CN101299014A - Method for measuring mechanical impurities content in coal oil - Google Patents

Abstract

The present invention relates to a method for measuring the content of mechanical impurity in the coal oil. Through measuring the mechanical impurity of the coal oil with a 49 glass fiber filter, the technical problems of long measuring time, low working efficiency for analyzing and inferior stability of the weighting data in existing method that a moderate speed qualitative filter is used for measuring the content of mechanical impurity in the coal oil. Because the material of 49 glass fiber filter is a glass fiber with diameter from a few micrometers to tens of micrometers, and the specificity of structure makes that the moisture in the air is not easily absorbed, the stability of the measured data is good and can totally satisfy the measurement request. The measurement time is shortened by one third to one half compared with that of the measurement when the moderate speed qualitative filter is used, namely the time of each experiment can be shortened for 3 to 5 hours.

Description

The measuring method of content of impurities in a kind of kerosene

Technical field

The present invention relates to a kind of method of measuring content of impurities in the kerosene.

Background technology

The measuring method of kerosene content of impurities generally adopts the middling speed qualitative filter paper, because the middling speed qualitative filter paper is not easy constant weight, blank filter paper often needs oven dry ability constant weight three or four times, and band sample filter paper also is like this, cause kerosene machinery impurity determination chronic, surveying work efficient is low; In addition, because the qualitative filter paper hydroscopicity is strong, the weighing data poor stability.

The measuring method detailed process of kerosene content of impurities is as follows: at first carry out blank test, with the folding funnel of putting into of ∮ 11 middling speed qualitative filter papers, with 50mL ether-alcohol mixeding liquid by behind the filter paper, in air, dry 10min, put into the measuring cup oven dry, drying time is 1.5h for the first time, puts into exsiccator, weighing behind the 40min, the record weighing data; Put into exsiccator after once more filter paper being put into baking oven oven dry 1h, weighing behind the 40min, record weighing data; Put into exsiccator after for the third time filter paper being put into baking oven oven dry 1h, weighing behind the 40min is the filter paper constant weight, otherwise proceeds the 4th oven dry when the difference of weighing result is no more than 0.0004g for the second time and for the third time.Filter paper after the constant weight carries out kerosene and filters, and the drying course after the filtration is identical with blank test, also needs at least three oven dry.

Then content of impurities is calculated as follows in the kerosene:

$\frac{m_2-m_1}{m}\×100\%$

Wherein: m ₂---band sample filter paper average quality, g;

m ₁---blank filter paper average quality, g;

M---the kerosene quality of filtering, g.

Because the middling speed qualitative filter paper is not easy constant weight, blank filter paper often needs oven dry ability constant weight three or four times, and band sample filter paper also is so, causes kerosene machinery impurity measurement chronic, and analytical work efficient is low; In addition, because the qualitative filter paper hydroscopicity is strong, the weighing data poor stability; Because the filter velocity of middling speed qualitative filter paper is slow, also to use vacuum pump to carry out aided filter in case of necessity.Therefore, the improvement research of carrying out the measuring method of kerosene content of impurities has certain application value.

Summary of the invention

The present invention seeks to propose the assay method of content of impurities in a kind of kerosene, it has solved, and the minute that method that existing employing middling speed qualitative filter paper measures content of impurities in the kerosene brings is long, analytical work efficient is low, the technical matters of weighing data poor stability.

Technical solution of the present invention is:

1] blank filter paper oven dry a: blank 49 type glass fiber filter paper are put into baking oven dry 1.5h, take out constant weight 40min in exsiccator, weigh with scale and write down the blank filter paper quality; Put into exsiccator constant weight 40min after once more filter paper being put into baking oven oven dry 1h, weigh with scale and write down the blank filter paper quality;

2] kerosene filters: kerosene is filtered according to the normal filtration method with 49 type glass fiber filter paper;

3] band mechanical impurity filter paper oven dry: the 49 type glass fiber filter paper that will finish filtration are put into baking oven dries 1.5h, takes out back constant weight 40min in exsiccator, weighs with scale and recording strip sample filter paper quality; Put into exsiccator constant weight 40min after once more filter paper being put into baking oven oven dry 1h, weigh with scale and recording strip sample filter paper quality;

4] calculating machine impurity content: calculate content of impurities in the kerosene in accordance with the following methods:

$\frac{m_2-m_1}{m}\×100\%$

Wherein: m ₂---band sample filter paper average quality, g;

m ₁---blank filter paper average quality, g;

M---the kerosene quality of filtering, g.

The advantage that the present invention has is:

1, measurement data good stability.Because the material of 49 type glass fiber filter paper is diameters is several microns to tens microns glass fibre, the singularity of structure causes it to be difficult for absorbing airborne moisture.And the middling speed qualitative filter paper adopts refining pure white wood pulp or cotton pulp to make, and fiber is elongated and flexible, and tough and tensile folding has good absorbability, and the absorbability that water in air is divided is also very strong.So 49 type glass fiber filter paper are difficult for absorbing airborne moisture in the process of filtration and weighing, the data stability of weighing is good.

2, Measuring Time shortens greatly.49 type glass fiber filter paper are difficult for absorbing airborne moisture in the process of filtration and weighing, the data stability of weighing is good, so blank filter paper oven dry and the oven dry of band mechanical impurity filter paper only need twice constant weight process to get final product respectively, and the middling speed qualitative filter paper needs the constant weight process respectively three to four times, by experiment as can be known, adopt 49 type glass fiber filter paper to carry out the measurement of kerosene mechanical impurity and shorten 1/3rd to 1/2nd than the time of adopting the middling speed qualitative filter paper, promptly each measuring process can shorten the time three by five hours.In addition, because the material of glass fiber filter paper is a glass fibre, the resistance to kerosene in the filtration is little, so velocity ratio is fast with the middling speed qualitative filter paper when filtering, also can save the regular hour.Absorb because 49 type glass fiber filter paper are divided hardly water in air, and this filter paper is crisp, frangibility, so can be placed directly on the balance on goods and services during weighing and carry out, need not be placed in the measuring cup the yet corresponding test period that reduced.

3, measuring equipment is simple.49 type glass fiber filter paper are divided hardly water in air and are absorbed, so can be placed directly on the balance on goods and services during weighing and carry out, and do not need to use measuring cup.Especially 49 type glass fiber filter paper are little to the resistance of kerosene, so do not need to use vacuum pump to carry out aided filter when filtering.

4, can adapt to the environmental requirement of kerosene impurity measurement.49 type glass fiber filter paper are the filter paper of being made by the fiber that melten glass pulls into or blows out, and the qualitative filter paper with respect to adopting refining pure white wood pulp or cotton pulp to make has good heat resistance, corrosion resistance.

Embodiment

One, 49 type glass fiber filter paper can satisfy the test of kerosene machinery impurity analysis:

1, high temperature resistant test

It is 110 ℃ baking oven that the blank 49 type glass fiber filter paper of a ∮ 11 are put into temperature, and oven dry 1.5h takes out constant weight 40min in exsiccator, weighing, record data; The baking oven of putting into 110 ℃ is once more dried 1.5h, carries out constant weight, record data once more.Under 110 ℃ temperature, carry out repeatedly the oven dry of 9h until glass fiber filter paper.The filter paper qualitative data is compared, and quality does not change, and outward appearance does not also have obvious change.And 9h is considerably beyond required drying time in the practical measurement.

Test figure sees Table 1, proves that this filter paper satisfies the requirement of kerosene machinery impurity analysis test temperature condition fully.

The high temperature resistant test figure of table 1 49 type glass fiber filter paper

Drying time (h)	1.5	3	4.5	6	7.5	9
							Filter paper quality (g)	0.4742	0.4741	0.4741	0.4744	0.4744	0.4742

2, solvent corrosion test

Filter paper needs to filter earlier the alcohol-ether organic solvent in the kerosene machinery impurity analysis, therefore needs the anti-solvent corrosion test of checking glass fiber filter paper.According to the blank test method of middling speed qualitative filter paper, 50mL ether-alcohol mixeding liquid by after this glass fiber filter paper, is observed outward appearance, filter paper does not have significant change.In air, dry in the air behind the 10min, put into baking oven, carry out, write down the result of twice weighing, find that twice oven dry of glass fiber filter paper just reached constant weight according to the program of blank test; With the test weighing data contrast of not passing through organic solvent, error is in the 0.0002g scope.

Test figure sees Table 2, illustrates that the alcohol-ether solvent has no effect to 49 type glass fiber filter paper, and this filter paper satisfies the requirement of kerosene machinery impurity analysis test solvent fully.

Table 2 49 type glass fiber filter paper solvent corrosion test figures

3,49 type glass fiber filter paper and middling speed qualitative filter paper moisture absorption speed contrast test

49 type glass fiber filter paper and middling speed qualitative filter paper are directly put into balance respectively, measure the situation of change of its quality, concrete data see Table 3, by table 3 data as can be seen, 49 type glass fiber filter paper divide absorption very little to water in air, and the moisture absorption degree of middling speed qualitative filter paper is far longer than glass fiber filter paper.For kerosene machinery impurity determination method is gravimetric method, uses 49 type glass fiber filter paper to be more suitable for.

Table 3 filter paper moisture absorption speed contrast test

Time	3 seconds	10 seconds	30 seconds	60 seconds
					Glass fiber filter paper quality (g)	0.4696	0.4696	0.4696	0.4698
Middling speed quantitative filter paper quality (g)	0.4776	0.4785	0.4811	0.4900

Two, 49 type glass fiber filter paper are to the test of kerosene machinery impurity analysis:

Because two test findings of 49 type glass fiber filter paper all satisfy kerosene machinery impurity determination conditional request, therefore, carried out repeatedly the test of kerosene machinery impurity determination, test is carried out according to measurement (analysis) method in the operation " the provisional technical conditions of YTJR-71-97 space flight kerosene ".

1] instrument and equipment: glass funnel; Surface plate; Reagent bottle; The 150mL beaker; Exsiccator.

2] reagent: be made into the alcohol-ether mixed liquor in 4: 1 by volume with 95% ethanol and ether.

3] preliminary work: 49 type glass fiber filter paper are folded be placed in the glass funnel, alcohol-ether mixed liquor with 50mL filters, after having filtered, filter paper was air drying 10 minutes, then filter paper is placed in the surface plate of spacious lid, drying is 1.5 hours in 105～110 ℃ of baking ovens, surface plate was moved in the exsiccator cooling after 40 minutes, carry out weighing, claim accurate to 0.0002g, and then put into baking oven (105～110 ℃) dry 1 hour, cooling weighing after 40 minutes in exsiccator is no more than 0.0004g until the difference of twice weighing.

4] test procedure:

A. will be contained in the kerosene that filters in the vial (be no more than bottle volume 3/4) and shake and made it to mix in 5 minutes, take by weighing the 100g sample;

B. constant weight is good filter paper is placed in the glass funnel that fixes, and sample is poured on the filter paper along glass bar, and the specimen height of pouring into during filtration in the funnel must not surpass 3/4 of filter paper;

C. remaining in precipitation in the beaker divides with 50mL alcohol-ether mixed liquor and is flushed on the filter paper for three times.After flushing finishes, air drying 10 minutes, the filter paper that will have precipitation then is placed on the surface plate, drying is 1.5 hours in 105～110 ℃ of baking ovens, put into exsiccator cooling 40 minutes, carry out weighing, claim accurate to 0.0002g, repeat the operation of dry (be 1 hour drying time for the second time) cooling and weighing, till the difference between double weighing is no more than 0.0004g; General needs dry weighing twice, if content of impurities is no more than the scope of kerosene technical requirement, drying and weighing for the second time handled and also can be omitted.

5] calculate:

Sample content of impurities X (%) by formula (11) calculates:

$X=\frac{m_2-m_1}{m}\×100$

In the formula: m ₂---have the average quality of the filter paper and the surface plate of mechanical impurity, g;

m ₁---the average quality of filter paper and surface plate, g;

M---the quality of the kerosene that filters, g.

6] precision: two results' of same operator's replication is poor, should not surpass 0.005%.

Measure calculating and the results are shown in Table 4 data, glass fiber filter paper is fit to carry out the test of kerosene machinery impurity analysis.

Table 4 uses glass fiber filter paper to measure kerosene machinery dirl butter result

Continuous table 4

When testing with glass fiber filter paper, compare test with the middling speed quantitative filter paper, because middling speed quantitative filter paper hydroscopicity is strong, therefore, the oven dry constant weight need be placed in the measuring cup carries out.Blank filter paper is for twice a constant weight, and weighing data is stable, the results are shown in Table 5 with what test several times.As can be seen from Table 5, when using the middling speed quantitative filter paper to measure, blank filter paper often need be carried out oven dry ability constant weight three times, and data are difficult for stable, and carry sample filter paper also is difficult for constant weight, causes analysis time long, and analysis efficiency is low.

Table 5 uses the middling speed quantitative filter paper to measure mechanical impurity test figure in the kerosene

Continuous table 5

Two kinds of filter paper income analysis the results are shown in Table 6, and as can be seen from Table 6, the error of using two kinds of filter paper income analysis results is within allowed band.And analysis efficiency differs widely.

Table 6 glass fiber filter paper measurement result and the contrast of middling speed quantitative filter paper measurement result

Three, the principle of the invention: in the work of kerosene machinery impurity analysis, replace the middling speed quantitative filter paper, only need to get final product constant weight through twice oven dry, good stability with 49 type glass fiber filter paper; Data stabilization in the weighing process, affected by environment hardly; Shorten analysis time greatly, and work efficiency improves greatly; Error in allowed limits.Because 49 its materials of type glass fiber filter paper are diameters is several microns to tens microns glass fibre, the singularity of structure causes it to be difficult for absorbing airborne moisture, and good heat-resisting, corrosion resistance are arranged, therefore easy constant weight, weighing data good stability.Through test and analysis, the effect of other glass fiber filter paper is bad.Make and the middling speed qualitative filter paper is wood pulp or cotton pulp, easily absorb airborne moisture.

Claims (1)

1, the measuring method of content of impurities in a kind of kerosene, it is characterized in that: it may further comprise the steps:

1] blank filter paper oven dry a: blank 49 type glass fiber filter paper are put into baking oven dry 1.5h, take out constant weight 40min in exsiccator, weigh with scale and write down the blank filter paper quality; Put into exsiccator constant weight 40min after once more filter paper being put into baking oven oven dry 1h, weigh with scale and write down the blank filter paper quality;

2] kerosene filters: kerosene is filtered according to the normal filtration method with 49 type glass fiber filter paper;

3] band mechanical impurity filter paper oven dry: the 49 type glass fiber filter paper that will finish filtration are put into baking oven dries 1.5h, takes out back constant weight 40min in exsiccator, weighs with scale and recording strip sample filter paper quality; Put into exsiccator constant weight 40min after once more filter paper being put into baking oven oven dry 1h, weigh with scale and recording strip sample filter paper quality;

4] calculating machine impurity content: calculate content of impurities in the kerosene in accordance with the following methods:

$\frac{m_2-m_1}{m}\×100\%$

Wherein: m ₂---band sample filter paper average quality, g;

m ₁---blank filter paper average quality, g;

M---the kerosene quality of filtering, g.