CN85105502A - The rapid test method of gold content in gold-silver alloy and Jin-Yin-aldary - Google Patents
The rapid test method of gold content in gold-silver alloy and Jin-Yin-aldary Download PDFInfo
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- CN85105502A CN85105502A CN 85105502 CN85105502A CN85105502A CN 85105502 A CN85105502 A CN 85105502A CN 85105502 CN85105502 CN 85105502 CN 85105502 A CN85105502 A CN 85105502A CN 85105502 A CN85105502 A CN 85105502A
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Abstract
The invention provides the new method of gold content in a kind of fast measuring gold-silver alloy and the Jin-Yin-aldary.This method adopts and adds a large amount of potassium chloride, and adds the concentrated hydrochloric acid and the concentrated nitric acid solution heating for dissolving of mixing by a certain percentage, adds certain excessive mohr salt solution again, with the back titration of potassium dichromate standard solution.Use this method gold content in the working sample exactly.Accuracy of measurement height, absolute error are in ± 0.2%, and be simultaneously simple to operate, grasps easily, just can finish the overall process of mensuration in two hours.And the gold that is consumed in the mensuration process can reclaim, and is very suitable for the analysis of daily productive gold content.
Description
The present invention relates to the mensuration of gold content in a kind of alloy, specifically a new method of utilizing between Mohr's salt-potassium dichromate method by measure to measure gold content.
In prior art, the mensuration of gold content in gold-silver alloy and Jin-Yin-aldary normally adopts gravimetric method, volumetric method and instrumental analysis.Though the gravimetric determination accuracy is high, it is miscellaneous to measure formality, once measures to take 3 day time and just can finish, and is not suitable for the analysis in the daily production; The instrumental analysis finding speed is fast, but error is bigger, and is special bigger for the high sample determination error of content.And the instrument cost is big, can not widespread usage on producing; The method of volumetric determination gold is a lot, and iodimetric titration is more ancient method, but because of the iodimetric titration selectivity is not high, it is cumbersome to measure formality, and error is also bigger.Other volumetric methods are as using Aa
3+, p-phenylenediamine (PPD), ascorbic acid, hydrazine sulfate, metol, benzenediol, N-amino-phenol, Ti
3+, Cr
2+, Cu
+ 1, Sn
2+VO
+ 1Deng direct titration to measure gold.But because above-mentioned metallic salt and organic reagent all are unsettled, condition determination harshness, error are big, cause their application to be restricted.
Task of the present invention be by provide a kind of need not expensive exact instrument, can obtain higher accuracy of measurement, while method is simple and easy, favorable reproducibility, grasp easily, the method for gold content in practical fast measuring gold-silver alloy and the Jin-Yin-aldary.
The solution of the above-mentioned task of the present invention is by adopting the indirect volumetric method of Mohr's salt-potassium dichromate to realize.The mensuration of gold content in the gold-silver alloy of high-load silver and Jin-Yin-aldary.
Following reaction, take place in concentrated hydrochloric acid and concentrated nitric acid solution heating for dissolving that gold-silver alloy and Jin-Yin-aldary sample mixes with the certain proportion amount in the presence of a large amount of chlorides:
Copper then generates Cu
2+, after sample dissolution is complete, under in check heated condition, be evaporated near doing, adding the suitable quantity of water dilution, when separating out the AgCl precipitation again, control Cl in the solution
-Concentration makes less than 1 molar concentration, to avoid Cl
-Interference to gold is measured makes Au simultaneously again
3+By Fe
2+Be reduced to metallic gold fully.
At this moment the AgCl in the solution precipitates and Cu
2+Deng the mensuration of not disturbing gold.When adding certain excessive standard mohr salt solution (is iron ammonium sulfate (NH
4)
2Fe(SO
4)
26H
2O) with Au
3+Reaction, remaining mohr salt solution is with standard K
2Cr
2O
7The solution residual titration it, its reaction is as follows:
When going into excessive K a little
2Cr
2O
7Behind the solution, for example the aniline sodium sulfonate is oxidized for indicator, makes solution colour that significantly sudden change take place, and the expression titration end-point is according to the K of Mohr's salt addition and consumption
2Cr
2O
7The consumption of solution, the gold content in just can calculation sample.
In the following formula: V '
Fe2+--adds the volume (milliliter) of standard mohr salt solution
V
Fe2+/Au--standard mohr salt solution is to the titer (grams per milliliter) of gold
W
Sample-weigh the weight (gram) of alloy sample
According to the method for gold content in mensuration gold-silver alloy provided by the invention and the Jin-Yin-aldary, have fast, the whole mensuration process of finding speed and about 2 hours, can finish, the weight/power ratio method needs 3 day time faster; Accuracy of measurement height, absolute error are in ± 0.2%, and this is than much higher with the large-scale expensive equipment accuracy of measurement; The favorable reproducibility of experiment, interference such as a large amount of silver that are not subjected to exist in the sample, copper; Assay method is simple, and practicality is good, as long as just can carry out with general glass apparatus, the golden sample that each simultaneously mensuration is consumed can reclaim, and is applicable to very much regular production analytical work.
Be the most preferred embodiment that the present invention proposes below.
Weigh 0.18 gram (being accurate to 0.0001 gram) gold-silver alloy or Jin-Yin-aldary sample in small, broken bits in 250 ml beakers, add solid potassium chloride 4～5 grams, 6～10 milliliters of 25～40 milliliters of concentrated hydrochloric acids (proportion 1.19) and red fuming nitric acid (RFNA)s (proportion 1.40), being heated to sample on the sand Lip river dissolves fully, under the low-temperature heat state, be evaporated near doing, after the cooling, wash wall of cup and watch glass for 10 milliliters with 1: 1 hydrochloric acid solution, under low-temperature heat state in the sand bath, be evaporated near doing again, after the cooling, add 25 ml waters and stir, make and separate out the AgCL precipitation, add 75 ml waters again, stir it.
Under constantly stirring, add 40～50 milliliters of 0.08N standard mohr salt solutions lentamente exactly, and continue to stir one minute, add 15 milliliters of sulfuric acid-phosphoric acid mixed liquors and stir it, add 5 of 0.5% diphenylamine sulfonic acid sodium salt indicator, with 0.05NK
2Cr
2O
7Standard solution titration becomes aubergine to solution from bottle green be terminal point.
Calculate Au% according to the addition of Mohr's salt standard solution and the residual titration amount of potassium dichromate standard solution.
According to the above embodiments measurement result such as following table:
*Check with gravimetric method through Fujian Measuring Technology Inst., recording No. 1 gold-silver alloy foil sample gold content is 70.95%; No. 3 gold-silver alloy sample gold content is 60.10%.
＊＊Caley E.R.，Shank L.W;Ohio J.Sci.，68，100（1968）;
РЖХИМ.，1968，22Г
Determination data is found out from last table, can record satisfied result with method of the present invention.
Claims (6)
1, a kind of method of measuring the gold content of gold-silver alloy and Jin-Yin-aldary, this method comprises the following steps:
(A), make the sample in small, broken bits of a kind of gold-silver alloy that contains high-load silver and Jin-Yin-aldary in the presence of a large amount of chlorides, add the concentrated hydrochloric acid and the concentrated nitric acid solution heating for dissolving of mixing by a certain percentage, form Au
3+, [AgCl
3]
2-, Cn
2+
(B), above-mentioned solution is evaporated near doing under in check heated condition, add the suitable quantity of water dilution, silver nitride precipitation is separated out.
(C), the silver nitride precipitation of separating out after will diluting, add certain excessive standard mohr salt solution [ferrous sulfate amine (NH
4)
2Fe (SO
4)
26H
2O], make Au
3+Reduced metal gold Au ↓.
(D), with remaining mohr salt solution standard K in the above-mentioned solution
2Cr
2O
7The solution residual titration it, from the K that consumes
2Cr
2O
7Standard solution calculates the gold content of sample.
6Fe
2+(residue)+K
2Cr
2O
7+ 14H
+=6Fe
3++ 2Cr
3++ 7H
2O+2K
+
Wherein: V '
Fe2+-adds the volume (milliliter) of standard mohr salt solution
T
Fe2+/Au-standard mohr salt solution is to the titer (grams per milliliter) of gold
W
Sample-weigh the weight (gram) that contains golden sample.
2, according to the described assay method of claim 1, it is characterized in that above-mentioned chloride is potassium chloride or sodium chloride, but the most handy potassium chloride.
3,, when it is characterized in that above-mentioned sample is the gold-silver alloy sample,, increase the consumption of chloride and concentrated hydrochloric acid, to promote the dissolving of sample along with the increase of silver content according to the described assay method of claim 1.
4,, when it is characterized in that above-mentioned sample is gold-aldary or the Jin-Yin that contains small amount of silver-aldary sample, need not add chloride, but will increase the red fuming nitric acid (RFNA) consumption, so that sample dissolution is complete according to the described assay method of claim 1.
5, according to the described assay method of claim 1, it is characterized in that sample evaporation near dry and cold but after, thin up, when separating out silver nitride precipitation, control the chlorine ion concentration in the solution, make less than 1 molar concentration, with the interference of avoiding chlorion that gold is measured, make Au simultaneously again
3+By Fe
2+Be reduced to metallic gold fully.
6, according to the described assay method of claim 1, it is characterized in that adding the standard mohr salt solution after, continue to stir one minute, make Au
3+Be reduced to metallic gold fully.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105502 CN85105502A (en) | 1985-07-15 | 1985-07-15 | The rapid test method of gold content in gold-silver alloy and Jin-Yin-aldary |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105502 CN85105502A (en) | 1985-07-15 | 1985-07-15 | The rapid test method of gold content in gold-silver alloy and Jin-Yin-aldary |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN85105502A true CN85105502A (en) | 1987-01-14 |
Family
ID=4794519
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85105502 Pending CN85105502A (en) | 1985-07-15 | 1985-07-15 | The rapid test method of gold content in gold-silver alloy and Jin-Yin-aldary |
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|---|---|
| CN (1) | CN85105502A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101149316B (en) * | 2007-11-08 | 2010-09-29 | 南京晨光集团有限责任公司 | Gold base alloy chemical composition analytical method |
-
1985
- 1985-07-15 CN CN 85105502 patent/CN85105502A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101149316B (en) * | 2007-11-08 | 2010-09-29 | 南京晨光集团有限责任公司 | Gold base alloy chemical composition analytical method |
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