CN102937587A - Method for rapidly measuring rapidly available potassium content in compound fertilizer through flame photometry - Google Patents

Abstract

The invention relates to a method for rapidly measuring rapidly available potassium content in a compound fertilizer through a flame photometry and solves the technical problems that in prior art, manual operation steps are cumbersome, the analysis time is long, and large quantities of manpower, material resources and financial resources are wasted. According to a large number of tests, the method for rapidly measuring the rapidly available potassium content in the compound fertilizer through the flame photometry has the advantages of being simple, convenient, rapid and high in precision degree and accuracy and reducing the assay cost, and the method can be widely used in the measurement of the available potassium in the compound fertilizer.

Description

The method of a kind of flame photometry Fast Measurement composite fertilizer effective K content

Technical field

The present invention relates to a kind of assay method of quick-acting potassium content, particularly the method for a kind of flame photometry Fast Measurement composite fertilizer effective K content.

Background technology

Composite fertilizer's effective K content is an important indicator of composite fertilizer's nutrient, according to national standard, adopts the gravimetric determination of tetraphenyl borate potassium, though accuracy is high, and complex operation, analysis time is long, and each analysis approximately needs 6 hours, and the drug price costliness of using.Chengwu County bureau of agriculture clay fertilizer station is through repeatedly studying for many years, test, proving, invented a kind of employing flame spectrophotometric determination composite fertilizer effective K content, it is easy and simple to handle, quick, each needs about 0.5 hour, do not need very expensive medicine, save the chemical examination cost, directly from typical curve, read the content of composite fertilizer's effective K, and there is all advantages such as higher of degree of accuracy and accuracy.

Summary of the invention

The technical matters that the present invention mainly solves is to provide the method for a kind of flame photometry Fast Measurement composite fertilizer effective K content.

For solving the problems of the technologies described above, the technical scheme that the present invention adopts is:

The method of a kind of flame photometry Fast Measurement composite fertilizer effective K content comprises the following steps:

One, the preparation of liquid to be measured

Really take composite fertilizer's sample that 1.0000g pulverizes in the 200ml Erlenmeyer flask, add 6-7 and drip concentrated hydrochloric acid, then add 20ml distilled water, low temperature boils 10min, coolingly with distilled water, shifts in the 100ml volumetric flask and is settled to scale afterwards, places clarification or dry the filtration;

Two, the mensuration of liquid to be measured

Draw the clear liquid of above-mentioned liquid to be measured or filtrate 5ml in the 100ml volumetric flask, add water and be settled to scale, directly measure on flame photometer after shaking up, read its reading on galvanometer.；

Three, the drafting of typical curve

Accurately take the analytical pure sulfuric acid potassium 0.0000 through the dry 2h of 105 degree, 0.3739, 0.5983, 0.7479, 0.8975, 1.1218, 1.3462g, 1.4958 gram, be placed in respectively the volumetric flask of 1000ml, add water, be settled to scale, shake up and obtain and be equivalent to composite fertilizer containing available potassium 0, 5%, 0.8%, 10%, 12%, 15%, 18%, 20% standard solution, till but above-mentioned solution long preservation to appearance precipitates, draw respectively above-mentioned standard solution 5ml in the 100ml volumetric flask, add water and be settled to scale, after shaking up, on flame photometer, directly measure, read the reading on each comfortable galvanometer, then do horizontal ordinate with being equivalent to composite fertilizer's effective K content percentage, do ordinate with the galvanometer reading and make typical curve,

Four, result is calculated

The percent value checked on typical curve according to the galvanometer reading of sample is the percentage composition of this sample effective K.

Described analytical pure sulfuric acid potassium content is 99.5%.

The invention has the beneficial effects as follows: with the effective potassium in flame spectrophotometric determination composite fertilizer have easy, quick, reduce the chemical examination cost, preci-sion and accuracy is higher advantage all, can be widely used in composite fertilizer the effectively mensuration of potassium.

Embodiment

Below preferred embodiment of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made to more explicit defining.

The embodiment of the present invention comprises:

One, the key instrument and the reagent that adopt

1, flame photometer

2, ten thousand/balance

3, the adjustable electric furnace of 1000W

4, concentrated hydrochloric acid, analytical pure sulfuric acid potassium (content 99.5%)

Two, standard operation solution preparation

Accurately take nucleic acid potassium 0,0.3739g, 0.5983g, 0.7479g, 0.8975g, 1.218g, 1.3462g, 1.4958g through 105 ℃ of dry 2h, be placed in respectively the volumetric flask of 1000ml, add water, be settled to scale, shake up, so, obtain and be equivalent to composite fertilizer containing K2O, 0,5%, 8%, 10%, 12%, 15%, 18%, 20% standard operation solution.

Three, sample preparation methods

Accurately take the composite fertilizer sample of 1.0000g through grinding in the 200ml Erlenmeyer flask, add 6-7 and drip concentrated hydrochloric acid, adding distil water 20ml again, low temperature boils that 10min is cooling to be shifted in the 250ml volumetric flask and be settled to scale with distilled water afterwards, place clarification or dry the filtration, draw the clear liquid of above-mentioned liquid to be measured or filtrate 5ml in the 100ml volumetric flask, adding distil water is settled to scale, directly measure on flame photometer after shaking up, read the reading of its bolt flowmeter.

Four, Specification Curve of Increasing method

Absorb respectively 5ml and be equivalent to composite fertilizer containing K2O, 0,5%, 8%, 10%, 12%, 15%, 18%, 20% standard operation solution is in the 100ml volumetric flask, be settled to scale with distilled water diluting, then on flame photometer, measure, read galvanometer reading separately, do horizontal ordinate with being equivalent to composite fertilizer's available potassium percentage composition, do ordinate with the galvanometer reading and make typical curve.

Five, result is calculated

The percent value checked on typical curve according to the galvanometer reading of sample is the content of this sample effective K.

Six, discuss

1, contrast test

10 kinds of samples are carried out to contrast test by tetraphenyl borate potassium gravimetric method and flame photometry respectively, and measurement result (table 1) shows that two kinds of methods are all in the permissible error scope

Table 1 contrast test

Flame photometry	Tetraphenyl borate potassium gravimetric method	Absolute error
			17.87	17.93	0.06
19.26	19.17	0.09
			14.24	14.38	0.14
15.34	15.17	0.17
			14.93	14.65	0.28
11.84	12.03	0.19
			15.46	15.65	0.19
6.87	6.93	0.06
			4.92	5.08	0.16
17.09	16.96	0.13

2, precision and accuracy test

By test method (flame photometry), sample is measured, every kind of sample replicate determination 5 times, measurement result (table 2) shows that the assay method preci-sion and accuracy is higher.

The test of table 2 preci-sion and accuracy

3, recovery test

To the recovery that adds the standard solution assay method in sample solution, measurement result (table 3) shows, K ₂The recovery of O is: 98.8-100.6%

Table 3 recovery of standard addition test findings

Six, brief summary

By a large amount of tests, show, with the effective potassium in flame spectrophotometric determination composite fertilizer have easy, quick, reduce the chemical examination cost, preci-sion and accuracy is higher advantage all, can be widely used in composite fertilizer the effectively mensuration of potassium.

The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.

Claims (2)

1. the method for a flame photometry Fast Measurement composite fertilizer effective K content, is characterized in that, comprises the following steps:

One, the preparation of liquid to be measured

Really take composite fertilizer's sample that 1.0000g pulverizes in the 200ml Erlenmeyer flask, add 6-7 and drip concentrated hydrochloric acid, then add 20ml distilled water, low temperature boils 10min, coolingly with distilled water, shifts in the 100ml volumetric flask and is settled to scale afterwards, places clarification or dry the filtration;

Two, the mensuration of liquid to be measured

Draw the clear liquid of above-mentioned liquid to be measured or filtrate 5ml in the 100ml volumetric flask, add water and be settled to scale, directly measure on flame photometer after shaking up, read its reading on galvanometer.；

Three, the drafting of typical curve

Accurately take the analytical pure sulfuric acid potassium 0.0000 through the dry 2h of 105 degree, 0.3739, 0.5983, 0.7479, 0.8975, 1.1218, 1.3462g, 1.4958 gram, be placed in respectively the volumetric flask of 1000ml, add water, be settled to scale, shake up and obtain and be equivalent to composite fertilizer containing available potassium 0, 5%, 0.8%, 10%, 12%, 15%, 18%, 20% standard solution, till but above-mentioned solution long preservation to appearance precipitates, draw respectively above-mentioned standard solution 5ml in the 100ml volumetric flask, add water and be settled to scale, after shaking up, on flame photometer, directly measure, read the reading on each comfortable galvanometer, then do horizontal ordinate with being equivalent to composite fertilizer's effective K content percentage, do ordinate with the galvanometer reading and make typical curve,

Four, result is calculated

The percent value checked on typical curve according to the galvanometer reading of sample is the percentage composition of this sample effective K.

2. according to the described method of claim 1 any one, it is characterized in that, described analytical pure sulfuric acid potassium content is 99.5%.