sample size, add 1ml pure water;

3. be airtightly placed in (see Fig. 1) in anticorrosion efficient digestion tank outer tank, fasten, compression bolts pressurizes; Wherein, anticorrosion efficient digestion tank is see (patent No.: ZL201220612911.6).

4., in 240 DEG C of baking ovens, 12 hours are cleared up;

5., after cooling, take out polytetrafluoroethylliner liner, uncap, visible solid molten mass;

6. add 6mlHCl, fully dissolve, and with distilled water diluting constant volume to 100mL, solution is limpid, bright, without residue, dissolve completely;

7. ICP-OES is adopted to test SiO ₂, Al ₂o ₃, Fe ₂o ₃, MgO, CaO, K ₂o, TiO ₂deng element (see table 1).

Table 1 hemipelagic sediment GBW07314 macroelement test result

By test data interpretation of result in table 1, all macroelement test result deviations are all less than 1% (MnO ₂be 2.65%), except Fe ₂o ₃slightly exceed outside range of uncertainty, other element result are all in scope, and the method is applicable to the macroelement that ICP-OES method measures marine sediment samples, is tested the macroelement method of testing of compatibly quality sample.

Claims

1. the method for macroelement in an ICP-OES Simultaneously test oceanic sediment, it is characterized in that: sample oceanic sediment is added in anticorrosion efficient sample-dissolving tank, add NaOH and pure water again, under the cryogenic conditions of 240-280 DEG C, clear up 12-24 hour, form approximate molten state aqueous slkali environment, to oceanic sediment silicate efficient melting in sample, finally be decomposed into the basic anhydride under aqueous slkali condition, after cooling, under hydrochloric acid condition, double decomposition, dissolve completely, form metal chloride, silicon is then uniformly distributed in the solution with the form of silicic acid, then by the macroelement in ICP-OES working sample.

2. by the method for macroelement in ICP-OES Simultaneously test oceanic sediment according to claim 1, it is characterized in that: described double decomposition forms metal chloride, silicon is then uniformly distributed in the solution with the form of silicic acid, then by the SiO in ICP-OES working sample ₂, Al ₂o ₃, Fe ₂o ₃, MgO, CaO, K ₂o, TiO ₂macroelement.