CN101109710B - Method for measuring magnesium oxide and calcium oxide content in magnesium calcium vitamin C preparation - Google Patents
Method for measuring magnesium oxide and calcium oxide content in magnesium calcium vitamin C preparation Download PDFInfo
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Abstract
The invention provides a content-determining method for a Mg-Ca vitamin C preparation. A specimen containing magnesium oxide and calcium oxide totally 0.4mmol is taken and placed into a porcelain crucible; a small amount of water is added; the mixture is heated slowly and shaken from time to time, so that the mixture is completely wet; heating is continued till no smoke exists. The mixture is placed in a 500-600 centigrade hi-temperature resistance oven, cooled, moistened by a small amount of water, some 10-40% chlorhydric acid is added; the mixture is boiled so as to become dissolved, then cooled to room temperature, filtered; the filter paper is washed by 10-40% chlorhydric acid for 2-3 times; the filtering solution and the washing fluid are mixed, diluted by water to desired quantity, now the specimen solution is obtained. Some specimen solution is fetched, diluted by a specified dilution way, the volume of the Disodium Edetate diluting solution consumed by the total magnesium oxide and calcium oxide is recorded and calculated. The method is rapid, accurate and easy, is applicable for quantitative determining of any mixture containing Mg and Ca.
Description
Technical field
The present invention relates to food or medicine field of measuring technique, the content assaying method of magnesium oxide and calcium oxide in specifically a kind of magnesium calcium vitamin C preparation.
Background technology
Endemic fluorosis is a kind of to invade bone and tooth, and relate to a kind of biomass geochemistry disease of each tissue of whole body, bone and tooth be fluorine mainly store tissue, the content of fluorine in bone and tooth is to judge whether prevent and treat the fluorosis medicine effectively generally acknowledges one of index.The Rao of India Osmania medical college, scholars such as S, R in 1975 report and use serpentine treatment fluorosis of bone, obtain sure curative effect.Shangguan of Xi'an Medical University in 1977 deposits the homemade serpentine of usefulness such as the people and produces the peaceful sheet of fluorine and carry out the fluorosis of bone treatment, and is evident in efficacy.Adopt serpentine, lime carbonate and vitamin C to form the magnesium calcium vitamin C sheet of compound, its quality standard has been recorded into national standard, and standard No. is: WS-10001-(HD-1407)-2003.Serpentine is that (the ideal composition formula is the chemical constitution silicate that mainly contains magnesium: Mg
6[Si
4O
10] (OH)
8), can obviously reduce fluorosis of bone patient's serum acid phosphatase, lactic dehydrogenase ester, serum inorganic phosphorus and urine F
-Ion concentration.Thereby significantly improve functional status, joint motion, the muscular strength of fluorosis of bone, the power of shaking hands; Lime carbonate can generate insoluble calcium fluoride with fluoride and promote dental calcium to form; Vitamin C can promote capillary and little blood vessel hyperplasia, improves whole body circulation and participates in the synthetic immunologic function of keeping between neurotransmitter, collagen and histocyte, and increases the resistibility that infects etc.In sum, the magnesium calcium vitamin C sheet is having unique curative effect aspect the treatment fluorosis of bone, and toxic and side effect is less.
In former national standard content assaying method,, time-consuming because of the cumbersome complexity of test sample pre-treatment process.Contain silicate in the concrete test sample, porcelain crucible seriously corroded after 700～800 ℃ of calcinings forms the gelatin thing of glass and makes filtration difficulty in the pre-treatment, adopts the nitric acid of high concentration easily to make filter paper corrosion failure when filtering, thereby cause the recovery on the low side, the method poor reproducibility.In addition, adopt the titration method of stipulating in the primary standard, the titration end-point hop is not obvious, causes the terminal point determining difficulty, accurately quantitative measurement.
Summary of the invention
The objective of the invention is at the above-mentioned technical matters that exists in the former national standard, provide a kind of have measure accurately, favorable reproducibility, easy and simple to handle, analyze new fast magnesium calcium vitamin C preparation or contain magnesium and the content assaying method of calcium constituent potpourri.
Technical solution of the present invention is:
(1) get and be equivalent to contain magnesium oxide and the calcium oxide total amount is the test sample of 0.4mmol, porphyrize is put in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continue to be heated to cigarette to the greatest extent; Place 500～600 ℃ of high temperature resistance furnaces to calcine 20～60 minutes, take out, put cold, wetting with little water, add 10%～40% aqueous hydrochloric acid solution of 10～15ml, heated and boiled made dissolving in 2～10 minutes, be cooled to room temperature, filter, filter paper is washed 2～3 times with 10%～40% hydrochloric acid solution, each 3ml, with a small amount of washing 1～2 time, merging filtrate and washing lotion are put in the 250ml measuring bottle again, thin up is need testing solution to scale;
(2) mensuration of magnesium oxide, calcium oxide total amount: get need testing solution 25ml, place conical flask, add water 10～30ml, add each 2～10ml of 2%～10% sodium potassium tartrate tetrahydrate and 10%～40% triethanolamine aqueous solution, shake up, ammonia-ammonium chloride buffer 5～the 15ml that adds pH10 ± 0.1, cupferron 20mg～50mg shakes up again, adds K-B indicator 20mg～50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blue-green;
(3) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the conical flask, add water 10～30ml, add each 2～10ml of 2%～10% sodium potassium tartrate tetrahydrate and 10%～40% triethanolamine aqueous solution, shake up, add 20% sodium hydroxide solution, 5～15ml, cupferron 20mg～50mg, shake up again, add K-B indicator 20mg～50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blueness, and every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the CaO of 2.805mg;
(4) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, be the volume of magnesium oxide consumption Calcium Disodium Versenate vs, every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the MgO of 2.015mg.
Assay method is combined as:
(1) preparation of need testing solution: get and be equivalent to contain magnesium oxide and the calcium oxide total amount is the test sample of 0.4mmol, porphyrize is put in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continue to be heated to cigarette to the greatest extent; Place 500～550 ℃ of high temperature resistance furnace calcinings 30 minutes, take out, put cold, wetting with little water, add the 10ml of 19% hydrochloric acid solution, heated and boiled made dissolving in 5 minutes, be cooled to room temperature, filter, filter paper is washed 3 times with 19% hydrochloric acid solution, each 3ml, again with a small amount of washing 2 times, merge five filtrate and washing lotion, put in the 250ml measuring bottle, thin up is need testing solution to scale.
(2) mensuration of magnesium oxide calcium oxide total amount: precision is measured need testing solution 25ml, put in the conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 5% sodium potassium tartrate tetrahydrate and 33%, shake up, ammonia-ammonium chloride buffer the 10ml that adds pH10 ± 0.1, cupferron 50mg shakes up again, adds K-B indicator 50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blue-green;
(3) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 5% sodium potassium tartrate tetrahydrate and 33%, shake up, add 20% sodium hydroxide solution 10ml, cupferron 50mg shakes up again, add K-B indicator 50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blueness, and every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the CaO of 2.805mg;
(4) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, be the volume of magnesium oxide consumption Calcium Disodium Versenate vs, every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the MgO of 2.015mg.
The good effect that the present invention has compared with the prior art is: in former national standard content assaying method, because of the cumbersome complexity of test sample pre-treatment process, time-consuming, the recovery is on the low side, the method poor reproducibility.In addition, adopt the titration method of stipulating in the primary standard, the titration end-point hop is not obvious, causes the terminal point determining difficulty, accurately quantitative measurement.Adopt the assay method of being set up, easy, method is accurate, favorable reproducibility.
The methodology demonstration test of the inventive method is as follows:
Linear relationship is investigated: precision takes by weighing the magnesium powder respectively, lime carbonate is an amount of, adds hydrochloric acid solution (1 → 2) dissolving.Demarcate the concentration that obtains mixing the reference substance storing solution with Calcium Disodium Versenate vs (0.05mol/L); Get calcium, the magnesium ion titer is measured according to above-mentioned (2)～(5) method.The amount of taking be original test solution normally the amount of taking 50%, 75%, 100%, 125%, 150%, i.e. 12.5ml, 18.75ml, 25ml, 31.25ml, 37.5ml.The volume V that consumes Calcium Disodium Versenate vs (0.05mol/L) with calcium, magnesium ion returns the amount of calcium, magnesium ion, and draws typical curve.Calculating calcium ion complexometric titration least square linear regression equation is:
V
1＝0.4556m
1+0.1084，r
1＝0.9995
The result shows that calcium ion is in the scope of 2.506mg～7.515mg, and consuming the volume of Calcium Disodium Versenate vs (0.05mol/L) and the measurer of calcium ion has good linear relationship.
Magnesium ion complexometric titration regression equation is:
V
2＝0.8248m
2-0.1093，r
2＝0.9998。
The result shows that magnesium ion is in the scope of 3.357mg～10.071mg, and magnesium ion consumes the volume of Calcium Disodium Versenate vs (0.05mol/L) and the measurer of magnesium ion has good linear relationship.
Recovery test: precision takes by weighing the magnesium powder respectively, lime carbonate is an amount of, and with an amount of dissolving of hydrochloric acid solution (1 → 2), dilute with water is made Ca
2+ Std0.3mol/L, Mg
2+ Std0.5mol/L solution, be used as the reference substance storing solution; Precision is measured reference substance storing solution 0.5ml, demarcates with Calcium Disodium Versenate vs (0.05mol/L), gets reference substance storing solution concentration, gets with a collection of each about 0.4g of magnesium calcium vitamin C preparation test sample powder in porcelain crucible, totally 12 parts, is numbered 1～12 respectively.Wherein, the 1st～3 part does not add the reference substance storing solution, the 4th～6 part adds reference substance storing solution 1.5ml, the 7th～9 part adds reference substance storing solution 2.6ml, and the 10th～12 part adds reference substance storing solution 3.6ml, presses under the preparation of need testing solution, begin operation from " calcining ", measure by above-mentioned (2)～(5) method, calculate recovery rate, data result sees the following form.
Table 1: calcium ion recovery test result
As a result, recovery test shows that average recovery rate can be with the Ca in the magnesium calcium vitamin C preparation with the extracting method of design greater than 95.0%
2+Ion is accurately measured.
Table 2: magnesium recovery test
As a result, recovery test shows that average recovery rate can be with the Mg in the magnesium calcium vitamin C preparation with the extracting method of design greater than 95.0%
2+Ion is accurately measured.
Replica test
Get 6 parts of same batch of sample preparation, measure, obtain the RSD% value with method according to assay.RSD% must be less than 3%.
Table 3: replica test data
The result shows that RSD% less than 3%, meets the requirements.
The precision test
Get same sample and survey 5 times continuously, obtain RSD%, RSD% must be less than 3%.
Table 4: precision experimental result
The result shows that RSD% is all less than 3%, and precision is better.
The stability of need testing solution: after the preparation of the need testing solution of magnesium calcium vitamin C preparation finished, respectively at the content of measuring magnesium oxide and calcium oxide in 1,2,4,6,8,12,24,36 hour, RSD% was all less than 1.0%.Need testing solution is comparatively stable.
Embodiment
Embodiment 1
(1) instrument and reagent:
Test sample: magnesium calcium vitamin C sheet: test sample numbering: 2007-1,2007-2,2007-3,2007-4,2007-5,2007-6,2007-7,2007-8,2007-9,2007-10; Specification: every contains serpentine 50mg.
Check reference substance: lime carbonate, specification: analyze pure (lime carbonate indicates content 99.0%); The magnesium powder, specification: analyze pure (magnesium indicates content 99.0%).
Instrument and reagent reagent: water is heavily to steam distilled water; Hydrochloric acid, Calcium Disodium Versenate, NaOH, sodium potassium tartrate tetrahydrate, triethanolamine, ammonium chloride, cupferron (diethyl-dithio sodium formate), it is AG that K-B indicator (acid chromium blue k mixed porphyrize with naphthol green B with 1: 2, add again grind well after 50 times potassium nitrate mixes formulated) waits.
Used Container transfer pipet (25ml, 10ml, 5ml), volumetric flask (250ml), all calibrated country one, the goods of inferior quality standard of meeting of acid dropper (10ml).
(2) preparation of need testing solution: get 20 of test samples, the accurate title, decide, porphyrize, and precision takes by weighing in right amount (being equivalent to 8 amount approximately), puts in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continue to be heated to cigarette to the greatest extent; Place 500～550 ℃ of high temperature resistance furnace calcinings 30 minutes, take out, put cold, wetting with little water, add the 10ml of 19% hydrochloric acid solution, heated and boiled made dissolving in 5 minutes, be cooled to room temperature, filter, filter paper is washed 3 times with 19% hydrochloric acid solution, each 3ml, again with a small amount of washing 2 times, merge five filtrate and washing lotion, put in the 250ml measuring bottle, thin up is need testing solution to scale.
(3) mensuration of magnesium oxide, calcium oxide total amount: precision is measured need testing solution 25ml, put in the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 5% sodium potassium tartrate tetrahydrate and 33%, shake up, ammonification-ammonium chloride buffer (pH10 ± 0.1) 10ml, the about 50mg of cupferron shakes up again, adds the about 50mg of K-B indicator, with Calcium Disodium Versenate vs (0.05mol/L) titration, disappearing to the solution redness becomes blue-green.
(4) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 5% sodium potassium tartrate tetrahydrate and 33%, shake up, add 20% sodium hydroxide solution 10ml, the about 50mg of cupferron shakes up again, add the about 50mg of K-B indicator, with Calcium Disodium Versenate vs (0.05mol/L) titration, disappearing to the solution redness becomes blueness, and every 1ml Calcium Disodium Versenate vs (0.05mol/L) is equivalent to the CaO of 2.805mg.
(5) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, and has both consumed the volume of Calcium Disodium Versenate vs for magnesium oxide.Every 1ml Calcium Disodium Versenate vs (0.05mol/L) is equivalent to the MgO of 2.015mg.
Sample determination: get the magnesium calcium vitamin C preparation of different batches, test according to above-mentioned (2)～(5) method, test result sees Table 5:
Magnesium calcium vitamin C preparation prescription is serpentine: lime carbonate: vitamin C: auxiliary material [50: 25: 12.5: 12.5 (they heavily are 0.1g calculating by sheet)] and think every theory of this product contain magnesium in magnesium oxide greater than 14mg, calcic in calcium oxide greater than 13mg, in conjunction with the result of above many batches of test sample assays.Therefore, can in the magnesium calcium vitamin C preparation quality standard regulation content limit be: every of this product contain magnesium in magnesium oxide greater than 13mg, calcic in calcium oxide greater than 10mg.
Table 5: different batches test sample and former national standard measurement result contrast table
Embodiment 2
(1) test sample
Magnesium calcium vitamin C capsule: test sample numbering: 2007J-1,2007J-2,2007J-3,2007J-4,2007J-5,2007J-6,2007J-7,2007J-8,2007J-9,2007J-10; Specification: every contains serpentine 50mg.
(2) preparation of need testing solution: get the content under the content uniformity item, mix, precision takes by weighing in right amount (being equivalent to 8 amount approximately), puts in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continues to be heated to cigarette to the greatest extent.Place 560～600 ℃ of high temperature resistance furnace calcinings 60 minutes, take out, put cold, wetting with little water, add the 10ml of 40% hydrochloric acid solution, heated and boiled made dissolving in 5 minutes, be cooled to room temperature, filter, filter paper is washed 2 times with 40% hydrochloric acid solution, each 3ml, again with a small amount of washing 2 times, merge five filtrate and washing lotion, put in the 250ml measuring bottle, thin up is need testing solution to scale.
(3) mensuration of magnesium oxide calcium oxide total amount: precision is measured need testing solution 25ml, put in the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 10% sodium potassium tartrate tetrahydrate and 10%, shake up, ammonification-ammonium chloride buffer (pH10 ± 0.1) 10ml, the about 50mg of cupferron shakes up again, adds the about 50mg of K-B indicator, with Calcium Disodium Versenate vs (0.05mol/L) titration, disappearing to the solution redness becomes blue-green.
(4) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the 250ml conical flask, add water 20ml, each 5ml of triethanolamine aqueous solution that adds 10% sodium potassium tartrate tetrahydrate and 10%, shake up, add 20% sodium hydroxide solution 10ml, the about 50mg of cupferron, shake up again, add the about 50mg of K-B indicator, with Calcium Disodium Versenate vs (0.05mol/L) titration, disappearing to the solution redness becomes blueness, and every 1ml Calcium Disodium Versenate vs (0.05mol/L) is equivalent to the CaO of 2.805mg.
(5) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, and has both consumed the volume of Calcium Disodium Versenate vs for magnesium oxide.Every 1ml Calcium Disodium Versenate vs (0.05mol/L) is equivalent to the MgO of 2.015mg.
Embodiment 3
(1) test sample
Magnesium calcium vitamin C powder: test sample numbering: 2007S-1,2007S-2,2007S-3,2007S-4,2007S-5,2007S-6,2007S-7,2007S-8,2007S-9,2007S-10; Specification: every bag contains serpentine 600mg.
(2) this product is got in the preparation of need testing solution, mixes, and precision takes by weighing in right amount (being equivalent to contain magnesium oxide and calcium oxide total amount 0.4mmol approximately), puts in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continues to be heated to cigarette to the greatest extent.Place 560～600 ℃ of high temperature resistance furnace calcinings 20 minutes, take out, put cold, wetting with little water, add the 10ml of 10% hydrochloric acid solution, heated and boiled made dissolving in 5 minutes, be cooled to room temperature, filter, filter paper is washed 2 times with 10% hydrochloric acid solution, each 3ml, again with a small amount of washing 2 times, merge five filtrate and washing lotion, put in the 250ml measuring bottle, thin up is need testing solution to scale.
(3) mensuration of magnesium oxide calcium oxide total amount: precision is measured need testing solution 25ml, put in the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 2% sodium potassium tartrate tetrahydrate and 10%, shake up, ammonification-ammonium chloride buffer (pH10 ± 0.1) 10ml, the about 50mg of cupferron shakes up again, adds the about 20mg of K-B indicator, with Calcium Disodium Versenate vs (0.05mol/L) titration, disappearing to the solution redness becomes blue-green.
(4) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 2% sodium potassium tartrate tetrahydrate and 10%, shake up, add 20% sodium hydroxide solution 10ml, the about 50mg of cupferron shakes up again, add the about 20mg of K-B indicator, with Calcium Disodium Versenate vs (0.05mol/L) titration, disappearing to the solution redness becomes blueness, and every 1ml Calcium Disodium Versenate vs (0.05mol/L) is equivalent to the CaO of 2.805mg.
(5) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, and has both consumed the volume of Calcium Disodium Versenate vs for magnesium oxide.Every 1ml Calcium Disodium Versenate vs (0.05mol/L) is equivalent to the MgO of 2.015mg.
Claims (2)
1. magnesium oxide and calcium oxide content assay method in the magnesium calcium vitamin C preparation, this method comprises the steps:
(1) get and be equivalent to contain magnesium oxide and the calcium oxide total amount is the test sample of 0.4mmol, porphyrize is put in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continue to be heated to cigarette to the greatest extent; Place 500～600 ℃ of high temperature resistance furnaces to calcine 20～60 minutes, take out, put cold, wetting with little water, add 10%～40% aqueous hydrochloric acid solution of 10～15ml, heated and boiled made dissolving in 2～10 minutes, be cooled to room temperature, filter, filter paper is washed 2～3 times with 10%～40% hydrochloric acid solution, each 3ml, with a small amount of washing 1～2 time, merging filtrate and washing lotion are put in the 250ml measuring bottle again, thin up is need testing solution to scale;
(2) mensuration of magnesium oxide, calcium oxide total amount: get need testing solution 25ml, place conical flask, add water 10～30ml, add each 2～10ml of 2%～10% sodium potassium tartrate tetrahydrate and 10%～40% triethanolamine aqueous solution, shake up, ammonia-ammonium chloride buffer 5～the 15ml that adds pH10 ± 0.1, cupferron 20mg～50mg shakes up again, adds K-B indicator 20mg～50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blue-green;
(3) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the conical flask, add water 10～30ml, add each 2～10ml of 2%～10% sodium potassium tartrate tetrahydrate and 10%～40% triethanolamine aqueous solution, shake up, add 20% sodium hydroxide solution, 5～15ml, cupferron 20mg～50mg, shake up again, add K-B indicator 20mg～50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blueness, and every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the CaO of 2.805mg;
(4) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, be the volume of magnesium oxide consumption Calcium Disodium Versenate vs, every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the MgO of 2.015mg.
2. magnesium oxide and calcium oxide content assay method in the described magnesium calcium vitamin C preparation of claim 1 is characterized in that assay method is:
(1) preparation of need testing solution: get and be equivalent to contain magnesium oxide and the calcium oxide total amount is the test sample of 0.4mmol, porphyrize is put in the porcelain crucible, adds low amounts of water, and slowly heating and jolting constantly make its complete wetting, continue to be heated to cigarette to the greatest extent; Place 500～550 ℃ of high temperature resistance furnace calcinings 30 minutes, take out, put cold, wetting with little water, add the 10ml of 19% hydrochloric acid solution, heated and boiled made dissolving in 5 minutes, be cooled to room temperature, filter, filter paper is washed 3 times with 19% hydrochloric acid solution, each 3ml, with a small amount of washing 2 times, merging filtrate and five washing lotions are put in the 250ml measuring bottle again, thin up is need testing solution to scale.
(2) mensuration of magnesium oxide calcium oxide total amount: precision is measured need testing solution 25ml, put in the conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 5% sodium potassium tartrate tetrahydrate and 33%, shake up, ammonia-ammonium chloride buffer the 10ml that adds pH10 ± 0.1, cupferron 50mg shakes up again, adds K-B indicator 50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blue-green;
(3) calcium oxide content is measured: precision is measured need testing solution 25ml, put in the conical flask, add water 20ml, add each 5ml of triethanolamine aqueous solution of 5% sodium potassium tartrate tetrahydrate and 33%, shake up, add 20% sodium hydroxide solution 10ml, cupferron 50mg shakes up again, add K-B indicator 50mg, with Calcium Disodium Versenate vs 0.05mol/L titration, disappearing to the solution redness becomes blueness, and every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the CaO of 2.805mg;
(4) content of magnesia is measured: the volume of the Calcium Disodium Versenate vs that magnesium oxide, the total quantitative determination of calcium oxide are consumed deducts the volume that calcium oxide content is measured the Calcium Disodium Versenate vs that is consumed, be the volume of magnesium oxide consumption Calcium Disodium Versenate vs, every 1ml 0.05mol/L Calcium Disodium Versenate vs is equivalent to the MgO of 2.015mg.
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